# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_exp_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H86 Co2 Dy2 N2 O20' _chemical_formula_weight 1406.01 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9410(4) _cell_length_b 11.2485(4) _cell_length_c 12.2043(5) _cell_angle_alpha 104.787(3) _cell_angle_beta 90.745(3) _cell_angle_gamma 94.220(3) _cell_volume 1447.50(9) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5475 _cell_measurement_theta_min 3.7042 _cell_measurement_theta_max 28.7987 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 710 _exptl_absorpt_coefficient_mu 3.183 _exptl_absorpt_correction_T_min 0.54401 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _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 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1158 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18734 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6252 _reflns_number_gt 5086 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0423P)^2^+1.4130P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6252 _refine_ls_number_parameters 314 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.092 _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 C11 C 0.6029(5) 0.6566(5) 0.3508(4) 0.0325(12) Uani 1 1 d . A . C12 C 0.7139(5) 1.1529(5) 0.7785(4) 0.0339(12) Uani 1 1 d . . . C13 C 0.8235(5) 0.7953(5) 0.6299(4) 0.0337(12) Uani 1 1 d . A . C14 C 0.6106(8) 1.0050(7) 0.1378(6) 0.068(2) Uani 1 1 d . . . H14A H 0.6855 1.0433 0.1159 0.081 Uiso 1 1 calc R . . H14B H 0.5534 0.9861 0.0731 0.081 Uiso 1 1 calc R . . C15 C 0.3636(5) 0.7940(5) 0.4486(5) 0.0357(12) Uani 1 1 d . A . H15A H 0.3312 0.8164 0.5232 0.054 Uiso 1 1 calc R . . H15B H 0.4026 0.7184 0.4386 0.054 Uiso 1 1 calc R . . H15C H 0.2981 0.7830 0.3930 0.054 Uiso 1 1 calc R . . C21 C 0.6304(7) 0.5219(6) 0.3040(5) 0.0514(17) Uani 1 1 d . . . C22 C 0.8126(5) 1.2332(6) 0.8596(5) 0.0499(16) Uani 1 1 d D . . C23 C 0.9243(5) 0.7279(5) 0.6647(5) 0.0369(13) Uani 1 1 d . . . C24 C 0.5616(11) 1.0890(8) 0.2256(8) 0.117(5) Uani 1 1 d . . . H24A H 0.6269 1.1500 0.2617 0.141 Uiso 1 1 calc R . . H24B H 0.5022 1.1315 0.1934 0.141 Uiso 1 1 calc R . . C31 C 0.7604(11) 0.5305(10) 0.2546(11) 0.145(5) Uani 1 1 d . . . H31A H 0.8186 0.5705 0.3146 0.218 Uiso 1 1 calc R . . H31B H 0.7592 0.5773 0.1989 0.218 Uiso 1 1 calc R . . H31C H 0.7834 0.4490 0.2197 0.218 Uiso 1 1 calc R . . C41 C 0.5519(15) 0.4597(9) 0.2077(12) 0.200(9) Uani 1 1 d . . . H41A H 0.5501 0.5099 0.1549 0.300 Uiso 1 1 calc R . . H41B H 0.4704 0.4456 0.2325 0.300 Uiso 1 1 calc R . . H41C H 0.5828 0.3821 0.1715 0.300 Uiso 1 1 calc R . . C51 C 0.6460(12) 0.4584(8) 0.3942(8) 0.122(5) Uani 1 1 d . . . H51A H 0.7002 0.5089 0.4530 0.182 Uiso 1 1 calc R . . H51B H 0.6802 0.3811 0.3633 0.182 Uiso 1 1 calc R . . H51C H 0.5677 0.4437 0.4250 0.182 Uiso 1 1 calc R . . C32 C 0.7792(14) 1.3694(11) 0.8822(14) 0.101(3) Uani 0.516(8) 1 d PD A 1 H32A H 0.8397 1.4223 0.9332 0.152 Uiso 0.516(8) 1 calc PR A 1 H32B H 0.7002 1.3769 0.9155 0.152 Uiso 0.516(8) 1 calc PR A 1 H32C H 0.7771 1.3929 0.8120 0.152 Uiso 0.516(8) 1 calc PR A 1 C42 C 0.9369(10) 1.2244(16) 0.8068(12) 0.101(3) Uani 0.516(8) 1 d PD A 1 H42A H 0.9973 1.2759 0.8589 0.152 Uiso 0.516(8) 1 calc PR A 1 H42B H 0.9343 1.2511 0.7382 0.152 Uiso 0.516(8) 1 calc PR A 1 H42C H 0.9580 1.1404 0.7898 0.152 Uiso 0.516(8) 1 calc PR A 1 C52 C 0.8110(14) 1.1979(16) 0.9707(10) 0.101(3) Uani 0.516(8) 1 d PD A 1 H52A H 0.8726 1.2487 1.0219 0.152 Uiso 0.516(8) 1 calc PR A 1 H52B H 0.8274 1.1128 0.9579 0.152 Uiso 0.516(8) 1 calc PR A 1 H52C H 0.7318 1.2096 1.0029 0.152 Uiso 0.516(8) 1 calc PR A 1 C32' C 0.7648(14) 1.3156(15) 0.9657(11) 0.101(3) Uani 0.484(8) 1 d PD A 2 H32D H 0.8323 1.3630 1.0115 0.152 Uiso 0.484(8) 1 calc PR A 2 H32E H 0.7210 1.2658 1.0078 0.152 Uiso 0.484(8) 1 calc PR A 2 H32F H 0.7106 1.3703 0.9451 0.152 Uiso 0.484(8) 1 calc PR A 2 C42' C 0.8919(14) 1.3063(16) 0.7944(12) 0.101(3) Uani 0.484(8) 1 d PD A 2 H42D H 0.9539 1.3577 0.8447 0.152 Uiso 0.484(8) 1 calc PR A 2 H42E H 0.8418 1.3569 0.7632 0.152 Uiso 0.484(8) 1 calc PR A 2 H42F H 0.9302 1.2504 0.7341 0.152 Uiso 0.484(8) 1 calc PR A 2 C52' C 0.8939(14) 1.1412(13) 0.8959(15) 0.101(3) Uani 0.484(8) 1 d PD A 2 H52D H 0.9582 1.1863 0.9475 0.152 Uiso 0.484(8) 1 calc PR A 2 H52E H 0.9291 1.0909 0.8301 0.152 Uiso 0.484(8) 1 calc PR A 2 H52F H 0.8445 1.0896 0.9325 0.152 Uiso 0.484(8) 1 calc PR A 2 C33 C 0.8762(8) 0.6077(8) 0.6876(8) 0.087(3) Uani 1 1 d . . . H33A H 0.9431 0.5675 0.7099 0.131 Uiso 1 1 calc R . . H33B H 0.8361 0.5555 0.6201 0.131 Uiso 1 1 calc R . . H33C H 0.8187 0.6237 0.7473 0.131 Uiso 1 1 calc R . . C34 C 0.7669(6) 0.8885(8) 0.2034(5) 0.062(2) Uani 1 1 d . . . H34A H 0.7913 0.8048 0.1809 0.074 Uiso 1 1 calc R . . H34B H 0.8194 0.9380 0.1658 0.074 Uiso 1 1 calc R . . C43 C 1.0190(7) 0.7005(9) 0.5687(7) 0.084(3) Uani 1 1 d . . . H43A H 1.0837 0.6575 0.5910 0.125 Uiso 1 1 calc R . . H43B H 1.0528 0.7768 0.5557 0.125 Uiso 1 1 calc R . . H43C H 0.9788 0.6505 0.5003 0.125 Uiso 1 1 calc R . . C44 C 0.7867(6) 0.9346(9) 0.3228(5) 0.074(3) Uani 1 1 d . A . H44A H 0.8454 0.8859 0.3482 0.089 Uiso 1 1 calc R . . H44B H 0.8229 1.0188 0.3386 0.089 Uiso 1 1 calc R . . C53 C 0.9895(8) 0.8091(9) 0.7691(7) 0.084(3) Uani 1 1 d . . . H53A H 1.0542 0.7666 0.7922 0.126 Uiso 1 1 calc R . . H53B H 0.9325 0.8290 0.8289 0.126 Uiso 1 1 calc R . . H53C H 1.0236 0.8837 0.7529 0.126 Uiso 1 1 calc R . . C54 C 0.6102(7) 0.7825(7) 0.0626(5) 0.0582(19) Uani 1 1 d . . . H54A H 0.5276 0.7877 0.0353 0.070 Uiso 1 1 calc R . . H54B H 0.6098 0.7074 0.0878 0.070 Uiso 1 1 calc R . . C64 C 0.6938(7) 0.7694(7) -0.0367(5) 0.0573(19) Uani 1 1 d . . . H64A H 0.7769 0.7639 -0.0110 0.069 Uiso 1 1 calc R . . H64B H 0.6689 0.6932 -0.0930 0.069 Uiso 1 1 calc R . . N1 N 0.6386(4) 0.8885(4) 0.1631(3) 0.0318(10) Uani 1 1 d . . . O11 O 0.5698(3) 0.7105(3) 0.2755(3) 0.0323(8) Uani 1 1 d . . . O12 O 0.7465(3) 1.0676(4) 0.7015(3) 0.0387(9) Uani 1 1 d . . . O13 O 0.7250(4) 0.8001(4) 0.6833(3) 0.0396(9) Uani 1 1 d . . . O14 O 0.5064(3) 1.0447(3) 0.3068(3) 0.0277(8) Uani 1 1 d . . . O15 O 0.4523(3) 0.8907(3) 0.4353(3) 0.0257(7) Uani 1 1 d . . . O21 O 0.6133(4) 0.7046(3) 0.4542(3) 0.0374(9) Uani 1 1 d . . . O22 O 0.3946(3) 0.8162(3) 0.2010(3) 0.0337(8) Uani 1 1 d . . . O23 O 0.8383(4) 0.8476(4) 0.5514(3) 0.0406(9) Uani 1 1 d . . . O24 O 0.6829(3) 0.9328(3) 0.3845(3) 0.0285(8) Uani 1 1 d . . . O34 O 0.6923(8) 0.8635(7) -0.0851(5) 0.128(3) Uani 1 1 d . . . H34 H 0.7390 0.8527 -0.1382 0.191 Uiso 1 1 calc R . . Co2 Co 0.53788(6) 0.87899(6) 0.29568(5) 0.02390(15) Uani 1 1 d . . . Dy1 Dy 0.63551(2) 0.91418(2) 0.559438(19) 0.02729(9) 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 C11 0.041(3) 0.024(3) 0.031(3) 0.005(2) 0.004(2) -0.003(2) C12 0.036(3) 0.039(3) 0.023(3) 0.004(2) 0.001(2) -0.003(2) C13 0.036(3) 0.039(3) 0.027(3) 0.009(2) -0.002(2) 0.009(2) C14 0.104(6) 0.069(5) 0.050(4) 0.040(4) 0.041(4) 0.041(4) C15 0.038(3) 0.039(3) 0.035(3) 0.018(3) 0.004(2) 0.001(2) C21 0.075(5) 0.031(3) 0.047(4) 0.005(3) 0.001(3) 0.013(3) C22 0.035(3) 0.059(4) 0.044(4) -0.006(3) -0.004(3) 0.001(3) C23 0.031(3) 0.048(3) 0.039(3) 0.026(3) -0.013(2) 0.003(2) C24 0.199(11) 0.069(6) 0.120(8) 0.067(6) 0.128(8) 0.074(7) C31 0.148(11) 0.094(8) 0.197(13) 0.022(8) 0.090(10) 0.073(8) C41 0.270(19) 0.039(5) 0.244(17) -0.046(8) -0.153(15) 0.032(8) C51 0.243(14) 0.058(6) 0.076(6) 0.023(5) 0.027(7) 0.066(7) C32 0.073(6) 0.125(8) 0.085(6) -0.001(5) -0.032(4) -0.022(5) C42 0.073(6) 0.125(8) 0.085(6) -0.001(5) -0.032(4) -0.022(5) C52 0.073(6) 0.125(8) 0.085(6) -0.001(5) -0.032(4) -0.022(5) C32' 0.073(6) 0.125(8) 0.085(6) -0.001(5) -0.032(4) -0.022(5) C42' 0.073(6) 0.125(8) 0.085(6) -0.001(5) -0.032(4) -0.022(5) C52' 0.073(6) 0.125(8) 0.085(6) -0.001(5) -0.032(4) -0.022(5) C33 0.087(7) 0.074(6) 0.119(8) 0.049(6) 0.009(5) 0.036(5) C34 0.032(3) 0.120(7) 0.033(3) 0.019(4) 0.009(3) 0.010(4) C43 0.064(5) 0.132(8) 0.073(5) 0.045(5) 0.021(4) 0.064(5) C44 0.029(3) 0.157(8) 0.035(4) 0.027(4) 0.006(3) -0.012(4) C53 0.060(5) 0.122(8) 0.076(6) 0.038(6) -0.015(4) 0.012(5) C54 0.068(5) 0.065(5) 0.030(3) -0.007(3) 0.018(3) -0.004(4) C64 0.060(4) 0.075(5) 0.028(3) -0.001(3) 0.012(3) 0.002(4) N1 0.036(3) 0.037(3) 0.022(2) 0.0073(19) 0.0078(18) 0.004(2) O11 0.041(2) 0.0273(19) 0.0275(19) 0.0042(16) 0.0044(16) 0.0063(16) O12 0.031(2) 0.044(2) 0.036(2) 0.0003(18) 0.0010(16) 0.0068(17) O13 0.040(2) 0.051(3) 0.031(2) 0.0154(19) 0.0071(17) 0.0153(18) O14 0.034(2) 0.0276(19) 0.0247(18) 0.0110(15) 0.0059(14) 0.0052(15) O15 0.0314(19) 0.0234(18) 0.0224(17) 0.0064(14) 0.0059(14) -0.0009(14) O21 0.053(2) 0.030(2) 0.030(2) 0.0083(17) 0.0002(17) 0.0098(17) O22 0.032(2) 0.041(2) 0.0255(19) 0.0040(17) 0.0001(15) 0.0037(16) O23 0.043(2) 0.050(2) 0.034(2) 0.0173(19) 0.0079(17) 0.0155(19) O24 0.0282(19) 0.034(2) 0.0230(17) 0.0058(15) 0.0014(14) 0.0074(15) O34 0.230(9) 0.110(6) 0.057(4) 0.033(4) 0.082(5) 0.049(6) Co2 0.0270(4) 0.0260(4) 0.0191(3) 0.0059(3) 0.0029(3) 0.0036(3) Dy1 0.03260(15) 0.03037(15) 0.01999(13) 0.00679(10) 0.00195(9) 0.00829(10) _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 C11 O21 1.240(6) . ? C11 O11 1.285(6) . ? C11 C21 1.531(8) . ? C12 O12 1.236(6) . ? C12 O22 1.272(6) 2_676 ? C12 C22 1.528(8) . ? C13 O23 1.253(6) . ? C13 O13 1.263(6) . ? C13 C23 1.499(7) . ? C13 Dy1 2.775(5) . ? C14 C24 1.379(10) . ? C14 N1 1.473(8) . ? C15 O15 1.446(6) . ? C21 C41 1.440(12) . ? C21 C51 1.470(10) . ? C21 C31 1.558(12) . ? C22 C52 1.507(9) . ? C22 C42 1.511(9) . ? C22 C32' 1.512(9) . ? C22 C42' 1.519(9) . ? C22 C52' 1.555(9) . ? C22 C32 1.557(9) . ? C23 C53 1.501(10) . ? C23 C33 1.508(10) . ? C23 C43 1.561(9) . ? C24 O14 1.348(7) . ? C34 C44 1.424(9) . ? C34 N1 1.481(7) . ? C44 O24 1.372(7) . ? C54 N1 1.487(7) . ? C54 C64 1.512(8) . ? C64 O34 1.338(9) . ? N1 Co2 1.990(4) . ? O11 Co2 1.907(4) . ? O12 Dy1 2.360(4) . ? O13 Dy1 2.455(4) . ? O14 Co2 1.891(3) . ? O14 Dy1 2.253(3) 2_676 ? O15 Co2 1.934(3) . ? O15 Dy1 2.446(3) 2_676 ? O15 Dy1 2.454(3) . ? O21 Dy1 2.372(4) . ? O22 C12 1.272(6) 2_676 ? O22 Co2 1.914(4) . ? O23 Dy1 2.388(4) . ? O24 Co2 1.881(3) . ? O24 Dy1 2.261(3) . ? Co2 Dy1 3.2824(11) 2_676 ? Co2 Dy1 3.2949(14) . ? Dy1 O14 2.253(3) 2_676 ? Dy1 O15 2.446(3) 2_676 ? Dy1 Co2 3.2824(11) 2_676 ? 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 O21 C11 O11 125.5(5) . . ? O21 C11 C21 119.7(5) . . ? O11 C11 C21 114.8(5) . . ? O12 C12 O22 127.4(5) . 2_676 ? O12 C12 C22 118.2(5) . . ? O22 C12 C22 114.4(5) 2_676 . ? O23 C13 O13 121.3(5) . . ? O23 C13 C23 120.4(5) . . ? O13 C13 C23 118.4(5) . . ? O23 C13 Dy1 59.1(3) . . ? O13 C13 Dy1 62.2(3) . . ? C23 C13 Dy1 178.2(4) . . ? C24 C14 N1 115.1(5) . . ? C41 C21 C51 117.5(9) . . ? C41 C21 C11 112.2(6) . . ? C51 C21 C11 112.4(6) . . ? C41 C21 C31 104.6(10) . . ? C51 C21 C31 104.5(8) . . ? C11 C21 C31 103.9(6) . . ? C52 C22 C42 112.6(6) . . ? C52 C22 C32' 58.1(7) . . ? C42 C22 C32' 133.7(10) . . ? C52 C22 C42' 140.9(9) . . ? C42 C22 C42' 43.3(7) . . ? C32' C22 C42' 111.8(6) . . ? C52 C22 C12 109.4(7) . . ? C42 C22 C12 110.9(7) . . ? C32' C22 C12 114.8(7) . . ? C42' C22 C12 108.7(7) . . ? C52 C22 C52' 53.1(7) . . ? C42 C22 C52' 65.4(7) . . ? C32' C22 C52' 108.0(6) . . ? C42' C22 C52' 107.7(6) . . ? C12 C22 C52' 105.3(7) . . ? C52 C22 C32 108.2(6) . . ? C42 C22 C32 108.2(6) . . ? C32' C22 C32 50.8(7) . . ? C42' C22 C32 67.9(7) . . ? C12 C22 C32 107.5(7) . . ? C52' C22 C32 146.4(9) . . ? C13 C23 C53 108.8(6) . . ? C13 C23 C33 111.9(5) . . ? C53 C23 C33 109.8(6) . . ? C13 C23 C43 109.5(5) . . ? C53 C23 C43 107.9(6) . . ? C33 C23 C43 108.8(6) . . ? O14 C24 C14 117.2(7) . . ? C44 C34 N1 114.5(5) . . ? O24 C44 C34 114.5(5) . . ? N1 C54 C64 117.8(6) . . ? O34 C64 C54 112.9(7) . . ? C14 N1 C34 113.6(6) . . ? C14 N1 C54 110.7(5) . . ? C34 N1 C54 109.7(5) . . ? C14 N1 Co2 104.8(3) . . ? C34 N1 Co2 104.7(3) . . ? C54 N1 Co2 113.2(4) . . ? C11 O11 Co2 128.3(3) . . ? C12 O12 Dy1 132.4(4) . . ? C13 O13 Dy1 90.7(3) . . ? C24 O14 Co2 112.2(4) . . ? C24 O14 Dy1 142.6(4) . 2_676 ? Co2 O14 Dy1 104.41(14) . 2_676 ? C15 O15 Co2 121.7(3) . . ? C15 O15 Dy1 113.9(3) . 2_676 ? Co2 O15 Dy1 96.35(13) . 2_676 ? C15 O15 Dy1 112.9(3) . . ? Co2 O15 Dy1 96.60(14) . . ? Dy1 O15 Dy1 113.44(13) 2_676 . ? C11 O21 Dy1 131.5(3) . . ? C12 O22 Co2 126.3(3) 2_676 . ? C13 O23 Dy1 94.1(3) . . ? C44 O24 Co2 114.1(3) . . ? C44 O24 Dy1 137.0(4) . . ? Co2 O24 Dy1 105.03(16) . . ? O24 Co2 O14 90.11(15) . . ? O24 Co2 O11 91.48(15) . . ? O14 Co2 O11 176.80(14) . . ? O24 Co2 O22 176.81(16) . . ? O14 Co2 O22 92.62(15) . . ? O11 Co2 O22 85.72(16) . . ? O24 Co2 O15 87.73(15) . . ? O14 Co2 O15 88.05(14) . . ? O11 Co2 O15 94.79(15) . . ? O22 Co2 O15 94.01(15) . . ? O24 Co2 N1 86.39(17) . . ? O14 Co2 N1 86.83(16) . . ? O11 Co2 N1 90.50(17) . . ? O22 Co2 N1 92.11(17) . . ? O15 Co2 N1 172.19(17) . . ? O24 Co2 Dy1 97.44(11) . 2_676 ? O14 Co2 Dy1 41.66(10) . 2_676 ? O11 Co2 Dy1 140.71(11) . 2_676 ? O22 Co2 Dy1 85.70(11) . 2_676 ? O15 Co2 Dy1 47.79(10) . 2_676 ? N1 Co2 Dy1 128.08(13) . 2_676 ? O24 Co2 Dy1 41.51(10) . . ? O14 Co2 Dy1 97.94(10) . . ? O11 Co2 Dy1 85.08(10) . . ? O22 Co2 Dy1 139.45(11) . . ? O15 Co2 Dy1 47.73(10) . . ? N1 Co2 Dy1 127.35(13) . . ? Dy1 Co2 Dy1 77.05(3) 2_676 . ? O14 Dy1 O24 143.14(12) 2_676 . ? O14 Dy1 O12 79.33(13) 2_676 . ? O24 Dy1 O12 111.16(13) . . ? O14 Dy1 O21 111.47(13) 2_676 . ? O24 Dy1 O21 79.23(13) . . ? O12 Dy1 O21 147.38(13) . . ? O14 Dy1 O23 135.51(12) 2_676 . ? O24 Dy1 O23 80.87(12) . . ? O12 Dy1 O23 76.23(13) . . ? O21 Dy1 O23 75.13(14) . . ? O14 Dy1 O15 68.78(11) 2_676 2_676 ? O24 Dy1 O15 80.42(11) . 2_676 ? O12 Dy1 O15 73.06(12) . 2_676 ? O21 Dy1 O15 139.43(12) . 2_676 ? O23 Dy1 O15 134.94(13) . 2_676 ? O14 Dy1 O15 81.08(12) 2_676 . ? O24 Dy1 O15 68.06(12) . . ? O12 Dy1 O15 139.22(12) . . ? O21 Dy1 O15 73.34(12) . . ? O23 Dy1 O15 138.99(12) . . ? O15 Dy1 O15 66.56(13) 2_676 . ? O14 Dy1 O13 84.41(12) 2_676 . ? O24 Dy1 O13 132.05(12) . . ? O12 Dy1 O13 75.60(14) . . ? O21 Dy1 O13 75.06(13) . . ? O23 Dy1 O13 53.81(13) . . ? O15 Dy1 O13 141.74(12) 2_676 . ? O15 Dy1 O13 137.19(12) . . ? O14 Dy1 C13 110.62(14) 2_676 . ? O24 Dy1 C13 106.24(14) . . ? O12 Dy1 C13 75.04(15) . . ? O21 Dy1 C13 72.36(15) . . ? O23 Dy1 C13 26.75(14) . . ? O15 Dy1 C13 147.59(14) 2_676 . ? O15 Dy1 C13 145.68(14) . . ? O13 Dy1 C13 27.08(14) . . ? O14 Dy1 Co2 33.93(8) 2_676 2_676 ? O24 Dy1 Co2 115.73(9) . 2_676 ? O12 Dy1 Co2 67.07(9) . 2_676 ? O21 Dy1 Co2 137.93(10) . 2_676 ? O23 Dy1 Co2 143.05(10) . 2_676 ? O15 Dy1 Co2 35.85(8) 2_676 2_676 ? O15 Dy1 Co2 76.78(8) . 2_676 ? O13 Dy1 Co2 110.49(9) . 2_676 ? C13 Dy1 Co2 130.89(11) . 2_676 ? O14 Dy1 Co2 116.25(9) 2_676 . ? O24 Dy1 Co2 33.45(9) . . ? O12 Dy1 Co2 137.38(10) . . ? O21 Dy1 Co2 67.11(9) . . ? O23 Dy1 Co2 106.88(9) . . ? O15 Dy1 Co2 76.63(8) 2_676 . ? O15 Dy1 Co2 35.68(7) . . ? O13 Dy1 Co2 141.33(9) . . ? C13 Dy1 Co2 126.16(11) . . ? Co2 Dy1 Co2 102.95(3) 2_676 . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.399 _refine_diff_density_min -1.029 _refine_diff_density_rms 0.135 _database_code_depnum_ccdc_archive 'CCDC 958224'