# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Zhao, Bin' _publ_contact_author_email zhaobin@nankai.edu.cn _publ_section_title ; Investigation on Structures, Luminescent and Magnetic Properties of LnIII-M (M = FeIIHS, CoII) Coordination Polymers ; _publ_author_name 'Bin Zhao' data_13 _database_code_depnum_ccdc_archive 'CCDC 630836' #TrackingRef '630836.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Co3 Eu2 N6 O37' _chemical_formula_weight 1705.54 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6/mcc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 15.2806(10) _cell_length_b 15.2806(10) _cell_length_c 15.393(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3112.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 3774 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 25.86 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1682 _exptl_absorpt_coefficient_mu 2.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.590888 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADBAS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15944 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 26.34 _reflns_number_total 1103 _reflns_number_gt 765 _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. ISOR: the parameter to go anisotropic restraint to appointed atoms, is applied for water molecule O5. ; _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^)+(0.0326P)^2^+8.7497P] 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 1103 _refine_ls_number_parameters 76 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.001 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 Eu1 Eu 0.3333 0.6667 0.2500 0.01582(16) Uani 1 6 d S . . Co1 Co 0.5000 1.0000 0.0000 0.0162(2) Uani 1 4 d S . . O1 O 0.3882(2) 0.8024(2) 0.14265(18) 0.0281(7) Uani 1 1 d . . . O2 O 0.3867(3) 0.9400(2) 0.0928(2) 0.0350(8) Uani 1 1 d . . . O3 O 0.5135(3) 0.8662(3) 0.0000 0.0279(10) Uani 1 2 d S . . H3A H 0.4796 0.8310 -0.0430 0.033 Uiso 1 1 d R . . N1 N 0.23832(16) 0.76168(16) 0.2500 0.0209(9) Uani 1 2 d S . . C1 C 0.3539(3) 0.8635(3) 0.1385(3) 0.0241(9) Uani 1 1 d . . . C2 C 0.2649(3) 0.8396(3) 0.1960(3) 0.0243(10) Uani 1 1 d . . . C3 C 0.2147(4) 0.8929(4) 0.1934(3) 0.0350(12) Uani 1 1 d . . . H3 H 0.2338 0.9461 0.1546 0.042 Uiso 1 1 calc R . . C4 C 0.1348(2) 0.8652(2) 0.2500 0.0448(17) Uani 1 2 d S . . H4 H 0.0996 0.9004 0.2500 0.054 Uiso 1 2 calc SR . . O4 O 0.2672(9) 0.0537(12) 0.0000 0.183(6) Uani 1 2 d S . . O5 O 0.0000 0.0000 0.2500 0.330(12) Uani 1 12 d SU . . 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 Eu1 0.01678(19) 0.01678(19) 0.0139(2) 0.000 0.000 0.00839(9) Co1 0.0184(6) 0.0137(5) 0.0134(5) 0.000 0.000 0.0056(5) O1 0.0338(19) 0.0272(15) 0.0265(15) 0.0093(13) 0.0116(14) 0.0176(15) O2 0.042(2) 0.0286(19) 0.0371(18) 0.0176(16) 0.0184(17) 0.0201(16) O3 0.032(3) 0.024(2) 0.025(2) 0.000 0.000 0.012(2) N1 0.0212(17) 0.0212(17) 0.022(2) 0.001(2) 0.001(2) 0.0118(19) C1 0.023(2) 0.024(2) 0.020(2) 0.0023(19) 0.0038(19) 0.0081(19) C2 0.025(2) 0.020(2) 0.027(2) 0.0074(19) 0.006(2) 0.011(2) C3 0.037(3) 0.031(3) 0.043(3) 0.016(2) 0.010(2) 0.022(2) C4 0.040(3) 0.040(3) 0.069(5) 0.015(5) 0.015(5) 0.031(3) O4 0.160(10) 0.346(18) 0.091(7) 0.000 0.000 0.163(12) O5 0.325(12) 0.325(12) 0.341(16) 0.000 0.000 0.162(6) _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 Eu1 O1 2.449(3) 2_665 ? Eu1 O1 2.449(3) 11 ? Eu1 O1 2.449(3) . ? Eu1 O1 2.449(3) 10_665 ? Eu1 O1 2.449(3) 3_565 ? Eu1 O1 2.449(3) 12_565 ? Eu1 N1 2.515(4) . ? Eu1 N1 2.515(4) 3_565 ? Eu1 N1 2.515(4) 2_665 ? Co1 O2 2.071(3) 16 ? Co1 O2 2.071(3) 4_675 ? Co1 O2 2.071(3) . ? Co1 O2 2.071(3) 13_675 ? Co1 O3 2.155(4) 13_675 ? Co1 O3 2.155(4) . ? O1 C1 1.281(5) . ? O2 C1 1.235(5) . ? O3 H3A 0.8470 . ? N1 C2 1.338(5) 10_665 ? N1 C2 1.338(5) . ? C1 C2 1.506(6) . ? C2 C3 1.370(6) . ? C3 C4 1.383(6) . ? C3 H3 0.9300 . ? C4 C3 1.383(6) 10_665 ? C4 H4 0.9300 . ? 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 O1 Eu1 O1 145.50(14) 2_665 11 ? O1 Eu1 O1 79.44(10) 2_665 . ? O1 Eu1 O1 85.64(14) 11 . ? O1 Eu1 O1 85.64(14) 2_665 10_665 ? O1 Eu1 O1 79.44(11) 11 10_665 ? O1 Eu1 O1 128.19(14) . 10_665 ? O1 Eu1 O1 79.44(10) 2_665 3_565 ? O1 Eu1 O1 128.19(14) 11 3_565 ? O1 Eu1 O1 79.44(10) . 3_565 ? O1 Eu1 O1 145.50(14) 10_665 3_565 ? O1 Eu1 O1 128.19(14) 2_665 12_565 ? O1 Eu1 O1 79.44(10) 11 12_565 ? O1 Eu1 O1 145.50(14) . 12_565 ? O1 Eu1 O1 79.44(10) 10_665 12_565 ? O1 Eu1 O1 85.64(14) 3_565 12_565 ? O1 Eu1 N1 72.75(7) 2_665 . ? O1 Eu1 N1 72.75(7) 11 . ? O1 Eu1 N1 64.09(7) . . ? O1 Eu1 N1 64.09(7) 10_665 . ? O1 Eu1 N1 137.18(7) 3_565 . ? O1 Eu1 N1 137.18(7) 12_565 . ? O1 Eu1 N1 137.18(7) 2_665 3_565 ? O1 Eu1 N1 64.09(7) 11 3_565 ? O1 Eu1 N1 72.75(7) . 3_565 ? O1 Eu1 N1 137.18(7) 10_665 3_565 ? O1 Eu1 N1 64.09(7) 3_565 3_565 ? O1 Eu1 N1 72.75(7) 12_565 3_565 ? N1 Eu1 N1 120.0 . 3_565 ? O1 Eu1 N1 64.09(7) 2_665 2_665 ? O1 Eu1 N1 137.18(7) 11 2_665 ? O1 Eu1 N1 137.18(7) . 2_665 ? O1 Eu1 N1 72.75(7) 10_665 2_665 ? O1 Eu1 N1 72.75(7) 3_565 2_665 ? O1 Eu1 N1 64.09(7) 12_565 2_665 ? N1 Eu1 N1 120.0 . 2_665 ? N1 Eu1 N1 120.0 3_565 2_665 ? O2 Co1 O2 180.0 16 4_675 ? O2 Co1 O2 87.2(2) 16 . ? O2 Co1 O2 92.8(2) 4_675 . ? O2 Co1 O2 92.8(2) 16 13_675 ? O2 Co1 O2 87.2(2) 4_675 13_675 ? O2 Co1 O2 180.0(2) . 13_675 ? O2 Co1 O3 87.99(12) 16 13_675 ? O2 Co1 O3 92.01(12) 4_675 13_675 ? O2 Co1 O3 87.99(12) . 13_675 ? O2 Co1 O3 92.01(12) 13_675 13_675 ? O2 Co1 O3 92.01(12) 16 . ? O2 Co1 O3 87.99(12) 4_675 . ? O2 Co1 O3 92.01(12) . . ? O2 Co1 O3 87.99(12) 13_675 . ? O3 Co1 O3 180.000(1) 13_675 . ? C1 O1 Eu1 124.0(3) . . ? C1 O2 Co1 131.8(3) . . ? Co1 O3 H3A 106.5 . . ? C2 N1 C2 119.0(5) 10_665 . ? C2 N1 Eu1 120.5(2) 10_665 . ? C2 N1 Eu1 120.5(2) . . ? O2 C1 O1 126.7(4) . . ? O2 C1 C2 117.0(4) . . ? O1 C1 C2 116.3(4) . . ? N1 C2 C3 122.4(4) . . ? N1 C2 C1 114.6(4) . . ? C3 C2 C1 123.0(4) . . ? C2 C3 C4 118.1(4) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C3 C4 C3 120.0(6) 10_665 . ? C3 C4 H4 120.0 10_665 . ? C3 C4 H4 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Eu1 O1 C1 81.9(4) 2_665 . . . ? O1 Eu1 O1 C1 -66.9(3) 11 . . . ? O1 Eu1 O1 C1 6.0(3) 10_665 . . . ? O1 Eu1 O1 C1 162.9(3) 3_565 . . . ? O1 Eu1 O1 C1 -131.1(3) 12_565 . . . ? N1 Eu1 O1 C1 6.0(3) . . . . ? N1 Eu1 O1 C1 -131.1(3) 3_565 . . . ? N1 Eu1 O1 C1 113.1(3) 2_665 . . . ? O2 Co1 O2 C1 101.8(4) 16 . . . ? O2 Co1 O2 C1 -78.2(4) 4_675 . . . ? O2 Co1 O2 C1 -36.1(5) 13_675 . . . ? O3 Co1 O2 C1 -170.1(4) 13_675 . . . ? O3 Co1 O2 C1 9.9(4) . . . . ? O1 Eu1 N1 C2 91.1(2) 2_665 . . 10_665 ? O1 Eu1 N1 C2 -88.9(2) 11 . . 10_665 ? O1 Eu1 N1 C2 177.5(2) . . . 10_665 ? O1 Eu1 N1 C2 -2.5(2) 10_665 . . 10_665 ? O1 Eu1 N1 C2 143.0(2) 3_565 . . 10_665 ? O1 Eu1 N1 C2 -37.0(2) 12_565 . . 10_665 ? N1 Eu1 N1 C2 -133.8(2) 3_565 . . 10_665 ? N1 Eu1 N1 C2 46.2(2) 2_665 . . 10_665 ? O1 Eu1 N1 C2 -88.9(2) 2_665 . . . ? O1 Eu1 N1 C2 91.1(2) 11 . . . ? O1 Eu1 N1 C2 -2.5(2) . . . . ? O1 Eu1 N1 C2 177.5(2) 10_665 . . . ? O1 Eu1 N1 C2 -37.0(2) 3_565 . . . ? O1 Eu1 N1 C2 143.0(2) 12_565 . . . ? N1 Eu1 N1 C2 46.2(2) 3_565 . . . ? N1 Eu1 N1 C2 -133.8(2) 2_665 . . . ? Co1 O2 C1 O1 4.3(7) . . . . ? Co1 O2 C1 C2 -176.3(3) . . . . ? Eu1 O1 C1 O2 171.0(3) . . . . ? Eu1 O1 C1 C2 -8.5(5) . . . . ? C2 N1 C2 C3 -0.5(4) 10_665 . . . ? Eu1 N1 C2 C3 179.5(4) . . . . ? C2 N1 C2 C1 179.6(4) 10_665 . . . ? Eu1 N1 C2 C1 -0.4(4) . . . . ? O2 C1 C2 N1 -174.0(4) . . . . ? O1 C1 C2 N1 5.5(6) . . . . ? O2 C1 C2 C3 6.1(7) . . . . ? O1 C1 C2 C3 -174.3(4) . . . . ? N1 C2 C3 C4 1.1(7) . . . . ? C1 C2 C3 C4 -179.1(4) . . . . ? C2 C3 C4 C3 -0.5(3) . . . 10_665 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.861 _refine_diff_density_min -0.964 _refine_diff_density_rms 0.106 #===END data_16 _database_code_depnum_ccdc_archive 'CCDC 630837' #TrackingRef '- Ln-L1-Co.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Co3 Dy2 N6 O37' _chemical_formula_weight 1726.62 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 hexagonal _symmetry_space_group_name_H-M P6/mcc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 15.2196(8) _cell_length_b 15.2196(8) _cell_length_c 15.4737(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3104.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5875 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 26.37 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1694 _exptl_absorpt_coefficient_mu 3.264 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.744949 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15971 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 26.38 _reflns_number_total 1108 _reflns_number_gt 818 _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. ; _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^)+(0.0227P)^2^+10.9811P] 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 1108 _refine_ls_number_parameters 80 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.177 _refine_ls_shift/su_max 0.000 _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 0.3333 0.6667 0.2500 0.01592(14) Uani 1 6 d S . . Co1 Co 0.5000 0.5000 0.5000 0.0170(2) Uani 1 4 d S . . O1 O 0.3871(3) 0.4487(2) 0.4075(2) 0.0346(8) Uani 1 1 d . . . O2 O 0.3888(2) 0.5878(2) 0.35662(18) 0.0263(6) Uani 1 1 d . . . O3 O 0.4856(3) 0.3507(3) 0.5000 0.0267(9) Uani 1 2 d S . . H3A H 0.5129 0.3490 0.5469 0.07(2) Uiso 1 1 d R . . N1 N 0.23940(16) 0.4788(3) 0.2500 0.0196(9) Uani 1 2 d S . . C1 C 0.3547(3) 0.4927(3) 0.3608(3) 0.0232(9) Uani 1 1 d . . . C2 C 0.2661(3) 0.4274(3) 0.3036(3) 0.0239(9) Uani 1 1 d . . . C3 C 0.2148(4) 0.3226(3) 0.3062(3) 0.0359(11) Uani 1 1 d . . . H3 H 0.2339 0.2884 0.3449 0.051(16) Uiso 1 1 calc R . . C4 C 0.1348(2) 0.2695(5) 0.2500 0.0453(17) Uani 1 2 d S . . H4 H 0.0995 0.1990 0.2500 0.11(4) Uiso 1 2 calc SR . . O4 O 0.2654(9) 0.2114(10) 0.5000 0.185(6) Uani 1 2 d S . . O5 O 0.0000 0.0000 0.177(5) 0.27(4) Uani 0.50 6 d SP . . 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 0.01750(16) 0.01750(16) 0.0128(2) 0.000 0.000 0.00875(8) Co1 0.0197(6) 0.0214(6) 0.0141(4) 0.000 0.000 0.0134(4) O1 0.0430(19) 0.0290(16) 0.0343(17) -0.0030(15) -0.0204(16) 0.0198(15) O2 0.0328(17) 0.0252(16) 0.0219(13) -0.0014(13) -0.0103(13) 0.0153(14) O3 0.033(2) 0.027(2) 0.024(2) 0.000 0.000 0.018(2) N1 0.0193(15) 0.022(2) 0.018(2) 0.000 -0.004(2) 0.0112(11) C1 0.023(2) 0.030(2) 0.0190(18) -0.0023(18) -0.0045(17) 0.0154(18) C2 0.024(2) 0.025(2) 0.024(2) 0.0017(18) -0.0031(18) 0.0137(18) C3 0.040(3) 0.026(2) 0.045(3) 0.003(2) -0.012(2) 0.018(2) C4 0.042(3) 0.017(3) 0.069(5) 0.000 -0.020(4) 0.0087(14) O4 0.140(10) 0.188(12) 0.100(7) 0.000 0.000 -0.013(9) O5 0.15(2) 0.15(2) 0.51(13) 0.000 0.000 0.073(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 Dy1 O2 2.427(3) 11 ? Dy1 O2 2.427(3) 2_665 ? Dy1 O2 2.427(3) 12_565 ? Dy1 O2 2.427(3) 3_565 ? Dy1 O2 2.427(3) 10_665 ? Dy1 O2 2.427(3) . ? Dy1 N1 2.476(4) 3_565 ? Dy1 N1 2.476(4) . ? Dy1 N1 2.476(4) 2_665 ? Co1 O1 2.066(3) . ? Co1 O1 2.066(3) 13_666 ? Co1 O1 2.066(3) 4_665 ? Co1 O1 2.066(3) 16_556 ? Co1 O3 2.171(4) . ? Co1 O3 2.171(4) 13_666 ? O1 C1 1.243(5) . ? O2 C1 1.271(5) . ? O3 H3A 0.8430 . ? N1 C2 1.335(5) . ? N1 C2 1.335(5) 11 ? C1 C2 1.501(6) . ? C2 C3 1.382(6) . ? C3 C4 1.381(6) . ? C3 H3 0.9300 . ? C4 C3 1.381(6) 11 ? C4 H4 0.9300 . ? 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 O2 144.92(14) 11 2_665 ? O2 Dy1 O2 78.86(10) 11 12_565 ? O2 Dy1 O2 86.27(13) 2_665 12_565 ? O2 Dy1 O2 86.27(14) 11 3_565 ? O2 Dy1 O2 78.86(10) 2_665 3_565 ? O2 Dy1 O2 129.27(14) 12_565 3_565 ? O2 Dy1 O2 78.86(10) 11 10_665 ? O2 Dy1 O2 129.27(14) 2_665 10_665 ? O2 Dy1 O2 78.86(10) 12_565 10_665 ? O2 Dy1 O2 144.92(14) 3_565 10_665 ? O2 Dy1 O2 129.27(14) 11 . ? O2 Dy1 O2 78.86(10) 2_665 . ? O2 Dy1 O2 144.92(14) 12_565 . ? O2 Dy1 O2 78.86(10) 3_565 . ? O2 Dy1 O2 86.27(13) 10_665 . ? O2 Dy1 N1 72.46(7) 11 3_565 ? O2 Dy1 N1 72.46(7) 2_665 3_565 ? O2 Dy1 N1 64.64(7) 12_565 3_565 ? O2 Dy1 N1 64.64(7) 3_565 3_565 ? O2 Dy1 N1 136.86(7) 10_665 3_565 ? O2 Dy1 N1 136.86(7) . 3_565 ? O2 Dy1 N1 64.64(7) 11 . ? O2 Dy1 N1 136.86(7) 2_665 . ? O2 Dy1 N1 136.86(7) 12_565 . ? O2 Dy1 N1 72.46(7) 3_565 . ? O2 Dy1 N1 72.46(7) 10_665 . ? O2 Dy1 N1 64.64(7) . . ? N1 Dy1 N1 120.0 3_565 . ? O2 Dy1 N1 136.86(7) 11 2_665 ? O2 Dy1 N1 64.64(7) 2_665 2_665 ? O2 Dy1 N1 72.46(7) 12_565 2_665 ? O2 Dy1 N1 136.86(7) 3_565 2_665 ? O2 Dy1 N1 64.64(7) 10_665 2_665 ? O2 Dy1 N1 72.46(7) . 2_665 ? N1 Dy1 N1 120.0 3_565 2_665 ? N1 Dy1 N1 120.0 . 2_665 ? O1 Co1 O1 180.000(1) . 13_666 ? O1 Co1 O1 92.3(2) . 4_665 ? O1 Co1 O1 87.7(2) 13_666 4_665 ? O1 Co1 O1 87.7(2) . 16_556 ? O1 Co1 O1 92.3(2) 13_666 16_556 ? O1 Co1 O1 180.000(1) 4_665 16_556 ? O1 Co1 O3 88.55(12) . . ? O1 Co1 O3 91.45(12) 13_666 . ? O1 Co1 O3 91.45(12) 4_665 . ? O1 Co1 O3 88.55(12) 16_556 . ? O1 Co1 O3 91.45(12) . 13_666 ? O1 Co1 O3 88.55(12) 13_666 13_666 ? O1 Co1 O3 88.55(12) 4_665 13_666 ? O1 Co1 O3 91.45(12) 16_556 13_666 ? O3 Co1 O3 180.000(1) . 13_666 ? C1 O1 Co1 132.7(3) . . ? C1 O2 Dy1 123.5(3) . . ? Co1 O3 H3A 103.8 . . ? C2 N1 C2 119.0(5) . 11 ? C2 N1 Dy1 120.5(2) . . ? C2 N1 Dy1 120.5(2) 11 . ? O1 C1 O2 126.7(4) . . ? O1 C1 C2 116.9(4) . . ? O2 C1 C2 116.4(3) . . ? N1 C2 C3 122.2(4) . . ? N1 C2 C1 114.5(4) . . ? C3 C2 C1 123.3(4) . . ? C4 C3 C2 118.6(4) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C3 119.2(6) . 11 ? C3 C4 H4 120.4 . . ? C3 C4 H4 120.4 11 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co1 O1 C1 -21(98) 13_666 . . . ? O1 Co1 O1 C1 -77.9(4) 4_665 . . . ? O1 Co1 O1 C1 102.1(4) 16_556 . . . ? O3 Co1 O1 C1 -169.3(4) . . . . ? O3 Co1 O1 C1 10.7(4) 13_666 . . . ? O2 Dy1 O2 C1 6.0(3) 11 . . . ? O2 Dy1 O2 C1 162.4(3) 2_665 . . . ? O2 Dy1 O2 C1 -130.9(3) 12_565 . . . ? O2 Dy1 O2 C1 81.7(4) 3_565 . . . ? O2 Dy1 O2 C1 -66.4(3) 10_665 . . . ? N1 Dy1 O2 C1 113.6(3) 3_565 . . . ? N1 Dy1 O2 C1 6.0(3) . . . . ? N1 Dy1 O2 C1 -130.9(3) 2_665 . . . ? O2 Dy1 N1 C2 177.3(2) 11 . . . ? O2 Dy1 N1 C2 -37.7(2) 2_665 . . . ? O2 Dy1 N1 C2 142.3(2) 12_565 . . . ? O2 Dy1 N1 C2 -88.4(2) 3_565 . . . ? O2 Dy1 N1 C2 91.6(2) 10_665 . . . ? O2 Dy1 N1 C2 -2.7(2) . . . . ? N1 Dy1 N1 C2 -133.9(2) 3_565 . . . ? N1 Dy1 N1 C2 46.1(2) 2_665 . . . ? O2 Dy1 N1 C2 -2.7(2) 11 . . 11 ? O2 Dy1 N1 C2 142.3(2) 2_665 . . 11 ? O2 Dy1 N1 C2 -37.7(2) 12_565 . . 11 ? O2 Dy1 N1 C2 91.6(2) 3_565 . . 11 ? O2 Dy1 N1 C2 -88.4(2) 10_665 . . 11 ? O2 Dy1 N1 C2 177.3(2) . . . 11 ? N1 Dy1 N1 C2 46.1(2) 3_565 . . 11 ? N1 Dy1 N1 C2 -133.9(2) 2_665 . . 11 ? Co1 O1 C1 O2 3.2(7) . . . . ? Co1 O1 C1 C2 -176.8(3) . . . . ? Dy1 O2 C1 O1 171.8(3) . . . . ? Dy1 O2 C1 C2 -8.2(5) . . . . ? C2 N1 C2 C3 -0.7(4) 11 . . . ? Dy1 N1 C2 C3 179.3(4) . . . . ? C2 N1 C2 C1 -180.0(4) 11 . . . ? Dy1 N1 C2 C1 0.0(4) . . . . ? O1 C1 C2 N1 -174.9(3) . . . . ? O2 C1 C2 N1 5.1(5) . . . . ? O1 C1 C2 C3 5.8(7) . . . . ? O2 C1 C2 C3 -174.1(4) . . . . ? N1 C2 C3 C4 1.4(7) . . . . ? C1 C2 C3 C4 -179.4(4) . . . . ? C2 C3 C4 C3 -0.7(3) . . . 11 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.505 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.101 # Attachment '630839.cif' data_15 _database_code_depnum_ccdc_archive 'CCDC 630839' #TrackingRef '630839.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H42 Co3 N6 O36 Tb2' _chemical_formula_weight 1701.45 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 Hexagonal _symmetry_space_group_name_H-M P6/mcc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 15.288(4) _cell_length_b 15.288(4) _cell_length_c 15.571(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3152(2) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 3446 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 26.12 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1670 _exptl_absorpt_coefficient_mu 3.086 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.613773 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16034 _diffrn_reflns_av_R_equivalents 0.0805 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 26.27 _reflns_number_total 1111 _reflns_number_gt 736 _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. ; _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^)+(0.0292P)^2^+11.5169P] 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 1111 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Tb1 Tb 0.6667 0.3333 0.2500 0.01604(16) Uani 1 6 d S . . Co1 Co 0.5000 0.0000 0.0000 0.0165(2) Uani 1 4 d S . . O1 O 0.5871(2) 0.1983(2) 0.14337(19) 0.0276(8) Uani 1 1 d . . . O2 O 0.4471(3) 0.0605(3) 0.0924(2) 0.0353(9) Uani 1 1 d . . . O3 O 0.6483(3) 0.1350(4) 0.0000 0.0277(11) Uani 1 2 d S . . H3A H 0.6601 0.1842 0.0327 0.033 Uiso 0.50 1 d PR . . H3B H 0.6946 0.1386 -0.0327 0.033 Uiso 0.50 1 d PR . . N1 N 0.4776(4) 0.23878(18) 0.2500 0.0198(10) Uani 1 2 d S . . C1 C 0.4912(4) 0.1371(4) 0.1387(3) 0.0254(11) Uani 1 1 d . . . C2 C 0.4261(4) 0.1610(3) 0.1962(3) 0.0243(10) Uani 1 1 d . . . C3 C 0.3211(4) 0.1071(4) 0.1935(4) 0.0363(13) Uani 1 1 d . . . H3 H 0.2870 0.0542 0.1549 0.044 Uiso 1 1 calc R . . C4 C 0.2689(5) 0.1345(3) 0.2500 0.0439(19) Uani 1 2 d S . . H4 H 0.1987 0.0993 0.2500 0.053 Uiso 1 2 calc SR . . O4 O 0.7888(10) 0.0520(12) 0.0000 0.179(6) Uani 1 2 d S . . 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 0.01745(19) 0.01745(19) 0.0132(2) 0.000 0.000 0.00873(10) Co1 0.0219(7) 0.0141(5) 0.0130(5) 0.000 0.000 0.0086(6) O1 0.028(2) 0.0285(17) 0.0231(15) -0.0091(13) 0.0016(15) 0.0115(16) O2 0.033(2) 0.029(2) 0.035(2) -0.0171(17) 0.0019(17) 0.0092(17) O3 0.025(3) 0.028(3) 0.028(3) 0.000 0.000 0.011(2) N1 0.021(2) 0.0206(18) 0.018(2) -0.003(3) 0.000 0.0107(12) C1 0.032(3) 0.029(3) 0.017(2) -0.002(2) 0.001(2) 0.018(2) C2 0.025(3) 0.021(2) 0.025(2) -0.004(2) 0.001(2) 0.011(2) C3 0.025(3) 0.035(3) 0.044(3) -0.016(3) -0.004(3) 0.011(2) C4 0.018(3) 0.038(3) 0.069(5) -0.017(5) 0.000 0.0088(16) O4 0.186(12) 0.310(18) 0.104(8) 0.000 0.000 0.172(13) _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 O1 2.447(3) . ? Tb1 O1 2.447(3) 10_665 ? Tb1 O1 2.447(3) 11_655 ? Tb1 O1 2.447(3) 2_655 ? Tb1 O1 2.447(3) 12 ? Tb1 O1 2.447(3) 3_665 ? Tb1 N1 2.504(5) 2_655 ? Tb1 N1 2.504(5) 3_665 ? Tb1 N1 2.504(5) . ? Co1 O2 2.080(3) 13_655 ? Co1 O2 2.080(3) 16 ? Co1 O2 2.080(3) 4_655 ? Co1 O2 2.080(3) . ? Co1 O3 2.173(5) 13_655 ? Co1 O3 2.173(5) . ? O1 C1 1.288(6) . ? O2 C1 1.247(6) . ? O3 H3A 0.8500 . ? O3 H3B 0.8500 . ? N1 C2 1.342(5) . ? N1 C2 1.342(5) 12 ? C1 C2 1.514(6) . ? C2 C3 1.390(6) . ? C3 C4 1.386(6) . ? C3 H3 0.9300 . ? C4 C3 1.386(6) 12 ? C4 H4 0.9300 . ? 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 O1 Tb1 O1 145.03(16) . 10_665 ? O1 Tb1 O1 86.09(15) . 11_655 ? O1 Tb1 O1 79.02(12) 10_665 11_655 ? O1 Tb1 O1 79.02(12) . 2_655 ? O1 Tb1 O1 86.09(15) 10_665 2_655 ? O1 Tb1 O1 129.02(16) 11_655 2_655 ? O1 Tb1 O1 129.02(16) . 12 ? O1 Tb1 O1 79.02(12) 10_665 12 ? O1 Tb1 O1 79.02(12) 11_655 12 ? O1 Tb1 O1 145.03(16) 2_655 12 ? O1 Tb1 O1 79.02(12) . 3_665 ? O1 Tb1 O1 129.02(16) 10_665 3_665 ? O1 Tb1 O1 145.03(16) 11_655 3_665 ? O1 Tb1 O1 79.02(12) 2_655 3_665 ? O1 Tb1 O1 86.09(15) 12 3_665 ? O1 Tb1 N1 72.52(8) . 2_655 ? O1 Tb1 N1 72.52(8) 10_665 2_655 ? O1 Tb1 N1 64.51(8) 11_655 2_655 ? O1 Tb1 N1 64.51(8) 2_655 2_655 ? O1 Tb1 N1 136.95(8) 12 2_655 ? O1 Tb1 N1 136.95(8) 3_665 2_655 ? O1 Tb1 N1 136.95(8) . 3_665 ? O1 Tb1 N1 64.51(8) 10_665 3_665 ? O1 Tb1 N1 136.95(8) 11_655 3_665 ? O1 Tb1 N1 72.52(8) 2_655 3_665 ? O1 Tb1 N1 72.52(8) 12 3_665 ? O1 Tb1 N1 64.51(8) 3_665 3_665 ? N1 Tb1 N1 120.0 2_655 3_665 ? O1 Tb1 N1 64.51(8) . . ? O1 Tb1 N1 136.95(8) 10_665 . ? O1 Tb1 N1 72.52(8) 11_655 . ? O1 Tb1 N1 136.95(8) 2_655 . ? O1 Tb1 N1 64.51(8) 12 . ? O1 Tb1 N1 72.52(8) 3_665 . ? N1 Tb1 N1 120.0 2_655 . ? N1 Tb1 N1 120.0 3_665 . ? O2 Co1 O2 92.5(2) 13_655 16 ? O2 Co1 O2 87.5(2) 13_655 4_655 ? O2 Co1 O2 180.0(2) 16 4_655 ? O2 Co1 O2 180.0(2) 13_655 . ? O2 Co1 O2 87.5(2) 16 . ? O2 Co1 O2 92.5(2) 4_655 . ? O2 Co1 O3 91.76(13) 13_655 13_655 ? O2 Co1 O3 88.24(13) 16 13_655 ? O2 Co1 O3 91.76(13) 4_655 13_655 ? O2 Co1 O3 88.24(13) . 13_655 ? O2 Co1 O3 88.24(13) 13_655 . ? O2 Co1 O3 91.76(13) 16 . ? O2 Co1 O3 88.24(13) 4_655 . ? O2 Co1 O3 91.76(13) . . ? O3 Co1 O3 180.0(4) 13_655 . ? C1 O1 Tb1 123.8(3) . . ? C1 O2 Co1 132.0(3) . . ? Co1 O3 H3A 120.0 . . ? Co1 O3 H3B 120.1 . . ? H3A O3 H3B 120.0 . . ? C2 N1 C2 119.0(5) . 12 ? C2 N1 Tb1 120.5(3) . . ? C2 N1 Tb1 120.5(3) 12 . ? O2 C1 O1 126.9(4) . . ? O2 C1 C2 117.1(4) . . ? O1 C1 C2 116.0(4) . . ? N1 C2 C3 122.4(5) . . ? N1 C2 C1 114.7(4) . . ? C3 C2 C1 122.9(4) . . ? C4 C3 C2 118.0(5) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C3 C4 C3 120.2(7) . 12 ? C3 C4 H4 119.9 . . ? C3 C4 H4 119.9 12 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Tb1 O1 C1 131.4(4) 10_665 . . . ? O1 Tb1 O1 C1 66.9(3) 11_655 . . . ? O1 Tb1 O1 C1 -162.1(4) 2_655 . . . ? O1 Tb1 O1 C1 -5.6(3) 12 . . . ? O1 Tb1 O1 C1 -81.3(4) 3_665 . . . ? N1 Tb1 O1 C1 131.4(4) 2_655 . . . ? N1 Tb1 O1 C1 -113.1(3) 3_665 . . . ? N1 Tb1 O1 C1 -5.6(3) . . . . ? O2 Co1 O2 C1 -144.7(4) 13_655 . . . ? O2 Co1 O2 C1 -102.4(5) 16 . . . ? O2 Co1 O2 C1 77.6(5) 4_655 . . . ? O3 Co1 O2 C1 169.3(5) 13_655 . . . ? O3 Co1 O2 C1 -10.7(5) . . . . ? O1 Tb1 N1 C2 2.3(2) . . . . ? O1 Tb1 N1 C2 -142.8(3) 10_665 . . . ? O1 Tb1 N1 C2 -91.8(3) 11_655 . . . ? O1 Tb1 N1 C2 37.2(3) 2_655 . . . ? O1 Tb1 N1 C2 -177.7(2) 12 . . . ? O1 Tb1 N1 C2 88.2(3) 3_665 . . . ? N1 Tb1 N1 C2 -46.5(2) 2_655 . . . ? N1 Tb1 N1 C2 133.5(2) 3_665 . . . ? O1 Tb1 N1 C2 -177.7(2) . . . 12 ? O1 Tb1 N1 C2 37.2(3) 10_665 . . 12 ? O1 Tb1 N1 C2 88.2(3) 11_655 . . 12 ? O1 Tb1 N1 C2 -142.8(3) 2_655 . . 12 ? O1 Tb1 N1 C2 2.3(2) 12 . . 12 ? O1 Tb1 N1 C2 -91.8(3) 3_665 . . 12 ? N1 Tb1 N1 C2 133.5(2) 2_655 . . 12 ? N1 Tb1 N1 C2 -46.5(2) 3_665 . . 12 ? Co1 O2 C1 O1 -3.8(8) . . . . ? Co1 O2 C1 C2 176.7(3) . . . . ? Tb1 O1 C1 O2 -171.7(4) . . . . ? Tb1 O1 C1 C2 7.8(6) . . . . ? C2 N1 C2 C3 0.7(4) 12 . . . ? Tb1 N1 C2 C3 -179.3(4) . . . . ? C2 N1 C2 C1 -179.6(5) 12 . . . ? Tb1 N1 C2 C1 0.4(5) . . . . ? O2 C1 C2 N1 174.5(4) . . . . ? O1 C1 C2 N1 -5.1(6) . . . . ? O2 C1 C2 C3 -5.8(8) . . . . ? O1 C1 C2 C3 174.6(5) . . . . ? N1 C2 C3 C4 -1.3(8) . . . . ? C1 C2 C3 C4 179.0(4) . . . . ? C2 C3 C4 C3 0.6(4) . . . 12 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.27 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.847 _refine_diff_density_min -1.050 _refine_diff_density_rms 0.116 # Attachment '630840.cif' data_17 _database_code_depnum_ccdc_archive 'CCDC 630840' #TrackingRef '630840.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H42 Co3 N6 O36 Yb2' _chemical_formula_weight 1729.69 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6/mcc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 15.0144(8) _cell_length_b 15.0144(8) _cell_length_c 15.6165(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3048.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5082 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 26.34 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1690 _exptl_absorpt_coefficient_mu 3.938 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6942 _exptl_absorpt_correction_T_max 0.9254 _exptl_absorpt_process_details sadbas _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15667 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0197 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.34 _reflns_number_total 1090 _reflns_number_gt 795 _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. ; _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^)+(0.0392P)^2^+11.5791P] 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 1090 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.000 _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 Yb1 Yb 0.3333 0.6667 0.2500 0.01625(17) Uani 1 6 d S . . Co1 Co 0.5000 0.5000 0.0000 0.0160(3) Uani 1 4 d S . . O1 O 0.4096(3) 0.6092(3) 0.1446(2) 0.0257(7) Uani 1 1 d . . . O2 O 0.5505(3) 0.6130(3) 0.0916(2) 0.0351(9) Uani 1 1 d . . . O3 O 0.6507(4) 0.5144(4) 0.0000 0.0276(11) Uani 1 2 d S . . H3A H 0.6968 0.5561 0.0314 0.033 Uiso 0.50 1 d PR . . H3B H 0.6618 0.4769 -0.0314 0.033 Uiso 0.50 1 d PR . . N1 N 0.5200(4) 0.7600(2) 0.2500 0.0199(10) Uani 1 2 d S . . C1 C 0.7316(6) 0.8658(3) 0.2500 0.0414(19) Uani 1 2 d S . . H1A H 0.8032 0.9016 0.2500 0.050 Uiso 1 2 calc SR . . C2 C 0.6782(4) 0.7858(4) 0.1927(4) 0.0350(13) Uani 1 1 d . . . H2A H 0.7128 0.7678 0.1532 0.042 Uiso 1 1 calc R . . C3 C 0.5724(4) 0.7340(4) 0.1961(3) 0.0232(10) Uani 1 1 d . . . C4 C 0.5059(4) 0.6444(4) 0.1387(3) 0.0245(10) Uani 1 1 d . . . O4 O 0.7942(12) 0.7455(10) 0.0000 0.167(6) Uani 1 2 d S . . 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 Yb1 0.01810(19) 0.01810(19) 0.0125(2) 0.000 0.000 0.00905(10) Co1 0.0209(7) 0.0191(6) 0.0121(5) 0.000 0.000 0.0130(5) O1 0.0264(19) 0.029(2) 0.0208(15) -0.0090(15) -0.0011(15) 0.0136(15) O2 0.0298(19) 0.043(2) 0.036(2) -0.0201(19) -0.0023(18) 0.0206(18) O3 0.027(3) 0.029(3) 0.029(3) 0.000 0.000 0.016(2) N1 0.021(3) 0.0204(18) 0.018(2) -0.002(2) 0.000 0.0107(13) C1 0.019(3) 0.035(3) 0.065(5) -0.012(4) 0.000 0.0093(16) C2 0.026(3) 0.038(3) 0.042(3) -0.013(3) 0.001(3) 0.017(2) C3 0.025(2) 0.026(3) 0.021(2) -0.004(2) 0.000(2) 0.014(2) C4 0.031(3) 0.024(2) 0.020(2) -0.002(2) -0.002(2) 0.015(2) O4 0.191(14) 0.137(11) 0.105(8) 0.000 0.000 0.032(11) _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 Yb1 O1 2.399(3) 12_565 ? Yb1 O1 2.399(3) 3_565 ? Yb1 O1 2.399(3) 2_665 ? Yb1 O1 2.399(3) 11 ? Yb1 O1 2.399(3) . ? Yb1 O1 2.399(3) 10_665 ? Yb1 N1 2.428(5) 2_665 ? Yb1 N1 2.428(5) 3_565 ? Yb1 N1 2.428(5) . ? Co1 O2 2.052(3) 13_665 ? Co1 O2 2.052(3) . ? Co1 O2 2.052(3) 16 ? Co1 O2 2.052(3) 4_665 ? Co1 O3 2.163(5) . ? Co1 O3 2.163(5) 13_665 ? O1 C4 1.270(6) . ? O2 C4 1.235(6) . ? O3 H3A 0.8230 . ? O3 H3B 0.8231 . ? N1 C3 1.337(5) 12_565 ? N1 C3 1.337(5) . ? C1 C2 1.387(7) . ? C1 C2 1.387(7) 12_565 ? C1 H1A 0.9300 . ? C2 C3 1.377(7) . ? C2 H2A 0.9300 . ? C3 C4 1.506(6) . ? 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 O1 Yb1 O1 143.73(16) 12_565 3_565 ? O1 Yb1 O1 87.07(16) 12_565 2_665 ? O1 Yb1 O1 78.09(12) 3_565 2_665 ? O1 Yb1 O1 78.09(12) 12_565 11 ? O1 Yb1 O1 87.07(16) 3_565 11 ? O1 Yb1 O1 131.13(16) 2_665 11 ? O1 Yb1 O1 131.13(16) 12_565 . ? O1 Yb1 O1 78.09(12) 3_565 . ? O1 Yb1 O1 78.09(12) 2_665 . ? O1 Yb1 O1 143.73(16) 11 . ? O1 Yb1 O1 78.09(12) 12_565 10_665 ? O1 Yb1 O1 131.13(16) 3_565 10_665 ? O1 Yb1 O1 143.73(16) 2_665 10_665 ? O1 Yb1 O1 78.09(12) 11 10_665 ? O1 Yb1 O1 87.07(16) . 10_665 ? O1 Yb1 N1 71.86(8) 12_565 2_665 ? O1 Yb1 N1 71.86(8) 3_565 2_665 ? O1 Yb1 N1 65.56(8) 2_665 2_665 ? O1 Yb1 N1 65.56(8) 11 2_665 ? O1 Yb1 N1 136.46(8) . 2_665 ? O1 Yb1 N1 136.46(8) 10_665 2_665 ? O1 Yb1 N1 136.46(8) 12_565 3_565 ? O1 Yb1 N1 65.56(8) 3_565 3_565 ? O1 Yb1 N1 136.46(8) 2_665 3_565 ? O1 Yb1 N1 71.86(8) 11 3_565 ? O1 Yb1 N1 71.86(8) . 3_565 ? O1 Yb1 N1 65.56(8) 10_665 3_565 ? N1 Yb1 N1 120.0 2_665 3_565 ? O1 Yb1 N1 65.56(8) 12_565 . ? O1 Yb1 N1 136.46(8) 3_565 . ? O1 Yb1 N1 71.86(8) 2_665 . ? O1 Yb1 N1 136.46(8) 11 . ? O1 Yb1 N1 65.56(8) . . ? O1 Yb1 N1 71.86(8) 10_665 . ? N1 Yb1 N1 120.000(1) 2_665 . ? N1 Yb1 N1 120.0 3_565 . ? O2 Co1 O2 180.0(2) 13_665 . ? O2 Co1 O2 91.7(2) 13_665 16 ? O2 Co1 O2 88.3(2) . 16 ? O2 Co1 O2 88.3(2) 13_665 4_665 ? O2 Co1 O2 91.7(2) . 4_665 ? O2 Co1 O2 180.0 16 4_665 ? O2 Co1 O3 91.02(14) 13_665 . ? O2 Co1 O3 88.98(14) . . ? O2 Co1 O3 88.98(14) 16 . ? O2 Co1 O3 91.02(14) 4_665 . ? O2 Co1 O3 88.98(14) 13_665 13_665 ? O2 Co1 O3 91.02(14) . 13_665 ? O2 Co1 O3 91.02(14) 16 13_665 ? O2 Co1 O3 88.98(14) 4_665 13_665 ? O3 Co1 O3 180.0 . 13_665 ? C4 O1 Yb1 123.3(3) . . ? C4 O2 Co1 133.1(3) . . ? Co1 O3 H3A 121.0 . . ? Co1 O3 H3B 119.3 . . ? H3A O3 H3B 119.7 . . ? C3 N1 C3 118.8(6) 12_565 . ? C3 N1 Yb1 120.6(3) 12_565 . ? C3 N1 Yb1 120.6(3) . . ? C2 C1 C2 119.9(7) . 12_565 ? C2 C1 H1A 120.1 . . ? C2 C1 H1A 120.1 12_565 . ? C3 C2 C1 118.0(5) . . ? C3 C2 H2A 121.0 . . ? C1 C2 H2A 121.0 . . ? N1 C3 C2 122.7(5) . . ? N1 C3 C4 114.3(4) . . ? C2 C3 C4 123.0(4) . . ? O2 C4 O1 127.3(5) . . ? O2 C4 C3 116.9(5) . . ? O1 C4 C3 115.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Yb1 O1 C4 4.7(3) 12_565 . . . ? O1 Yb1 O1 C4 160.1(4) 3_565 . . . ? O1 Yb1 O1 C4 80.0(4) 2_665 . . . ? O1 Yb1 O1 C4 -132.0(4) 11 . . . ? O1 Yb1 O1 C4 -66.7(4) 10_665 . . . ? N1 Yb1 O1 C4 113.3(4) 2_665 . . . ? N1 Yb1 O1 C4 -132.0(4) 3_565 . . . ? N1 Yb1 O1 C4 4.7(3) . . . . ? O2 Co1 O2 C4 0(100) 13_665 . . . ? O2 Co1 O2 C4 103.1(5) 16 . . . ? O2 Co1 O2 C4 -76.9(5) 4_665 . . . ? O3 Co1 O2 C4 -167.9(5) . . . . ? O3 Co1 O2 C4 12.1(5) 13_665 . . . ? O1 Yb1 N1 C3 -1.9(2) 12_565 . . 12_565 ? O1 Yb1 N1 C3 142.0(3) 3_565 . . 12_565 ? O1 Yb1 N1 C3 93.3(3) 2_665 . . 12_565 ? O1 Yb1 N1 C3 -38.0(3) 11 . . 12_565 ? O1 Yb1 N1 C3 178.1(2) . . . 12_565 ? O1 Yb1 N1 C3 -86.7(3) 10_665 . . 12_565 ? N1 Yb1 N1 C3 47.1(2) 2_665 . . 12_565 ? N1 Yb1 N1 C3 -132.9(2) 3_565 . . 12_565 ? O1 Yb1 N1 C3 178.1(2) 12_565 . . . ? O1 Yb1 N1 C3 -38.0(3) 3_565 . . . ? O1 Yb1 N1 C3 -86.7(3) 2_665 . . . ? O1 Yb1 N1 C3 142.0(3) 11 . . . ? O1 Yb1 N1 C3 -1.9(2) . . . . ? O1 Yb1 N1 C3 93.3(3) 10_665 . . . ? N1 Yb1 N1 C3 -132.9(2) 2_665 . . . ? N1 Yb1 N1 C3 47.1(2) 3_565 . . . ? C2 C1 C2 C3 -1.1(4) 12_565 . . . ? C3 N1 C3 C2 -1.2(4) 12_565 . . . ? Yb1 N1 C3 C2 178.8(4) . . . . ? C3 N1 C3 C4 179.6(5) 12_565 . . . ? Yb1 N1 C3 C4 -0.4(5) . . . . ? C1 C2 C3 N1 2.3(8) . . . . ? C1 C2 C3 C4 -178.6(4) . . . . ? Co1 O2 C4 O1 2.9(9) . . . . ? Co1 O2 C4 C3 -177.5(3) . . . . ? Yb1 O1 C4 O2 173.1(4) . . . . ? Yb1 O1 C4 C3 -6.5(6) . . . . ? N1 C3 C4 O2 -175.4(4) . . . . ? C2 C3 C4 O2 5.4(8) . . . . ? N1 C3 C4 O1 4.3(6) . . . . ? C2 C3 C4 O1 -174.9(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.955 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.133 # Attachment '772801.cif' data_21 _database_code_depnum_ccdc_archive 'CCDC 772801' #TrackingRef '772801.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H26 Co2 Dy N3 O24' _chemical_formula_weight 984.81 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' 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.939(5) _cell_length_b 24.460(14) _cell_length_c 18.213(9) _cell_angle_alpha 90.00 _cell_angle_beta 110.34(2) _cell_angle_gamma 90.00 _cell_volume 3734(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7444 _cell_measurement_theta_min 2.0481 _cell_measurement_theta_max 28.0692 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1940 _exptl_absorpt_coefficient_mu 2.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5902 _exptl_absorpt_correction_T_max 0.5902 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27283 _diffrn_reflns_av_R_equivalents 0.1868 _diffrn_reflns_av_sigmaI/netI 0.1497 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6525 _reflns_number_gt 4630 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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. Rint value is higher than 0.1, and the results maybe originated from the poor single crystal quality, although much effort has been made. The residual peaks are 3.59 and 3.42, and the distances to the nearest atom Dy1 are 0.98 and 1.00, respectively. ; _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^)+(0.0778P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6525 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.2034 _refine_ls_wR_factor_gt 0.1829 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.45778(6) 0.68633(2) 0.42194(3) 0.0228(2) Uani 1 1 d . . . Co1 Co 1.00225(18) 0.83171(7) 0.48509(9) 0.0357(4) Uani 1 1 d . . . Co2 Co 0.07286(17) 0.90972(6) 0.07413(8) 0.0272(4) Uani 1 1 d . . . C1 C 0.6468(14) 0.8014(5) 0.4034(6) 0.033(3) Uani 1 1 d . . . C2 C 0.4929(13) 0.8047(5) 0.3326(6) 0.027(3) Uani 1 1 d . . . C3 C 0.4601(13) 0.8492(5) 0.2816(7) 0.033(3) Uani 1 1 d . . . H3 H 0.5315 0.8782 0.2902 0.040 Uiso 1 1 calc R . . C4 C 0.3150(12) 0.8494(4) 0.2160(6) 0.026(2) Uani 1 1 d . . . C5 C 0.2156(12) 0.8031(5) 0.2095(6) 0.028(3) Uani 1 1 d . . . H5 H 0.1183 0.8012 0.1685 0.034 Uiso 1 1 calc R . . C6 C 0.2600(12) 0.7611(5) 0.2623(6) 0.027(2) Uani 1 1 d . . . C7 C 0.1612(12) 0.7105(5) 0.2566(6) 0.027(3) Uani 1 1 d . . . C8 C 0.5891(14) 0.6086(5) 0.3056(7) 0.036(3) Uani 1 1 d . . . C9 C 0.5100(12) 0.5655(5) 0.3392(6) 0.026(2) Uani 1 1 d . . . C10 C 0.5160(13) 0.5111(5) 0.3281(6) 0.030(3) Uani 1 1 d . . . H10 H 0.5715 0.4979 0.2970 0.036 Uiso 1 1 calc R . . C11 C 0.4406(13) 0.4745(4) 0.3623(6) 0.029(3) Uani 1 1 d . . . C12 C 0.3588(14) 0.4955(4) 0.4081(6) 0.030(3) Uani 1 1 d . . . H12 H 0.3052 0.4722 0.4309 0.037 Uiso 1 1 calc R . . C13 C 0.3573(12) 0.5506(4) 0.4196(6) 0.026(2) Uani 1 1 d . . . C14 C 0.2850(13) 0.5788(5) 0.4734(6) 0.030(3) Uani 1 1 d . . . C15 C 0.7665(13) 0.6479(4) 0.5794(6) 0.024(2) Uani 1 1 d . . . C16 C 0.6958(12) 0.6910(4) 0.6147(6) 0.023(2) Uani 1 1 d . . . C17 C 0.7628(13) 0.7097(5) 0.6913(6) 0.029(3) Uani 1 1 d . . . H17 H 0.8567 0.6944 0.7250 0.035 Uiso 1 1 calc R . . C18 C 0.6864(13) 0.7525(5) 0.7174(6) 0.030(3) Uani 1 1 d . . . C19 C 0.5441(13) 0.7731(5) 0.6652(7) 0.032(3) Uani 1 1 d . . . H19 H 0.4905 0.8008 0.6808 0.039 Uiso 1 1 calc R . . C20 C 0.4827(12) 0.7524(4) 0.5903(6) 0.026(2) Uani 1 1 d . . . C21 C 0.3314(13) 0.7728(5) 0.5276(6) 0.030(3) Uani 1 1 d . . . N1 N 0.3988(11) 0.7625(4) 0.3245(5) 0.029(2) Uani 1 1 d . . . N2 N 0.4334(10) 0.5864(4) 0.3857(5) 0.026(2) Uani 1 1 d . . . N3 N 0.5542(10) 0.7141(4) 0.5644(5) 0.028(2) Uani 1 1 d . . . O1 O 0.6561(9) 0.7587(3) 0.4457(4) 0.0303(18) Uani 1 1 d . . . O2 O 0.7482(9) 0.8390(3) 0.4177(4) 0.0347(19) Uani 1 1 d . . . O3 O 0.2793(9) 0.8906(3) 0.1656(4) 0.037(2) Uani 1 1 d . . . O4 O 0.2094(9) 0.6781(3) 0.3144(4) 0.0341(19) Uani 1 1 d . . . O5 O 0.0383(9) 0.7030(3) 0.1964(4) 0.038(2) Uani 1 1 d . . . O6 O 0.5877(9) 0.6582(3) 0.3312(4) 0.0328(18) Uani 1 1 d . . . O7 O 0.6528(12) 0.5949(4) 0.2582(5) 0.056(3) Uani 1 1 d . . . O8 O 0.4542(9) 0.4195(3) 0.3572(5) 0.037(2) Uani 1 1 d . . . H8 H 0.5405 0.4163 0.3452 0.056 Uiso 1 1 d R . . O9 O 0.3034(9) 0.6318(3) 0.4776(4) 0.0312(18) Uani 1 1 d . . . O10 O 0.2117(8) 0.5522(3) 0.5087(4) 0.0295(18) Uani 1 1 d . . . O11 O 0.6933(8) 0.6389(3) 0.5050(4) 0.0267(17) Uani 1 1 d . . . O12 O 0.8992(8) 0.6263(3) 0.6206(4) 0.0274(17) Uani 1 1 d . . . O13 O 0.7529(9) 0.7708(3) 0.7908(4) 0.036(2) Uani 1 1 d . . . H13 H 0.8501 0.7721 0.8024 0.055 Uiso 1 1 calc R . . O14 O 0.2492(9) 0.8087(3) 0.5474(5) 0.038(2) Uani 1 1 d . . . O15 O 0.2952(9) 0.7512(3) 0.4605(4) 0.0339(19) Uani 1 1 d . . . O16 O 0.9970(13) 0.8799(4) 0.5793(6) 0.075(3) Uani 1 1 d . . . H16A H 0.9094 0.8938 0.5787 0.090 Uiso 1 1 d R . . H16B H 1.0822 0.8857 0.6179 0.090 Uiso 1 1 d R . . O17 O 1.0537(13) 0.9023(4) 0.4356(6) 0.081(4) Uani 1 1 d . . . H17A H 0.9781 0.9198 0.4024 0.097 Uiso 1 1 d R . . H17B H 1.1491 0.9137 0.4482 0.097 Uiso 1 1 d R . . O18 O 1.0077(10) 0.7877(4) 0.3893(5) 0.051(2) Uani 1 1 d . . . H18A H 0.9225 0.7827 0.3504 0.061 Uiso 1 1 d R . . H18B H 1.0954 0.7746 0.3888 0.061 Uiso 1 1 d R . . O19 O 0.9505(9) 0.7636(3) 0.5456(4) 0.039(2) Uani 1 1 d . . . H19A H 0.8548 0.7530 0.5348 0.047 Uiso 1 1 d R . . H19B H 1.0259 0.7471 0.5805 0.047 Uiso 1 1 d R . . O20 O 0.0512(11) 0.8360(3) 0.0108(5) 0.047(2) Uani 1 1 d . . . H20A H -0.0107 0.8108 0.0150 0.057 Uiso 1 1 d R . . H20B H 0.1051 0.8317 -0.0192 0.057 Uiso 1 1 d R . . O21 O -0.1265(10) 0.9398(4) -0.0225(5) 0.046(2) Uani 1 1 d . . . H21B H -0.2302 0.9414 -0.0468 0.056 Uiso 1 1 d R . . H21A H -0.0919 0.9710 0.0015 0.056 Uiso 1 1 d R . . O22 O 0.0707(11) 0.9834(4) 0.1306(5) 0.053(2) Uani 1 1 d . . . H22A H 0.0115 0.9866 0.1582 0.064 Uiso 1 1 d R . . H22B H 0.1280 1.0102 0.1266 0.064 Uiso 1 1 d R . . O23 O 0.9994(18) 0.0900(7) 0.1982(12) 0.166(8) Uani 1 1 d . . . O24 O 0.960(4) 0.9250(10) 0.2756(10) 0.298(18) 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 Dy1 0.0259(3) 0.0241(3) 0.0181(3) 0.0017(2) 0.0071(2) -0.0002(2) Co1 0.0285(9) 0.0419(10) 0.0322(9) 0.0009(7) 0.0047(7) 0.0028(7) Co2 0.0289(8) 0.0280(9) 0.0242(8) 0.0048(6) 0.0085(7) 0.0002(6) C1 0.039(7) 0.033(7) 0.022(6) 0.001(5) 0.004(5) -0.005(6) C2 0.023(6) 0.038(7) 0.024(6) 0.004(5) 0.011(5) -0.001(5) C3 0.033(7) 0.028(6) 0.040(7) 0.006(5) 0.013(6) 0.009(5) C4 0.030(6) 0.021(6) 0.022(6) 0.007(4) 0.003(5) -0.002(5) C5 0.013(5) 0.045(7) 0.021(6) 0.004(5) -0.001(4) -0.005(5) C6 0.024(6) 0.039(7) 0.016(5) 0.007(5) 0.005(5) -0.004(5) C7 0.017(6) 0.030(6) 0.032(6) 0.002(5) 0.006(5) 0.002(5) C8 0.040(7) 0.037(7) 0.033(7) -0.003(6) 0.014(6) 0.007(6) C9 0.031(6) 0.031(7) 0.022(6) -0.001(5) 0.017(5) -0.005(5) C10 0.031(6) 0.033(7) 0.029(6) -0.005(5) 0.014(5) 0.004(5) C11 0.032(6) 0.019(6) 0.032(6) -0.004(5) 0.005(5) -0.009(5) C12 0.050(7) 0.014(6) 0.031(6) 0.004(5) 0.018(6) -0.002(5) C13 0.026(6) 0.029(6) 0.023(6) -0.009(5) 0.009(5) -0.007(5) C14 0.029(6) 0.034(7) 0.024(6) 0.004(5) 0.004(5) 0.005(5) C15 0.033(6) 0.025(6) 0.017(5) 0.007(4) 0.011(5) -0.005(5) C16 0.023(6) 0.037(7) 0.011(5) -0.008(4) 0.007(4) 0.000(5) C17 0.029(6) 0.030(6) 0.031(6) 0.008(5) 0.015(5) -0.002(5) C18 0.035(7) 0.033(7) 0.023(6) -0.001(5) 0.010(5) 0.008(5) C19 0.033(7) 0.034(7) 0.035(7) -0.008(5) 0.019(6) 0.003(5) C20 0.024(6) 0.027(6) 0.025(6) -0.008(5) 0.007(5) 0.014(5) C21 0.026(6) 0.035(7) 0.025(6) 0.007(5) 0.003(5) -0.002(5) N1 0.033(5) 0.022(5) 0.031(5) 0.009(4) 0.012(4) -0.002(4) N2 0.026(5) 0.032(5) 0.018(4) -0.003(4) 0.006(4) -0.005(4) N3 0.032(5) 0.031(6) 0.018(5) -0.003(4) 0.006(4) 0.002(4) O1 0.034(4) 0.024(4) 0.030(4) 0.006(3) 0.008(4) -0.004(3) O2 0.028(4) 0.029(5) 0.038(5) 0.008(4) -0.001(4) -0.005(4) O3 0.031(4) 0.040(5) 0.037(5) 0.020(4) 0.009(4) 0.001(4) O4 0.041(5) 0.035(5) 0.025(4) 0.012(3) 0.009(4) -0.003(4) O5 0.036(5) 0.040(5) 0.029(4) 0.009(4) 0.000(4) -0.010(4) O6 0.047(5) 0.028(5) 0.029(4) -0.001(3) 0.021(4) -0.005(4) O7 0.102(8) 0.036(5) 0.057(6) -0.008(4) 0.062(6) -0.011(5) O8 0.046(5) 0.025(4) 0.048(5) -0.005(4) 0.026(4) -0.001(4) O9 0.041(5) 0.029(5) 0.030(4) 0.003(3) 0.021(4) -0.001(4) O10 0.031(4) 0.027(4) 0.035(4) 0.000(3) 0.017(4) -0.003(3) O11 0.034(4) 0.026(4) 0.019(4) -0.007(3) 0.007(3) 0.005(3) O12 0.023(4) 0.035(4) 0.021(4) -0.010(3) 0.002(3) 0.007(3) O13 0.031(4) 0.049(5) 0.019(4) -0.012(4) -0.005(3) 0.010(4) O14 0.032(5) 0.041(5) 0.033(5) -0.014(4) 0.001(4) 0.010(4) O15 0.028(4) 0.047(5) 0.022(4) -0.007(4) 0.003(3) 0.001(4) O16 0.072(7) 0.070(8) 0.071(7) -0.026(6) 0.010(6) 0.021(6) O17 0.073(8) 0.080(8) 0.075(8) 0.015(6) 0.005(6) -0.010(6) O18 0.031(5) 0.078(7) 0.037(5) -0.010(5) 0.004(4) 0.015(5) O19 0.032(5) 0.050(5) 0.028(4) 0.004(4) 0.000(4) 0.004(4) O20 0.070(6) 0.031(5) 0.058(6) -0.004(4) 0.043(5) -0.008(4) O21 0.039(5) 0.050(6) 0.039(5) 0.024(4) 0.000(4) -0.014(4) O22 0.053(6) 0.043(6) 0.069(7) -0.003(5) 0.029(5) -0.001(4) O23 0.103(11) 0.136(14) 0.23(2) -0.108(14) 0.023(12) 0.028(10) O24 0.55(5) 0.21(3) 0.074(12) 0.010(14) 0.03(2) -0.02(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O9 2.384(7) . ? Dy1 O4 2.405(8) . ? Dy1 O15 2.415(8) . ? Dy1 O11 2.420(7) . ? Dy1 O6 2.426(8) . ? Dy1 O1 2.435(7) . ? Dy1 N1 2.500(8) . ? Dy1 N2 2.523(9) . ? Dy1 N3 2.527(8) . ? Co1 O18 2.065(9) . ? Co1 O17 2.071(11) . ? Co1 O16 2.095(10) . ? Co1 O19 2.134(8) . ? Co1 O14 2.176(8) 1_655 ? Co1 O2 2.182(7) . ? Co2 O3 2.064(7) . ? Co2 O22 2.079(9) . ? Co2 O20 2.113(8) . ? Co2 O21 2.154(8) . ? Co2 O12 2.193(7) 4_475 ? Co2 O10 2.205(7) 4_575 ? C1 O2 1.254(13) . ? C1 O1 1.283(13) . ? C1 C2 1.526(15) . ? C2 N1 1.307(13) . ? C2 C3 1.394(15) . ? C3 C4 1.426(14) . ? C3 H3 0.9300 . ? C4 O3 1.326(12) . ? C4 C5 1.419(15) . ? C5 C6 1.369(14) . ? C5 H5 0.9300 . ? C6 N1 1.358(13) . ? C6 C7 1.502(15) . ? C7 O5 1.268(12) . ? C7 O4 1.269(12) . ? C8 O7 1.235(14) . ? C8 O6 1.301(14) . ? C8 C9 1.512(16) . ? C9 C10 1.349(14) . ? C9 N2 1.361(13) . ? C10 C11 1.392(15) . ? C10 H10 0.9300 . ? C11 O8 1.357(12) . ? C11 C12 1.384(15) . ? C12 C13 1.366(14) . ? C12 H12 0.9300 . ? C13 N2 1.378(13) . ? C13 C14 1.515(15) . ? C14 O10 1.249(13) . ? C14 O9 1.305(13) . ? C15 O12 1.277(12) . ? C15 O11 1.301(11) . ? C15 C16 1.488(14) . ? C16 C17 1.390(14) . ? C16 N3 1.398(13) . ? C17 C18 1.419(15) . ? C17 H17 0.9300 . ? C18 O13 1.338(12) . ? C18 C19 1.391(15) . ? C19 C20 1.377(14) . ? C19 H19 0.9300 . ? C20 N3 1.310(13) . ? C20 C21 1.520(14) . ? C21 O15 1.267(13) . ? C21 O14 1.275(13) . ? O8 H8 0.8753 . ? O10 Co2 2.205(7) 4_576 ? O12 Co2 2.193(7) 4_676 ? O13 H13 0.8200 . ? O14 Co1 2.176(8) 1_455 ? O16 H16A 0.8500 . ? O16 H16B 0.8500 . ? O17 H17A 0.8501 . ? O17 H17B 0.8499 . ? O18 H18A 0.8500 . ? O18 H18B 0.8499 . ? O19 H19A 0.8500 . ? O19 H19B 0.8500 . ? O20 H20A 0.8500 . ? O20 H20B 0.8499 . ? O21 H21B 0.8784 . ? O21 H21A 0.8803 . ? O22 H22A 0.8500 . ? O22 H22B 0.8499 . ? 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 O9 Dy1 O4 78.0(3) . . ? O9 Dy1 O15 75.4(3) . . ? O4 Dy1 O15 79.2(3) . . ? O9 Dy1 O11 88.4(3) . . ? O4 Dy1 O11 145.6(2) . . ? O15 Dy1 O11 127.9(2) . . ? O9 Dy1 O6 128.0(3) . . ? O4 Dy1 O6 86.9(3) . . ? O15 Dy1 O6 149.7(3) . . ? O11 Dy1 O6 76.8(2) . . ? O9 Dy1 O1 145.5(2) . . ? O4 Dy1 O1 127.9(2) . . ? O15 Dy1 O1 86.8(3) . . ? O11 Dy1 O1 79.4(2) . . ? O6 Dy1 O1 80.6(3) . . ? O9 Dy1 N1 135.1(3) . . ? O4 Dy1 N1 65.0(3) . . ? O15 Dy1 N1 73.5(3) . . ? O11 Dy1 N1 136.4(3) . . ? O6 Dy1 N1 76.1(3) . . ? O1 Dy1 N1 63.0(3) . . ? O9 Dy1 N2 63.8(3) . . ? O4 Dy1 N2 74.6(3) . . ? O15 Dy1 N2 135.0(3) . . ? O11 Dy1 N2 71.1(2) . . ? O6 Dy1 N2 64.2(3) . . ? O1 Dy1 N2 138.0(3) . . ? N1 Dy1 N2 124.0(3) . . ? O9 Dy1 N3 75.8(3) . . ? O4 Dy1 N3 138.4(3) . . ? O15 Dy1 N3 63.2(3) . . ? O11 Dy1 N3 64.8(3) . . ? O6 Dy1 N3 134.6(3) . . ? O1 Dy1 N3 69.8(3) . . ? N1 Dy1 N3 116.2(3) . . ? N2 Dy1 N3 119.8(3) . . ? O18 Co1 O17 89.6(4) . . ? O18 Co1 O16 177.2(4) . . ? O17 Co1 O16 87.6(5) . . ? O18 Co1 O19 95.9(4) . . ? O17 Co1 O19 174.5(4) . . ? O16 Co1 O19 86.9(4) . . ? O18 Co1 O14 89.4(3) . 1_655 ? O17 Co1 O14 96.0(4) . 1_655 ? O16 Co1 O14 91.4(3) . 1_655 ? O19 Co1 O14 83.8(3) . 1_655 ? O18 Co1 O2 83.9(3) . . ? O17 Co1 O2 91.8(4) . . ? O16 Co1 O2 95.7(4) . . ? O19 Co1 O2 89.1(3) . . ? O14 Co1 O2 169.6(3) 1_655 . ? O3 Co2 O22 87.5(3) . . ? O3 Co2 O20 97.7(3) . . ? O22 Co2 O20 174.4(4) . . ? O3 Co2 O21 172.2(3) . . ? O22 Co2 O21 87.7(4) . . ? O20 Co2 O21 87.3(4) . . ? O3 Co2 O12 98.8(3) . 4_475 ? O22 Co2 O12 91.6(3) . 4_475 ? O20 Co2 O12 85.7(3) . 4_475 ? O21 Co2 O12 87.5(3) . 4_475 ? O3 Co2 O10 91.1(3) . 4_575 ? O22 Co2 O10 90.3(3) . 4_575 ? O20 Co2 O10 91.6(3) . 4_575 ? O21 Co2 O10 82.8(3) . 4_575 ? O12 Co2 O10 170.1(3) 4_475 4_575 ? O2 C1 O1 125.6(10) . . ? O2 C1 C2 120.7(10) . . ? O1 C1 C2 113.7(10) . . ? N1 C2 C3 124.2(10) . . ? N1 C2 C1 114.2(9) . . ? C3 C2 C1 121.6(10) . . ? C2 C3 C4 118.7(10) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? O3 C4 C5 123.8(9) . . ? O3 C4 C3 120.9(9) . . ? C5 C4 C3 115.3(9) . . ? C6 C5 C4 121.4(9) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? N1 C6 C5 121.6(10) . . ? N1 C6 C7 115.1(9) . . ? C5 C6 C7 123.3(9) . . ? O5 C7 O4 124.6(10) . . ? O5 C7 C6 119.5(9) . . ? O4 C7 C6 115.8(9) . . ? O7 C8 O6 124.6(12) . . ? O7 C8 C9 119.2(11) . . ? O6 C8 C9 116.2(10) . . ? C10 C9 N2 121.2(10) . . ? C10 C9 C8 125.4(10) . . ? N2 C9 C8 113.4(9) . . ? C9 C10 C11 121.1(10) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? O8 C11 C12 119.2(10) . . ? O8 C11 C10 122.6(10) . . ? C12 C11 C10 118.1(10) . . ? C13 C12 C11 119.6(10) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 N2 121.7(10) . . ? C12 C13 C14 125.3(10) . . ? N2 C13 C14 112.9(9) . . ? O10 C14 O9 124.5(10) . . ? O10 C14 C13 120.9(10) . . ? O9 C14 C13 114.6(10) . . ? O12 C15 O11 124.7(10) . . ? O12 C15 C16 119.1(9) . . ? O11 C15 C16 115.8(9) . . ? C17 C16 N3 120.1(10) . . ? C17 C16 C15 124.6(10) . . ? N3 C16 C15 115.3(8) . . ? C16 C17 C18 119.3(10) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? O13 C18 C19 123.0(10) . . ? O13 C18 C17 118.9(10) . . ? C19 C18 C17 118.1(10) . . ? C20 C19 C18 119.9(10) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? N3 C20 C19 122.9(10) . . ? N3 C20 C21 112.5(9) . . ? C19 C20 C21 124.5(10) . . ? O15 C21 O14 125.6(10) . . ? O15 C21 C20 116.7(10) . . ? O14 C21 C20 117.7(9) . . ? C2 N1 C6 118.7(9) . . ? C2 N1 Dy1 122.6(7) . . ? C6 N1 Dy1 118.6(7) . . ? C9 N2 C13 118.4(9) . . ? C9 N2 Dy1 120.7(7) . . ? C13 N2 Dy1 120.6(7) . . ? C20 N3 C16 119.7(8) . . ? C20 N3 Dy1 121.8(7) . . ? C16 N3 Dy1 118.2(6) . . ? C1 O1 Dy1 126.4(7) . . ? C1 O2 Co1 126.3(7) . . ? C4 O3 Co2 131.5(7) . . ? C7 O4 Dy1 125.0(7) . . ? C8 O6 Dy1 125.1(7) . . ? C11 O8 H8 102.3 . . ? C14 O9 Dy1 127.6(7) . . ? C14 O10 Co2 123.5(7) . 4_576 ? C15 O11 Dy1 125.7(6) . . ? C15 O12 Co2 125.2(6) . 4_676 ? C18 O13 H13 109.5 . . ? C21 O14 Co1 127.6(7) . 1_455 ? C21 O15 Dy1 125.3(7) . . ? Co1 O16 H16A 119.8 . . ? Co1 O16 H16B 120.2 . . ? H16A O16 H16B 120.0 . . ? Co1 O17 H17A 119.3 . . ? Co1 O17 H17B 120.8 . . ? H17A O17 H17B 120.0 . . ? Co1 O18 H18A 120.1 . . ? Co1 O18 H18B 119.9 . . ? H18A O18 H18B 120.0 . . ? Co1 O19 H19A 120.1 . . ? Co1 O19 H19B 119.9 . . ? H19A O19 H19B 120.0 . . ? Co2 O20 H20A 120.6 . . ? Co2 O20 H20B 119.4 . . ? H20A O20 H20B 120.0 . . ? Co2 O21 H21B 148.7 . . ? Co2 O21 H21A 80.9 . . ? H21B O21 H21A 109.8 . . ? Co2 O22 H22A 119.0 . . ? Co2 O22 H22B 121.0 . . ? H22A O22 H22B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.586 _refine_diff_density_min -2.045 _refine_diff_density_rms 0.239 # Attachment '772802.cif' data_23 _database_code_depnum_ccdc_archive 'CCDC 772802' #TrackingRef '772802.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 Co2 Er N3 O26' _chemical_formula_weight 1025.60 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9328(18) _cell_length_b 24.341(5) _cell_length_c 18.192(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.27(3) _cell_angle_gamma 90.00 _cell_volume 3710.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8641 _cell_measurement_theta_min 1.4572 _cell_measurement_theta_max 27.8445 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2028 _exptl_absorpt_coefficient_mu 3.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5651 _exptl_absorpt_correction_T_max 0.5651 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22405 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6487 _reflns_number_gt 5519 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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. ISOR: the parameter to go anisotropic restraint to appointed atoms, is applied for disordered water molecule O26 and O26'. The residual peak is 2.644, and the distance to the nearest atom Co2 is 0.84. ; _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^)+(0.0631P)^2^+11.1775P] 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 6487 _refine_ls_number_parameters 498 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.067 _refine_ls_shift/su_mean 0.002 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 Er1 Er 0.04426(3) 0.812694(10) 0.082541(13) 0.01622(11) Uani 1 1 d . A . Co1 Co -0.57284(10) 0.90643(3) -0.06926(4) 0.0211(2) Uani 1 1 d . . . Co2 Co 0.50102(11) 0.66934(4) 0.02301(5) 0.0319(2) Uani 1 1 d . . . C1 C 0.1738(7) 0.7265(2) -0.0211(3) 0.0207(13) Uani 1 1 d . A . C2 C 0.0228(8) 0.7469(2) -0.0834(3) 0.0203(12) Uani 1 1 d . A . C3 C -0.0340(8) 0.7264(3) -0.1584(3) 0.0235(13) Uani 1 1 d . . . H3 H 0.0213 0.6991 -0.1740 0.028 Uiso 1 1 calc R . . C4 C -0.1766(8) 0.7476(3) -0.2106(3) 0.0219(13) Uani 1 1 d . . . C5 C -0.2564(7) 0.7889(3) -0.1848(3) 0.0223(13) Uani 1 1 d . . . H5 H -0.3520 0.8037 -0.2180 0.027 Uiso 1 1 calc R . . C6 C -0.1874(7) 0.8070(2) -0.1083(3) 0.0165(12) Uani 1 1 d . A . C7 C -0.2646(7) 0.8494(2) -0.0723(3) 0.0186(12) Uani 1 1 d . . . C8 C 0.2145(8) 0.9168(2) 0.0297(3) 0.0187(13) Uani 1 1 d . A . C9 C 0.1393(7) 0.9463(2) 0.0806(3) 0.0169(12) Uani 1 1 d . A . C10 C 0.1370(8) 1.0024(2) 0.0890(3) 0.0224(13) Uani 1 1 d . . . H10 H 0.1921 1.0250 0.0660 0.027 Uiso 1 1 calc R . . C11 C 0.0507(8) 1.0250(2) 0.1327(3) 0.0233(13) Uani 1 1 d . . . C12 C -0.0220(8) 0.9892(3) 0.1701(3) 0.0253(14) Uani 1 1 d . . . H12 H -0.0783 1.0026 0.2008 0.030 Uiso 1 1 calc R . . C13 C -0.0081(7) 0.9334(2) 0.1605(3) 0.0183(12) Uani 1 1 d . A . C14 C -0.0848(9) 0.8909(3) 0.1967(3) 0.0288(15) Uani 1 1 d . A . C15 C 0.3420(8) 0.7897(3) 0.2458(3) 0.0216(13) Uani 1 1 d . A . C16 C 0.2432(7) 0.7389(2) 0.2413(3) 0.0194(12) Uani 1 1 d . A . C17 C 0.2869(8) 0.6965(3) 0.2946(3) 0.0238(13) Uani 1 1 d . . . H17 H 0.3841 0.6981 0.3357 0.029 Uiso 1 1 calc R . . C18 C 0.1877(8) 0.6513(2) 0.2878(3) 0.0231(13) Uani 1 1 d . . . C19 C 0.0420(8) 0.6515(3) 0.2234(3) 0.0247(14) Uani 1 1 d . . . H19 H -0.0296 0.6225 0.2156 0.030 Uiso 1 1 calc R . . C20 C 0.0080(8) 0.6956(2) 0.1722(3) 0.0197(13) Uani 1 1 d . A . C21 C -0.1444(7) 0.6992(2) 0.1017(3) 0.0200(13) Uani 1 1 d . A . N1 N -0.0517(6) 0.7861(2) -0.0577(3) 0.0193(10) Uani 1 1 d . . . N2 N 0.0663(6) 0.91165(19) 0.1147(3) 0.0187(11) Uani 1 1 d . . . N3 N 0.1026(6) 0.7385(2) 0.1792(3) 0.0197(11) Uani 1 1 d . . . O1 O 0.2577(6) 0.69190(18) -0.0396(3) 0.0300(11) Uani 1 1 d . . . O2 O 0.2043(6) 0.74772(18) 0.0457(2) 0.0277(10) Uani 1 1 d . . . O3 O -0.2428(6) 0.72885(19) -0.2837(2) 0.0309(11) Uani 1 1 d . . . H3A H -0.3212 0.7475 -0.3073 0.037 Uiso 1 1 d R . . O4 O -0.3952(5) 0.87118(17) -0.1139(2) 0.0228(9) Uani 1 1 d . A . O5 O -0.1926(5) 0.85882(17) -0.0002(2) 0.0211(9) Uani 1 1 d . A . O6 O 0.1966(5) 0.86551(17) 0.0262(2) 0.0233(9) Uani 1 1 d . . . O7 O 0.2898(6) 0.94421(17) -0.0054(2) 0.0246(10) Uani 1 1 d . . . O8 O 0.0394(6) 1.07928(18) 0.1366(3) 0.0323(11) Uani 1 1 d . . . H8A H -0.0461 1.0872 0.1450 0.039 Uiso 1 1 d R . . O9 O -0.1441(9) 0.9047(2) 0.2455(4) 0.0572(18) Uani 1 1 d . . . O10 O -0.0800(6) 0.84161(17) 0.1729(2) 0.0246(10) Uani 1 1 d . . . O11 O 0.2917(6) 0.82148(18) 0.1875(2) 0.0287(11) Uani 1 1 d . . . O12 O 0.4640(6) 0.7968(2) 0.3031(3) 0.0354(12) Uani 1 1 d . . . O13 O 0.2222(5) 0.61047(18) 0.3384(2) 0.0284(10) Uani 1 1 d . . . O14 O -0.1554(5) 0.74181(17) 0.0599(2) 0.0244(10) Uani 1 1 d . . . O15 O -0.2469(6) 0.66236(18) 0.0887(3) 0.0303(11) Uani 1 1 d . . . O16 O -0.5628(8) 0.8327(2) -0.0122(4) 0.0577(18) Uani 1 1 d . A . O17 O -0.3723(14) 0.9402(17) 0.0234(17) 0.031(7) Uani 0.60(8) 1 d P A 1 O17' O -0.391(3) 0.9181(18) 0.0447(18) 0.025(7) Uani 0.40(8) 1 d P A 2 O18 O -0.5604(8) 0.9815(2) -0.1201(4) 0.0570(17) Uani 1 1 d . A . O19 O 0.4452(11) 0.6040(3) 0.0802(4) 0.097(3) Uani 1 1 d . . . O20 O 0.5003(10) 0.6152(3) -0.0656(5) 0.081(2) Uani 1 1 d . . . O21 O 0.5566(6) 0.73356(19) -0.0433(2) 0.0305(10) Uani 1 1 d . . . O22 O 0.4997(7) 0.7189(3) 0.1148(3) 0.0582(17) Uani 1 1 d . . . O23 O 0.5138(12) 0.8981(5) 0.1774(6) 0.149(5) Uani 1 1 d . . . O24 O 0.569(2) 0.5809(5) 0.2348(6) 0.210(9) Uani 1 1 d . . . O25 O 0.708(5) 0.6206(14) 0.861(2) 0.47(3) Uani 1 1 d . . . O26 O 0.400(4) 0.0070(11) 0.7331(15) 0.109(13) Uani 0.36(3) 1 d PU B 1 O26' O 0.215(5) -0.0147(14) 0.691(2) 0.250(18) Uani 0.64(3) 1 d PU B 2 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 Er1 0.01565(17) 0.01686(17) 0.01463(15) 0.00100(9) 0.00330(11) 0.00039(10) Co1 0.0189(5) 0.0226(4) 0.0212(4) -0.0057(3) 0.0060(3) 0.0006(3) Co2 0.0156(5) 0.0487(6) 0.0260(4) 0.0039(4) 0.0004(3) 0.0030(4) C1 0.013(3) 0.021(3) 0.024(3) -0.005(2) 0.001(2) -0.001(2) C2 0.015(3) 0.023(3) 0.022(3) 0.001(2) 0.005(2) 0.002(2) C3 0.023(4) 0.027(3) 0.020(3) -0.006(2) 0.006(2) 0.005(3) C4 0.024(4) 0.027(3) 0.017(3) -0.003(2) 0.009(2) 0.002(3) C5 0.017(3) 0.029(3) 0.018(3) 0.005(2) 0.002(2) 0.006(3) C6 0.014(3) 0.017(3) 0.019(3) 0.003(2) 0.007(2) 0.000(2) C7 0.015(3) 0.018(3) 0.024(3) 0.002(2) 0.007(2) -0.001(2) C8 0.021(3) 0.016(3) 0.018(3) -0.001(2) 0.006(2) 0.005(2) C9 0.012(3) 0.022(3) 0.018(2) -0.002(2) 0.007(2) 0.000(2) C10 0.020(4) 0.019(3) 0.027(3) 0.000(2) 0.007(3) -0.001(2) C11 0.025(4) 0.016(3) 0.028(3) -0.001(2) 0.007(3) 0.002(2) C12 0.027(4) 0.026(3) 0.025(3) -0.004(3) 0.012(3) -0.001(3) C13 0.018(3) 0.018(3) 0.019(3) 0.001(2) 0.007(2) 0.001(2) C14 0.034(4) 0.033(4) 0.023(3) -0.001(3) 0.014(3) -0.004(3) C15 0.023(4) 0.024(3) 0.017(3) 0.002(2) 0.006(2) -0.004(3) C16 0.012(3) 0.025(3) 0.018(3) 0.004(2) 0.001(2) 0.000(2) C17 0.016(3) 0.031(3) 0.021(3) 0.004(2) 0.001(2) 0.002(3) C18 0.024(4) 0.016(3) 0.028(3) 0.005(2) 0.007(3) 0.002(2) C19 0.016(3) 0.027(3) 0.026(3) 0.005(3) 0.001(2) -0.004(3) C20 0.017(3) 0.020(3) 0.019(3) 0.002(2) 0.003(2) 0.000(2) C21 0.015(3) 0.021(3) 0.020(3) -0.003(2) 0.002(2) 0.001(2) N1 0.019(3) 0.019(3) 0.019(2) 0.000(2) 0.0055(19) 0.000(2) N2 0.017(3) 0.021(3) 0.018(2) 0.0007(19) 0.0050(19) 0.002(2) N3 0.017(3) 0.019(3) 0.018(2) 0.0024(19) -0.0003(19) -0.001(2) O1 0.023(3) 0.032(3) 0.028(2) -0.0074(18) 0.0001(19) 0.0109(19) O2 0.024(3) 0.034(3) 0.021(2) -0.0031(18) 0.0029(17) 0.0109(19) O3 0.028(3) 0.040(3) 0.0173(19) -0.0083(18) -0.0019(17) 0.013(2) O4 0.016(2) 0.028(2) 0.0227(19) -0.0021(17) 0.0043(17) 0.0055(18) O5 0.021(2) 0.025(2) 0.0137(17) -0.0011(16) 0.0022(16) 0.0044(17) O6 0.023(3) 0.022(2) 0.029(2) 0.0008(17) 0.0142(18) -0.0004(18) O7 0.029(3) 0.022(2) 0.031(2) 0.0022(18) 0.0195(19) -0.0006(18) O8 0.031(3) 0.020(2) 0.051(3) -0.005(2) 0.021(2) 0.0051(19) O9 0.101(6) 0.034(3) 0.071(4) -0.015(3) 0.073(4) -0.017(3) O10 0.032(3) 0.020(2) 0.025(2) -0.0005(17) 0.0142(18) -0.0029(19) O11 0.024(3) 0.026(2) 0.026(2) 0.0071(18) -0.0037(18) -0.0083(19) O12 0.029(3) 0.037(3) 0.028(2) 0.010(2) -0.006(2) -0.013(2) O13 0.020(3) 0.026(2) 0.034(2) 0.0180(19) 0.0026(18) 0.0000(18) O14 0.022(3) 0.023(2) 0.0219(19) 0.0075(17) -0.0004(17) -0.0004(17) O15 0.023(3) 0.023(2) 0.037(2) 0.0080(19) -0.0006(19) -0.0043(19) O16 0.075(5) 0.045(3) 0.080(4) 0.026(3) 0.060(4) 0.029(3) O17 0.023(5) 0.038(14) 0.033(8) -0.014(9) 0.009(4) -0.002(5) O17' 0.024(8) 0.022(12) 0.029(8) 0.007(9) 0.009(6) 0.000(7) O18 0.061(5) 0.024(3) 0.098(5) 0.000(3) 0.044(4) -0.005(3) O19 0.102(7) 0.092(6) 0.076(5) 0.035(4) 0.004(4) -0.041(5) O20 0.087(6) 0.053(4) 0.096(5) -0.039(4) 0.023(4) -0.005(4) O21 0.023(3) 0.035(3) 0.027(2) 0.0039(19) 0.0010(18) 0.002(2) O22 0.028(3) 0.096(5) 0.043(3) -0.026(3) 0.002(2) 0.008(3) O23 0.091(8) 0.175(10) 0.132(8) 0.092(8) -0.025(6) -0.075(7) O24 0.40(3) 0.130(10) 0.062(6) -0.003(6) 0.032(10) -0.017(12) O25 0.65(7) 0.39(4) 0.56(6) -0.08(4) 0.47(6) 0.03(4) O26 0.123(16) 0.105(15) 0.099(15) -0.002(8) 0.037(9) 0.001(9) O26' 0.25(2) 0.26(2) 0.25(2) 0.000(10) 0.098(11) -0.001(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 Er1 O6 2.349(4) . ? Er1 O11 2.378(4) . ? Er1 O2 2.378(4) . ? Er1 O10 2.386(4) . ? Er1 O5 2.408(4) . ? Er1 O14 2.412(4) . ? Er1 N3 2.448(5) . ? Er1 N2 2.470(5) . ? Er1 N1 2.479(5) . ? Co1 O13 2.052(4) 4_475 ? Co1 O16 2.059(5) . ? Co1 O18 2.067(6) . ? Co1 O17 2.153(11) . ? Co1 O17' 2.164(16) . ? Co1 O7 2.164(4) 1_455 ? Co1 O4 2.192(4) . ? Co2 O19 2.054(7) . ? Co2 O22 2.063(5) . ? Co2 O20 2.081(7) . ? Co2 O21 2.135(5) . ? Co2 O1 2.147(5) . ? Co2 O15 2.159(5) 1_655 ? C1 O1 1.249(7) . ? C1 O2 1.260(7) . ? C1 C2 1.514(8) . ? C2 N1 1.337(8) . ? C2 C3 1.374(8) . ? C3 C4 1.397(9) . ? C4 O3 1.335(7) . ? C4 C5 1.405(9) . ? C5 C6 1.385(8) . ? C6 N1 1.342(8) . ? C6 C7 1.510(8) . ? C7 O5 1.265(7) . ? C7 O4 1.266(7) . ? C8 O6 1.257(7) . ? C8 O7 1.267(7) . ? C8 C9 1.502(8) . ? C9 N2 1.342(8) . ? C9 C10 1.376(8) . ? C10 C11 1.396(9) . ? C11 O8 1.329(7) . ? C11 C12 1.398(9) . ? C12 C13 1.380(8) . ? C13 N2 1.343(8) . ? C13 C14 1.511(9) . ? C14 O9 1.226(8) . ? C14 O10 1.282(8) . ? C15 O12 1.232(7) . ? C15 O11 1.262(7) . ? C15 C16 1.505(8) . ? C16 N3 1.367(7) . ? C16 C17 1.376(8) . ? C17 C18 1.392(9) . ? C18 O13 1.316(7) . ? C18 C19 1.418(9) . ? C19 C20 1.383(8) . ? C20 N3 1.320(8) . ? C20 C21 1.516(8) . ? C21 O15 1.245(8) . ? C21 O14 1.268(7) . ? O7 Co1 2.164(4) 1_655 ? O13 Co1 2.052(4) 4_676 ? O15 Co2 2.159(5) 1_455 ? 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 O6 Er1 O11 77.48(15) . . ? O6 Er1 O2 75.27(16) . . ? O11 Er1 O2 78.67(16) . . ? O6 Er1 O10 128.08(14) . . ? O11 Er1 O10 86.85(16) . . ? O2 Er1 O10 149.15(14) . . ? O6 Er1 O5 89.34(15) . . ? O11 Er1 O5 146.24(14) . . ? O2 Er1 O5 128.15(13) . . ? O10 Er1 O5 77.03(14) . . ? O6 Er1 O14 145.37(14) . . ? O11 Er1 O14 128.89(14) . . ? O2 Er1 O14 87.56(16) . . ? O10 Er1 O14 80.54(15) . . ? O5 Er1 O14 77.84(14) . . ? O6 Er1 N3 134.90(16) . . ? O11 Er1 N3 65.30(15) . . ? O2 Er1 N3 73.29(16) . . ? O10 Er1 N3 75.93(16) . . ? O5 Er1 N3 135.69(16) . . ? O14 Er1 N3 63.60(15) . . ? O6 Er1 N2 63.83(15) . . ? O11 Er1 N2 75.32(16) . . ? O2 Er1 N2 135.12(17) . . ? O10 Er1 N2 64.36(15) . . ? O5 Er1 N2 70.98(15) . . ? O14 Er1 N2 137.00(16) . . ? N3 Er1 N2 124.74(15) . . ? O6 Er1 N1 74.93(16) . . ? O11 Er1 N1 138.05(17) . . ? O2 Er1 N1 64.16(15) . . ? O10 Er1 N1 135.11(16) . . ? O5 Er1 N1 64.05(15) . . ? O14 Er1 N1 70.52(15) . . ? N3 Er1 N1 117.29(16) . . ? N2 Er1 N1 117.94(15) . . ? O13 Co1 O16 96.2(3) 4_475 . ? O13 Co1 O18 89.0(2) 4_475 . ? O16 Co1 O18 174.6(3) . . ? O13 Co1 O17 169.1(10) 4_475 . ? O16 Co1 O17 93.4(13) . . ? O18 Co1 O17 81.6(14) . . ? O13 Co1 O17' 166.2(14) 4_475 . ? O16 Co1 O17' 75.2(15) . . ? O18 Co1 O17' 100.0(15) . . ? O17 Co1 O17' 19.1(4) . . ? O13 Co1 O7 90.79(18) 4_475 1_455 ? O16 Co1 O7 91.92(18) . 1_455 ? O18 Co1 O7 89.6(2) . 1_455 ? O17 Co1 O7 83.7(4) . 1_455 ? O17' Co1 O7 78.9(6) . 1_455 ? O13 Co1 O4 99.97(16) 4_475 . ? O16 Co1 O4 86.28(19) . . ? O18 Co1 O4 91.3(2) . . ? O17 Co1 O4 85.8(4) . . ? O17' Co1 O4 90.4(7) . . ? O7 Co1 O4 169.22(16) 1_455 . ? O19 Co2 O22 88.4(3) . . ? O19 Co2 O20 88.1(4) . . ? O22 Co2 O20 176.4(3) . . ? O19 Co2 O21 176.0(3) . . ? O22 Co2 O21 95.6(2) . . ? O20 Co2 O21 88.0(3) . . ? O19 Co2 O1 95.0(3) . . ? O22 Co2 O1 89.5(2) . . ? O20 Co2 O1 91.2(3) . . ? O21 Co2 O1 84.51(18) . . ? O19 Co2 O15 92.8(3) . 1_655 ? O22 Co2 O15 84.0(2) . 1_655 ? O20 Co2 O15 95.8(3) . 1_655 ? O21 Co2 O15 88.17(17) . 1_655 ? O1 Co2 O15 169.68(18) . 1_655 ? O1 C1 O2 125.9(6) . . ? O1 C1 C2 118.8(5) . . ? O2 C1 C2 115.3(5) . . ? N1 C2 C3 123.3(6) . . ? N1 C2 C1 113.2(5) . . ? C3 C2 C1 123.4(5) . . ? C2 C3 C4 118.5(6) . . ? O3 C4 C3 122.5(5) . . ? O3 C4 C5 118.4(6) . . ? C3 C4 C5 119.0(5) . . ? C6 C5 C4 117.6(5) . . ? N1 C6 C5 123.4(5) . . ? N1 C6 C7 113.7(5) . . ? C5 C6 C7 122.8(5) . . ? O5 C7 O4 125.1(5) . . ? O5 C7 C6 115.4(5) . . ? O4 C7 C6 119.5(5) . . ? O6 C8 O7 125.3(5) . . ? O6 C8 C9 115.4(5) . . ? O7 C8 C9 119.2(5) . . ? N2 C9 C10 123.0(5) . . ? N2 C9 C8 112.1(5) . . ? C10 C9 C8 124.8(5) . . ? C9 C10 C11 119.1(6) . . ? O8 C11 C10 119.3(6) . . ? O8 C11 C12 122.5(6) . . ? C10 C11 C12 118.2(6) . . ? C13 C12 C11 118.4(6) . . ? N2 C13 C12 123.5(5) . . ? N2 C13 C14 113.5(5) . . ? C12 C13 C14 122.9(6) . . ? O9 C14 O10 125.0(6) . . ? O9 C14 C13 120.2(6) . . ? O10 C14 C13 114.8(5) . . ? O12 C15 O11 125.4(6) . . ? O12 C15 C16 119.4(5) . . ? O11 C15 C16 115.2(5) . . ? N3 C16 C17 122.0(6) . . ? N3 C16 C15 113.9(5) . . ? C17 C16 C15 124.0(5) . . ? C16 C17 C18 121.0(6) . . ? O13 C18 C17 123.2(6) . . ? O13 C18 C19 120.5(6) . . ? C17 C18 C19 116.3(5) . . ? C20 C19 C18 118.9(6) . . ? N3 C20 C19 124.3(6) . . ? N3 C20 C21 113.1(5) . . ? C19 C20 C21 122.6(6) . . ? O15 C21 O14 125.2(5) . . ? O15 C21 C20 120.3(5) . . ? O14 C21 C20 114.5(5) . . ? C2 N1 C6 118.1(5) . . ? C2 N1 Er1 120.6(4) . . ? C6 N1 Er1 121.0(4) . . ? C9 N2 C13 117.6(5) . . ? C9 N2 Er1 121.0(4) . . ? C13 N2 Er1 121.0(4) . . ? C20 N3 C16 117.4(5) . . ? C20 N3 Er1 123.0(4) . . ? C16 N3 Er1 119.5(4) . . ? C1 O1 Co2 128.4(4) . . ? C1 O2 Er1 126.4(4) . . ? C7 O4 Co1 125.3(4) . . ? C7 O5 Er1 125.8(4) . . ? C8 O6 Er1 127.2(4) . . ? C8 O7 Co1 123.1(4) . 1_655 ? C14 O10 Er1 126.0(4) . . ? C15 O11 Er1 125.5(4) . . ? C18 O13 Co1 130.6(4) . 4_676 ? C21 O14 Er1 125.7(4) . . ? C21 O15 Co2 127.3(4) . 1_455 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.644 _refine_diff_density_min -1.445 _refine_diff_density_rms 0.172 # Attachment '772803.CIF' data_9 _database_code_depnum_ccdc_archive 'CCDC 772803' #TrackingRef '772803.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Er2 Fe3 N6 O37' _chemical_formula_weight 1726.90 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6/mcc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' '-y, -x, -z+1/2' 'x-y, -y, -z+1/2' 'x, x-y, -z+1/2' 'y, x, -z+1/2' '-x+y, y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' 'y, x, z-1/2' '-x+y, y, z-1/2' '-x, -x+y, z-1/2' '-y, -x, z-1/2' 'x-y, -y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 15.165(7) _cell_length_b 15.165(7) _cell_length_c 15.713(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3129(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 984 _cell_measurement_theta_min 1.55 _cell_measurement_theta_max 26.24 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 3.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5469 _exptl_absorpt_correction_T_max 0.7253 _exptl_absorpt_process_details SADBAS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16725 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 26.38 _reflns_number_total 1115 _reflns_number_gt 773 _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. ISOR: the parameter to go anisotropic restraint to appointed atoms, is applied for water molecule O5. ; _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^)+(0.0579P)^2^+0.7951P] 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 1115 _refine_ls_number_parameters 77 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.002 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 Er1 Er 0.3333 0.6667 0.2500 0.02202(18) Uani 1 6 d S . . Fe1 Fe 0.5000 0.5000 0.0000 0.0203(3) Uani 1 4 d S . . O1 O 0.4107(2) 0.6104(2) 0.1445(2) 0.0315(7) Uani 1 1 d . . . O2 O 0.5508(2) 0.6157(2) 0.0912(2) 0.0432(8) Uani 1 1 d . . . O3 O 0.6524(3) 0.5125(3) 0.0000 0.0348(11) Uani 1 2 d S . . N1 N 0.5209(3) 0.76047(17) 0.2500 0.0244(10) Uani 1 2 d S . . C1 C 0.7293(5) 0.8647(2) 0.2500 0.0493(19) Uani 1 2 d S . . H1 H 0.8001 0.9001 0.2500 0.059 Uiso 1 2 calc SR . . C2 C 0.6771(3) 0.7860(4) 0.1934(4) 0.0438(13) Uani 1 1 d . . . H2 H 0.7115 0.7680 0.1544 0.053 Uiso 1 1 calc R . . C3 C 0.5727(3) 0.7351(3) 0.1964(3) 0.0295(9) Uani 1 1 d . . . C4 C 0.5066(4) 0.6466(3) 0.1393(3) 0.0314(10) Uani 1 1 d . . . O5 O 0.0000 0.0000 0.2500 0.330(12) Uani 1 12 d SU . . O4 O 0.7920(11) 0.7380(9) 1.0000 0.224(6) Uani 1 2 d S . . 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 Er1 0.0241(2) 0.0241(2) 0.0179(3) 0.000 0.000 0.01205(10) Fe1 0.0261(6) 0.0232(6) 0.0164(6) 0.000 0.000 0.0158(4) O1 0.0320(17) 0.0346(17) 0.0289(16) -0.0088(13) -0.0010(13) 0.0174(14) O2 0.0396(19) 0.053(2) 0.043(2) -0.0218(18) -0.0011(17) 0.0271(17) O3 0.029(2) 0.038(2) 0.036(3) 0.000 0.000 0.0158(19) N1 0.027(2) 0.0245(17) 0.022(2) -0.003(2) 0.000 0.0136(12) C1 0.020(3) 0.042(3) 0.078(5) -0.017(4) 0.000 0.0099(15) C2 0.032(2) 0.048(3) 0.052(3) -0.016(3) 0.005(2) 0.020(2) C3 0.032(2) 0.029(2) 0.029(3) -0.007(2) 0.000(2) 0.0176(19) C4 0.038(3) 0.033(2) 0.025(2) -0.003(2) 0.001(2) 0.019(2) O5 0.325(12) 0.325(12) 0.342(17) 0.000 0.000 0.162(6) O4 0.226(13) 0.179(11) 0.115(9) 0.000 0.000 -0.013(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 Er1 O1 2.419(3) 9_565 ? Er1 O1 2.419(3) 5_565 ? Er1 O1 2.419(3) 3_665 ? Er1 O1 2.419(3) 11 ? Er1 O1 2.419(3) 7_665 ? Er1 O1 2.419(3) . ? Er1 N1 2.464(5) 3_665 ? Er1 N1 2.464(5) 5_565 ? Er1 N1 2.464(5) . ? Fe1 O2 2.092(3) 13_665 ? Fe1 O2 2.092(3) . ? Fe1 O2 2.092(3) 16 ? Fe1 O2 2.092(3) 4_665 ? Fe1 O3 2.223(4) 13_665 ? Fe1 O3 2.223(4) . ? O1 C4 1.275(5) . ? O2 C4 1.246(5) . ? N1 C3 1.332(5) 9_565 ? N1 C3 1.332(5) . ? C1 C2 1.377(6) . ? C1 C2 1.377(6) 9_565 ? C1 H1 0.9300 . ? C2 C3 1.373(5) . ? C2 H2 0.9300 . ? C3 C4 1.506(6) . ? 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 O1 Er1 O1 144.45(12) 9_565 5_565 ? O1 Er1 O1 87.00(15) 9_565 3_665 ? O1 Er1 O1 78.22(12) 5_565 3_665 ? O1 Er1 O1 78.22(12) 9_565 11 ? O1 Er1 O1 87.00(15) 5_565 11 ? O1 Er1 O1 130.32(13) 3_665 11 ? O1 Er1 O1 78.22(12) 9_565 7_665 ? O1 Er1 O1 130.32(13) 5_565 7_665 ? O1 Er1 O1 144.45(13) 3_665 7_665 ? O1 Er1 O1 78.22(12) 11 7_665 ? O1 Er1 O1 130.32(13) 9_565 . ? O1 Er1 O1 78.22(12) 5_565 . ? O1 Er1 O1 78.22(12) 3_665 . ? O1 Er1 O1 144.45(12) 11 . ? O1 Er1 O1 87.00(15) 7_665 . ? O1 Er1 N1 72.23(6) 9_565 3_665 ? O1 Er1 N1 72.23(6) 5_565 3_665 ? O1 Er1 N1 65.16(6) 3_665 3_665 ? O1 Er1 N1 65.16(6) 11 3_665 ? O1 Er1 N1 136.50(8) 7_665 3_665 ? O1 Er1 N1 136.50(8) . 3_665 ? O1 Er1 N1 136.50(8) 9_565 5_565 ? O1 Er1 N1 65.16(6) 5_565 5_565 ? O1 Er1 N1 136.50(8) 3_665 5_565 ? O1 Er1 N1 72.23(6) 11 5_565 ? O1 Er1 N1 65.16(6) 7_665 5_565 ? O1 Er1 N1 72.23(6) . 5_565 ? N1 Er1 N1 120.0 3_665 5_565 ? O1 Er1 N1 65.16(6) 9_565 . ? O1 Er1 N1 136.50(8) 5_565 . ? O1 Er1 N1 72.23(6) 3_665 . ? O1 Er1 N1 136.50(8) 11 . ? O1 Er1 N1 72.23(6) 7_665 . ? O1 Er1 N1 65.16(6) . . ? N1 Er1 N1 120.000(1) 3_665 . ? N1 Er1 N1 120.0 5_565 . ? O2 Fe1 O2 180.00(19) 13_665 . ? O2 Fe1 O2 93.49(19) 13_665 16 ? O2 Fe1 O2 86.51(19) . 16 ? O2 Fe1 O2 86.51(19) 13_665 4_665 ? O2 Fe1 O2 93.49(19) . 4_665 ? O2 Fe1 O2 180.0 16 4_665 ? O2 Fe1 O3 89.85(12) 13_665 13_665 ? O2 Fe1 O3 90.15(12) . 13_665 ? O2 Fe1 O3 90.15(12) 16 13_665 ? O2 Fe1 O3 89.85(12) 4_665 13_665 ? O2 Fe1 O3 90.15(12) 13_665 . ? O2 Fe1 O3 89.85(12) . . ? O2 Fe1 O3 89.85(12) 16 . ? O2 Fe1 O3 90.15(12) 4_665 . ? O3 Fe1 O3 180.0 13_665 . ? C4 O1 Er1 122.9(3) . . ? C4 O2 Fe1 133.5(3) . . ? C3 N1 C3 118.6(5) 9_565 . ? C3 N1 Er1 120.7(2) 9_565 . ? C3 N1 Er1 120.7(2) . . ? C2 C1 C2 120.3(6) . 9_565 ? C2 C1 H1 119.8 . . ? C2 C1 H1 119.8 9_565 . ? C3 C2 C1 117.8(5) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? N1 C3 C2 122.7(4) . . ? N1 C3 C4 114.1(4) . . ? C2 C3 C4 123.1(4) . . ? O2 C4 O1 126.1(4) . . ? O2 C4 C3 117.0(4) . . ? O1 C4 C3 116.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Er1 O1 C4 4.3(3) 9_565 . . . ? O1 Er1 O1 C4 160.3(3) 5_565 . . . ? O1 Er1 O1 C4 80.0(4) 3_665 . . . ? O1 Er1 O1 C4 -132.3(3) 11 . . . ? O1 Er1 O1 C4 -67.5(3) 7_665 . . . ? N1 Er1 O1 C4 112.5(3) 3_665 . . . ? N1 Er1 O1 C4 -132.3(3) 5_565 . . . ? N1 Er1 O1 C4 4.3(3) . . . . ? O2 Fe1 O2 C4 2(100) 13_665 . . . ? O2 Fe1 O2 C4 104.7(4) 16 . . . ? O2 Fe1 O2 C4 -75.3(4) 4_665 . . . ? O3 Fe1 O2 C4 14.5(4) 13_665 . . . ? O3 Fe1 O2 C4 -165.5(4) . . . . ? O1 Er1 N1 C3 -1.7(2) 9_565 . . 9_565 ? O1 Er1 N1 C3 142.8(2) 5_565 . . 9_565 ? O1 Er1 N1 C3 93.3(2) 3_665 . . 9_565 ? O1 Er1 N1 C3 -37.2(2) 11 . . 9_565 ? O1 Er1 N1 C3 -86.7(2) 7_665 . . 9_565 ? O1 Er1 N1 C3 178.3(2) . . . 9_565 ? N1 Er1 N1 C3 47.3(2) 3_665 . . 9_565 ? N1 Er1 N1 C3 -132.7(2) 5_565 . . 9_565 ? O1 Er1 N1 C3 178.3(2) 9_565 . . . ? O1 Er1 N1 C3 -37.2(2) 5_565 . . . ? O1 Er1 N1 C3 -86.7(2) 3_665 . . . ? O1 Er1 N1 C3 142.8(2) 11 . . . ? O1 Er1 N1 C3 93.3(2) 7_665 . . . ? O1 Er1 N1 C3 -1.7(2) . . . . ? N1 Er1 N1 C3 -132.7(2) 3_665 . . . ? N1 Er1 N1 C3 47.3(2) 5_565 . . . ? C2 C1 C2 C3 -0.8(3) 9_565 . . . ? C3 N1 C3 C2 -0.9(4) 9_565 . . . ? Er1 N1 C3 C2 179.1(4) . . . . ? C3 N1 C3 C4 179.6(4) 9_565 . . . ? Er1 N1 C3 C4 -0.4(4) . . . . ? C1 C2 C3 N1 1.7(7) . . . . ? C1 C2 C3 C4 -178.9(4) . . . . ? Fe1 O2 C4 O1 0.6(7) . . . . ? Fe1 O2 C4 C3 -179.3(3) . . . . ? Er1 O1 C4 O2 173.9(3) . . . . ? Er1 O1 C4 C3 -6.2(5) . . . . ? N1 C3 C4 O2 -176.0(4) . . . . ? C2 C3 C4 O2 4.6(7) . . . . ? N1 C3 C4 O1 4.1(6) . . . . ? C2 C3 C4 O1 -175.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.438 _refine_diff_density_min -1.066 _refine_diff_density_rms 0.124 # Attachment '772804.cif' data_18 _database_code_depnum_ccdc_archive 'CCDC 772804' #TrackingRef '772804.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H40 Co2 Eu N3 O31' _chemical_formula_sum 'C21 H40 Co2 Eu N3 O31' _chemical_formula_weight 1100.38 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9767(4) _cell_length_b 23.9151(10) _cell_length_c 18.6746(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.497(4) _cell_angle_gamma 90.00 _cell_volume 3730.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7914 _cell_measurement_theta_min 2.4314 _cell_measurement_theta_max 29.0776 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.959 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 2.654 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7772 _exptl_absorpt_correction_T_max 0.9013 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14276 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.10 _reflns_number_total 6597 _reflns_number_gt 5126 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _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. ISOR: the parameter to go anisotropic restraint t o appointed atoms, is applied for C1, C14 and C18. The significant residual peaks are 3.98, 3.76, 3.65 and 2.06, and those peaks are around Eu1 with distances of 0.93, 1.03, 1.03 and 1.04, respectively. ; _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^)+(0.0950P)^2^+61.2353P] 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 SHELXL _refine_ls_extinction_coef 0.0017(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6597 _refine_ls_number_parameters 525 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0988 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.1965 _refine_ls_wR_factor_gt 0.1881 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _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 Eu1 Eu 0.44627(6) 0.80955(2) 0.40905(3) 0.0113(2) Uani 1 1 d . . . Co1 Co 1.06306(17) 0.90215(6) 0.55650(9) 0.0169(4) Uani 1 1 d . . . Co2 Co -0.00749(17) 0.66350(7) 0.46378(9) 0.0212(4) Uani 1 1 d . . . C1 C 0.7559(12) 0.8475(4) 0.5633(6) 0.014(2) Uani 1 1 d U . . C2 C 0.6822(13) 0.8043(5) 0.5989(6) 0.016(2) Uani 1 1 d . . . C3 C 0.7451(13) 0.7882(5) 0.6771(7) 0.020(2) Uani 1 1 d . . . H3 H 0.8359 0.8055 0.7116 0.024 Uiso 1 1 calc R . . C4 C 0.6677(14) 0.7456(5) 0.7013(7) 0.022(3) Uani 1 1 d . . . C5 C 0.5255(12) 0.7235(5) 0.6492(6) 0.019(2) Uani 1 1 d . . . H5 H 0.4688 0.6968 0.6649 0.022 Uiso 1 1 calc R . . C6 C 0.4691(12) 0.7422(5) 0.5725(6) 0.015(2) Uani 1 1 d . . . C7 C 0.3220(12) 0.7213(5) 0.5117(6) 0.018(2) Uani 1 1 d . . . C8 C 0.6382(13) 0.6961(5) 0.3878(7) 0.018(2) Uani 1 1 d . . . C9 C 0.4827(13) 0.6931(5) 0.3164(6) 0.018(2) Uani 1 1 d . . . C10 C 0.4521(13) 0.6505(5) 0.2648(7) 0.021(2) Uani 1 1 d . . . H10 H 0.5254 0.6216 0.2718 0.025 Uiso 1 1 calc R . . C11 C 0.3050(13) 0.6509(5) 0.1995(6) 0.020(2) Uani 1 1 d . . . C12 C 0.2011(13) 0.6966(5) 0.1937(6) 0.018(2) Uani 1 1 d . . . H12 H 0.1030 0.6991 0.1531 0.022 Uiso 1 1 calc R . . C13 C 0.2488(13) 0.7375(5) 0.2497(6) 0.017(2) Uani 1 1 d . . . C14 C 0.1427(13) 0.7875(5) 0.2488(6) 0.014(2) Uani 1 1 d U . . C15 C 0.5749(12) 0.8941(5) 0.3002(6) 0.017(2) Uani 1 1 d . . . C16 C 0.4984(12) 0.9355(5) 0.3375(6) 0.017(2) Uani 1 1 d . . . C17 C 0.5154(12) 0.9925(5) 0.3331(6) 0.017(2) Uani 1 1 d . . . H17 H 0.5694 1.0073 0.3034 0.020 Uiso 1 1 calc R . . C18 C 0.4510(12) 1.0277(5) 0.3736(6) 0.016(2) Uani 1 1 d U . . C19 C 0.3644(12) 1.0035(5) 0.4147(6) 0.015(2) Uani 1 1 d . . . H19 H 0.3141 1.0255 0.4402 0.018 Uiso 1 1 calc R . . C20 C 0.3562(12) 0.9465(5) 0.4161(6) 0.017(2) Uani 1 1 d . . . C21 C 0.2765(13) 0.9149(5) 0.4633(6) 0.018(2) Uani 1 1 d . . . N1 N 0.5480(10) 0.7820(4) 0.5480(5) 0.0151(19) Uani 1 1 d . . . N2 N 0.3841(10) 0.7376(4) 0.3101(5) 0.016(2) Uani 1 1 d . . . N3 N 0.4232(11) 0.9115(4) 0.3794(6) 0.021(2) Uani 1 1 d . . . O1 O 0.6845(9) 0.8556(3) 0.4926(4) 0.0184(17) Uani 1 1 d . . . O2 O 0.8873(9) 0.8693(3) 0.6033(4) 0.0192(17) Uani 1 1 d . . . O3 O 0.7283(9) 0.7295(4) 0.7740(4) 0.0221(18) Uani 1 1 d . . . H3A H 0.6553 0.7218 0.7888 0.033 Uiso 1 1 calc R . . O4 O 0.2336(9) 0.6869(3) 0.5298(5) 0.0212(18) Uani 1 1 d . . . O5 O 0.2909(9) 0.7413(3) 0.4439(4) 0.0216(18) Uani 1 1 d . . . O6 O 0.6509(9) 0.7392(3) 0.4297(4) 0.0177(17) Uani 1 1 d . . . O7 O 0.7394(9) 0.6578(3) 0.4002(5) 0.0236(18) Uani 1 1 d . . . O8 O 0.2700(9) 0.6097(3) 0.1485(4) 0.0205(17) Uani 1 1 d . . . O9 O 0.0196(9) 0.7967(3) 0.1896(5) 0.0243(19) Uani 1 1 d . . . O10 O 0.1896(9) 0.8183(3) 0.3084(5) 0.0209(18) Uani 1 1 d . . . O11 O 0.5666(8) 0.8429(3) 0.3183(4) 0.0185(17) Uani 1 1 d . . . O12 O 0.6431(11) 0.9100(4) 0.2566(5) 0.029(2) Uani 1 1 d . . . O13 O 0.4669(9) 1.0827(3) 0.3753(5) 0.0208(17) Uani 1 1 d . . . H13 H 0.5459 1.0925 0.3628 0.031 Uiso 1 1 d R . . O14 O 0.2011(9) 0.9426(3) 0.4969(4) 0.0174(17) Uani 1 1 d . . . O15 O 0.2954(8) 0.8623(3) 0.4673(4) 0.0161(16) Uani 1 1 d . . . O16 O 1.0358(9) 0.9814(3) 0.5935(5) 0.0228(18) Uani 1 1 d . . . H16A H 1.0467 0.9864 0.6436 0.027 Uiso 1 1 d R . . H16B H 1.1166 1.0017 0.5917 0.027 Uiso 1 1 d R . . O17 O 0.8736(9) 0.9187(3) 0.4495(4) 0.0227(18) Uani 1 1 d . . . H17A H 0.8084 0.8976 0.4625 0.027 Uiso 1 1 d R . . H17B H 0.8666 0.9044 0.4040 0.027 Uiso 1 1 d R . . O18 O 1.0692(11) 0.8247(3) 0.5109(5) 0.030(2) Uani 1 1 d . . . H18A H 1.0430 0.7929 0.5260 0.036 Uiso 1 1 d R . . H18B H 1.1638 0.8194 0.5095 0.036 Uiso 1 1 d R . . O19 O -0.0602(9) 0.7259(3) 0.5340(4) 0.0208(18) Uani 1 1 d . . . H19A H -0.0362 0.7184 0.5820 0.025 Uiso 1 1 d R . . H19B H -0.1628 0.7302 0.5138 0.025 Uiso 1 1 d R . . O20 O -0.0141(10) 0.7168(5) 0.3773(5) 0.039(2) Uani 1 1 d . . . H20A H 0.0425 0.7479 0.3979 0.047 Uiso 1 1 d R . . H20B H -0.0039 0.7170 0.3317 0.047 Uiso 1 1 d R . . O21 O 0.0437(12) 0.6007(4) 0.4016(5) 0.041(2) Uani 1 1 d . . . H21A H 0.1115 0.5732 0.4036 0.049 Uiso 1 1 d R . . H21B H 0.0338 0.6166 0.3557 0.049 Uiso 1 1 d R . . O22 O -0.0033(10) 0.6034(4) 0.5395(5) 0.032(2) Uani 1 1 d . . . H22A H -0.0541 0.6053 0.5716 0.039 Uiso 1 1 d R . . H22B H 0.0310 0.5691 0.5449 0.039 Uiso 1 1 d R . . O23 O 0.9696(10) 0.8903(4) 0.3314(5) 0.032(2) Uani 1 1 d . . . H23A H 0.9181 0.8756 0.2851 0.038 Uiso 1 1 d R . . H23B H 1.0711 0.8821 0.3445 0.038 Uiso 1 1 d R . . O24 O 0.3277(12) 0.5177(5) 0.3154(6) 0.046(3) Uani 1 1 d . . . H24A H 0.3187 0.4836 0.2975 0.055 Uiso 1 1 d R . . H24B H 0.2581 0.5411 0.2897 0.055 Uiso 1 1 d R . . O25 O 1.0226(14) 0.5764(4) 0.2536(5) 0.049(3) Uani 1 1 d . . . H25A H 0.9718 0.6007 0.2172 0.059 Uiso 1 1 d R . . H25B H 0.9545 0.5524 0.2612 0.059 Uiso 1 1 d R . . O26 O 0.2893(12) 0.5243(5) 0.4603(6) 0.053(3) Uani 1 1 d . . . H26A H 0.3378 0.5542 0.4838 0.064 Uiso 1 1 d R . . H26B H 0.3139 0.5132 0.4217 0.064 Uiso 1 1 d R . . O27 O 0.0667(12) 0.9665(5) 0.2362(6) 0.047(3) Uani 1 1 d . . . H27A H 0.0927 0.9575 0.2848 0.057 Uiso 1 1 d R . . H27B H -0.0341 0.9799 0.2206 0.057 Uiso 1 1 d R . . O28 O 0.8390(12) 0.6065(4) 0.6378(6) 0.046(3) Uani 1 1 d . . . H28B H 0.7376 0.6038 0.6160 0.055 Uiso 1 1 d R . . H28A H 0.8695 0.6303 0.6763 0.055 Uiso 1 1 d R . . O29 O 0.6436(13) 0.5439(5) 0.4098(6) 0.059(3) Uani 1 1 d . . . H29A H 0.6919 0.5641 0.3860 0.070 Uiso 1 1 d R . . H29B H 0.5469 0.5356 0.3833 0.070 Uiso 1 1 d R . . O30 O 0.2599(13) 0.5535(5) 0.6427(6) 0.054(3) Uani 1 1 d . . . H30B H 0.2392 0.5637 0.6828 0.065 Uiso 1 1 d R . . H30A H 0.2475 0.5171 0.6340 0.065 Uiso 1 1 d R . . O31 O 0.5139(14) 0.9092(5) 0.0798(7) 0.059(3) Uani 1 1 d . . . H31A H 0.5154 0.8740 0.0653 0.071 Uiso 1 1 d R . . H31B H 0.4280 0.9143 0.0916 0.071 Uiso 1 1 d 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 Eu1 0.0060(3) 0.0132(3) 0.0140(3) -0.0008(2) 0.0030(2) 0.0000(2) Co1 0.0128(7) 0.0175(8) 0.0204(8) 0.0026(6) 0.0061(6) 0.0000(6) Co2 0.0096(7) 0.0296(9) 0.0222(8) -0.0007(7) 0.0033(6) -0.0007(6) C1 0.009(4) 0.015(4) 0.019(4) -0.002(3) 0.007(3) 0.001(3) C2 0.014(5) 0.015(6) 0.020(6) 0.004(5) 0.005(5) 0.005(4) C3 0.007(5) 0.024(6) 0.025(6) -0.004(5) 0.001(5) -0.001(4) C4 0.023(6) 0.021(6) 0.023(6) 0.001(5) 0.010(5) -0.003(5) C5 0.011(5) 0.019(6) 0.027(6) 0.006(5) 0.007(5) -0.004(4) C6 0.008(5) 0.024(6) 0.013(5) -0.001(4) 0.001(4) -0.004(4) C7 0.008(5) 0.024(6) 0.020(6) -0.004(5) 0.004(4) -0.001(5) C8 0.012(5) 0.014(6) 0.024(6) 0.002(5) 0.003(5) 0.003(4) C9 0.015(6) 0.023(6) 0.020(6) -0.004(5) 0.009(5) -0.002(5) C10 0.017(6) 0.014(6) 0.030(6) 0.000(5) 0.008(5) 0.003(4) C11 0.013(5) 0.021(6) 0.023(6) -0.004(5) 0.005(5) -0.008(4) C12 0.005(5) 0.028(7) 0.017(5) -0.001(5) -0.001(4) 0.001(4) C13 0.015(5) 0.013(5) 0.024(6) -0.003(5) 0.008(5) 0.003(4) C14 0.017(4) 0.017(4) 0.007(4) 0.001(3) 0.003(3) 0.001(3) C15 0.006(5) 0.024(6) 0.020(6) 0.001(5) 0.003(4) 0.000(4) C16 0.007(5) 0.030(7) 0.010(5) 0.001(5) -0.001(4) 0.000(4) C17 0.009(5) 0.023(6) 0.017(5) -0.001(5) 0.003(4) -0.003(4) C18 0.011(4) 0.020(4) 0.017(4) 0.001(3) 0.003(3) 0.002(3) C19 0.008(5) 0.019(6) 0.017(5) -0.001(4) 0.004(4) -0.004(4) C20 0.008(5) 0.033(7) 0.011(5) -0.002(5) 0.005(4) -0.004(5) C21 0.016(5) 0.019(6) 0.019(6) -0.003(5) 0.007(5) -0.006(5) N1 0.010(4) 0.016(5) 0.020(5) -0.001(4) 0.006(4) 0.000(4) N2 0.006(4) 0.026(5) 0.014(4) 0.001(4) 0.002(4) 0.001(4) N3 0.011(5) 0.026(6) 0.030(5) 0.002(4) 0.012(4) 0.005(4) O1 0.013(4) 0.020(4) 0.019(4) 0.001(3) 0.002(3) -0.004(3) O2 0.014(4) 0.020(4) 0.024(4) 0.003(3) 0.008(3) -0.005(3) O3 0.015(4) 0.035(5) 0.017(4) 0.004(4) 0.006(3) -0.006(4) O4 0.012(4) 0.018(4) 0.031(5) 0.007(3) 0.004(3) -0.005(3) O5 0.011(4) 0.032(5) 0.020(4) 0.003(4) 0.003(3) -0.004(3) O6 0.012(4) 0.020(4) 0.017(4) -0.004(3) 0.000(3) 0.002(3) O7 0.016(4) 0.020(4) 0.032(5) -0.002(4) 0.004(4) -0.001(3) O8 0.017(4) 0.022(4) 0.024(4) -0.008(3) 0.009(3) -0.002(3) O9 0.012(4) 0.032(5) 0.025(4) 0.000(4) 0.002(3) 0.010(3) O10 0.009(4) 0.018(4) 0.031(5) -0.004(3) 0.003(3) 0.002(3) O11 0.011(4) 0.017(4) 0.029(4) 0.000(3) 0.009(3) 0.001(3) O12 0.038(5) 0.025(5) 0.028(5) 0.004(4) 0.016(4) 0.004(4) O13 0.017(4) 0.014(4) 0.032(5) 0.005(3) 0.010(3) 0.004(3) O14 0.019(4) 0.021(4) 0.017(4) 0.001(3) 0.011(3) 0.000(3) O15 0.009(4) 0.017(4) 0.023(4) -0.005(3) 0.007(3) 0.001(3) O16 0.022(4) 0.019(4) 0.031(4) -0.002(4) 0.013(4) -0.003(3) O17 0.021(4) 0.028(5) 0.018(4) 0.006(3) 0.005(3) -0.004(4) O18 0.033(5) 0.017(5) 0.050(6) -0.002(4) 0.028(5) -0.003(4) O19 0.008(4) 0.030(5) 0.021(4) -0.001(3) 0.002(3) -0.002(3) O20 0.019(5) 0.059(7) 0.034(5) 0.015(5) 0.003(4) -0.004(4) O21 0.044(6) 0.047(6) 0.026(5) -0.009(4) 0.007(4) 0.020(5) O22 0.028(5) 0.028(5) 0.041(5) 0.015(4) 0.013(4) 0.009(4) O23 0.019(4) 0.041(6) 0.030(5) -0.001(4) 0.003(4) 0.007(4) O24 0.035(6) 0.060(7) 0.040(6) -0.007(5) 0.010(5) -0.001(5) O25 0.068(8) 0.045(6) 0.028(5) 0.003(5) 0.010(5) -0.003(5) O26 0.040(6) 0.065(8) 0.047(6) -0.004(6) 0.007(5) 0.002(5) O27 0.038(6) 0.065(8) 0.035(6) -0.003(5) 0.009(5) -0.009(5) O28 0.037(6) 0.044(6) 0.055(7) 0.001(5) 0.013(5) -0.011(5) O29 0.041(6) 0.062(8) 0.055(7) 0.009(6) -0.002(5) -0.008(6) O30 0.042(6) 0.067(8) 0.046(6) 0.007(6) 0.007(5) 0.010(6) O31 0.057(8) 0.060(8) 0.064(8) 0.008(6) 0.026(6) -0.003(6) _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 Eu1 O15 2.385(7) . ? Eu1 O5 2.386(8) . ? Eu1 O10 2.390(8) . ? Eu1 O1 2.403(7) . ? Eu1 O6 2.415(7) . ? Eu1 N2 2.435(9) . ? Eu1 O11 2.452(8) . ? Eu1 N3 2.493(10) . ? Eu1 N1 2.503(9) . ? Co1 O8 2.036(8) 4_676 ? Co1 O18 2.047(8) . ? Co1 O16 2.063(8) . ? Co1 O17 2.133(7) . ? Co1 O14 2.172(8) 1_655 ? Co1 O2 2.210(8) . ? Co2 O22 2.007(9) . ? Co2 O20 2.042(9) . ? Co2 O21 2.052(9) . ? Co2 O4 2.136(8) . ? Co2 O7 2.148(8) 1_455 ? Co2 O19 2.150(8) . ? C1 O1 1.254(13) . ? C1 O2 1.256(13) . ? C1 C2 1.506(15) . ? C2 N1 1.341(14) . ? C2 C3 1.411(16) . ? C3 C4 1.399(17) . ? C3 H3 0.9300 . ? C4 O3 1.321(14) . ? C4 C5 1.395(16) . ? C5 C6 1.404(15) . ? C5 H5 0.9300 . ? C6 N1 1.363(14) . ? C6 C7 1.478(14) . ? C7 O4 1.271(14) . ? C7 O5 1.286(13) . ? C8 O7 1.251(13) . ? C8 O6 1.274(13) . ? C8 C9 1.538(15) . ? C9 C10 1.361(16) . ? C9 N2 1.361(15) . ? C10 C11 1.432(16) . ? C10 H10 0.9300 . ? C11 O8 1.325(14) . ? C11 C12 1.415(16) . ? C12 C13 1.381(16) . ? C12 H12 0.9300 . ? C13 N2 1.320(14) . ? C13 C14 1.525(15) . ? C14 O9 1.264(13) . ? C14 O10 1.271(13) . ? C15 O12 1.243(14) . ? C15 O11 1.280(13) . ? C15 C16 1.513(16) . ? C16 N3 1.335(14) . ? C16 C17 1.378(16) . ? C17 C18 1.391(16) . ? C17 H17 0.9300 . ? C18 O13 1.320(13) . ? C18 C19 1.404(15) . ? C19 C20 1.364(15) . ? C19 H19 0.9300 . ? C20 N3 1.356(14) . ? C20 C21 1.523(15) . ? C21 O14 1.266(14) . ? C21 O15 1.269(13) . ? O3 H3A 0.8200 . ? O7 Co2 2.148(8) 1_655 ? O8 Co1 2.036(8) 4_475 ? O13 H13 0.8559 . ? O14 Co1 2.172(7) 1_455 ? O16 H16A 0.9119 . ? O16 H16B 0.8829 . ? O17 H17A 0.8724 . ? O17 H17B 0.8968 . ? O18 H18A 0.8730 . ? O18 H18B 0.8682 . ? O19 H19A 0.8600 . ? O19 H19B 0.8645 . ? O20 H20A 0.9038 . ? O20 H20B 0.8888 . ? O21 H21A 0.8863 . ? O21 H21B 0.9116 . ? O22 H22A 0.8782 . ? O22 H22B 0.8687 . ? O23 H23A 0.8897 . ? O23 H23B 0.8748 . ? O24 H24A 0.8728 . ? O24 H24B 0.8455 . ? O25 H25A 0.8843 . ? O25 H25B 0.8879 . ? O26 H26A 0.8668 . ? O26 H26B 0.8700 . ? O27 H27A 0.8778 . ? O27 H27B 0.9018 . ? O28 H28B 0.8525 . ? O28 H28A 0.8792 . ? O29 H29A 0.8727 . ? O29 H29B 0.8497 . ? O30 H30B 0.8696 . ? O30 H30A 0.8854 . ? O31 H31A 0.8871 . ? O31 H31B 0.8837 . ? 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 O15 Eu1 O5 75.6(3) . . ? O15 Eu1 O10 76.6(3) . . ? O5 Eu1 O10 77.4(3) . . ? O15 Eu1 O1 88.9(3) . . ? O5 Eu1 O1 127.3(3) . . ? O10 Eu1 O1 147.4(3) . . ? O15 Eu1 O6 145.2(3) . . ? O5 Eu1 O6 88.1(3) . . ? O10 Eu1 O6 130.1(2) . . ? O1 Eu1 O6 76.8(3) . . ? O15 Eu1 N2 135.2(3) . . ? O5 Eu1 N2 74.3(3) . . ? O10 Eu1 N2 65.0(3) . . ? O1 Eu1 N2 135.9(3) . . ? O6 Eu1 N2 65.1(3) . . ? O15 Eu1 O11 127.6(3) . . ? O5 Eu1 O11 149.3(3) . . ? O10 Eu1 O11 88.3(3) . . ? O1 Eu1 O11 77.7(3) . . ? O6 Eu1 O11 80.5(3) . . ? N2 Eu1 O11 75.0(3) . . ? O15 Eu1 N3 64.5(3) . . ? O5 Eu1 N3 136.1(3) . . ? O10 Eu1 N3 76.3(3) . . ? O1 Eu1 N3 71.2(3) . . ? O6 Eu1 N3 135.5(3) . . ? N2 Eu1 N3 123.0(3) . . ? O11 Eu1 N3 63.3(3) . . ? O15 Eu1 N1 73.7(3) . . ? O5 Eu1 N1 64.2(3) . . ? O10 Eu1 N1 135.9(3) . . ? O1 Eu1 N1 63.1(3) . . ? O6 Eu1 N1 71.6(3) . . ? N2 Eu1 N1 119.7(3) . . ? O11 Eu1 N1 135.7(3) . . ? N3 Eu1 N1 117.2(3) . . ? O8 Co1 O18 94.0(4) 4_676 . ? O8 Co1 O16 91.6(3) 4_676 . ? O18 Co1 O16 174.4(4) . . ? O8 Co1 O17 169.8(3) 4_676 . ? O18 Co1 O17 85.0(3) . . ? O16 Co1 O17 89.5(3) . . ? O8 Co1 O14 88.8(3) 4_676 1_655 ? O18 Co1 O14 94.7(3) . 1_655 ? O16 Co1 O14 85.5(3) . 1_655 ? O17 Co1 O14 81.2(3) . 1_655 ? O8 Co1 O2 100.3(3) 4_676 . ? O18 Co1 O2 88.5(3) . . ? O16 Co1 O2 90.3(3) . . ? O17 Co1 O2 89.8(3) . . ? O14 Co1 O2 170.1(3) 1_655 . ? O22 Co2 O20 172.9(4) . . ? O22 Co2 O21 85.6(4) . . ? O20 Co2 O21 87.5(4) . . ? O22 Co2 O4 91.6(3) . . ? O20 Co2 O4 91.3(3) . . ? O21 Co2 O4 97.4(4) . . ? O22 Co2 O7 95.0(3) . 1_455 ? O20 Co2 O7 83.3(3) . 1_455 ? O21 Co2 O7 92.9(4) . 1_455 ? O4 Co2 O7 168.1(3) . 1_455 ? O22 Co2 O19 91.1(3) . . ? O20 Co2 O19 95.7(4) . . ? O21 Co2 O19 176.8(4) . . ? O4 Co2 O19 82.5(3) . . ? O7 Co2 O19 87.5(3) 1_455 . ? O1 C1 O2 124.7(10) . . ? O1 C1 C2 115.7(9) . . ? O2 C1 C2 119.4(9) . . ? N1 C2 C3 122.7(10) . . ? N1 C2 C1 112.6(9) . . ? C3 C2 C1 124.7(10) . . ? C4 C3 C2 118.4(10) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? O3 C4 C5 122.2(10) . . ? O3 C4 C3 118.6(10) . . ? C5 C4 C3 119.1(10) . . ? C4 C5 C6 119.1(10) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? N1 C6 C5 121.8(9) . . ? N1 C6 C7 114.0(9) . . ? C5 C6 C7 124.2(10) . . ? O4 C7 O5 124.8(10) . . ? O4 C7 C6 118.9(10) . . ? O5 C7 C6 116.2(10) . . ? O7 C8 O6 125.7(10) . . ? O7 C8 C9 119.6(10) . . ? O6 C8 C9 114.7(9) . . ? C10 C9 N2 124.7(11) . . ? C10 C9 C8 122.1(10) . . ? N2 C9 C8 113.1(9) . . ? C9 C10 C11 118.8(11) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? O8 C11 C12 123.0(10) . . ? O8 C11 C10 120.5(10) . . ? C12 C11 C10 116.5(10) . . ? C13 C12 C11 118.5(10) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? N2 C13 C12 125.6(10) . . ? N2 C13 C14 112.5(9) . . ? C12 C13 C14 121.9(10) . . ? O9 C14 O10 124.6(10) . . ? O9 C14 C13 119.3(9) . . ? O10 C14 C13 116.1(9) . . ? O12 C15 O11 123.9(11) . . ? O12 C15 C16 121.1(10) . . ? O11 C15 C16 115.1(10) . . ? N3 C16 C17 123.4(10) . . ? N3 C16 C15 113.6(10) . . ? C17 C16 C15 122.8(10) . . ? C16 C17 C18 119.3(10) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? O13 C18 C17 123.5(10) . . ? O13 C18 C19 118.4(10) . . ? C17 C18 C19 118.1(10) . . ? C20 C19 C18 117.9(10) . . ? C20 C19 H19 121.0 . . ? C18 C19 H19 121.0 . . ? N3 C20 C19 124.7(10) . . ? N3 C20 C21 112.1(10) . . ? C19 C20 C21 123.1(10) . . ? O14 C21 O15 125.0(10) . . ? O14 C21 C20 118.5(10) . . ? O15 C21 C20 116.5(10) . . ? C2 N1 C6 118.8(9) . . ? C2 N1 Eu1 121.5(7) . . ? C6 N1 Eu1 119.7(7) . . ? C13 N2 C9 115.9(9) . . ? C13 N2 Eu1 122.2(7) . . ? C9 N2 Eu1 121.8(7) . . ? C16 N3 C20 116.4(10) . . ? C16 N3 Eu1 122.1(7) . . ? C20 N3 Eu1 120.5(7) . . ? C1 O1 Eu1 127.0(7) . . ? C1 O2 Co1 124.3(7) . . ? C4 O3 H3A 109.5 . . ? C7 O4 Co2 128.0(7) . . ? C7 O5 Eu1 125.8(7) . . ? C8 O6 Eu1 125.0(7) . . ? C8 O7 Co2 127.3(7) . 1_655 ? C11 O8 Co1 127.7(7) . 4_475 ? C14 O10 Eu1 123.6(7) . . ? C15 O11 Eu1 125.3(7) . . ? C18 O13 H13 111.1 . . ? C21 O14 Co1 122.0(7) . 1_455 ? C21 O15 Eu1 125.7(7) . . ? Co1 O16 H16A 118.9 . . ? Co1 O16 H16B 107.0 . . ? H16A O16 H16B 100.7 . . ? Co1 O17 H17A 91.0 . . ? Co1 O17 H17B 124.8 . . ? H17A O17 H17B 102.8 . . ? Co1 O18 H18A 127.1 . . ? Co1 O18 H18B 108.7 . . ? H18A O18 H18B 105.2 . . ? Co2 O19 H19A 117.6 . . ? Co2 O19 H19B 104.8 . . ? H19A O19 H19B 107.3 . . ? Co2 O20 H20A 109.1 . . ? Co2 O20 H20B 140.9 . . ? H20A O20 H20B 99.6 . . ? Co2 O21 H21A 144.1 . . ? Co2 O21 H21B 105.2 . . ? H21A O21 H21B 100.3 . . ? Co2 O22 H22A 124.3 . . ? Co2 O22 H22B 132.3 . . ? H22A O22 H22B 102.6 . . ? H23A O23 H23B 107.5 . . ? H24A O24 H24B 117.1 . . ? H25A O25 H25B 110.9 . . ? H26A O26 H26B 116.0 . . ? H27A O27 H27B 105.9 . . ? H28B O28 H28A 113.4 . . ? H29A O29 H29B 115.1 . . ? H30B O30 H30A 112.5 . . ? H31A O31 H31B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.984 _refine_diff_density_min -1.766 _refine_diff_density_rms 0.256 # Attachment '772805.cif' data_19 _database_code_depnum_ccdc_archive 'CCDC 772805' #TrackingRef '772805.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H40 Co2 Gd N3 O31' _chemical_formula_weight 1105.67 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8952(18) _cell_length_b 24.379(5) _cell_length_c 18.159(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.94(3) _cell_angle_gamma 90.00 _cell_volume 3701.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 7847 _cell_measurement_theta_min 1.6705 _cell_measurement_theta_max 27.9083 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2212 _exptl_absorpt_coefficient_mu 2.772 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6353 _exptl_absorpt_correction_T_max 0.6654 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27848 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.10 _reflns_number_total 6518 _reflns_number_gt 6027 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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. ISOR: the parameter to go anisotropic restraint to appointed atoms, is applied for O17 and O18. The significant residual peak is 4.69, and the distance to the nearest atom Co1 is 0.91. ; _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^)+(0.0192P)^2^+60.7321P] 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 6518 _refine_ls_number_parameters 543 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.128 _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 Gd1 Gd 0.55007(5) 0.813062(16) 0.08242(2) 0.01500(13) Uani 1 1 d . . . Co1 Co 1.00739(15) 0.67036(6) 0.02204(8) 0.0360(4) Uani 1 1 d . . . Co2 Co -0.06652(14) 0.90864(5) -0.07077(7) 0.0199(3) Uani 1 1 d . . . C1 C 0.6801(10) 0.7272(3) -0.0248(5) 0.0201(18) Uani 1 1 d . . . C2 C 0.5276(10) 0.7474(3) -0.0859(5) 0.0165(17) Uani 1 1 d . . . C3 C 0.4697(10) 0.7260(4) -0.1610(5) 0.0226(19) Uani 1 1 d . . . H3 H 0.5238 0.6982 -0.1768 0.027 Uiso 1 1 d R . . C4 C 0.3276(10) 0.7475(3) -0.2120(5) 0.0187(18) Uani 1 1 d . . . C5 C 0.2498(10) 0.7897(4) -0.1867(5) 0.0213(18) Uani 1 1 d . . . H5 H 0.1555 0.8049 -0.2202 0.026 Uiso 1 1 d R . . C6 C 0.3177(10) 0.8076(3) -0.1105(4) 0.0159(17) Uani 1 1 d . . . C7 C 0.2406(10) 0.8504(3) -0.0750(5) 0.0169(17) Uani 1 1 d . . . C8 C 0.7229(10) 0.9196(3) 0.0311(5) 0.0172(17) Uani 1 1 d . . . C9 C 0.6437(9) 0.9483(3) 0.0811(4) 0.0155(17) Uani 1 1 d . . . C10 C 0.6371(10) 1.0042(3) 0.0883(5) 0.0168(17) Uani 1 1 d . . . H10 H 0.6919 1.0272 0.0653 0.020 Uiso 1 1 d R . . C11 C 0.5467(10) 1.0261(3) 0.1307(5) 0.0194(18) Uani 1 1 d . . . C12 C 0.4744(11) 0.9900(4) 0.1679(5) 0.025(2) Uani 1 1 d . . . H12 H 0.4155 1.0032 0.1978 0.029 Uiso 1 1 d R . . C13 C 0.4920(10) 0.9349(3) 0.1593(5) 0.0160(17) Uani 1 1 d . . . C14 C 0.4144(11) 0.8923(4) 0.1955(5) 0.026(2) Uani 1 1 d . . . C15 C 0.8508(10) 0.7883(4) 0.2486(5) 0.0218(19) Uani 1 1 d . . . C16 C 0.7486(10) 0.7376(3) 0.2418(5) 0.0165(17) Uani 1 1 d . . . C17 C 0.7958(11) 0.6954(3) 0.2952(5) 0.0216(18) Uani 1 1 d . . . H17 H 0.8943 0.6967 0.3354 0.026 Uiso 1 1 calc R . . C18 C 0.6928(10) 0.6501(3) 0.2882(5) 0.0209(18) Uani 1 1 d . . . C19 C 0.5488(10) 0.6509(3) 0.2242(5) 0.0203(18) Uani 1 1 d . . . H19 H 0.4768 0.6220 0.2165 0.024 Uiso 1 1 d R . . C20 C 0.5137(9) 0.6944(3) 0.1726(5) 0.0183(17) Uani 1 1 d . . . C21 C 0.3624(11) 0.6984(3) 0.1027(5) 0.0223(19) Uani 1 1 d . . . N1 N 0.4540(8) 0.7869(3) -0.0605(4) 0.0156(14) Uani 1 1 d . . . N2 N 0.5701(8) 0.9131(3) 0.1149(4) 0.0162(14) Uani 1 1 d . . . N3 N 0.6101(8) 0.7376(3) 0.1808(4) 0.0178(15) Uani 1 1 d . . . O1 O 0.7621(7) 0.6916(2) -0.0430(3) 0.0272(14) Uani 1 1 d . . . O2 O 0.7116(7) 0.7481(2) 0.0427(3) 0.0217(13) Uani 1 1 d . . . O3 O 0.2586(7) 0.7286(2) -0.2855(3) 0.0253(14) Uani 1 1 d . . . H3B H 0.3205 0.7079 -0.2964 0.038 Uiso 1 1 d R . . O4 O 0.3094(7) 0.8595(2) -0.0029(3) 0.0180(12) Uani 1 1 d . . . O5 O 0.1132(7) 0.8729(2) -0.1165(3) 0.0193(12) Uani 1 1 d . . . O6 O 0.7948(7) 0.9467(2) -0.0052(3) 0.0214(13) Uani 1 1 d . . . O7 O 0.7081(7) 0.8682(2) 0.0274(3) 0.0197(13) Uani 1 1 d . . . O8 O 0.5334(7) 1.0806(2) 0.1335(4) 0.0264(14) Uani 1 1 d . . . H8 H 0.4452 1.0884 0.1356 0.040 Uiso 1 1 d R . . O9 O 0.3515(11) 0.9064(3) 0.2428(5) 0.056(2) Uani 1 1 d . . . O10 O 0.4202(7) 0.8434(2) 0.1728(3) 0.0213(13) Uani 1 1 d . . . O11 O 0.7989(7) 0.8218(2) 0.1907(3) 0.0225(13) Uani 1 1 d . . . O12 O 0.9747(7) 0.7946(2) 0.3049(3) 0.0260(14) Uani 1 1 d . . . O13 O 0.3514(7) 0.7404(2) 0.0606(3) 0.0224(13) Uani 1 1 d . . . O14 O 0.2601(7) 0.6613(2) 0.0907(4) 0.0271(14) Uani 1 1 d . . . O15 O 0.7277(7) 0.6094(2) 0.3388(4) 0.0264(14) Uani 1 1 d . . . O16 O 1.0054(9) 0.7200(4) 0.1136(4) 0.062(3) Uani 1 1 d . . . O17 O 0.9465(13) 0.6084(4) 0.0803(6) 0.086(3) Uani 1 1 d U . . H17A H 0.8506 0.5986 0.0766 0.103 Uiso 1 1 d R . . H17B H 1.0177 0.5826 0.0947 0.103 Uiso 1 1 d R . . O18 O 1.0226(12) 0.6158(4) -0.0598(6) 0.073(3) Uani 1 1 d U . . H18A H 0.9365 0.5975 -0.0852 0.088 Uiso 1 1 d R . . H18B H 1.1049 0.6076 -0.0732 0.088 Uiso 1 1 d R . . O19 O 1.0636(7) 0.7351(2) -0.0429(3) 0.0261(14) Uani 1 1 d . . . O20 O -0.0504(9) 0.8356(3) -0.0117(5) 0.047(2) Uani 1 1 d . . . O21 O 0.1296(9) 0.9361(4) 0.0281(5) 0.063(3) Uani 1 1 d . . . O22 O -0.0557(9) 0.9843(3) -0.1204(4) 0.0398(18) Uani 1 1 d . . . O23 O 0.0933(13) 0.5800(4) 0.2353(5) 0.078(3) Uani 1 1 d . . . O24 O 0.1074(14) 0.9971(4) 0.2713(6) 0.082(3) Uani 1 1 d . . . O25 O 0.571(2) 0.9925(7) 0.6388(9) 0.142(6) Uani 1 1 d . . . O26 O 0.0180(16) 0.8951(7) 0.1752(11) 0.179(9) Uani 1 1 d . . . O27 O 0.2871(18) 0.9688(10) 0.6610(10) 0.181(9) Uani 1 1 d . . . O28 O 0.653(2) 0.5640(9) 0.0291(12) 0.204(10) Uani 1 1 d . . . O29 O 0.141(3) 0.5134(12) 0.0143(12) 0.249(13) Uani 1 1 d . . . O30 O 0.179(3) 0.6223(10) 0.8312(18) 0.121(14) Uani 0.50(3) 1 d P A 1 O30' O 0.430(8) 0.5995(13) 0.9075(16) 0.29(4) Uani 0.50(3) 1 d P A 2 O31 O 0.742(4) 0.5951(11) 0.8160(17) 0.082(15) Uani 0.37(4) 1 d P B 1 O31' O 0.879(6) 0.559(3) 0.792(2) 0.35(4) Uani 0.63(4) 1 d P B 2 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 Gd1 0.0156(2) 0.0141(2) 0.0159(2) 0.00061(16) 0.00622(16) 0.00016(17) Co1 0.0171(7) 0.0598(10) 0.0285(7) 0.0145(6) 0.0042(6) 0.0050(6) Co2 0.0186(6) 0.0224(6) 0.0206(6) -0.0048(5) 0.0089(5) 0.0006(5) C1 0.017(4) 0.020(4) 0.024(5) 0.000(3) 0.007(4) -0.001(4) C2 0.015(4) 0.017(4) 0.019(4) -0.001(3) 0.008(3) -0.001(3) C3 0.023(5) 0.024(5) 0.024(5) 0.000(4) 0.014(4) 0.006(4) C4 0.019(5) 0.023(4) 0.016(4) 0.001(3) 0.007(3) 0.000(4) C5 0.019(5) 0.025(5) 0.020(4) 0.002(4) 0.008(4) 0.003(4) C6 0.019(4) 0.017(4) 0.014(4) 0.005(3) 0.009(3) 0.005(3) C7 0.021(5) 0.015(4) 0.019(4) -0.004(3) 0.012(4) -0.002(3) C8 0.016(4) 0.013(4) 0.021(4) 0.001(3) 0.005(4) 0.000(3) C9 0.010(4) 0.019(4) 0.013(4) -0.002(3) 0.000(3) -0.002(3) C10 0.020(4) 0.013(4) 0.017(4) 0.002(3) 0.005(3) -0.002(3) C11 0.025(5) 0.010(4) 0.024(4) -0.004(3) 0.009(4) 0.001(3) C12 0.025(5) 0.024(5) 0.032(5) -0.002(4) 0.020(4) 0.002(4) C13 0.022(5) 0.013(4) 0.019(4) -0.007(3) 0.014(4) -0.006(3) C14 0.034(5) 0.023(5) 0.030(5) -0.001(4) 0.024(4) -0.004(4) C15 0.019(5) 0.026(5) 0.019(4) 0.000(4) 0.006(4) 0.001(4) C16 0.019(4) 0.016(4) 0.017(4) 0.001(3) 0.009(3) -0.005(3) C17 0.023(5) 0.020(5) 0.022(4) 0.003(3) 0.009(4) 0.003(4) C18 0.020(5) 0.018(4) 0.026(5) 0.008(3) 0.010(4) 0.002(4) C19 0.020(5) 0.019(4) 0.023(4) 0.004(3) 0.009(4) 0.002(4) C20 0.011(4) 0.023(4) 0.019(4) 0.005(3) 0.003(3) 0.002(3) C21 0.026(5) 0.019(5) 0.023(4) 0.006(4) 0.010(4) 0.001(4) N1 0.014(4) 0.016(3) 0.021(4) 0.001(3) 0.011(3) -0.001(3) N2 0.017(4) 0.014(3) 0.018(3) 0.001(3) 0.006(3) 0.000(3) N3 0.016(4) 0.019(4) 0.017(3) 0.004(3) 0.003(3) 0.000(3) O1 0.028(4) 0.026(3) 0.028(3) 0.000(3) 0.009(3) 0.014(3) O2 0.021(3) 0.023(3) 0.020(3) -0.004(2) 0.006(3) 0.003(3) O3 0.024(3) 0.030(3) 0.021(3) -0.011(3) 0.008(3) 0.007(3) O4 0.017(3) 0.019(3) 0.015(3) -0.002(2) 0.003(2) 0.003(2) O5 0.018(3) 0.021(3) 0.019(3) -0.003(2) 0.005(3) 0.002(2) O6 0.024(3) 0.021(3) 0.025(3) -0.001(3) 0.016(3) 0.000(3) O7 0.025(3) 0.018(3) 0.021(3) -0.001(2) 0.015(3) -0.003(2) O8 0.022(3) 0.016(3) 0.045(4) -0.003(3) 0.017(3) 0.002(3) O9 0.094(7) 0.032(4) 0.076(6) -0.013(4) 0.071(6) -0.013(4) O10 0.025(3) 0.019(3) 0.025(3) -0.001(2) 0.016(3) -0.005(3) O11 0.016(3) 0.025(3) 0.020(3) 0.004(2) -0.002(2) -0.007(3) O12 0.018(3) 0.028(3) 0.026(3) 0.008(3) 0.000(3) -0.005(3) O13 0.019(3) 0.021(3) 0.026(3) 0.003(3) 0.007(3) -0.002(3) O14 0.021(3) 0.024(3) 0.031(3) 0.004(3) 0.002(3) -0.002(3) O15 0.018(3) 0.023(3) 0.036(4) 0.009(3) 0.006(3) -0.002(3) O16 0.032(4) 0.109(8) 0.039(4) -0.033(5) 0.003(4) 0.016(5) O17 0.070(6) 0.087(6) 0.093(6) 0.037(5) 0.016(5) -0.011(5) O18 0.069(6) 0.060(5) 0.078(6) -0.032(5) 0.008(5) 0.002(4) O19 0.024(3) 0.028(3) 0.025(3) 0.004(3) 0.006(3) 0.003(3) O20 0.058(5) 0.036(4) 0.066(5) 0.018(4) 0.047(4) 0.024(4) O21 0.027(4) 0.100(7) 0.047(5) -0.049(5) -0.008(4) 0.024(4) O22 0.042(4) 0.026(4) 0.060(5) -0.006(3) 0.028(4) -0.006(3) O23 0.105(8) 0.074(7) 0.046(5) 0.014(5) 0.014(5) -0.003(6) O24 0.112(9) 0.064(6) 0.068(7) 0.007(5) 0.028(6) 0.013(6) O25 0.170(15) 0.135(13) 0.117(12) -0.003(10) 0.045(11) -0.030(11) O26 0.075(9) 0.181(16) 0.222(18) 0.117(14) -0.026(10) -0.058(10) O27 0.095(11) 0.31(3) 0.124(13) 0.095(15) 0.025(10) 0.033(13) O28 0.195(19) 0.26(2) 0.21(2) -0.106(17) 0.128(17) -0.147(18) O29 0.24(2) 0.34(3) 0.127(16) -0.063(19) 0.021(17) 0.05(2) O30 0.12(2) 0.097(19) 0.18(3) 0.031(18) 0.09(2) 0.082(17) O30' 0.63(11) 0.11(3) 0.052(17) 0.023(16) 0.03(3) -0.16(4) O31 0.11(3) 0.059(19) 0.06(2) 0.011(14) 0.005(17) -0.010(16) O31' 0.26(5) 0.68(11) 0.12(3) -0.08(4) 0.09(3) -0.20(6) _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 Gd1 O7 2.395(5) . ? Gd1 O2 2.409(6) . ? Gd1 O11 2.418(6) . ? Gd1 O10 2.422(5) . ? Gd1 O13 2.437(6) . ? Gd1 O4 2.450(5) . ? Gd1 N3 2.492(6) . ? Gd1 N2 2.502(6) . ? Gd1 N1 2.521(7) . ? Co1 O17 2.021(9) . ? Co1 O18 2.033(9) . ? Co1 O16 2.062(7) . ? Co1 O19 2.129(6) . ? Co1 O1 2.160(6) . ? Co1 O14 2.178(6) 1_655 ? Co2 O15 2.047(6) 4_475 ? Co2 O20 2.059(7) . ? Co2 O22 2.069(7) . ? Co2 O21 2.139(7) . ? Co2 O6 2.192(6) 1_455 ? Co2 O5 2.215(6) . ? C1 O1 1.248(10) . ? C1 O2 1.268(10) . ? C1 C2 1.512(12) . ? C2 N1 1.332(10) . ? C2 C3 1.386(12) . ? C3 C4 1.391(12) . ? C3 H3 0.9301 . ? C4 O3 1.346(10) . ? C4 C5 1.402(12) . ? C5 C6 1.378(11) . ? C5 H5 0.9300 . ? C6 N1 1.341(10) . ? C6 C7 1.508(11) . ? C7 O5 1.254(10) . ? C7 O4 1.261(9) . ? C8 O6 1.253(10) . ? C8 O7 1.259(9) . ? C8 C9 1.498(11) . ? C9 N2 1.347(10) . ? C9 C10 1.374(11) . ? C10 C11 1.394(11) . ? C10 H10 0.9300 . ? C11 O8 1.337(10) . ? C11 C12 1.393(12) . ? C12 C13 1.369(12) . ? C12 H12 0.9299 . ? C13 N2 1.340(10) . ? C13 C14 1.516(11) . ? C14 O9 1.224(11) . ? C14 O10 1.269(10) . ? C15 O12 1.231(10) . ? C15 O11 1.286(10) . ? C15 C16 1.514(11) . ? C16 N3 1.346(10) . ? C16 C17 1.378(11) . ? C17 C18 1.414(12) . ? C17 H17 0.9300 . ? C18 O15 1.314(10) . ? C18 C19 1.406(12) . ? C19 C20 1.380(11) . ? C19 H19 0.9301 . ? C20 N3 1.334(10) . ? C20 C21 1.506(12) . ? C21 O14 1.247(10) . ? C21 O13 1.263(10) . ? O3 H3B 0.8200 . ? O6 Co2 2.192(6) 1_655 ? O8 H8 0.8200 . ? O14 Co1 2.178(6) 1_455 ? O15 Co2 2.047(6) 4_676 ? O17 H17A 0.8663 . ? O17 H17B 0.8676 . ? O18 H18A 0.8697 . ? O18 H18B 0.8699 . ? 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 O7 Gd1 O2 75.5(2) . . ? O7 Gd1 O11 77.6(2) . . ? O2 Gd1 O11 80.1(2) . . ? O7 Gd1 O10 126.51(19) . . ? O2 Gd1 O10 151.01(19) . . ? O11 Gd1 O10 86.4(2) . . ? O7 Gd1 O13 146.72(19) . . ? O2 Gd1 O13 87.0(2) . . ? O11 Gd1 O13 127.50(19) . . ? O10 Gd1 O13 81.06(19) . . ? O7 Gd1 O4 89.29(19) . . ? O2 Gd1 O4 126.61(18) . . ? O11 Gd1 O4 146.48(19) . . ? O10 Gd1 O4 76.80(19) . . ? O13 Gd1 O4 78.70(19) . . ? O7 Gd1 N3 134.5(2) . . ? O2 Gd1 N3 74.1(2) . . ? O11 Gd1 N3 64.5(2) . . ? O10 Gd1 N3 77.0(2) . . ? O13 Gd1 N3 63.0(2) . . ? O4 Gd1 N3 136.2(2) . . ? O7 Gd1 N2 63.0(2) . . ? O2 Gd1 N2 135.2(2) . . ? O11 Gd1 N2 75.5(2) . . ? O10 Gd1 N2 63.6(2) . . ? O13 Gd1 N2 137.4(2) . . ? O4 Gd1 N2 71.0(2) . . ? N3 Gd1 N2 124.7(2) . . ? O7 Gd1 N1 75.7(2) . . ? O2 Gd1 N1 63.5(2) . . ? O11 Gd1 N1 139.0(2) . . ? O10 Gd1 N1 134.6(2) . . ? O13 Gd1 N1 71.1(2) . . ? O4 Gd1 N1 63.23(19) . . ? N3 Gd1 N1 117.8(2) . . ? N2 Gd1 N1 117.4(2) . . ? O17 Co1 O18 89.4(5) . . ? O17 Co1 O16 86.5(5) . . ? O18 Co1 O16 174.1(4) . . ? O17 Co1 O19 177.9(4) . . ? O18 Co1 O19 89.6(3) . . ? O16 Co1 O19 94.6(3) . . ? O17 Co1 O1 93.7(4) . . ? O18 Co1 O1 93.7(3) . . ? O16 Co1 O1 90.9(3) . . ? O19 Co1 O1 84.5(2) . . ? O17 Co1 O14 91.9(3) . 1_655 ? O18 Co1 O14 92.2(3) . 1_655 ? O16 Co1 O14 83.6(3) . 1_655 ? O19 Co1 O14 90.0(2) . 1_655 ? O1 Co1 O14 171.9(2) . 1_655 ? O15 Co2 O20 96.7(3) 4_475 . ? O15 Co2 O22 90.2(3) 4_475 . ? O20 Co2 O22 173.1(3) . . ? O15 Co2 O21 172.1(3) 4_475 . ? O20 Co2 O21 86.7(4) . . ? O22 Co2 O21 86.6(4) . . ? O15 Co2 O6 90.7(2) 4_475 1_455 ? O20 Co2 O6 92.0(2) . 1_455 ? O22 Co2 O6 88.7(2) . 1_455 ? O21 Co2 O6 82.0(3) . 1_455 ? O15 Co2 O5 100.2(2) 4_475 . ? O20 Co2 O5 85.7(2) . . ? O22 Co2 O5 92.3(2) . . ? O21 Co2 O5 87.2(2) . . ? O6 Co2 O5 169.0(2) 1_455 . ? O1 C1 O2 125.3(8) . . ? O1 C1 C2 119.5(7) . . ? O2 C1 C2 115.1(7) . . ? N1 C2 C3 123.5(8) . . ? N1 C2 C1 114.0(7) . . ? C3 C2 C1 122.5(7) . . ? C2 C3 C4 117.5(8) . . ? C2 C3 H3 121.4 . . ? C4 C3 H3 121.1 . . ? O3 C4 C3 122.4(7) . . ? O3 C4 C5 117.9(7) . . ? C3 C4 C5 119.8(8) . . ? C6 C5 C4 117.8(8) . . ? C6 C5 H5 121.2 . . ? C4 C5 H5 121.0 . . ? N1 C6 C5 123.0(7) . . ? N1 C6 C7 114.1(7) . . ? C5 C6 C7 122.8(7) . . ? O5 C7 O4 124.5(7) . . ? O5 C7 C6 119.7(7) . . ? O4 C7 C6 115.8(7) . . ? O6 C8 O7 124.1(7) . . ? O6 C8 C9 120.1(7) . . ? O7 C8 C9 115.8(7) . . ? N2 C9 C10 123.0(7) . . ? N2 C9 C8 112.4(7) . . ? C10 C9 C8 124.5(7) . . ? C9 C10 C11 118.9(7) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.4 . . ? O8 C11 C12 123.1(8) . . ? O8 C11 C10 118.5(7) . . ? C12 C11 C10 118.4(7) . . ? C13 C12 C11 118.3(8) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.8 . . ? N2 C13 C12 124.1(7) . . ? N2 C13 C14 113.3(7) . . ? C12 C13 C14 122.5(7) . . ? O9 C14 O10 125.0(8) . . ? O9 C14 C13 119.7(8) . . ? O10 C14 C13 115.3(7) . . ? O12 C15 O11 124.8(8) . . ? O12 C15 C16 120.8(8) . . ? O11 C15 C16 114.4(7) . . ? N3 C16 C17 123.5(7) . . ? N3 C16 C15 115.0(7) . . ? C17 C16 C15 121.4(8) . . ? C16 C17 C18 119.2(8) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? O15 C18 C19 121.3(8) . . ? O15 C18 C17 122.4(8) . . ? C19 C18 C17 116.3(7) . . ? C20 C19 C18 120.2(8) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 120.1 . . ? N3 C20 C19 122.9(8) . . ? N3 C20 C21 113.5(7) . . ? C19 C20 C21 123.5(8) . . ? O14 C21 O13 125.5(8) . . ? O14 C21 C20 119.3(7) . . ? O13 C21 C20 115.1(8) . . ? C2 N1 C6 118.4(7) . . ? C2 N1 Gd1 120.3(5) . . ? C6 N1 Gd1 120.8(5) . . ? C13 N2 C9 117.0(7) . . ? C13 N2 Gd1 121.2(5) . . ? C9 N2 Gd1 121.3(5) . . ? C20 N3 C16 117.7(7) . . ? C20 N3 Gd1 122.0(5) . . ? C16 N3 Gd1 120.1(5) . . ? C1 O1 Co1 126.5(6) . . ? C1 O2 Gd1 126.6(5) . . ? C4 O3 H3B 109.5 . . ? C7 O4 Gd1 125.8(5) . . ? C7 O5 Co2 124.5(5) . . ? C8 O6 Co2 123.0(5) . 1_655 ? C8 O7 Gd1 127.0(5) . . ? C11 O8 H8 109.4 . . ? C14 O10 Gd1 126.1(5) . . ? C15 O11 Gd1 125.6(5) . . ? C21 O13 Gd1 126.1(6) . . ? C21 O14 Co1 125.2(6) . 1_455 ? C18 O15 Co2 131.0(5) . 4_676 ? Co1 O17 H17A 126.7 . . ? Co1 O17 H17B 113.7 . . ? H17A O17 H17B 114.9 . . ? Co1 O18 H18A 117.2 . . ? Co1 O18 H18B 128.8 . . ? H18A O18 H18B 114.0 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 4.685 _refine_diff_density_min -2.374 _refine_diff_density_rms 0.186 #===END data_22 _database_code_depnum_ccdc_archive 'CCDC 772806' #TrackingRef '- Ln-L2-Co.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H28 Co2 Ho N3 O25' _chemical_formula_weight 1005.25 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9629(18) _cell_length_b 24.304(5) _cell_length_c 18.353(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.35(3) _cell_angle_gamma 90.00 _cell_volume 3748.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6660 _cell_measurement_theta_min 1.4499 _cell_measurement_theta_max 27.8445 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 3.057 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5799 _exptl_absorpt_correction_T_max 0.5799 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22751 _diffrn_reflns_av_R_equivalents 0.0838 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6557 _reflns_number_gt 5040 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0713P)^2^+16.6457P] 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 6557 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1661 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _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 Co2 Co 0.99991(16) 0.32987(7) 0.47178(9) 0.0400(4) Uani 1 1 d . . . Co1 Co 0.07476(15) 0.40412(6) 0.06651(8) 0.0304(3) Uani 1 1 d . . . Ho1 Ho 0.45733(5) 0.188782(18) 0.41511(2) 0.02186(16) Uani 1 1 d . . . C1 C 0.3267(11) 0.2748(4) 0.5173(6) 0.031(2) Uani 1 1 d . . . C2 C 0.4790(11) 0.2542(4) 0.5797(6) 0.030(2) Uani 1 1 d . . . C3 C 0.5317(11) 0.2740(5) 0.6552(6) 0.032(2) Uani 1 1 d . . . H3A H 0.4753 0.3007 0.6711 0.038 Uiso 1 1 d R . . C4 C 0.6721(11) 0.2522(4) 0.7052(5) 0.026(2) Uani 1 1 d . . . C5 C 0.7518(11) 0.2107(5) 0.6805(5) 0.032(2) Uani 1 1 d . . . H5 H 0.8458 0.1954 0.7140 0.038 Uiso 1 1 d R . . C6 C 0.6868(10) 0.1940(4) 0.6039(5) 0.023(2) Uani 1 1 d . . . C7 C 0.7633(10) 0.1518(4) 0.5684(5) 0.025(2) Uani 1 1 d . . . C8 C 0.2894(11) 0.0842(4) 0.4686(6) 0.029(2) Uani 1 1 d . . . C9 C 0.3621(10) 0.0557(4) 0.4191(5) 0.027(2) Uani 1 1 d . . . C10 C 0.3666(11) -0.0008(4) 0.4126(5) 0.028(2) Uani 1 1 d . . . H10 H 0.3127 -0.0232 0.4363 0.034 Uiso 1 1 d R . . C11 C 0.4530(11) -0.0242(4) 0.3710(6) 0.030(2) Uani 1 1 d . . . C12 C 0.5221(12) 0.0120(5) 0.3304(6) 0.038(3) Uani 1 1 d . . . H12 H 0.5753 -0.0020 0.2990 0.045 Uiso 1 1 d R . . C13 C 0.5106(11) 0.0682(4) 0.3399(5) 0.027(2) Uani 1 1 d . . . C14 C 0.5836(13) 0.1095(5) 0.3025(6) 0.040(3) Uani 1 1 d . . . C15 C 0.1591(11) 0.2117(4) 0.2542(5) 0.028(2) Uani 1 1 d . . . C16 C 0.2604(10) 0.2616(4) 0.2586(6) 0.027(2) Uani 1 1 d . . . C17 C 0.2141(11) 0.3038(4) 0.2046(6) 0.034(2) Uani 1 1 d . . . H17 H 0.1160 0.3020 0.1646 0.041 Uiso 1 1 d R . . C18 C 0.3127(11) 0.3484(5) 0.2100(5) 0.030(2) Uani 1 1 d . . . C19 C 0.4593(11) 0.3478(4) 0.2735(6) 0.031(2) Uani 1 1 d . . . H19 H 0.5315 0.3764 0.2798 0.037 Uiso 1 1 d R . . C20 C 0.4941(12) 0.3054(4) 0.3251(6) 0.032(2) Uani 1 1 d . . . C21 C 0.6469(11) 0.3010(4) 0.3942(6) 0.029(2) Uani 1 1 d . . . N1 N 0.5526(8) 0.2155(4) 0.5540(4) 0.0253(17) Uani 1 1 d . . . N2 N 0.4356(9) 0.0899(3) 0.3848(4) 0.0222(16) Uani 1 1 d . . . N3 N 0.3979(8) 0.2613(3) 0.3182(4) 0.0240(17) Uani 1 1 d . . . O1 O 0.2422(7) 0.3092(3) 0.5354(4) 0.0394(18) Uani 1 1 d . . . O2 O 0.2992(8) 0.2540(3) 0.4502(4) 0.0344(17) Uani 1 1 d . . . O3 O 0.7379(8) 0.2701(3) 0.7794(4) 0.0393(18) Uani 1 1 d . . . H3 H 0.6729 0.2887 0.7907 0.059 Uiso 1 1 d R . . O4 O 0.8940(7) 0.1303(3) 0.6098(4) 0.0309(16) Uani 1 1 d . . . O5 O 0.6931(7) 0.1431(3) 0.4972(4) 0.0312(16) Uani 1 1 d . . . O6 O 0.3065(7) 0.1367(3) 0.4717(4) 0.0323(16) Uani 1 1 d . . . O7 O 0.2134(8) 0.0585(3) 0.5039(4) 0.0342(16) Uani 1 1 d . . . O8 O 0.4627(8) -0.0785(3) 0.3659(4) 0.0372(17) Uani 1 1 d . . . H8 H 0.5396 -0.0881 0.3504 0.056 Uiso 1 1 d R . . O9 O 0.5792(8) 0.1588(3) 0.3249(4) 0.0303(15) Uani 1 1 d . . . O10 O 0.6385(11) 0.0957(4) 0.2526(5) 0.064(3) Uani 1 1 d . . . O11 O 0.2097(7) 0.1789(3) 0.3118(4) 0.0330(16) Uani 1 1 d . . . O12 O 0.0349(9) 0.2038(3) 0.1971(4) 0.045(2) Uani 1 1 d . . . O13 O 0.2793(8) 0.3905(3) 0.1603(4) 0.0377(17) Uani 1 1 d . . . O14 O 0.6570(7) 0.2591(3) 0.4374(4) 0.0350(17) Uani 1 1 d . . . O15 O 0.7501(8) 0.3377(3) 0.4067(4) 0.0406(18) Uani 1 1 d . . . O16 O 0.9456(8) 0.2697(3) 0.5419(4) 0.0404(18) Uani 1 1 d . . . H16A H 0.9839 0.2882 0.5844 0.048 Uiso 1 1 d R . . H16B H 0.8437 0.2722 0.5192 0.048 Uiso 1 1 d R . . O17 O 0.9978(9) 0.2755(5) 0.3864(5) 0.089(4) Uani 1 1 d . . . H17A H 1.0930 0.2683 0.3870 0.107 Uiso 1 1 d R . . H17B H 0.9338 0.2478 0.3749 0.107 Uiso 1 1 d R . . O18 O 1.0598(13) 0.3921(5) 0.4104(6) 0.104(4) Uani 1 1 d . . . H18A H 1.1339 0.4038 0.4509 0.124 Uiso 1 1 d R . . H18B H 1.0651 0.4022 0.3660 0.124 Uiso 1 1 d R . . O19 O 0.9993(13) 0.3887(4) 0.5511(7) 0.091(4) Uani 1 1 d . . . H19A H 1.0974 0.3967 0.5762 0.109 Uiso 1 1 d R . . H19B H 0.9301 0.4043 0.5670 0.109 Uiso 1 1 d R . . O20 O 0.0539(10) 0.4800(4) 0.1087(6) 0.060(2) Uani 1 1 d . . . H20A H -0.0149 0.5024 0.0808 0.072 Uiso 1 1 d R . . H20B H 0.1138 0.4892 0.1541 0.072 Uiso 1 1 d R . . O21 O -0.1103(9) 0.4224(5) -0.0398(5) 0.084(4) Uani 1 1 d . . . H21A H -0.0877 0.4339 -0.0785 0.101 Uiso 1 1 d R . . H21B H -0.2069 0.4182 -0.0437 0.101 Uiso 1 1 d R . . O22 O 0.0762(12) 0.3285(4) 0.0175(6) 0.071(3) Uani 1 1 d . . . H22A H 0.0266 0.2960 0.0107 0.085 Uiso 1 1 d R . . H22B H 0.1651 0.3261 0.0082 0.085 Uiso 1 1 d R . . O23 O 0.9816(13) 0.1104(6) 0.3299(7) 0.113(5) Uani 1 1 d . . . O24 O 0.918(3) 0.4192(7) 0.2579(8) 0.204(10) Uani 1 1 d . . . O25 O 0.805(3) 0.3802(11) 0.6404(18) 0.267(13) 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 Co2 0.0251(7) 0.0510(10) 0.0379(8) 0.0026(7) 0.0032(6) 0.0007(7) Co1 0.0263(7) 0.0326(8) 0.0320(7) 0.0058(6) 0.0097(6) -0.0007(6) Ho1 0.0191(2) 0.0240(3) 0.0211(2) 0.00147(18) 0.00528(17) 0.00058(19) C1 0.029(5) 0.035(6) 0.025(5) -0.005(4) 0.005(4) -0.003(5) C2 0.020(4) 0.033(6) 0.039(6) 0.005(5) 0.012(4) 0.007(4) C3 0.025(5) 0.039(6) 0.030(5) 0.000(5) 0.008(4) -0.001(5) C4 0.026(5) 0.034(6) 0.020(5) 0.004(4) 0.009(4) 0.002(4) C5 0.026(5) 0.045(6) 0.022(5) 0.001(5) 0.005(4) -0.001(5) C6 0.023(4) 0.026(5) 0.017(4) -0.001(4) 0.004(4) 0.000(4) C7 0.023(5) 0.030(5) 0.022(5) 0.004(4) 0.005(4) 0.002(4) C8 0.029(5) 0.025(6) 0.031(5) -0.003(4) 0.007(4) -0.005(5) C9 0.019(4) 0.029(6) 0.030(5) 0.006(4) 0.004(4) 0.011(4) C10 0.023(5) 0.030(6) 0.032(5) 0.004(4) 0.012(4) 0.001(4) C11 0.025(5) 0.025(5) 0.039(6) 0.002(4) 0.009(4) -0.005(4) C12 0.030(5) 0.042(7) 0.047(6) -0.007(5) 0.021(5) 0.007(5) C13 0.026(5) 0.026(5) 0.029(5) -0.012(4) 0.011(4) -0.002(4) C14 0.043(6) 0.047(7) 0.037(6) -0.006(5) 0.022(5) -0.005(6) C15 0.029(5) 0.031(6) 0.025(5) 0.001(4) 0.011(4) 0.002(5) C16 0.019(4) 0.024(5) 0.033(5) 0.004(4) 0.003(4) 0.004(4) C17 0.023(5) 0.045(7) 0.025(5) 0.009(5) -0.003(4) -0.012(5) C18 0.022(4) 0.042(6) 0.025(5) 0.007(5) 0.006(4) 0.001(5) C19 0.023(5) 0.029(6) 0.037(6) 0.003(5) 0.005(4) -0.003(4) C20 0.030(5) 0.033(6) 0.031(5) 0.009(5) 0.006(4) 0.007(5) C21 0.025(5) 0.025(6) 0.035(6) 0.007(4) 0.008(4) 0.002(4) N1 0.021(4) 0.035(5) 0.017(4) -0.002(3) 0.003(3) 0.005(4) N2 0.033(4) 0.012(4) 0.024(4) 0.000(3) 0.013(3) -0.005(3) N3 0.026(4) 0.022(4) 0.021(4) 0.006(3) 0.004(3) -0.002(4) O1 0.021(3) 0.052(5) 0.042(4) -0.006(4) 0.006(3) 0.019(3) O2 0.031(4) 0.043(4) 0.023(4) -0.004(3) 0.002(3) 0.005(3) O3 0.039(4) 0.052(5) 0.024(4) -0.010(3) 0.008(3) 0.017(4) O4 0.025(3) 0.029(4) 0.036(4) -0.005(3) 0.007(3) 0.009(3) O5 0.027(3) 0.037(4) 0.029(4) -0.001(3) 0.010(3) 0.009(3) O6 0.027(3) 0.038(4) 0.036(4) -0.003(3) 0.015(3) -0.002(3) O7 0.039(4) 0.031(4) 0.040(4) 0.007(3) 0.023(3) 0.004(3) O8 0.034(4) 0.028(4) 0.053(5) -0.002(3) 0.020(3) -0.001(3) O9 0.038(4) 0.029(4) 0.028(4) -0.002(3) 0.017(3) -0.005(3) O10 0.094(7) 0.053(6) 0.075(6) -0.012(5) 0.067(6) -0.006(5) O11 0.024(3) 0.034(4) 0.032(4) 0.008(3) -0.002(3) -0.003(3) O12 0.037(4) 0.049(5) 0.037(4) 0.000(4) -0.004(3) -0.017(4) O13 0.032(4) 0.035(4) 0.042(4) 0.022(3) 0.006(3) 0.002(3) O14 0.022(3) 0.042(5) 0.037(4) 0.006(3) 0.005(3) -0.001(3) O15 0.028(4) 0.042(5) 0.046(4) 0.007(4) 0.004(3) -0.008(4) O16 0.026(3) 0.050(5) 0.040(4) 0.000(4) 0.005(3) 0.003(4) O17 0.026(4) 0.154(11) 0.073(7) -0.062(7) -0.002(4) 0.004(6) O18 0.096(8) 0.125(11) 0.071(7) 0.048(7) 0.004(6) -0.030(8) O19 0.076(7) 0.062(7) 0.111(9) -0.038(7) 0.004(6) 0.001(6) O20 0.063(5) 0.042(5) 0.075(6) 0.004(5) 0.025(5) 0.005(5) O21 0.033(4) 0.140(10) 0.064(6) 0.054(6) -0.005(4) -0.032(6) O22 0.090(7) 0.047(6) 0.107(8) -0.026(5) 0.073(7) -0.031(5) O23 0.078(7) 0.157(13) 0.078(8) 0.042(8) -0.005(6) -0.044(8) O24 0.36(3) 0.137(15) 0.071(9) -0.019(10) 0.024(14) -0.050(17) O25 0.32(3) 0.20(2) 0.32(3) -0.01(2) 0.17(3) 0.09(2) _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 Co2 O19 2.042(10) . ? Co2 O17 2.044(9) . ? Co2 O18 2.064(10) . ? Co2 O16 2.114(7) . ? Co2 O1 2.137(6) 1_655 ? Co2 O15 2.148(7) . ? Co1 O20 2.033(9) . ? Co1 O22 2.049(9) . ? Co1 O13 2.059(7) . ? Co1 O21 2.122(8) . ? Co1 O7 2.164(7) 4_565 ? Co1 O4 2.203(6) 4_465 ? Ho1 O6 2.343(6) . ? Ho1 O2 2.360(7) . ? Ho1 O11 2.377(6) . ? Ho1 O9 2.392(6) . ? Ho1 O5 2.398(6) . ? Ho1 O14 2.404(7) . ? Ho1 N3 2.429(7) . ? Ho1 N2 2.459(7) . ? Ho1 N1 2.477(7) . ? C1 O1 1.247(12) . ? C1 O2 1.274(11) . ? C1 C2 1.529(13) . ? C2 N1 1.326(12) . ? C2 C3 1.384(14) . ? C3 C4 1.380(13) . ? C3 H3A 0.9300 . ? C4 O3 1.353(11) . ? C4 C5 1.401(14) . ? C5 C6 1.382(13) . ? C5 H5 0.9301 . ? C6 N1 1.339(11) . ? C6 C7 1.503(13) . ? C7 O5 1.256(11) . ? C7 O4 1.266(11) . ? C8 O7 1.256(11) . ? C8 O6 1.283(11) . ? C8 C9 1.463(13) . ? C9 N2 1.345(12) . ? C9 C10 1.381(14) . ? C10 C11 1.384(13) . ? C10 H10 0.9299 . ? C11 O8 1.329(12) . ? C11 C12 1.426(14) . ? C12 C13 1.385(14) . ? C12 H12 0.9302 . ? C13 N2 1.340(11) . ? C13 C14 1.490(15) . ? C14 O10 1.227(12) . ? C14 O9 1.271(13) . ? C15 O12 1.251(11) . ? C15 O11 1.274(11) . ? C15 C16 1.500(13) . ? C16 N3 1.333(11) . ? C16 C17 1.386(13) . ? C17 C18 1.381(14) . ? C17 H17 0.9300 . ? C18 O13 1.334(12) . ? C18 C19 1.422(13) . ? C19 C20 1.358(14) . ? C19 H19 0.9301 . ? C20 N3 1.353(13) . ? C20 C21 1.513(13) . ? C21 O15 1.247(12) . ? C21 O14 1.274(11) . ? O1 Co2 2.137(6) 1_455 ? O3 H3 0.8201 . ? O4 Co1 2.203(6) 4_666 ? O7 Co1 2.164(7) 4_566 ? O8 H8 0.8648 . ? O16 H16A 0.8623 . ? O16 H16B 0.8643 . ? O17 H17A 0.8680 . ? O17 H17B 0.8626 . ? O18 H18A 0.8555 . ? O18 H18B 0.8682 . ? O19 H19A 0.8615 . ? O19 H19B 0.8597 . ? O20 H20A 0.8500 . ? O20 H20B 0.8499 . ? O21 H21A 0.8500 . ? O21 H21B 0.8500 . ? O22 H22A 0.8923 . ? O22 H22B 0.8732 . ? 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 O19 Co2 O17 175.8(5) . . ? O19 Co2 O18 86.7(5) . . ? O17 Co2 O18 89.4(5) . . ? O19 Co2 O16 89.5(4) . . ? O17 Co2 O16 94.4(4) . . ? O18 Co2 O16 175.9(4) . . ? O19 Co2 O1 91.7(4) . 1_655 ? O17 Co2 O1 90.2(3) . 1_655 ? O18 Co2 O1 93.6(4) . 1_655 ? O16 Co2 O1 84.8(3) . 1_655 ? O19 Co2 O15 94.2(4) . . ? O17 Co2 O15 84.3(3) . . ? O18 Co2 O15 92.9(4) . . ? O16 Co2 O15 89.1(3) . . ? O1 Co2 O15 171.5(3) 1_655 . ? O20 Co1 O22 175.1(4) . . ? O20 Co1 O13 90.0(3) . . ? O22 Co1 O13 94.8(4) . . ? O20 Co1 O21 90.8(4) . . ? O22 Co1 O21 84.6(5) . . ? O13 Co1 O21 170.5(3) . . ? O20 Co1 O7 88.2(3) . 4_565 ? O22 Co1 O7 92.9(3) . 4_565 ? O13 Co1 O7 90.2(3) . 4_565 ? O21 Co1 O7 80.4(3) . 4_565 ? O20 Co1 O4 91.7(3) . 4_465 ? O22 Co1 O4 86.3(3) . 4_465 ? O13 Co1 O4 100.9(3) . 4_465 ? O21 Co1 O4 88.5(3) . 4_465 ? O7 Co1 O4 168.9(3) 4_565 4_465 ? O6 Ho1 O2 75.4(2) . . ? O6 Ho1 O11 77.1(2) . . ? O2 Ho1 O11 78.6(2) . . ? O6 Ho1 O9 128.0(2) . . ? O2 Ho1 O9 148.8(2) . . ? O11 Ho1 O9 86.7(2) . . ? O6 Ho1 O5 89.4(2) . . ? O2 Ho1 O5 128.4(2) . . ? O11 Ho1 O5 146.0(2) . . ? O9 Ho1 O5 77.2(2) . . ? O6 Ho1 O14 145.0(2) . . ? O2 Ho1 O14 87.6(2) . . ? O11 Ho1 O14 129.8(2) . . ? O9 Ho1 O14 80.9(2) . . ? O5 Ho1 O14 77.3(2) . . ? O6 Ho1 N3 134.7(2) . . ? O2 Ho1 N3 73.3(2) . . ? O11 Ho1 N3 65.3(2) . . ? O9 Ho1 N3 75.6(2) . . ? O5 Ho1 N3 135.8(2) . . ? O14 Ho1 N3 64.5(2) . . ? O6 Ho1 N2 63.8(2) . . ? O2 Ho1 N2 135.2(2) . . ? O11 Ho1 N2 75.1(2) . . ? O9 Ho1 N2 64.2(2) . . ? O5 Ho1 N2 70.9(2) . . ? O14 Ho1 N2 136.8(2) . . ? N3 Ho1 N2 124.3(2) . . ? O6 Ho1 N1 74.4(2) . . ? O2 Ho1 N1 64.4(2) . . ? O11 Ho1 N1 137.7(2) . . ? O9 Ho1 N1 135.7(2) . . ? O5 Ho1 N1 64.0(2) . . ? O14 Ho1 N1 70.6(2) . . ? N3 Ho1 N1 118.2(3) . . ? N2 Ho1 N1 117.4(3) . . ? O1 C1 O2 126.3(9) . . ? O1 C1 C2 119.1(9) . . ? O2 C1 C2 114.6(9) . . ? N1 C2 C3 124.3(9) . . ? N1 C2 C1 113.0(8) . . ? C3 C2 C1 122.7(9) . . ? C4 C3 C2 116.6(9) . . ? C4 C3 H3A 121.9 . . ? C2 C3 H3A 121.5 . . ? O3 C4 C3 121.7(9) . . ? O3 C4 C5 117.6(8) . . ? C3 C4 C5 120.7(9) . . ? C6 C5 C4 117.3(9) . . ? C6 C5 H5 121.3 . . ? C4 C5 H5 121.3 . . ? N1 C6 C5 122.8(9) . . ? N1 C6 C7 114.0(8) . . ? C5 C6 C7 123.2(8) . . ? O5 C7 O4 125.4(9) . . ? O5 C7 C6 115.3(8) . . ? O4 C7 C6 119.2(8) . . ? O7 C8 O6 123.2(9) . . ? O7 C8 C9 121.5(9) . . ? O6 C8 C9 115.2(9) . . ? N2 C9 C10 122.7(9) . . ? N2 C9 C8 113.2(9) . . ? C10 C9 C8 123.9(9) . . ? C9 C10 C11 119.6(9) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.0 . . ? O8 C11 C10 120.6(9) . . ? O8 C11 C12 121.7(9) . . ? C10 C11 C12 117.6(9) . . ? C13 C12 C11 118.5(9) . . ? C13 C12 H12 121.0 . . ? C11 C12 H12 120.5 . . ? N2 C13 C12 122.8(9) . . ? N2 C13 C14 114.4(9) . . ? C12 C13 C14 122.9(9) . . ? O10 C14 O9 124.4(10) . . ? O10 C14 C13 120.9(11) . . ? O9 C14 C13 114.7(8) . . ? O12 C15 O11 123.9(9) . . ? O12 C15 C16 121.0(9) . . ? O11 C15 C16 115.2(8) . . ? N3 C16 C17 123.4(9) . . ? N3 C16 C15 114.3(8) . . ? C17 C16 C15 122.3(8) . . ? C18 C17 C16 120.3(8) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.7 . . ? O13 C18 C17 124.6(8) . . ? O13 C18 C19 119.5(9) . . ? C17 C18 C19 115.8(9) . . ? C20 C19 C18 120.2(9) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 119.9 . . ? N3 C20 C19 123.4(9) . . ? N3 C20 C21 112.5(8) . . ? C19 C20 C21 124.0(9) . . ? O15 C21 O14 124.7(9) . . ? O15 C21 C20 120.0(9) . . ? O14 C21 C20 115.2(9) . . ? C2 N1 C6 118.2(8) . . ? C2 N1 Ho1 121.1(6) . . ? C6 N1 Ho1 120.5(6) . . ? C13 N2 C9 118.4(8) . . ? C13 N2 Ho1 120.4(6) . . ? C9 N2 Ho1 120.8(6) . . ? C16 N3 C20 116.8(8) . . ? C16 N3 Ho1 120.5(6) . . ? C20 N3 Ho1 122.4(6) . . ? C1 O1 Co2 127.4(6) . 1_455 ? C1 O2 Ho1 126.7(6) . . ? C4 O3 H3 109.4 . . ? C7 O4 Co1 125.7(6) . 4_666 ? C7 O5 Ho1 126.1(6) . . ? C8 O6 Ho1 126.6(6) . . ? C8 O7 Co1 125.5(7) . 4_566 ? C11 O8 H8 111.7 . . ? C14 O9 Ho1 125.7(6) . . ? C15 O11 Ho1 124.3(6) . . ? C18 O13 Co1 128.1(6) . . ? C21 O14 Ho1 125.1(6) . . ? C21 O15 Co2 127.0(7) . . ? Co2 O16 H16A 95.0 . . ? Co2 O16 H16B 94.9 . . ? H16A O16 H16B 114.9 . . ? Co2 O17 H17A 112.1 . . ? Co2 O17 H17B 121.4 . . ? H17A O17 H17B 114.2 . . ? Co2 O18 H18A 92.4 . . ? Co2 O18 H18B 146.0 . . ? H18A O18 H18B 116.2 . . ? Co2 O19 H19A 106.5 . . ? Co2 O19 H19B 137.1 . . ? H19A O19 H19B 116.2 . . ? Co1 O20 H20A 119.8 . . ? Co1 O20 H20B 120.2 . . ? H20A O20 H20B 120.0 . . ? Co1 O21 H21A 120.0 . . ? Co1 O21 H21B 120.0 . . ? H21A O21 H21B 120.0 . . ? Co1 O22 H22A 140.9 . . ? Co1 O22 H22B 106.9 . . ? H22A O22 H22B 111.0 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.603 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.189 # Attachment '772807.cif' data_8 _database_code_depnum_ccdc_archive 'CCDC 772807' #TrackingRef '772807.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Fe3 Ho2 N6 O37' _chemical_formula_weight 1722.24 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6/mcc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 15.187(2) _cell_length_b 15.187(2) _cell_length_c 15.616(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3119.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 976 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 26.30 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 3.289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.837821 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16395 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 26.41 _reflns_number_total 1113 _reflns_number_gt 839 _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. ; _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^)+(0.0267P)^2^+6.9797P] 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 1113 _refine_ls_number_parameters 77 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0608 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.000 _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 Ho1 Ho 0.3333 0.6667 0.2500 0.01708(14) Uani 1 6 d S . . Fe2 Fe 0.5000 1.0000 0.0000 0.0178(2) Uani 1 4 d S . . O1 O 0.3883(2) 0.8002(2) 0.14427(17) 0.0274(7) Uani 1 1 d . . . O2 O 0.3851(2) 0.9356(2) 0.0916(2) 0.0363(8) Uani 1 1 d . . . O3 O 0.4868(3) 1.1381(3) 0.0000 0.0279(10) Uani 1 2 d S . . H3 H 0.5172 1.1735 -0.0415 0.034 Uiso 0.50 1 d PR . . N1 N 0.23969(16) 0.76031(16) 0.2500 0.0216(9) Uani 1 2 d S . . C1 C 0.3541(3) 0.8604(3) 0.1390(3) 0.0248(9) Uani 1 1 d . . . C2 C 0.2662(3) 0.8385(3) 0.1961(3) 0.0246(9) Uani 1 1 d . . . C3 C 0.2150(4) 0.8914(3) 0.1939(3) 0.0376(12) Uani 1 1 d . . . H3A H 0.2337 0.9444 0.1553 0.045 Uiso 1 1 d R . . C4 C 0.1349(2) 0.8651(2) 0.2500 0.0476(17) Uani 1 2 d S . . H4 H 0.0996 0.9004 0.2500 0.057 Uiso 1 2 d SR . . O4 O 0.2638(10) 0.0544(13) 0.0000 0.208(7) Uani 1 2 d S . . O5 O 0.0000 0.0000 0.190(6) 0.32(7) Uani 0.50 6 d SP . . 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 Ho1 0.01923(16) 0.01923(16) 0.01277(19) 0.000 0.000 0.00962(8) Fe2 0.0202(6) 0.0153(4) 0.0139(5) 0.000 0.000 0.0058(6) O1 0.0322(18) 0.0306(14) 0.0231(13) 0.0097(11) 0.0100(13) 0.0185(14) O2 0.045(2) 0.0320(18) 0.0357(17) 0.0190(15) 0.0200(16) 0.0223(16) O3 0.035(2) 0.025(2) 0.026(2) 0.000 0.000 0.016(2) N1 0.0218(15) 0.0218(15) 0.021(2) 0.002(2) 0.002(2) 0.0104(17) C1 0.028(2) 0.025(2) 0.0184(19) 0.0030(17) 0.0029(18) 0.0109(19) C2 0.029(2) 0.023(2) 0.021(2) 0.0055(18) 0.0046(18) 0.0119(19) C3 0.040(3) 0.031(3) 0.046(3) 0.020(2) 0.015(2) 0.021(2) C4 0.044(3) 0.044(3) 0.070(5) 0.021(4) 0.021(4) 0.034(3) O4 0.164(11) 0.40(2) 0.103(8) 0.000 0.000 0.172(14) O5 0.130(18) 0.130(18) 0.7(2) 0.000 0.000 0.065(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O1 2.417(3) 2_665 ? Ho1 O1 2.417(3) 11 ? Ho1 O1 2.417(3) 10_665 ? Ho1 O1 2.417(3) . ? Ho1 O1 2.417(3) 12_565 ? Ho1 O1 2.417(3) 3_565 ? Ho1 N1 2.463(4) . ? Ho1 N1 2.463(4) 3_565 ? Ho1 N1 2.463(4) 2_665 ? Fe2 O2 2.084(3) 16 ? Fe2 O2 2.084(3) 4_675 ? Fe2 O2 2.084(3) 13_675 ? Fe2 O2 2.084(3) . ? Fe2 O3 2.204(4) . ? Fe2 O3 2.204(4) 13_675 ? O1 C1 1.261(5) . ? O2 C1 1.239(5) . ? O3 H3 0.8200 . ? N1 C2 1.343(4) . ? N1 C2 1.343(4) 10_665 ? C1 C2 1.499(6) . ? C2 C3 1.368(6) . ? C3 C4 1.386(6) . ? C3 H3A 0.9300 . ? C4 C3 1.386(6) 10_665 ? C4 H4 0.9300 . ? 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 O1 Ho1 O1 145.16(14) 2_665 11 ? O1 Ho1 O1 86.82(13) 2_665 10_665 ? O1 Ho1 O1 78.45(10) 11 10_665 ? O1 Ho1 O1 78.45(10) 2_665 . ? O1 Ho1 O1 86.82(13) 11 . ? O1 Ho1 O1 129.43(13) 10_665 . ? O1 Ho1 O1 129.43(14) 2_665 12_565 ? O1 Ho1 O1 78.45(10) 11 12_565 ? O1 Ho1 O1 78.45(10) 10_665 12_565 ? O1 Ho1 O1 145.16(14) . 12_565 ? O1 Ho1 O1 78.45(10) 2_665 3_565 ? O1 Ho1 O1 129.43(14) 11 3_565 ? O1 Ho1 O1 145.16(14) 10_665 3_565 ? O1 Ho1 O1 78.45(10) . 3_565 ? O1 Ho1 O1 86.82(13) 12_565 3_565 ? O1 Ho1 N1 72.58(7) 2_665 . ? O1 Ho1 N1 72.58(7) 11 . ? O1 Ho1 N1 64.72(7) 10_665 . ? O1 Ho1 N1 64.72(7) . . ? O1 Ho1 N1 136.59(7) 12_565 . ? O1 Ho1 N1 136.59(7) 3_565 . ? O1 Ho1 N1 136.59(7) 2_665 3_565 ? O1 Ho1 N1 64.72(7) 11 3_565 ? O1 Ho1 N1 136.59(7) 10_665 3_565 ? O1 Ho1 N1 72.58(7) . 3_565 ? O1 Ho1 N1 72.58(7) 12_565 3_565 ? O1 Ho1 N1 64.72(7) 3_565 3_565 ? N1 Ho1 N1 120.0 . 3_565 ? O1 Ho1 N1 64.72(7) 2_665 2_665 ? O1 Ho1 N1 136.59(7) 11 2_665 ? O1 Ho1 N1 72.58(7) 10_665 2_665 ? O1 Ho1 N1 136.59(7) . 2_665 ? O1 Ho1 N1 64.72(7) 12_565 2_665 ? O1 Ho1 N1 72.58(7) 3_565 2_665 ? N1 Ho1 N1 120.0 . 2_665 ? N1 Ho1 N1 120.0 3_565 2_665 ? O2 Fe2 O2 180.000(1) 16 4_675 ? O2 Fe2 O2 93.31(19) 16 13_675 ? O2 Fe2 O2 86.69(19) 4_675 13_675 ? O2 Fe2 O2 86.69(19) 16 . ? O2 Fe2 O2 93.31(19) 4_675 . ? O2 Fe2 O2 180.0 13_675 . ? O2 Fe2 O3 89.62(12) 16 . ? O2 Fe2 O3 90.38(12) 4_675 . ? O2 Fe2 O3 90.38(12) 13_675 . ? O2 Fe2 O3 89.62(12) . . ? O2 Fe2 O3 90.38(12) 16 13_675 ? O2 Fe2 O3 89.62(12) 4_675 13_675 ? O2 Fe2 O3 89.62(12) 13_675 13_675 ? O2 Fe2 O3 90.38(12) . 13_675 ? O3 Fe2 O3 180.000(1) . 13_675 ? C1 O1 Ho1 124.0(3) . . ? C1 O2 Fe2 133.2(3) . . ? Fe2 O3 H3 109.5 . . ? C2 N1 C2 119.2(5) . 10_665 ? C2 N1 Ho1 120.4(2) . . ? C2 N1 Ho1 120.4(2) 10_665 . ? O2 C1 O1 127.2(4) . . ? O2 C1 C2 116.4(4) . . ? O1 C1 C2 116.4(3) . . ? N1 C2 C3 121.8(4) . . ? N1 C2 C1 114.2(3) . . ? C3 C2 C1 124.0(4) . . ? C2 C3 C4 119.3(4) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C3 118.6(6) . 10_665 ? C3 C4 H4 120.7 . . ? C3 C4 H4 120.7 10_665 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ho1 O1 C1 81.3(4) 2_665 . . . ? O1 Ho1 O1 C1 -67.0(3) 11 . . . ? O1 Ho1 O1 C1 5.2(3) 10_665 . . . ? O1 Ho1 O1 C1 -131.5(3) 12_565 . . . ? O1 Ho1 O1 C1 161.7(3) 3_565 . . . ? N1 Ho1 O1 C1 5.2(3) . . . . ? N1 Ho1 O1 C1 -131.5(3) 3_565 . . . ? N1 Ho1 O1 C1 113.0(3) 2_665 . . . ? O2 Fe2 O2 C1 103.9(4) 16 . . . ? O2 Fe2 O2 C1 -76.1(4) 4_675 . . . ? O2 Fe2 O2 C1 6(100) 13_675 . . . ? O3 Fe2 O2 C1 -166.5(4) . . . . ? O3 Fe2 O2 C1 13.5(4) 13_675 . . . ? O1 Ho1 N1 C2 -87.7(2) 2_665 . . . ? O1 Ho1 N1 C2 92.3(2) 11 . . . ? O1 Ho1 N1 C2 177.5(2) 10_665 . . . ? O1 Ho1 N1 C2 -2.5(2) . . . . ? O1 Ho1 N1 C2 142.8(2) 12_565 . . . ? O1 Ho1 N1 C2 -37.2(2) 3_565 . . . ? N1 Ho1 N1 C2 46.6(2) 3_565 . . . ? N1 Ho1 N1 C2 -133.4(2) 2_665 . . . ? O1 Ho1 N1 C2 92.3(2) 2_665 . . 10_665 ? O1 Ho1 N1 C2 -87.7(2) 11 . . 10_665 ? O1 Ho1 N1 C2 -2.5(2) 10_665 . . 10_665 ? O1 Ho1 N1 C2 177.5(2) . . . 10_665 ? O1 Ho1 N1 C2 -37.2(2) 12_565 . . 10_665 ? O1 Ho1 N1 C2 142.8(2) 3_565 . . 10_665 ? N1 Ho1 N1 C2 -133.4(2) 3_565 . . 10_665 ? N1 Ho1 N1 C2 46.6(2) 2_665 . . 10_665 ? Fe2 O2 C1 O1 0.8(7) . . . . ? Fe2 O2 C1 C2 -179.0(3) . . . . ? Ho1 O1 C1 O2 173.1(3) . . . . ? Ho1 O1 C1 C2 -7.0(5) . . . . ? C2 N1 C2 C3 -0.7(4) 10_665 . . . ? Ho1 N1 C2 C3 179.3(4) . . . . ? C2 N1 C2 C1 -179.7(4) 10_665 . . . ? Ho1 N1 C2 C1 0.3(4) . . . . ? O2 C1 C2 N1 -176.0(3) . . . . ? O1 C1 C2 N1 4.2(5) . . . . ? O2 C1 C2 C3 5.1(7) . . . . ? O1 C1 C2 C3 -174.8(4) . . . . ? N1 C2 C3 C4 1.4(7) . . . . ? C1 C2 C3 C4 -179.7(4) . . . . ? C2 C3 C4 C3 -0.7(3) . . . 10_665 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.475 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.090 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 772808' #TrackingRef '- Ln-L1-Fe.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Fe3 N6 Nd2 O37' _chemical_formula_weight 1680.86 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' Fe Fe 0.3463 0.8444 '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' Nd Nd -0.1943 3.0179 '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' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6/mcc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' '-y, -x, -z+1/2' 'x-y, -y, -z+1/2' 'x, x-y, -z+1/2' 'y, x, -z+1/2' '-x+y, y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' 'y, x, z-1/2' '-x+y, y, z-1/2' '-x, -x+y, z-1/2' '-y, -x, z-1/2' 'x-y, -y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 15.329(3) _cell_length_b 15.329(3) _cell_length_c 15.403(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3134.5(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 974 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 26.15 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 2.406 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.658676 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15963 _diffrn_reflns_av_R_equivalents 0.1127 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 26.19 _reflns_number_total 1095 _reflns_number_gt 782 _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. ; _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^)+(0.0325P)^2^+10.7357P] 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 1095 _refine_ls_number_parameters 77 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0831 _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 Nd1 Nd 0.6667 0.3333 0.2500 0.01777(19) Uani 1 6 d S . . Fe1 Fe 1.0000 0.5000 0.0000 0.0188(3) Uani 1 4 d S . . O1 O 0.8037(3) 0.4183(3) 0.1419(2) 0.0314(9) Uani 1 1 d . . . O2 O 0.9397(3) 0.5558(3) 0.0927(3) 0.0364(10) Uani 1 1 d . . . O3 O 1.1378(4) 0.6481(4) 0.0000 0.0285(12) Uani 1 2 d S . . N1 N 0.7628(2) 0.5256(4) 0.2500 0.0229(11) Uani 1 2 d S . . C1 C 0.8635(4) 0.5123(4) 0.1387(3) 0.0262(11) Uani 1 1 d . . . C2 C 0.8400(4) 0.5769(4) 0.1961(3) 0.0255(11) Uani 1 1 d . . . C3 C 0.8928(5) 0.6796(4) 0.1941(4) 0.0401(15) Uani 1 1 d . . . H3 H 0.9460 0.7137 0.1555 0.048 Uiso 1 1 calc R . . C4 C 0.8657(3) 0.7315(6) 0.2500 0.049(2) Uani 1 2 d S . . H4 H 0.9008 0.8015 0.2500 0.059 Uiso 1 2 calc SR . . O4 O 0.7321(13) 0.9445(18) 0.0000 0.232(10) Uani 1 2 d S . . O5 O 0.0000 0.0000 0.178(7) 0.32(7) Uani 0.50 6 d SP . . 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 Nd1 0.0185(2) 0.0185(2) 0.0163(3) 0.000 0.000 0.00925(11) Fe1 0.0152(6) 0.0222(9) 0.0179(6) 0.000 0.000 0.0086(8) O1 0.0291(19) 0.026(2) 0.0333(19) -0.0007(16) 0.0128(16) 0.0095(16) O2 0.030(2) 0.031(2) 0.038(2) -0.0016(18) 0.0201(19) 0.0078(18) O3 0.021(3) 0.024(3) 0.033(3) 0.000 0.000 0.005(2) N1 0.022(2) 0.023(3) 0.024(2) 0.000 0.002(3) 0.0114(13) C1 0.026(3) 0.033(3) 0.021(2) 0.000(2) 0.003(2) 0.015(3) C2 0.020(3) 0.027(3) 0.027(3) 0.002(2) 0.007(2) 0.009(2) C3 0.034(3) 0.031(3) 0.051(4) 0.003(3) 0.017(3) 0.014(3) C4 0.044(4) 0.017(4) 0.078(6) 0.000 0.018(6) 0.0085(18) O4 0.204(17) 0.47(3) 0.114(10) 0.000 0.000 0.23(2) O5 0.16(3) 0.16(3) 0.6(2) 0.000 0.000 0.078(14) _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 Nd1 O1 2.479(3) 5_665 ? Nd1 O1 2.479(3) 9 ? Nd1 O1 2.479(3) 7_665 ? Nd1 O1 2.479(3) . ? Nd1 O1 2.479(3) 3_655 ? Nd1 O1 2.479(3) 11_655 ? Nd1 N1 2.553(5) 5_665 ? Nd1 N1 2.553(5) 3_655 ? Nd1 N1 2.553(5) . ? Fe1 O2 2.101(4) 16 ? Fe1 O2 2.101(4) 4_765 ? Fe1 O2 2.101(4) . ? Fe1 O2 2.101(4) 13_765 ? Fe1 O3 2.196(5) 13_765 ? Fe1 O3 2.196(5) . ? O1 C1 1.264(6) . ? O2 C1 1.239(6) . ? N1 C2 1.333(6) 11_655 ? N1 C2 1.333(6) . ? C1 C2 1.500(7) . ? C2 C3 1.364(7) . ? C3 C4 1.370(7) . ? C3 H3 0.9300 . ? C4 C3 1.370(7) 11_655 ? C4 H4 0.9300 . ? 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 O1 Nd1 O1 125.86(16) 5_665 9 ? O1 Nd1 O1 85.56(17) 5_665 7_665 ? O1 Nd1 O1 79.84(13) 9 7_665 ? O1 Nd1 O1 79.84(13) 5_665 . ? O1 Nd1 O1 85.56(17) 9 . ? O1 Nd1 O1 147.61(16) 7_665 . ? O1 Nd1 O1 79.84(13) 5_665 3_655 ? O1 Nd1 O1 147.61(16) 9 3_655 ? O1 Nd1 O1 125.86(16) 7_665 3_655 ? O1 Nd1 O1 79.84(13) . 3_655 ? O1 Nd1 O1 147.61(16) 5_665 11_655 ? O1 Nd1 O1 79.84(13) 9 11_655 ? O1 Nd1 O1 79.84(13) 7_665 11_655 ? O1 Nd1 O1 125.86(16) . 11_655 ? O1 Nd1 O1 85.56(17) 3_655 11_655 ? O1 Nd1 N1 62.93(8) 5_665 5_665 ? O1 Nd1 N1 62.93(8) 9 5_665 ? O1 Nd1 N1 73.80(8) 7_665 5_665 ? O1 Nd1 N1 73.80(8) . 5_665 ? O1 Nd1 N1 137.22(9) 3_655 5_665 ? O1 Nd1 N1 137.22(9) 11_655 5_665 ? O1 Nd1 N1 73.80(8) 5_665 3_655 ? O1 Nd1 N1 137.22(9) 9 3_655 ? O1 Nd1 N1 62.93(8) 7_665 3_655 ? O1 Nd1 N1 137.22(9) . 3_655 ? O1 Nd1 N1 62.93(8) 3_655 3_655 ? O1 Nd1 N1 73.80(8) 11_655 3_655 ? N1 Nd1 N1 120.0 5_665 3_655 ? O1 Nd1 N1 137.22(9) 5_665 . ? O1 Nd1 N1 73.80(8) 9 . ? O1 Nd1 N1 137.22(9) 7_665 . ? O1 Nd1 N1 62.93(8) . . ? O1 Nd1 N1 73.80(8) 3_655 . ? O1 Nd1 N1 62.93(8) 11_655 . ? N1 Nd1 N1 120.000(1) 5_665 . ? N1 Nd1 N1 120.0 3_655 . ? O2 Fe1 O2 180.0(2) 16 4_765 ? O2 Fe1 O2 85.6(2) 16 . ? O2 Fe1 O2 94.4(2) 4_765 . ? O2 Fe1 O2 94.4(2) 16 13_765 ? O2 Fe1 O2 85.6(2) 4_765 13_765 ? O2 Fe1 O2 180.00(16) . 13_765 ? O2 Fe1 O3 91.68(14) 16 13_765 ? O2 Fe1 O3 88.32(14) 4_765 13_765 ? O2 Fe1 O3 91.68(14) . 13_765 ? O2 Fe1 O3 88.32(14) 13_765 13_765 ? O2 Fe1 O3 88.32(14) 16 . ? O2 Fe1 O3 91.68(14) 4_765 . ? O2 Fe1 O3 88.32(14) . . ? O2 Fe1 O3 91.68(14) 13_765 . ? O3 Fe1 O3 180.0 13_765 . ? C1 O1 Nd1 124.5(3) . . ? C1 O2 Fe1 131.1(4) . . ? C2 N1 C2 118.6(6) 11_655 . ? C2 N1 Nd1 120.7(3) 11_655 . ? C2 N1 Nd1 120.7(3) . . ? O2 C1 O1 126.0(5) . . ? O2 C1 C2 117.0(5) . . ? O1 C1 C2 116.9(4) . . ? N1 C2 C3 122.3(5) . . ? N1 C2 C1 114.4(5) . . ? C3 C2 C1 123.3(5) . . ? C2 C3 C4 118.6(6) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C3 119.6(7) . 11_655 ? C3 C4 H4 120.2 . . ? C3 C4 H4 120.2 11_655 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.19 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.490 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.104 # Attachment '- Ln-L1-Co.CIF' data_10 _database_code_depnum_ccdc_archive 'CCDC 772809' #TrackingRef '- Ln-L1-Co.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Co3 N6 O37 Pr2' _chemical_formula_weight 1683.44 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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6/mcc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 15.4997(9) _cell_length_b 15.4997(9) _cell_length_c 15.2348(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3169.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5328 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 26.35 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1666 _exptl_absorpt_coefficient_mu 2.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.697908 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16432 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 26.35 _reflns_number_total 1134 _reflns_number_gt 864 _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. ; _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^)+(0.0345P)^2^+8.2093P] 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 1134 _refine_ls_number_parameters 77 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.000 _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 Pr1 Pr 0.6667 0.3333 0.2500 0.01617(15) Uani 1 6 d S . . Co1 Co 0.5000 0.0000 0.0000 0.0176(2) Uani 1 4 d S . . O1 O 0.58129(19) 0.1953(2) 0.14083(17) 0.0312(7) Uani 1 1 d . . . O2 O 0.4450(2) 0.0576(2) 0.09420(19) 0.0350(7) Uani 1 1 d . . . O3 O 0.6437(3) 0.1329(3) 0.0000 0.0266(8) Uani 1 2 d S . . H3A H 0.6546 0.1813 0.0333 0.032 Uiso 0.50 1 d PR . . H3B H 0.6896 0.1371 -0.0333 0.032 Uiso 0.50 1 d PR . . N1 N 0.4742(3) 0.23709(15) 0.2500 0.0216(8) Uani 1 2 d S . . C1 C 0.4877(3) 0.1345(3) 0.1388(2) 0.0243(8) Uani 1 1 d . . . C2 C 0.4236(3) 0.1592(3) 0.1963(2) 0.0258(8) Uani 1 1 d . . . C3 C 0.3210(3) 0.1067(3) 0.1941(3) 0.0387(11) Uani 1 1 d . . . H3 H 0.2870 0.0535 0.1557 0.046 Uiso 1 1 calc R . . C4 C 0.2701(4) 0.1351(2) 0.2500 0.0462(16) Uani 1 2 d S . . H4 H 0.2008 0.1004 0.2500 0.055 Uiso 1 2 calc SR . . O4 O 0.7842(9) 0.0564(12) 0.0000 0.199(6) Uani 1 2 d S . . O5 O 1.0000 0.0000 0.184(4) 0.20(3) Uani 0.50 6 d SP . . 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 Pr1 0.01692(18) 0.01692(18) 0.0147(2) 0.000 0.000 0.00846(9) Co1 0.0214(5) 0.0144(4) 0.0154(4) 0.000 0.000 0.0078(4) O1 0.0279(15) 0.0300(14) 0.0288(14) -0.0122(12) 0.0029(11) 0.0094(12) O2 0.0292(15) 0.0298(16) 0.0370(15) -0.0170(13) 0.0016(13) 0.0080(13) O3 0.027(2) 0.0221(19) 0.0277(19) 0.000 0.000 0.0102(16) N1 0.023(2) 0.0214(14) 0.0211(19) -0.0041(17) 0.000 0.0115(10) C1 0.027(2) 0.0245(19) 0.0197(17) -0.0028(15) 0.0002(16) 0.0120(17) C2 0.0238(18) 0.0231(19) 0.028(2) -0.0050(16) -0.0016(16) 0.0096(16) C3 0.028(2) 0.033(2) 0.048(3) -0.018(2) -0.006(2) 0.0104(18) C4 0.018(3) 0.044(3) 0.068(4) -0.020(4) 0.000 0.0089(13) O4 0.178(10) 0.41(2) 0.089(6) 0.000 0.000 0.204(13) O5 0.090(11) 0.090(11) 0.43(8) 0.000 0.000 0.045(6) _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 Pr1 O1 2.503(2) . ? Pr1 O1 2.503(2) 10_665 ? Pr1 O1 2.503(2) 11_655 ? Pr1 O1 2.503(2) 2_655 ? Pr1 O1 2.503(2) 12 ? Pr1 O1 2.503(2) 3_665 ? Pr1 N1 2.584(4) 2_655 ? Pr1 N1 2.584(4) 3_665 ? Pr1 N1 2.584(4) . ? Co1 O2 2.084(3) 16 ? Co1 O2 2.084(3) . ? Co1 O2 2.084(3) 4_655 ? Co1 O2 2.084(3) 13_655 ? Co1 O3 2.148(4) 13_655 ? Co1 O3 2.148(4) . ? O1 C1 1.276(4) . ? O2 C1 1.237(4) . ? O3 H3A 0.8500 . ? O3 H3B 0.8500 . ? N1 C2 1.339(4) 12 ? N1 C2 1.339(4) . ? C1 C2 1.512(5) . ? C2 C3 1.378(5) . ? C3 C4 1.373(5) . ? C3 H3 0.9300 . ? C4 C3 1.373(5) 12 ? C4 H4 0.9300 . ? 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 O1 Pr1 O1 147.19(12) . 10_665 ? O1 Pr1 O1 84.49(13) . 11_655 ? O1 Pr1 O1 80.65(9) 10_665 11_655 ? O1 Pr1 O1 80.65(9) . 2_655 ? O1 Pr1 O1 84.49(13) 10_665 2_655 ? O1 Pr1 O1 125.50(11) 11_655 2_655 ? O1 Pr1 O1 125.50(11) . 12 ? O1 Pr1 O1 80.65(9) 10_665 12 ? O1 Pr1 O1 80.65(9) 11_655 12 ? O1 Pr1 O1 147.19(12) 2_655 12 ? O1 Pr1 O1 80.65(9) . 3_665 ? O1 Pr1 O1 125.50(11) 10_665 3_665 ? O1 Pr1 O1 147.19(12) 11_655 3_665 ? O1 Pr1 O1 80.65(9) 2_655 3_665 ? O1 Pr1 O1 84.49(13) 12 3_665 ? O1 Pr1 N1 73.60(6) . 2_655 ? O1 Pr1 N1 73.60(6) 10_665 2_655 ? O1 Pr1 N1 62.75(6) 11_655 2_655 ? O1 Pr1 N1 62.75(6) 2_655 2_655 ? O1 Pr1 N1 137.76(6) 12 2_655 ? O1 Pr1 N1 137.76(6) 3_665 2_655 ? O1 Pr1 N1 137.76(6) . 3_665 ? O1 Pr1 N1 62.75(6) 10_665 3_665 ? O1 Pr1 N1 137.76(6) 11_655 3_665 ? O1 Pr1 N1 73.60(6) 2_655 3_665 ? O1 Pr1 N1 73.60(6) 12 3_665 ? O1 Pr1 N1 62.75(6) 3_665 3_665 ? N1 Pr1 N1 120.0 2_655 3_665 ? O1 Pr1 N1 62.75(6) . . ? O1 Pr1 N1 137.76(6) 10_665 . ? O1 Pr1 N1 73.60(6) 11_655 . ? O1 Pr1 N1 137.76(6) 2_655 . ? O1 Pr1 N1 62.75(6) 12 . ? O1 Pr1 N1 73.60(6) 3_665 . ? N1 Pr1 N1 120.0 2_655 . ? N1 Pr1 N1 120.0 3_665 . ? O2 Co1 O2 87.04(17) 16 . ? O2 Co1 O2 180.00(17) 16 4_655 ? O2 Co1 O2 92.96(17) . 4_655 ? O2 Co1 O2 92.96(17) 16 13_655 ? O2 Co1 O2 180.00(17) . 13_655 ? O2 Co1 O2 87.04(17) 4_655 13_655 ? O2 Co1 O3 87.76(10) 16 13_655 ? O2 Co1 O3 87.76(10) . 13_655 ? O2 Co1 O3 92.24(10) 4_655 13_655 ? O2 Co1 O3 92.24(10) 13_655 13_655 ? O2 Co1 O3 92.24(10) 16 . ? O2 Co1 O3 92.24(10) . . ? O2 Co1 O3 87.76(10) 4_655 . ? O2 Co1 O3 87.76(10) 13_655 . ? O3 Co1 O3 180.0(3) 13_655 . ? C1 O1 Pr1 124.6(2) . . ? C1 O2 Co1 130.9(3) . . ? Co1 O3 H3A 120.0 . . ? Co1 O3 H3B 120.0 . . ? H3A O3 H3B 120.0 . . ? C2 N1 C2 119.0(4) 12 . ? C2 N1 Pr1 120.5(2) 12 . ? C2 N1 Pr1 120.5(2) . . ? O2 C1 O1 126.0(3) . . ? O2 C1 C2 117.4(3) . . ? O1 C1 C2 116.6(3) . . ? N1 C2 C3 122.1(4) . . ? N1 C2 C1 114.8(3) . . ? C3 C2 C1 123.1(3) . . ? C4 C3 C2 118.2(4) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C3 120.4(5) 12 . ? C3 C4 H4 119.8 12 . ? C3 C4 H4 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Pr1 O1 C1 129.8(3) 10_665 . . . ? O1 Pr1 O1 C1 66.6(3) 11_655 . . . ? O1 Pr1 O1 C1 -166.0(3) 2_655 . . . ? O1 Pr1 O1 C1 -7.8(3) 12 . . . ? O1 Pr1 O1 C1 -84.0(3) 3_665 . . . ? N1 Pr1 O1 C1 129.8(3) 2_655 . . . ? N1 Pr1 O1 C1 -113.4(3) 3_665 . . . ? N1 Pr1 O1 C1 -7.8(3) . . . . ? O2 Co1 O2 C1 -100.3(4) 16 . . . ? O2 Co1 O2 C1 79.7(4) 4_655 . . . ? O2 Co1 O2 C1 38.8(3) 13_655 . . . ? O3 Co1 O2 C1 171.8(4) 13_655 . . . ? O3 Co1 O2 C1 -8.2(4) . . . . ? O1 Pr1 N1 C2 -176.7(2) . . . 12 ? O1 Pr1 N1 C2 36.2(2) 10_665 . . 12 ? O1 Pr1 N1 C2 91.1(2) 11_655 . . 12 ? O1 Pr1 N1 C2 -143.8(2) 2_655 . . 12 ? O1 Pr1 N1 C2 3.3(2) 12 . . 12 ? O1 Pr1 N1 C2 -88.9(2) 3_665 . . 12 ? N1 Pr1 N1 C2 134.90(19) 2_655 . . 12 ? N1 Pr1 N1 C2 -45.10(19) 3_665 . . 12 ? O1 Pr1 N1 C2 3.3(2) . . . . ? O1 Pr1 N1 C2 -143.8(2) 10_665 . . . ? O1 Pr1 N1 C2 -88.9(2) 11_655 . . . ? O1 Pr1 N1 C2 36.2(2) 2_655 . . . ? O1 Pr1 N1 C2 -176.7(2) 12 . . . ? O1 Pr1 N1 C2 91.1(2) 3_665 . . . ? N1 Pr1 N1 C2 -45.10(19) 2_655 . . . ? N1 Pr1 N1 C2 134.90(19) 3_665 . . . ? Co1 O2 C1 O1 -5.2(6) . . . . ? Co1 O2 C1 C2 174.8(2) . . . . ? Pr1 O1 C1 O2 -169.1(3) . . . . ? Pr1 O1 C1 C2 10.9(5) . . . . ? C2 N1 C2 C3 0.6(3) 12 . . . ? Pr1 N1 C2 C3 -179.4(3) . . . . ? C2 N1 C2 C1 -179.8(4) 12 . . . ? Pr1 N1 C2 C1 0.2(4) . . . . ? O2 C1 C2 N1 173.2(3) . . . . ? O1 C1 C2 N1 -6.8(5) . . . . ? O2 C1 C2 C3 -7.2(6) . . . . ? O1 C1 C2 C3 172.8(4) . . . . ? N1 C2 C3 C4 -1.1(6) . . . . ? C1 C2 C3 C4 179.3(3) . . . . ? C2 C3 C4 C3 0.5(3) . . . 12 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.914 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.102 # Attachment '772810.CIF' data_021106d _database_code_depnum_ccdc_archive 'CCDC 772810' #TrackingRef '772810.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Fe3 N6 O37 Pr2' _chemical_formula_weight 1674.20 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6/mcc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 15.514(2) _cell_length_b 15.514(2) _cell_length_c 15.354(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3200.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 944 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 23.54 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 2.256 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.750839 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16438 _diffrn_reflns_av_R_equivalents 0.1123 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 26.28 _reflns_number_total 1135 _reflns_number_gt 865 _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. Rint value is higher than 0.1, and the results maybe originated from the poor single crystal quality, although much effort has been made. ; _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^)+(0.0513P)^2^+9.1960P] 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 1135 _refine_ls_number_parameters 76 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.000 _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 Pr1 Pr 0.3333 0.6667 0.2500 0.01657(19) Uani 1 6 d S . . Fe1 Fe 0.5000 1.0000 0.0000 0.0147(3) Uani 1 4 d S . . N1 N 0.23709(17) 0.76291(17) 0.2500 0.0218(10) Uani 1 2 d S . . O1 O 0.3860(2) 0.8046(2) 0.14102(19) 0.0322(7) Uani 1 1 d . . . O2 O 0.3874(2) 0.9424(2) 0.0943(2) 0.0368(8) Uani 1 1 d . . . O3 O 0.4892(3) 1.1339(3) 0.0000 0.0274(9) Uani 1 2 d S . . C1 C 0.2643(3) 0.8408(3) 0.1964(3) 0.0267(9) Uani 1 1 d . . . C2 C 0.2144(4) 0.8935(3) 0.1939(4) 0.0390(12) Uani 1 1 d . . . H2A H 0.2337 0.9465 0.1556 0.047 Uiso 1 1 calc R . . C3 C 0.1347(2) 0.8653(2) 0.2500 0.0484(19) Uani 1 2 d S . . H3A H 0.1001 0.8999 0.2500 0.058 Uiso 1 2 calc SR . . C4 C 0.3530(3) 0.8654(3) 0.1390(3) 0.0248(9) Uani 1 1 d . . . O4 O 0.2726(10) 0.0565(14) 0.0000 0.209(7) Uani 1 2 d S . . O5 O 0.0000 0.0000 0.2500 0.59(9) Uani 1 12 d S . . 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 Pr1 0.0172(2) 0.0172(2) 0.0154(3) 0.000 0.000 0.00858(11) Fe1 0.0170(6) 0.0113(5) 0.0129(5) 0.000 0.000 0.0051(5) N1 0.0205(16) 0.0205(16) 0.022(2) 0.0046(18) 0.0046(18) 0.0085(19) O1 0.0406(18) 0.0304(16) 0.0298(15) 0.0123(13) 0.0156(14) 0.0209(14) O2 0.0456(19) 0.0312(18) 0.0395(18) 0.0178(15) 0.0193(16) 0.0237(16) O3 0.031(2) 0.022(2) 0.029(2) 0.000 0.000 0.0129(19) C1 0.029(2) 0.024(2) 0.029(2) 0.0048(18) 0.0022(18) 0.0146(19) C2 0.041(3) 0.034(3) 0.048(3) 0.020(2) 0.014(2) 0.023(2) C3 0.045(3) 0.045(3) 0.074(5) 0.022(4) 0.022(4) 0.038(4) C4 0.028(2) 0.025(2) 0.0203(19) 0.0030(17) 0.0035(17) 0.0123(18) O4 0.180(12) 0.44(2) 0.089(7) 0.000 0.000 0.214(15) O5 0.083(13) 0.083(13) 1.6(3) 0.000 0.000 0.041(6) _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 Pr1 O1 2.510(3) 2_665 ? Pr1 O1 2.510(3) 11 ? Pr1 O1 2.510(3) 10_665 ? Pr1 O1 2.510(3) . ? Pr1 O1 2.510(3) 12_565 ? Pr1 O1 2.510(3) 3_565 ? Pr1 N1 2.586(5) . ? Pr1 N1 2.586(5) 3_565 ? Pr1 N1 2.586(5) 2_665 ? Fe1 O2 2.094(3) 16 ? Fe1 O2 2.094(3) 4_675 ? Fe1 O2 2.094(3) . ? Fe1 O2 2.094(3) 13_675 ? Fe1 O3 2.166(4) 13_675 ? Fe1 O3 2.166(4) . ? N1 C1 1.344(5) . ? N1 C1 1.344(5) 10_665 ? O1 C4 1.279(5) . ? O2 C4 1.243(5) . ? C1 C2 1.379(6) . ? C1 C4 1.513(6) . ? C2 C3 1.386(6) . ? C2 H2A 0.9300 . ? C3 C2 1.386(6) 10_665 ? C3 H3A 0.9300 . ? 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 O1 Pr1 O1 147.28(14) 2_665 11 ? O1 Pr1 O1 84.79(15) 2_665 10_665 ? O1 Pr1 O1 80.41(11) 11 10_665 ? O1 Pr1 O1 80.41(11) 2_665 . ? O1 Pr1 O1 84.79(15) 11 . ? O1 Pr1 O1 125.64(13) 10_665 . ? O1 Pr1 O1 125.64(13) 2_665 12_565 ? O1 Pr1 O1 80.41(11) 11 12_565 ? O1 Pr1 O1 80.41(11) 10_665 12_565 ? O1 Pr1 O1 147.28(14) . 12_565 ? O1 Pr1 O1 80.41(11) 2_665 3_565 ? O1 Pr1 O1 125.64(13) 11 3_565 ? O1 Pr1 O1 147.28(14) 10_665 3_565 ? O1 Pr1 O1 80.41(11) . 3_565 ? O1 Pr1 O1 84.79(15) 12_565 3_565 ? O1 Pr1 N1 73.64(7) 2_665 . ? O1 Pr1 N1 73.64(7) 11 . ? O1 Pr1 N1 62.82(6) 10_665 . ? O1 Pr1 N1 62.82(6) . . ? O1 Pr1 N1 137.60(7) 12_565 . ? O1 Pr1 N1 137.60(7) 3_565 . ? O1 Pr1 N1 137.60(7) 2_665 3_565 ? O1 Pr1 N1 62.82(6) 11 3_565 ? O1 Pr1 N1 137.60(7) 10_665 3_565 ? O1 Pr1 N1 73.64(7) . 3_565 ? O1 Pr1 N1 73.64(7) 12_565 3_565 ? O1 Pr1 N1 62.82(6) 3_565 3_565 ? N1 Pr1 N1 120.000(1) . 3_565 ? O1 Pr1 N1 62.82(6) 2_665 2_665 ? O1 Pr1 N1 137.60(7) 11 2_665 ? O1 Pr1 N1 73.64(7) 10_665 2_665 ? O1 Pr1 N1 137.60(7) . 2_665 ? O1 Pr1 N1 62.82(6) 12_565 2_665 ? O1 Pr1 N1 73.64(7) 3_565 2_665 ? N1 Pr1 N1 120.0 . 2_665 ? N1 Pr1 N1 120.0 3_565 2_665 ? O2 Fe1 O2 180.000(1) 16 4_675 ? O2 Fe1 O2 87.5(2) 16 . ? O2 Fe1 O2 92.54(19) 4_675 . ? O2 Fe1 O2 92.54(19) 16 13_675 ? O2 Fe1 O2 87.5(2) 4_675 13_675 ? O2 Fe1 O2 180.000(1) . 13_675 ? O2 Fe1 O3 92.20(11) 16 13_675 ? O2 Fe1 O3 87.80(11) 4_675 13_675 ? O2 Fe1 O3 92.20(11) . 13_675 ? O2 Fe1 O3 87.80(11) 13_675 13_675 ? O2 Fe1 O3 87.80(11) 16 . ? O2 Fe1 O3 92.20(11) 4_675 . ? O2 Fe1 O3 87.80(11) . . ? O2 Fe1 O3 92.20(11) 13_675 . ? O3 Fe1 O3 180.000(1) 13_675 . ? C1 N1 C1 119.1(5) . 10_665 ? C1 N1 Pr1 120.5(2) . . ? C1 N1 Pr1 120.5(2) 10_665 . ? C4 O1 Pr1 124.5(3) . . ? C4 O2 Fe1 131.2(3) . . ? N1 C1 C2 122.2(4) . . ? N1 C1 C4 114.9(4) . . ? C2 C1 C4 122.9(4) . . ? C1 C2 C3 118.2(4) . . ? C1 C2 H2A 120.9 . . ? C3 C2 H2A 120.9 . . ? C2 C3 C2 120.1(6) . 10_665 ? C2 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 10_665 . ? O2 C4 O1 125.7(4) . . ? O2 C4 C1 117.7(4) . . ? O1 C4 C1 116.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Pr1 N1 C1 -90.7(2) 2_665 . . . ? O1 Pr1 N1 C1 89.3(2) 11 . . . ? O1 Pr1 N1 C1 176.7(2) 10_665 . . . ? O1 Pr1 N1 C1 -3.3(2) . . . . ? O1 Pr1 N1 C1 143.9(2) 12_565 . . . ? O1 Pr1 N1 C1 -36.1(2) 3_565 . . . ? N1 Pr1 N1 C1 45.3(2) 3_565 . . . ? N1 Pr1 N1 C1 -134.7(2) 2_665 . . . ? O1 Pr1 N1 C1 89.3(2) 2_665 . . 10_665 ? O1 Pr1 N1 C1 -90.7(2) 11 . . 10_665 ? O1 Pr1 N1 C1 -3.3(2) 10_665 . . 10_665 ? O1 Pr1 N1 C1 176.7(2) . . . 10_665 ? O1 Pr1 N1 C1 -36.1(2) 12_565 . . 10_665 ? O1 Pr1 N1 C1 143.9(2) 3_565 . . 10_665 ? N1 Pr1 N1 C1 -134.7(2) 3_565 . . 10_665 ? N1 Pr1 N1 C1 45.3(2) 2_665 . . 10_665 ? O1 Pr1 O1 C4 84.1(4) 2_665 . . . ? O1 Pr1 O1 C4 -66.6(3) 11 . . . ? O1 Pr1 O1 C4 7.7(3) 10_665 . . . ? O1 Pr1 O1 C4 -129.8(3) 12_565 . . . ? O1 Pr1 O1 C4 165.9(3) 3_565 . . . ? N1 Pr1 O1 C4 7.7(3) . . . . ? N1 Pr1 O1 C4 -129.8(3) 3_565 . . . ? N1 Pr1 O1 C4 113.4(3) 2_665 . . . ? O2 Fe1 O2 C4 100.3(4) 16 . . . ? O2 Fe1 O2 C4 -79.7(4) 4_675 . . . ? O2 Fe1 O2 C4 -39(100) 13_675 . . . ? O3 Fe1 O2 C4 8.2(4) 13_675 . . . ? O3 Fe1 O2 C4 -171.8(4) . . . . ? C1 N1 C1 C2 -0.6(4) 10_665 . . . ? Pr1 N1 C1 C2 179.4(4) . . . . ? C1 N1 C1 C4 179.8(4) 10_665 . . . ? Pr1 N1 C1 C4 -0.2(4) . . . . ? N1 C1 C2 C3 1.1(7) . . . . ? C4 C1 C2 C3 -179.3(3) . . . . ? C1 C2 C3 C2 -0.5(3) . . . 10_665 ? Fe1 O2 C4 O1 5.4(7) . . . . ? Fe1 O2 C4 C1 -174.7(3) . . . . ? Pr1 O1 C4 O2 169.2(3) . . . . ? Pr1 O1 C4 C1 -10.7(5) . . . . ? N1 C1 C4 O2 -173.2(4) . . . . ? C2 C1 C4 O2 7.3(7) . . . . ? N1 C1 C4 O1 6.7(5) . . . . ? C2 C1 C4 O1 -172.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.28 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.949 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.128 # Attachment '772811.cif' data_12 _database_code_depnum_ccdc_archive 'CCDC 772811' #TrackingRef '772811.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Co3 N6 O37 Sm2' _chemical_formula_weight 1702.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6/mcc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 15.3092(14) _cell_length_b 15.3092(14) _cell_length_c 15.346(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3114.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 3050 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 25.81 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1678 _exptl_absorpt_coefficient_mu 2.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5840 _exptl_absorpt_correction_T_max 0.7346 _exptl_absorpt_process_details SADBAS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15942 _diffrn_reflns_av_R_equivalents 0.0913 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 26.41 _reflns_number_total 1113 _reflns_number_gt 721 _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. ; _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^)+(0.0373P)^2^+16.4966P] 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 1113 _refine_ls_number_parameters 76 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0981 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.076 _refine_ls_shift/su_mean 0.012 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 Sm1 Sm 0.6667 0.3333 0.2500 0.0169(2) Uani 1 6 d S . . Co1 Co 0.5000 0.0000 0.0000 0.0173(3) Uani 1 4 d S . . O1 O 0.5846(3) 0.1969(3) 0.1426(2) 0.0304(10) Uani 1 1 d . . . O2 O 0.4463(3) 0.0593(3) 0.0931(3) 0.0357(10) Uani 1 1 d . . . O3 O 0.6459(4) 0.1336(4) 0.0000 0.0278(13) Uani 1 2 d S . . H3A H 0.6570 0.1822 0.0333 0.033 Uiso 0.50 1 d PR . . H3B H 0.6920 0.1377 -0.0333 0.033 Uiso 0.50 1 d PR . . N1 N 0.4758(4) 0.2379(2) 0.2500 0.0217(12) Uani 1 2 d S . . C1 C 0.4900(4) 0.1359(4) 0.1384(4) 0.0261(13) Uani 1 1 d . . . C2 C 0.4248(4) 0.1600(4) 0.1964(4) 0.0268(13) Uani 1 1 d . . . C3 C 0.3214(5) 0.1069(5) 0.1939(5) 0.0383(16) Uani 1 1 d . . . H3 H 0.2871 0.0535 0.1553 0.046 Uiso 1 1 calc R . . C4 C 0.2698(6) 0.1349(3) 0.2500 0.047(2) Uani 1 2 d S . . H4 H 0.2003 0.1001 0.2500 0.056 Uiso 1 2 d SR . . O4 O 0.7882(12) 0.0564(16) 0.0000 0.191(8) Uani 1 2 d S . . O5 O 0.0000 0.0000 0.2500 0.63(12) Uani 1 12 d S . . 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 Sm1 0.0167(2) 0.0167(2) 0.0173(3) 0.000 0.000 0.00837(12) Co1 0.0205(8) 0.0134(6) 0.0173(6) 0.000 0.000 0.0079(7) O1 0.029(2) 0.027(2) 0.030(2) -0.0099(16) 0.0008(18) 0.0104(18) O2 0.030(2) 0.027(2) 0.042(2) -0.017(2) 0.000(2) 0.0084(19) O3 0.022(3) 0.020(3) 0.035(3) 0.000 0.000 0.006(2) N1 0.020(3) 0.021(2) 0.024(3) -0.001(3) 0.000 0.0101(14) C1 0.030(3) 0.026(3) 0.021(3) -0.003(2) -0.001(2) 0.013(3) C2 0.024(3) 0.020(3) 0.032(3) -0.007(3) 0.000(3) 0.008(2) C3 0.024(3) 0.030(4) 0.054(4) -0.014(3) -0.001(3) 0.008(3) C4 0.017(4) 0.041(4) 0.074(6) -0.016(6) 0.000 0.0086(19) O4 0.177(14) 0.38(3) 0.093(8) 0.000 0.000 0.198(17) O5 0.12(2) 0.12(2) 1.7(4) 0.000 0.000 0.059(11) _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 Sm1 O1 2.456(4) . ? Sm1 O1 2.456(4) 10_665 ? Sm1 O1 2.456(4) 11_655 ? Sm1 O1 2.456(4) 2_655 ? Sm1 O1 2.456(4) 12 ? Sm1 O1 2.456(4) 3_665 ? Sm1 N1 2.531(6) 2_655 ? Sm1 N1 2.531(6) 3_665 ? Sm1 N1 2.531(6) . ? Co1 O2 2.070(4) 4_655 ? Co1 O2 2.070(4) 13_655 ? Co1 O2 2.070(4) . ? Co1 O2 2.070(4) 16 ? Co1 O3 2.146(5) 13_655 ? Co1 O3 2.146(5) . ? O1 C1 1.274(7) . ? O2 C1 1.234(6) . ? O3 H3A 0.8470 . ? O3 H3B 0.8471 . ? N1 C2 1.333(6) . ? N1 C2 1.333(6) 12 ? C1 C2 1.514(8) . ? C2 C3 1.373(8) . ? C3 C4 1.373(7) . ? C3 H3 0.9300 . ? C4 C3 1.373(7) 12 ? C4 H4 0.9226 . ? 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 O1 Sm1 O1 145.88(18) . 10_665 ? O1 Sm1 O1 85.15(18) . 11_655 ? O1 Sm1 O1 79.90(14) 10_665 11_655 ? O1 Sm1 O1 79.90(14) . 2_655 ? O1 Sm1 O1 85.15(18) 10_665 2_655 ? O1 Sm1 O1 127.41(18) 11_655 2_655 ? O1 Sm1 O1 127.41(18) . 12 ? O1 Sm1 O1 79.89(14) 10_665 12 ? O1 Sm1 O1 79.89(14) 11_655 12 ? O1 Sm1 O1 145.88(19) 2_655 12 ? O1 Sm1 O1 79.89(14) . 3_665 ? O1 Sm1 O1 127.41(18) 10_665 3_665 ? O1 Sm1 O1 145.88(19) 11_655 3_665 ? O1 Sm1 O1 79.90(14) 2_655 3_665 ? O1 Sm1 O1 85.15(18) 12 3_665 ? O1 Sm1 N1 72.94(9) . 2_655 ? O1 Sm1 N1 72.94(9) 10_665 2_655 ? O1 Sm1 N1 63.71(9) 11_655 2_655 ? O1 Sm1 N1 63.71(9) 2_655 2_655 ? O1 Sm1 N1 137.42(9) 12 2_655 ? O1 Sm1 N1 137.42(9) 3_665 2_655 ? O1 Sm1 N1 137.42(9) . 3_665 ? O1 Sm1 N1 63.71(9) 10_665 3_665 ? O1 Sm1 N1 137.42(9) 11_655 3_665 ? O1 Sm1 N1 72.94(9) 2_655 3_665 ? O1 Sm1 N1 72.94(9) 12 3_665 ? O1 Sm1 N1 63.71(9) 3_665 3_665 ? N1 Sm1 N1 120.000(1) 2_655 3_665 ? O1 Sm1 N1 63.71(9) . . ? O1 Sm1 N1 137.42(9) 10_665 . ? O1 Sm1 N1 72.94(9) 11_655 . ? O1 Sm1 N1 137.42(9) 2_655 . ? O1 Sm1 N1 63.71(9) 12 . ? O1 Sm1 N1 72.94(9) 3_665 . ? N1 Sm1 N1 120.0 2_655 . ? N1 Sm1 N1 120.0 3_665 . ? O2 Co1 O2 87.3(3) 4_655 13_655 ? O2 Co1 O2 92.7(3) 4_655 . ? O2 Co1 O2 180.0(3) 13_655 . ? O2 Co1 O2 180.0(3) 4_655 16 ? O2 Co1 O2 92.7(3) 13_655 16 ? O2 Co1 O2 87.3(3) . 16 ? O2 Co1 O3 91.98(16) 4_655 13_655 ? O2 Co1 O3 91.98(16) 13_655 13_655 ? O2 Co1 O3 88.02(16) . 13_655 ? O2 Co1 O3 88.02(16) 16 13_655 ? O2 Co1 O3 88.02(16) 4_655 . ? O2 Co1 O3 88.02(16) 13_655 . ? O2 Co1 O3 91.98(16) . . ? O2 Co1 O3 91.98(16) 16 . ? O3 Co1 O3 180.0(5) 13_655 . ? C1 O1 Sm1 124.7(4) . . ? C1 O2 Co1 131.3(4) . . ? Co1 O3 H3A 119.6 . . ? Co1 O3 H3B 120.1 . . ? H3A O3 H3B 120.3 . . ? C2 N1 C2 119.1(6) . 12 ? C2 N1 Sm1 120.4(3) . . ? C2 N1 Sm1 120.4(3) 12 . ? O2 C1 O1 127.1(5) . . ? O2 C1 C2 116.9(5) . . ? O1 C1 C2 116.0(5) . . ? N1 C2 C3 122.2(5) . . ? N1 C2 C1 114.7(5) . . ? C3 C2 C1 123.1(5) . . ? C2 C3 C4 118.1(6) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C3 C4 C3 120.3(8) 12 . ? C3 C4 H4 119.8 12 . ? C3 C4 H4 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Sm1 O1 C1 131.1(4) 10_665 . . . ? O1 Sm1 O1 C1 67.1(4) 11_655 . . . ? O1 Sm1 O1 C1 -163.5(4) 2_655 . . . ? O1 Sm1 O1 C1 -6.2(4) 12 . . . ? O1 Sm1 O1 C1 -82.1(5) 3_665 . . . ? N1 Sm1 O1 C1 131.1(4) 2_655 . . . ? N1 Sm1 O1 C1 -112.9(4) 3_665 . . . ? N1 Sm1 O1 C1 -6.2(4) . . . . ? O2 Co1 O2 C1 78.6(5) 4_655 . . . ? O2 Co1 O2 C1 -143.2(5) 13_655 . . . ? O2 Co1 O2 C1 -101.4(5) 16 . . . ? O3 Co1 O2 C1 170.4(6) 13_655 . . . ? O3 Co1 O2 C1 -9.6(6) . . . . ? O1 Sm1 N1 C2 2.7(3) . . . . ? O1 Sm1 N1 C2 -143.1(3) 10_665 . . . ? O1 Sm1 N1 C2 -90.3(3) 11_655 . . . ? O1 Sm1 N1 C2 36.9(3) 2_655 . . . ? O1 Sm1 N1 C2 -177.3(3) 12 . . . ? O1 Sm1 N1 C2 89.7(3) 3_665 . . . ? N1 Sm1 N1 C2 -45.7(3) 2_655 . . . ? N1 Sm1 N1 C2 134.3(3) 3_665 . . . ? O1 Sm1 N1 C2 -177.3(3) . . . 12 ? O1 Sm1 N1 C2 36.9(3) 10_665 . . 12 ? O1 Sm1 N1 C2 89.7(3) 11_655 . . 12 ? O1 Sm1 N1 C2 -143.1(3) 2_655 . . 12 ? O1 Sm1 N1 C2 2.7(3) 12 . . 12 ? O1 Sm1 N1 C2 -90.3(3) 3_665 . . 12 ? N1 Sm1 N1 C2 134.3(3) 2_655 . . 12 ? N1 Sm1 N1 C2 -45.7(3) 3_665 . . 12 ? Co1 O2 C1 O1 -4.8(10) . . . . ? Co1 O2 C1 C2 176.0(4) . . . . ? Sm1 O1 C1 O2 -170.6(5) . . . . ? Sm1 O1 C1 C2 8.6(7) . . . . ? C2 N1 C2 C3 0.6(5) 12 . . . ? Sm1 N1 C2 C3 -179.4(5) . . . . ? C2 N1 C2 C1 -180.0(6) 12 . . . ? Sm1 N1 C2 C1 0.0(6) . . . . ? O2 C1 C2 N1 174.0(5) . . . . ? O1 C1 C2 N1 -5.3(7) . . . . ? O2 C1 C2 C3 -6.6(9) . . . . ? O1 C1 C2 C3 174.2(6) . . . . ? N1 C2 C3 C4 -1.1(10) . . . . ? C1 C2 C3 C4 179.5(5) . . . . ? C2 C3 C4 C3 0.5(5) . . . 12 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.244 _refine_diff_density_min -1.167 _refine_diff_density_rms 0.123 # Attachment '772812.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 772812' #TrackingRef '772812.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Fe3 N6 O37 Sm2' _chemical_formula_weight 1693.08 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6/mcc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 15.4050(14) _cell_length_b 15.4050(14) _cell_length_c 15.456(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3176.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 986 _cell_measurement_theta_min 3.73 _cell_measurement_theta_max 26.25 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 2.588 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.800237 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15956 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.22 _reflns_number_total 1114 _reflns_number_gt 722 _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. ; _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^)+(0.0553P)^2^+30.3424P] 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 1114 _refine_ls_number_parameters 78 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.1121 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.000 _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 Sm1 Sm 0.6667 0.3333 0.2500 0.0177(2) Uani 1 6 d S . . Fe1 Fe 0.5000 0.5000 0.0000 0.0145(3) Uani 1 4 d S . . N1 N 0.4757(5) 0.2379(2) 0.2500 0.0228(13) Uani 1 2 d S . . O1 O 0.4466(3) 0.3872(4) 0.0934(3) 0.0385(11) Uani 1 1 d . . . O2 O 0.5846(3) 0.3879(3) 0.1429(3) 0.0323(11) Uani 1 1 d . . . O3 O 0.6470(4) 0.5125(5) 0.0000 0.0295(14) Uani 1 2 d S . . O4 O 0.7871(14) 0.7314(13) 0.0000 0.198(9) Uani 1 2 d S . . C1 C 0.4900(5) 0.3540(5) 0.1384(4) 0.0273(13) Uani 1 1 d . . . C2 C 0.4247(4) 0.2648(4) 0.1965(4) 0.0283(14) Uani 1 1 d . . . C3 C 0.3212(5) 0.2144(5) 0.1938(5) 0.0396(18) Uani 1 1 d . . . H3A H 0.2872 0.2335 0.1555 0.029(18) Uiso 1 1 calc R . . C4 C 0.2696(7) 0.1348(3) 0.2500 0.050(3) Uani 1 2 d S . . H4 H 0.1999 0.1000 0.2500 0.10(5) Uiso 1 2 calc SR . . O5 O 0.0000 0.0000 0.2500 0.59(13) Uani 1 12 d S . . 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 Sm1 0.0176(3) 0.0176(3) 0.0181(3) 0.000 0.000 0.00878(13) Fe1 0.0177(9) 0.0153(8) 0.0144(7) 0.000 0.000 0.0111(6) N1 0.022(3) 0.021(2) 0.026(3) 0.001(3) 0.000 0.0108(16) O1 0.031(2) 0.044(3) 0.045(3) 0.018(2) 0.001(2) 0.022(2) O2 0.032(3) 0.038(3) 0.031(2) 0.011(2) 0.001(2) 0.021(2) O3 0.023(3) 0.032(3) 0.038(3) 0.000 0.000 0.017(3) O4 0.187(16) 0.163(15) 0.094(9) 0.000 0.000 -0.027(13) C1 0.031(3) 0.032(3) 0.022(3) 0.003(3) 0.000(3) 0.018(3) C2 0.025(3) 0.030(3) 0.035(4) 0.006(3) -0.001(3) 0.017(3) C3 0.026(3) 0.040(4) 0.054(5) 0.016(4) 0.000(3) 0.018(3) C4 0.016(4) 0.044(4) 0.081(7) 0.019(7) 0.000 0.008(2) O5 0.11(2) 0.11(2) 1.6(4) 0.000 0.000 0.056(11) _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 Sm1 O2 2.472(4) 11_655 ? Sm1 O2 2.472(4) 2_655 ? Sm1 O2 2.472(4) 3_665 ? Sm1 O2 2.472(4) 12 ? Sm1 O2 2.472(4) 10_665 ? Sm1 O2 2.472(4) . ? Sm1 N1 2.547(6) 2_655 ? Sm1 N1 2.547(6) . ? Sm1 N1 2.547(6) 3_665 ? Fe1 O1 2.085(4) 16 ? Fe1 O1 2.085(4) 4_665 ? Fe1 O1 2.085(4) . ? Fe1 O1 2.085(4) 13_665 ? Fe1 O3 2.174(6) . ? Fe1 O3 2.174(6) 13_665 ? N1 C2 1.342(7) . ? N1 C2 1.342(7) 12 ? O1 C1 1.239(7) . ? O2 C1 1.281(7) . ? C1 C2 1.525(8) . ? C2 C3 1.382(8) . ? C3 C4 1.384(8) . ? C3 H3A 0.9300 . ? C4 C3 1.384(8) 12 ? C4 H4 0.9300 . ? 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 Sm1 O2 127.4(2) 11_655 2_655 ? O2 Sm1 O2 84.9(2) 11_655 3_665 ? O2 Sm1 O2 80.05(15) 2_655 3_665 ? O2 Sm1 O2 80.05(15) 11_655 12 ? O2 Sm1 O2 84.9(2) 2_655 12 ? O2 Sm1 O2 145.7(2) 3_665 12 ? O2 Sm1 O2 80.05(15) 11_655 10_665 ? O2 Sm1 O2 145.7(2) 2_655 10_665 ? O2 Sm1 O2 127.4(2) 3_665 10_665 ? O2 Sm1 O2 80.05(15) 12 10_665 ? O2 Sm1 O2 145.7(2) 11_655 . ? O2 Sm1 O2 80.05(15) 2_655 . ? O2 Sm1 O2 80.05(15) 3_665 . ? O2 Sm1 O2 127.4(2) 12 . ? O2 Sm1 O2 84.9(2) 10_665 . ? O2 Sm1 N1 63.70(10) 11_655 2_655 ? O2 Sm1 N1 63.70(10) 2_655 2_655 ? O2 Sm1 N1 72.87(10) 3_665 2_655 ? O2 Sm1 N1 72.87(10) 12 2_655 ? O2 Sm1 N1 137.53(10) 10_665 2_655 ? O2 Sm1 N1 137.53(10) . 2_655 ? O2 Sm1 N1 137.53(10) 11_655 . ? O2 Sm1 N1 72.87(10) 2_655 . ? O2 Sm1 N1 137.53(10) 3_665 . ? O2 Sm1 N1 63.70(10) 12 . ? O2 Sm1 N1 72.87(10) 10_665 . ? O2 Sm1 N1 63.70(10) . . ? N1 Sm1 N1 120.0 2_655 . ? O2 Sm1 N1 72.87(10) 11_655 3_665 ? O2 Sm1 N1 137.53(10) 2_655 3_665 ? O2 Sm1 N1 63.70(10) 3_665 3_665 ? O2 Sm1 N1 137.53(10) 12 3_665 ? O2 Sm1 N1 63.70(10) 10_665 3_665 ? O2 Sm1 N1 72.87(10) . 3_665 ? N1 Sm1 N1 120.000(1) 2_655 3_665 ? N1 Sm1 N1 120.0 . 3_665 ? O1 Fe1 O1 180.0(3) 16 4_665 ? O1 Fe1 O1 87.6(3) 16 . ? O1 Fe1 O1 92.4(3) 4_665 . ? O1 Fe1 O1 92.4(3) 16 13_665 ? O1 Fe1 O1 87.6(3) 4_665 13_665 ? O1 Fe1 O1 180.0(2) . 13_665 ? O1 Fe1 O3 91.91(17) 16 . ? O1 Fe1 O3 88.09(17) 4_665 . ? O1 Fe1 O3 91.91(17) . . ? O1 Fe1 O3 88.09(17) 13_665 . ? O1 Fe1 O3 88.09(17) 16 13_665 ? O1 Fe1 O3 91.91(17) 4_665 13_665 ? O1 Fe1 O3 88.09(17) . 13_665 ? O1 Fe1 O3 91.91(17) 13_665 13_665 ? O3 Fe1 O3 180.0 . 13_665 ? C2 N1 C2 119.0(7) . 12 ? C2 N1 Sm1 120.5(4) . . ? C2 N1 Sm1 120.5(3) 12 . ? C1 O1 Fe1 131.5(4) . . ? C1 O2 Sm1 124.7(4) . . ? O1 C1 O2 127.0(6) . . ? O1 C1 C2 117.0(5) . . ? O2 C1 C2 116.0(5) . . ? N1 C2 C3 122.4(6) . . ? N1 C2 C1 114.7(5) . . ? C3 C2 C1 123.0(6) . . ? C4 C3 C2 117.9(6) . . ? C4 C3 H3A 121.0 . . ? C2 C3 H3A 121.0 . . ? C3 C4 C3 120.4(8) 12 . ? C3 C4 H4 119.8 12 . ? C3 C4 H4 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Sm1 N1 C2 143.0(4) 11_655 . . . ? O2 Sm1 N1 C2 -89.8(3) 2_655 . . . ? O2 Sm1 N1 C2 -37.0(4) 3_665 . . . ? O2 Sm1 N1 C2 177.4(3) 12 . . . ? O2 Sm1 N1 C2 90.2(3) 10_665 . . . ? O2 Sm1 N1 C2 -2.6(3) . . . . ? N1 Sm1 N1 C2 -134.3(3) 2_655 . . . ? N1 Sm1 N1 C2 45.7(3) 3_665 . . . ? O2 Sm1 N1 C2 -37.0(4) 11_655 . . 12 ? O2 Sm1 N1 C2 90.2(3) 2_655 . . 12 ? O2 Sm1 N1 C2 143.0(4) 3_665 . . 12 ? O2 Sm1 N1 C2 -2.6(3) 12 . . 12 ? O2 Sm1 N1 C2 -89.8(3) 10_665 . . 12 ? O2 Sm1 N1 C2 177.4(3) . . . 12 ? N1 Sm1 N1 C2 45.7(3) 2_655 . . 12 ? N1 Sm1 N1 C2 -134.3(3) 3_665 . . 12 ? O1 Fe1 O1 C1 101.0(6) 16 . . . ? O1 Fe1 O1 C1 -79.0(6) 4_665 . . . ? O1 Fe1 O1 C1 0(100) 13_665 . . . ? O3 Fe1 O1 C1 9.1(6) . . . . ? O3 Fe1 O1 C1 -170.9(6) 13_665 . . . ? O2 Sm1 O2 C1 -131.5(5) 11_655 . . . ? O2 Sm1 O2 C1 81.6(5) 2_655 . . . ? O2 Sm1 O2 C1 163.1(5) 3_665 . . . ? O2 Sm1 O2 C1 5.9(4) 12 . . . ? O2 Sm1 O2 C1 -67.5(5) 10_665 . . . ? N1 Sm1 O2 C1 112.5(5) 2_655 . . . ? N1 Sm1 O2 C1 5.9(4) . . . . ? N1 Sm1 O2 C1 -131.5(5) 3_665 . . . ? Fe1 O1 C1 O2 5.7(10) . . . . ? Fe1 O1 C1 C2 -175.9(4) . . . . ? Sm1 O2 C1 O1 170.4(5) . . . . ? Sm1 O2 C1 C2 -8.0(8) . . . . ? C2 N1 C2 C3 -0.6(5) 12 . . . ? Sm1 N1 C2 C3 179.4(5) . . . . ? C2 N1 C2 C1 -179.9(6) 12 . . . ? Sm1 N1 C2 C1 0.1(6) . . . . ? O1 C1 C2 N1 -173.8(5) . . . . ? O2 C1 C2 N1 4.8(8) . . . . ? O1 C1 C2 C3 7.0(10) . . . . ? O2 C1 C2 C3 -174.4(7) . . . . ? N1 C2 C3 C4 1.2(10) . . . . ? C1 C2 C3 C4 -179.6(5) . . . . ? C2 C3 C4 C3 -0.6(5) . . . 12 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.22 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.094 _refine_diff_density_min -1.012 _refine_diff_density_rms 0.124 # Attachment '772813.cif' data_20 _database_code_depnum_ccdc_archive 'CCDC 772813' #TrackingRef '772813.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H42 Co2 N3 O32 Tb' _chemical_formula_weight 1125.37 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' Co Co 0.3494 0.9721 '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' 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8872(18) _cell_length_b 23.960(5) _cell_length_c 18.493(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.57(3) _cell_angle_gamma 90.00 _cell_volume 3686.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6731 _cell_measurement_theta_min 2.5015 _cell_measurement_theta_max 25.0264 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 2.906 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5941 _exptl_absorpt_correction_T_max 0.8449 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26901 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6411 _reflns_number_gt 6107 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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. ISOR: the parameter to go anisotropic restraint to appointed atoms. SIMU: the parameter to set some atoms in limited range having the save shift parameters, and this parameter always is used with ISOR. Isor and Simu are applied for water molecules O20, O20', O21, O21', O22, O22', O30, O31, O32, O33 and O34. The significant residual peak are 4.98, 3.20, 2.39 and 2.27, which are close to Tb1, C19, O22 and Co2, and the distances are 0.75, 1.70, 1.43 and 0.87, respectively. ; _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^)+(0.0000P)^2^+228.4463P] 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 6411 _refine_ls_number_parameters 580 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0910 _refine_ls_wR_factor_ref 0.2012 _refine_ls_wR_factor_gt 0.1995 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.015 _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 0.4249(2) 0.90644(8) 0.42870(11) 0.0177(4) Uani 1 1 d . . . Tb1 Tb 0.04409(7) 0.69088(2) 0.07868(4) 0.01069(18) Uani 1 1 d . A . Co2 Co -0.4987(2) 0.83208(9) 0.02154(13) 0.0262(5) Uani 1 1 d . . . C1 C 0.2154(15) 0.5848(5) 0.0281(8) 0.016(3) Uani 1 1 d . A . C2 C 0.1417(15) 0.5562(5) 0.0780(8) 0.015(3) Uani 1 1 d . . . C3 C 0.1381(15) 0.4981(5) 0.0883(8) 0.016(3) Uani 1 1 d . . . H3 H 0.1929 0.4744 0.0664 0.019 Uiso 1 1 d R . . C4 C 0.0511(16) 0.4769(6) 0.1314(9) 0.020(3) Uani 1 1 d . . . C5 C -0.0200(16) 0.5133(6) 0.1685(9) 0.021(3) Uani 1 1 d . . . H5 H -0.0753 0.5001 0.1994 0.025 Uiso 1 1 d R . . C6 C -0.0055(16) 0.5699(6) 0.1575(8) 0.018(3) Uani 1 1 d . . . C7 C -0.0775(18) 0.6130(6) 0.1937(9) 0.024(3) Uani 1 1 d . A . C8 C 0.3430(15) 0.7137(5) 0.2402(8) 0.017(3) Uani 1 1 d U A . C9 C 0.2429(15) 0.7653(6) 0.2351(8) 0.018(3) Uani 1 1 d . A . C10 C 0.2893(17) 0.8078(6) 0.2904(9) 0.023(3) Uani 1 1 d . . . H10 H 0.3873 0.8060 0.3310 0.027 Uiso 1 1 d R . . C11 C 0.1854(16) 0.8535(6) 0.2830(9) 0.023(3) Uani 1 1 d . . . C12 C 0.0425(18) 0.8523(6) 0.2205(9) 0.025(3) Uani 1 1 d . . . H12 H -0.0317 0.8810 0.2137 0.030 Uiso 1 1 d R . . C13 C 0.0084(16) 0.8093(5) 0.1681(8) 0.018(3) Uani 1 1 d U A . C14 C -0.1459(17) 0.8051(6) 0.0970(9) 0.023(3) Uani 1 1 d . . . C15 C 0.1741(15) 0.7768(6) -0.0238(8) 0.017(3) Uani 1 1 d . A . C16 C 0.0249(17) 0.7550(5) -0.0851(8) 0.016(3) Uani 1 1 d . A . C17 C -0.0313(17) 0.7721(5) -0.1621(9) 0.021(3) Uani 1 1 d . . . H17 H 0.0255 0.7987 -0.1789 0.025 Uiso 1 1 d R . . C18 C -0.1710(18) 0.7501(6) -0.2127(9) 0.024(3) Uani 1 1 d . . . C19 C -0.2480(17) 0.7082(6) -0.1857(9) 0.022(3) Uani 1 1 d . . . H19 H -0.3398 0.6911 -0.2194 0.026 Uiso 1 1 d R . . C20 C -0.1877(15) 0.6926(5) -0.1096(7) 0.014(3) Uani 1 1 d . A . C21 C -0.2639(15) 0.6509(5) -0.0727(8) 0.016(3) Uani 1 1 d . A . N1 N 0.0688(13) 0.5909(4) 0.1119(7) 0.016(2) Uani 1 1 d . . . N2 N 0.1050(13) 0.7654(4) 0.1751(7) 0.017(2) Uani 1 1 d . . . N3 N -0.0517(14) 0.7147(5) -0.0594(7) 0.020(3) Uani 1 1 d . . . O1 O 0.2873(12) 0.5568(4) -0.0072(6) 0.024(2) Uani 1 1 d . . . O2 O 0.1972(11) 0.6368(4) 0.0236(6) 0.017(2) Uani 1 1 d . . . O3 O -0.136(2) 0.5998(5) 0.2430(9) 0.064(5) Uani 1 1 d . . . O4 O -0.0794(11) 0.6621(4) 0.1685(6) 0.018(2) Uani 1 1 d . . . O5 O 0.0411(12) 0.4206(4) 0.1356(7) 0.029(3) Uani 1 1 d . . . H5A H -0.0445 0.4123 0.1404 0.044 Uiso 1 1 d R . . O6 O 0.4700(11) 0.7065(4) 0.2962(6) 0.020(2) Uani 1 1 d . . . O7 O 0.2926(11) 0.6807(4) 0.1825(6) 0.020(2) Uani 1 1 d . . . O8 O -0.2485(11) 0.8422(4) 0.0868(6) 0.024(2) Uani 1 1 d . A . O9 O -0.1537(11) 0.7626(4) 0.0558(6) 0.021(2) Uani 1 1 d . A . O10 O 0.2183(11) 0.8930(4) 0.3350(7) 0.027(2) Uani 1 1 d . . . O11 O -0.1950(11) 0.6432(4) -0.0025(5) 0.019(2) Uani 1 1 d . . . O12 O -0.3920(10) 0.6279(4) -0.1145(5) 0.017(2) Uani 1 1 d . . . O13 O 0.2565(12) 0.8120(4) -0.0430(6) 0.025(2) Uani 1 1 d . . . O14 O 0.2008(11) 0.7570(4) 0.0422(6) 0.022(2) Uani 1 1 d . . . O15 O -0.2360(12) 0.7659(4) -0.2863(6) 0.024(2) Uani 1 1 d . . . H15 H -0.1725 0.7858 -0.2976 0.036 Uiso 1 1 d R . . O16 O 0.6179(15) 0.9261(6) 0.5336(8) 0.053(4) Uani 1 1 d U . . O17 O 0.4445(14) 0.9840(4) 0.3875(7) 0.036(3) Uani 1 1 d . . . O18 O 0.4203(18) 0.8291(5) 0.4746(9) 0.059(5) Uani 1 1 d . . . O19 O -0.4430(11) 0.7723(4) -0.0486(6) 0.024(2) Uani 1 1 d . A . O20 O -0.501(3) 0.7855(16) 0.1101(16) 0.034(6) Uani 0.50(5) 1 d PU A 1 O20' O -0.485(3) 0.7599(15) 0.0931(15) 0.029(6) Uani 0.50(5) 1 d PU A 2 O21 O -0.554(3) 0.8977(12) 0.0828(16) 0.052(7) Uani 0.62(4) 1 d PU A 1 O21' O -0.577(4) 0.8694(19) 0.103(2) 0.040(8) Uani 0.38(4) 1 d PU A 2 O22 O -0.516(2) 0.8994(9) -0.0479(14) 0.041(6) Uani 0.69(5) 1 d PU A 1 O22' O -0.489(5) 0.884(2) -0.079(3) 0.041(9) Uani 0.31(5) 1 d PU A 2 O23 O 0.605(2) 0.9951(6) 0.7617(8) 0.059(4) Uani 1 1 d . . . O24 O 0.594(2) 0.9226(6) 0.2409(9) 0.067(5) Uani 1 1 d . . . O25 O 0.5205(18) 0.8877(7) 0.6581(10) 0.078(6) Uani 1 1 d . . . O26 O 0.910(6) 0.0126(16) 0.857(2) 0.25(2) Uani 1 1 d . B 1 O27 O 0.778(3) 0.5275(17) 0.6664(16) 0.191(17) Uani 1 1 d . . . O28 O 0.638(4) 0.8884(11) 0.8339(17) 0.177(15) Uani 1 1 d . . . O29 O 0.257(5) 0.9033(12) 0.8083(17) 0.080(12) Uani 0.50 1 d P . . O30 O 0.036(4) 0.4077(14) 0.605(2) 0.176(13) Uani 1 1 d U . . O31 O 0.827(4) 0.4415(15) 0.606(2) 0.074(9) Uani 0.50 1 d PU . . O32 O 0.643(5) 0.5011(17) 0.515(2) 0.088(11) Uani 0.50 1 d PU C 1 O33 O 0.853(5) 0.0703(18) 0.957(2) 0.224(17) Uani 1 1 d U D 2 O34 O 0.778(8) 0.935(3) 0.949(4) 0.17(2) Uani 0.50 1 d PU E 2 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 0.0142(9) 0.0185(9) 0.0248(10) -0.0043(8) 0.0125(8) -0.0006(7) Tb1 0.0084(3) 0.0083(3) 0.0175(3) 0.0004(2) 0.0072(2) 0.0006(2) Co2 0.0140(9) 0.0261(11) 0.0353(12) -0.0061(9) 0.0048(9) -0.0019(8) C1 0.007(6) 0.017(7) 0.025(7) -0.003(6) 0.006(5) 0.002(5) C2 0.011(6) 0.012(6) 0.019(7) -0.002(5) 0.003(5) -0.002(5) C3 0.011(6) 0.016(7) 0.020(7) 0.001(5) 0.006(5) -0.002(5) C4 0.014(7) 0.015(7) 0.033(8) 0.002(6) 0.010(6) -0.005(5) C5 0.018(7) 0.022(7) 0.029(8) 0.004(6) 0.018(6) 0.004(6) C6 0.021(7) 0.016(7) 0.023(7) 0.009(6) 0.013(6) 0.004(5) C7 0.033(8) 0.024(8) 0.025(8) -0.002(6) 0.022(7) -0.005(6) C8 0.010(5) 0.016(6) 0.027(6) -0.002(5) 0.010(5) -0.002(4) C9 0.007(6) 0.022(7) 0.022(7) 0.001(6) 0.002(5) 0.003(5) C10 0.020(7) 0.024(7) 0.027(8) -0.009(6) 0.012(6) -0.001(6) C11 0.015(7) 0.024(7) 0.034(9) -0.007(6) 0.013(6) 0.000(6) C12 0.026(8) 0.023(7) 0.034(9) -0.014(7) 0.021(7) -0.005(6) C13 0.016(6) 0.010(5) 0.028(6) -0.006(5) 0.007(5) 0.002(5) C14 0.021(7) 0.016(7) 0.036(9) -0.003(6) 0.017(7) -0.001(6) C15 0.006(6) 0.021(7) 0.024(8) 0.001(6) 0.004(5) -0.001(5) C16 0.025(7) 0.010(6) 0.016(7) 0.006(5) 0.011(6) 0.006(5) C17 0.026(8) 0.010(6) 0.033(8) -0.002(6) 0.020(7) 0.004(5) C18 0.030(8) 0.021(7) 0.028(8) 0.008(6) 0.020(7) 0.003(6) C19 0.022(7) 0.015(7) 0.033(8) -0.003(6) 0.016(6) -0.002(6) C20 0.017(6) 0.013(6) 0.015(7) 0.002(5) 0.011(5) 0.000(5) C21 0.010(6) 0.011(6) 0.029(8) -0.002(6) 0.012(6) 0.002(5) N1 0.013(5) 0.007(5) 0.029(6) 0.004(5) 0.009(5) 0.002(4) N2 0.020(6) 0.009(5) 0.025(6) -0.003(5) 0.012(5) 0.002(4) N3 0.020(6) 0.018(6) 0.027(7) -0.006(5) 0.016(5) -0.008(5) O1 0.028(5) 0.019(5) 0.037(6) 0.001(4) 0.024(5) 0.001(4) O2 0.018(5) 0.011(4) 0.027(5) 0.003(4) 0.014(4) 0.004(4) O3 0.133(14) 0.021(6) 0.081(11) 0.016(7) 0.091(11) 0.012(8) O4 0.026(5) 0.008(4) 0.026(5) -0.003(4) 0.016(4) 0.003(4) O5 0.023(5) 0.013(5) 0.061(8) 0.005(5) 0.025(5) 0.004(4) O6 0.014(5) 0.021(5) 0.025(5) -0.001(4) 0.005(4) 0.005(4) O7 0.020(5) 0.017(5) 0.021(5) -0.008(4) 0.004(4) 0.003(4) O8 0.013(5) 0.010(5) 0.040(6) -0.002(4) 0.001(4) 0.005(4) O9 0.018(5) 0.017(5) 0.032(6) -0.005(4) 0.013(4) -0.002(4) O10 0.013(5) 0.018(5) 0.046(7) -0.016(5) 0.006(5) 0.003(4) O11 0.017(5) 0.020(5) 0.019(5) 0.002(4) 0.007(4) -0.004(4) O12 0.011(4) 0.024(5) 0.017(5) 0.003(4) 0.006(4) 0.004(4) O13 0.019(5) 0.022(5) 0.034(6) -0.001(5) 0.010(5) -0.003(4) O14 0.016(5) 0.027(5) 0.021(5) 0.007(4) 0.006(4) -0.006(4) O15 0.025(5) 0.024(5) 0.021(5) 0.006(4) 0.008(4) -0.002(4) O16 0.036(6) 0.068(7) 0.040(6) -0.026(6) -0.004(5) 0.018(5) O17 0.038(7) 0.022(6) 0.052(8) -0.005(5) 0.023(6) -0.012(5) O18 0.087(11) 0.032(7) 0.097(12) 0.029(7) 0.082(10) 0.031(7) O19 0.011(5) 0.039(6) 0.020(5) 0.005(4) 0.001(4) 0.007(4) O20 0.031(8) 0.036(10) 0.037(9) 0.001(8) 0.014(7) -0.008(7) O20' 0.028(8) 0.030(10) 0.028(9) 0.006(7) 0.010(7) -0.004(7) O21 0.045(9) 0.043(10) 0.059(9) -0.006(8) 0.008(7) 0.001(7) O21' 0.036(10) 0.045(11) 0.040(11) 0.002(8) 0.013(8) 0.002(8) O22 0.046(8) 0.038(8) 0.041(9) 0.003(7) 0.016(6) -0.005(6) O22' 0.041(11) 0.040(11) 0.045(12) 0.003(9) 0.021(8) 0.001(8) O23 0.083(11) 0.040(8) 0.039(8) -0.004(6) 0.004(8) 0.002(7) O24 0.082(11) 0.052(9) 0.045(9) -0.004(7) -0.004(8) 0.012(8) O25 0.049(9) 0.085(12) 0.070(11) 0.023(9) -0.018(8) -0.030(9) O26 0.31(5) 0.16(3) 0.20(4) -0.06(3) 0.00(4) 0.07(3) O27 0.098(18) 0.34(5) 0.13(2) -0.14(3) 0.030(17) -0.11(2) O28 0.24(4) 0.11(2) 0.15(3) 0.014(19) 0.03(2) -0.11(2) O29 0.14(3) 0.039(17) 0.035(16) -0.005(13) 0.004(19) 0.020(19) O30 0.177(15) 0.168(15) 0.172(15) 0.001(10) 0.049(10) 0.002(10) O31 0.075(12) 0.071(12) 0.077(13) 0.002(9) 0.026(9) -0.007(9) O32 0.091(14) 0.085(14) 0.087(14) -0.006(9) 0.029(10) 0.002(9) O33 0.224(19) 0.24(2) 0.218(19) -0.004(10) 0.085(11) 0.017(10) O34 0.17(3) 0.17(3) 0.17(3) -0.004(10) 0.060(13) 0.000(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 Co1 O17 2.039(11) . ? Co1 O18 2.045(12) . ? Co1 O10 2.060(10) . ? Co1 O16 2.143(12) . ? Co1 O1 2.167(9) 4_576 ? Co1 O12 2.208(9) 4_676 ? Tb1 O2 2.354(9) . ? Tb1 O14 2.359(9) . ? Tb1 O7 2.375(10) . ? Tb1 O9 2.388(9) . ? Tb1 O4 2.392(9) . ? Tb1 O11 2.415(9) . ? Tb1 N2 2.446(11) . ? Tb1 N3 2.459(12) . ? Tb1 N1 2.463(10) . ? Co2 O20 1.99(3) . ? Co2 O22 2.033(19) . ? Co2 O21' 2.07(3) . ? Co2 O21 2.09(2) . ? Co2 O19 2.104(11) . ? Co2 O13 2.136(10) 1_455 ? Co2 O8 2.139(10) . ? Co2 O20' 2.15(3) . ? Co2 O22' 2.27(5) . ? C1 O1 1.256(16) . ? C1 O2 1.256(16) . ? C1 C2 1.475(18) . ? C2 N1 1.338(17) . ? C2 C3 1.407(18) . ? C3 C4 1.387(18) . ? C3 H3 0.9301 . ? C4 O5 1.356(16) . ? C4 C5 1.392(19) . ? C5 C6 1.383(19) . ? C5 H5 0.9300 . ? C6 N1 1.339(17) . ? C6 C7 1.493(19) . ? C7 O3 1.235(18) . ? C7 O4 1.263(17) . ? C8 O6 1.246(17) . ? C8 O7 1.277(16) . ? C8 C9 1.507(18) . ? C9 N2 1.333(18) . ? C9 C10 1.40(2) . ? C10 C11 1.41(2) . ? C10 H10 0.9300 . ? C11 O10 1.306(17) . ? C11 C12 1.39(2) . ? C12 C13 1.373(19) . ? C12 H12 0.9301 . ? C13 N2 1.335(17) . ? C13 C14 1.53(2) . ? C14 O8 1.240(17) . ? C14 O9 1.258(17) . ? C15 O13 1.247(16) . ? C15 O14 1.252(17) . ? C15 C16 1.503(19) . ? C16 N3 1.359(17) . ? C16 C17 1.39(2) . ? C17 C18 1.37(2) . ? C17 H17 0.9301 . ? C18 O15 1.334(18) . ? C18 C19 1.400(19) . ? C19 C20 1.37(2) . ? C19 H19 0.9300 . ? C20 N3 1.348(18) . ? C20 C21 1.499(17) . ? C21 O11 1.239(17) . ? C21 O12 1.257(16) . ? O1 Co1 2.167(9) 4_575 ? O5 H5A 0.8200 . ? O12 Co1 2.208(9) 4_475 ? O13 Co2 2.136(10) 1_655 ? O15 H15 0.8200 . ? 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 O17 Co1 O18 176.3(6) . . ? O17 Co1 O10 89.8(5) . . ? O18 Co1 O10 93.8(6) . . ? O17 Co1 O16 89.5(6) . . ? O18 Co1 O16 87.1(7) . . ? O10 Co1 O16 171.8(4) . . ? O17 Co1 O1 88.4(4) . 4_576 ? O18 Co1 O1 92.5(4) . 4_576 ? O10 Co1 O1 90.9(4) . 4_576 ? O16 Co1 O1 80.9(5) . 4_576 ? O17 Co1 O12 92.0(4) . 4_676 ? O18 Co1 O12 86.4(4) . 4_676 ? O10 Co1 O12 100.9(4) . 4_676 ? O16 Co1 O12 87.3(4) . 4_676 ? O1 Co1 O12 168.1(4) 4_576 4_676 ? O2 Tb1 O14 75.9(3) . . ? O2 Tb1 O7 77.2(3) . . ? O14 Tb1 O7 79.9(3) . . ? O2 Tb1 O9 145.2(3) . . ? O14 Tb1 O9 86.4(3) . . ? O7 Tb1 O9 129.4(3) . . ? O2 Tb1 O4 128.2(3) . . ? O14 Tb1 O4 148.6(3) . . ? O7 Tb1 O4 86.1(3) . . ? O9 Tb1 O4 80.9(3) . . ? O2 Tb1 O11 89.2(3) . . ? O14 Tb1 O11 128.2(3) . . ? O7 Tb1 O11 145.0(3) . . ? O9 Tb1 O11 78.4(3) . . ? O4 Tb1 O11 77.1(3) . . ? O2 Tb1 N2 134.7(3) . . ? O14 Tb1 N2 73.5(4) . . ? O7 Tb1 N2 65.2(3) . . ? O9 Tb1 N2 64.2(4) . . ? O4 Tb1 N2 75.0(3) . . ? O11 Tb1 N2 136.0(3) . . ? O2 Tb1 N3 73.8(4) . . ? O14 Tb1 N3 64.6(3) . . ? O7 Tb1 N3 138.4(4) . . ? O9 Tb1 N3 71.6(4) . . ? O4 Tb1 N3 135.5(4) . . ? O11 Tb1 N3 63.7(3) . . ? N2 Tb1 N3 119.6(4) . . ? O2 Tb1 N1 63.8(3) . . ? O14 Tb1 N1 135.6(3) . . ? O7 Tb1 N1 73.9(3) . . ? O9 Tb1 N1 137.7(3) . . ? O4 Tb1 N1 64.5(3) . . ? O11 Tb1 N1 71.1(3) . . ? N2 Tb1 N1 123.4(4) . . ? N3 Tb1 N1 116.9(4) . . ? O20 Co2 O22 161.0(14) . . ? O20 Co2 O21' 62.7(17) . . ? O22 Co2 O21' 98.4(15) . . ? O20 Co2 O21 84.5(15) . . ? O22 Co2 O21 76.5(12) . . ? O21' Co2 O21 23.1(10) . . ? O20 Co2 O19 101.5(12) . . ? O22 Co2 O19 97.6(9) . . ? O21' Co2 O19 162.6(13) . . ? O21 Co2 O19 174.1(10) . . ? O20 Co2 O13 91.7(8) . 1_455 ? O22 Co2 O13 89.5(6) . 1_455 ? O21' Co2 O13 88.0(10) . 1_455 ? O21 Co2 O13 95.0(7) . 1_455 ? O19 Co2 O13 85.2(4) . 1_455 ? O20 Co2 O8 84.8(8) . . ? O22 Co2 O8 95.6(6) . . ? O21' Co2 O8 95.3(10) . . ? O21 Co2 O8 90.2(7) . . ? O19 Co2 O8 90.1(4) . . ? O13 Co2 O8 173.5(4) 1_455 . ? O20 Co2 O20' 19.7(8) . . ? O22 Co2 O20' 178.8(10) . . ? O21' Co2 O20' 82.1(16) . . ? O21 Co2 O20' 104.2(14) . . ? O19 Co2 O20' 81.8(10) . . ? O13 Co2 O20' 89.5(7) 1_455 . ? O8 Co2 O20' 85.4(7) . . ? O20 Co2 O22' 178.2(16) . . ? O22 Co2 O22' 20.3(11) . . ? O21' Co2 O22' 118.7(19) . . ? O21 Co2 O22' 96.7(17) . . ? O19 Co2 O22' 77.3(15) . . ? O13 Co2 O22' 89.4(11) 1_455 . ? O8 Co2 O22' 94.0(11) . . ? O20' Co2 O22' 159.1(18) . . ? O1 C1 O2 125.0(12) . . ? O1 C1 C2 119.8(12) . . ? O2 C1 C2 115.2(11) . . ? N1 C2 C3 120.9(12) . . ? N1 C2 C1 113.6(11) . . ? C3 C2 C1 125.5(12) . . ? C4 C3 C2 119.0(12) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.3 . . ? O5 C4 C3 117.3(13) . . ? O5 C4 C5 123.1(12) . . ? C3 C4 C5 119.6(13) . . ? C6 C5 C4 117.4(12) . . ? C6 C5 H5 121.3 . . ? C4 C5 H5 121.3 . . ? N1 C6 C5 123.6(12) . . ? N1 C6 C7 113.9(11) . . ? C5 C6 C7 122.4(12) . . ? O3 C7 O4 123.8(13) . . ? O3 C7 C6 120.6(13) . . ? O4 C7 C6 115.6(11) . . ? O6 C8 O7 124.0(12) . . ? O6 C8 C9 120.5(12) . . ? O7 C8 C9 115.4(12) . . ? N2 C9 C10 123.8(13) . . ? N2 C9 C8 113.8(12) . . ? C10 C9 C8 122.4(12) . . ? C9 C10 C11 118.7(14) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? O10 C11 C12 122.1(13) . . ? O10 C11 C10 121.5(14) . . ? C12 C11 C10 116.2(13) . . ? C13 C12 C11 121.0(14) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.7 . . ? N2 C13 C12 123.2(13) . . ? N2 C13 C14 112.5(11) . . ? C12 C13 C14 124.3(13) . . ? O8 C14 O9 127.3(14) . . ? O8 C14 C13 118.2(12) . . ? O9 C14 C13 114.5(12) . . ? O13 C15 O14 127.2(13) . . ? O13 C15 C16 118.1(12) . . ? O14 C15 C16 114.7(11) . . ? N3 C16 C17 121.5(13) . . ? N3 C16 C15 113.6(11) . . ? C17 C16 C15 124.9(12) . . ? C18 C17 C16 119.8(13) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? O15 C18 C17 123.4(13) . . ? O15 C18 C19 118.5(14) . . ? C17 C18 C19 118.1(14) . . ? C20 C19 C18 119.8(14) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.1 . . ? N3 C20 C19 122.1(12) . . ? N3 C20 C21 112.9(11) . . ? C19 C20 C21 125.0(12) . . ? O11 C21 O12 125.9(12) . . ? O11 C21 C20 116.2(11) . . ? O12 C21 C20 117.9(12) . . ? C2 N1 C6 119.2(11) . . ? C2 N1 Tb1 120.2(8) . . ? C6 N1 Tb1 120.2(8) . . ? C9 N2 C13 117.0(12) . . ? C9 N2 Tb1 120.6(9) . . ? C13 N2 Tb1 122.3(9) . . ? C20 N3 C16 118.5(12) . . ? C20 N3 Tb1 121.5(8) . . ? C16 N3 Tb1 119.7(9) . . ? C1 O1 Co1 123.7(9) . 4_575 ? C1 O2 Tb1 126.8(8) . . ? C7 O4 Tb1 125.1(8) . . ? C4 O5 H5A 109.2 . . ? C8 O7 Tb1 124.5(8) . . ? C14 O8 Co2 124.6(9) . . ? C14 O9 Tb1 126.5(9) . . ? C11 O10 Co1 129.4(9) . . ? C21 O11 Tb1 125.7(8) . . ? C21 O12 Co1 124.3(8) . 4_475 ? C15 O13 Co2 125.3(9) . 1_655 ? C15 O14 Tb1 127.2(8) . . ? C18 O15 H15 109.6 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 4.983 _refine_diff_density_min -3.504 _refine_diff_density_rms 0.283 # Attachment '772814.cif' data_24 _database_code_depnum_ccdc_archive 'CCDC 772814' #TrackingRef '772814.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H40 Co2 N3 O31 Tm' _chemical_formula_weight 1117.35 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8971(18) _cell_length_b 23.867(5) _cell_length_c 18.486(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.72(3) _cell_angle_gamma 90.00 _cell_volume 3671.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 7477 _cell_measurement_theta_min 2.5057 _cell_measurement_theta_max 25.0264 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.021 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 3.405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5492 _exptl_absorpt_correction_T_max 0.5492 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27158 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6431 _reflns_number_gt 6271 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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. ISOR: the parameter to go anisotropic restraint to appointed atoms. SIMU: the parameter to set some atoms in limited range having the save shift parameters, and this parameter always is used with ISOR. Isor and Simu are applied for water molecule o16, o16', o17, o17', o18, o19, o19', o20, o21, o22, o22', o31 and o31'. ; _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^)+(0.0244P)^2^+36.7671P] 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 6431 _refine_ls_number_parameters 591 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.002 _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 Tm1 Tm 0.04471(3) 0.808812(11) 0.079320(15) 0.01079(10) Uani 1 1 d . A . Co1 Co -0.57430(10) 0.90566(4) -0.07048(5) 0.01398(19) Uani 1 1 d . . . Co2 Co 0.50138(11) 0.66851(4) 0.02304(5) 0.0219(2) Uani 1 1 d . . . C1 C 0.1737(7) 0.7229(3) -0.0227(4) 0.0141(13) Uani 1 1 d . . . C2 C 0.0243(7) 0.7450(3) -0.0845(4) 0.0123(13) Uani 1 1 d . A . C3 C -0.0282(8) 0.7269(3) -0.1606(3) 0.0136(13) Uani 1 1 d . . . H3 H 0.0292 0.7004 -0.1771 0.016 Uiso 1 1 calc R B . C4 C -0.1696(8) 0.7498(3) -0.2112(3) 0.0139(13) Uani 1 1 d . B . C5 C -0.2487(7) 0.7908(3) -0.1853(4) 0.0141(13) Uani 1 1 d . . . H5 H -0.3418 0.8074 -0.2188 0.017 Uiso 1 1 calc R B . C6 C -0.1856(7) 0.8064(2) -0.1082(3) 0.0110(13) Uani 1 1 d . A . C7 C -0.2625(7) 0.8483(3) -0.0723(3) 0.0117(13) Uani 1 1 d . . . C8 C 0.2152(7) 0.9145(3) 0.0281(3) 0.0133(13) Uani 1 1 d . A . C9 C 0.1394(7) 0.9444(3) 0.0783(3) 0.0114(13) Uani 1 1 d . A . C10 C 0.1387(7) 1.0015(3) 0.0875(4) 0.0145(13) Uani 1 1 d . . . H10 H 0.1952 1.0249 0.0659 0.017 Uiso 1 1 calc R . . C11 C 0.0519(8) 1.0233(3) 0.1296(4) 0.0170(14) Uani 1 1 d . . . C12 C -0.0190(8) 0.9870(3) 0.1668(4) 0.0205(15) Uani 1 1 d . . . H12 H -0.0740 1.0007 0.1975 0.025 Uiso 1 1 calc R . . C13 C -0.0056(7) 0.9300(3) 0.1572(4) 0.0142(13) Uani 1 1 d . A . C14 C -0.0744(9) 0.8871(3) 0.1948(4) 0.0221(15) Uani 1 1 d . A . C15 C 0.3446(8) 0.7861(3) 0.2392(4) 0.0175(14) Uani 1 1 d . A . C16 C 0.2449(7) 0.7352(3) 0.2354(4) 0.0151(13) Uani 1 1 d . A . C17 C 0.2911(8) 0.6929(3) 0.2898(4) 0.0197(15) Uani 1 1 d . . . H17 H 0.3906 0.6945 0.3296 0.024 Uiso 1 1 calc R . . C18 C 0.1869(8) 0.6475(3) 0.2848(4) 0.0190(14) Uani 1 1 d . . . C19 C 0.0411(8) 0.6474(3) 0.2208(4) 0.0178(14) Uani 1 1 d . . . H19 H -0.0319 0.6182 0.2137 0.021 Uiso 1 1 calc R . . C20 C 0.0089(7) 0.6913(3) 0.1692(4) 0.0149(13) Uani 1 1 d . A . C21 C -0.1437(8) 0.6950(3) 0.0994(4) 0.0151(14) Uani 1 1 d . A . N1 N -0.0510(6) 0.7840(2) -0.0585(3) 0.0122(11) Uani 1 1 d . . . N2 N 0.0682(6) 0.9086(2) 0.1120(3) 0.0116(11) Uani 1 1 d . . . N3 N 0.1057(6) 0.7345(2) 0.1753(3) 0.0129(11) Uani 1 1 d . . . O1 O 0.2582(5) 0.68848(19) -0.0415(3) 0.0179(10) Uani 1 1 d . B . O2 O 0.2013(5) 0.74243(19) 0.0442(2) 0.0161(10) Uani 1 1 d . A . O3 O -0.2314(5) 0.73298(19) -0.2852(2) 0.0178(10) Uani 1 1 d . . . H3A H -0.3098 0.7517 -0.3087 0.021 Uiso 1 1 d R B . O4 O -0.3901(5) 0.87200(18) -0.1131(2) 0.0143(9) Uani 1 1 d . A . O5 O -0.1925(5) 0.85603(18) -0.0009(2) 0.0124(9) Uani 1 1 d . A . O6 O 0.1970(5) 0.86222(18) 0.0242(2) 0.0154(10) Uani 1 1 d . . . O7 O 0.2879(6) 0.94217(19) -0.0068(3) 0.0187(10) Uani 1 1 d . . . O8 O 0.0393(6) 1.07934(19) 0.1342(3) 0.0219(11) Uani 1 1 d . . . H8A H -0.0462 1.0872 0.1425 0.026 Uiso 1 1 d R . . O9 O -0.1300(9) 0.9001(2) 0.2439(4) 0.0513(19) Uani 1 1 d . . . O10 O -0.0757(5) 0.83714(18) 0.1693(2) 0.0139(9) Uani 1 1 d . . . O11 O 0.2931(5) 0.81944(19) 0.1823(3) 0.0183(10) Uani 1 1 d . . . O12 O 0.4701(5) 0.7940(2) 0.2961(3) 0.0200(10) Uani 1 1 d . . . O13 O 0.2206(5) 0.60720(19) 0.3357(3) 0.0226(11) Uani 1 1 d . . . O14 O -0.1539(5) 0.73731(18) 0.0568(2) 0.0162(10) Uani 1 1 d . . . O15 O -0.2482(5) 0.65820(19) 0.0881(3) 0.0205(10) Uani 1 1 d . . . O16 O -0.6076(17) 0.8244(4) -0.0385(8) 0.017(3) Uani 0.59(3) 1 d PU A 1 O16' O -0.551(3) 0.8314(6) -0.0112(12) 0.019(3) Uani 0.41(3) 1 d PU A 2 O17 O -0.361(2) 0.9397(11) 0.0251(11) 0.014(4) Uani 0.29(3) 1 d PU A 1 O17' O -0.3943(11) 0.9177(5) 0.0380(5) 0.019(2) Uani 0.71(3) 1 d PU A 2 O19 O 0.4277(16) 0.6275(9) 0.1025(8) 0.033(3) Uani 0.47(3) 1 d PU B 1 O19' O 0.4467(16) 0.6032(8) 0.0853(8) 0.038(3) Uani 0.53(3) 1 d PU B 2 O22 O 0.5064(16) 0.7166(9) 0.1089(9) 0.025(3) Uani 0.43(3) 1 d PU B 1 O22' O 0.5121(11) 0.7416(6) 0.0919(6) 0.021(3) Uani 0.57(3) 1 d PU B 2 O18 O -0.5500(6) 0.9843(2) -0.1082(3) 0.0275(12) Uani 1 1 d U A . O20 O 0.4879(8) 0.6017(3) -0.0504(4) 0.0553(18) Uani 1 1 d U B . O21 O 0.5593(5) 0.7267(2) -0.0494(3) 0.0208(10) Uani 1 1 d U B . O23 O 0.5246(8) 0.8858(3) 0.1582(4) 0.061(2) Uani 1 1 d . . . O24 O 0.5924(9) 0.5771(3) 0.2400(4) 0.0563(19) Uani 1 1 d . . . O25 O 0.3852(9) 0.0051(3) 0.7374(4) 0.0506(17) Uani 1 1 d . . . O26 O 0.6405(14) 0.6107(4) 0.8348(6) 0.133(5) Uani 1 1 d . . . O27 O 0.0717(17) 0.5146(6) 0.1450(8) 0.147(5) Uani 1 1 d . . . O28 O 0.2229(12) 0.0288(7) 0.3337(6) 0.146(6) Uani 1 1 d . . . O29 O 0.9547(17) 0.5939(6) 0.9029(7) 0.053(3) Uani 0.50 1 d P . . O30 O 0.2515(18) 0.5981(6) 0.8072(8) 0.064(4) Uani 0.50 1 d P . . O31 O 0.167(2) 0.5588(8) 0.0396(10) 0.099(5) Uani 0.595(16) 1 d PU C 1 O31' O 0.110(3) 0.6002(12) 0.0436(15) 0.099(5) Uani 0.405(16) 1 d PU C 2 O32 O 0.376(3) 0.0014(6) 0.4843(8) 0.102(8) Uani 0.50 1 d P . . O33 O 0.1625(18) 0.5575(6) 0.8857(9) 0.068(4) Uani 0.50 1 d P . . 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 Tm1 0.01074(15) 0.01089(16) 0.01068(15) 0.00073(10) 0.00371(11) 0.00035(10) Co1 0.0136(4) 0.0147(5) 0.0146(4) -0.0021(3) 0.0062(3) 0.0014(3) Co2 0.0128(5) 0.0275(5) 0.0213(5) 0.0051(4) 0.0009(4) 0.0010(4) C1 0.014(3) 0.010(3) 0.019(3) -0.004(3) 0.006(3) -0.002(3) C2 0.011(3) 0.012(3) 0.017(3) 0.003(2) 0.007(3) 0.002(2) C3 0.017(3) 0.013(3) 0.013(3) -0.002(2) 0.007(3) -0.002(3) C4 0.017(3) 0.015(3) 0.010(3) -0.001(2) 0.005(3) 0.002(3) C5 0.012(3) 0.015(3) 0.014(3) -0.002(3) 0.002(2) 0.001(3) C6 0.012(3) 0.008(3) 0.014(3) -0.005(2) 0.006(3) -0.005(2) C7 0.013(3) 0.013(3) 0.013(3) 0.003(2) 0.008(3) 0.002(3) C8 0.011(3) 0.017(3) 0.013(3) 0.006(3) 0.004(2) 0.002(3) C9 0.011(3) 0.014(3) 0.008(3) 0.002(2) 0.002(2) 0.000(2) C10 0.011(3) 0.015(3) 0.014(3) 0.001(3) 0.001(3) -0.001(3) C11 0.013(3) 0.014(3) 0.021(3) 0.000(3) 0.002(3) -0.002(3) C12 0.022(4) 0.022(4) 0.023(4) -0.005(3) 0.014(3) -0.001(3) C13 0.015(3) 0.013(3) 0.015(3) -0.005(3) 0.005(3) -0.001(3) C14 0.031(4) 0.022(4) 0.020(4) -0.003(3) 0.017(3) -0.003(3) C15 0.014(3) 0.020(4) 0.019(3) 0.001(3) 0.006(3) 0.000(3) C16 0.011(3) 0.016(3) 0.017(3) 0.000(3) 0.002(3) 0.001(3) C17 0.014(3) 0.023(4) 0.020(3) 0.007(3) 0.005(3) -0.002(3) C18 0.014(3) 0.016(4) 0.027(4) 0.009(3) 0.009(3) -0.001(3) C19 0.012(3) 0.017(3) 0.025(4) 0.003(3) 0.006(3) 0.002(3) C20 0.009(3) 0.015(3) 0.021(3) 0.006(3) 0.005(3) 0.000(3) C21 0.014(3) 0.013(3) 0.016(3) -0.001(3) 0.002(3) -0.001(3) N1 0.010(3) 0.017(3) 0.011(3) 0.000(2) 0.005(2) -0.001(2) N2 0.012(3) 0.009(3) 0.015(3) -0.002(2) 0.006(2) 0.004(2) N3 0.011(3) 0.012(3) 0.016(3) -0.001(2) 0.005(2) -0.003(2) O1 0.014(2) 0.017(2) 0.018(2) -0.0030(19) 0.0005(19) 0.0032(19) O2 0.014(2) 0.022(3) 0.011(2) -0.0021(18) 0.0031(18) 0.0056(19) O3 0.018(2) 0.022(3) 0.010(2) -0.0021(19) 0.0004(18) 0.0071(19) O4 0.015(2) 0.017(2) 0.010(2) -0.0005(18) 0.0027(18) 0.0015(19) O5 0.011(2) 0.017(2) 0.007(2) -0.0020(17) 0.0017(17) 0.0017(18) O6 0.018(2) 0.013(2) 0.019(2) 0.0006(18) 0.0099(19) -0.0022(18) O7 0.024(3) 0.014(2) 0.026(3) 0.002(2) 0.019(2) 0.003(2) O8 0.019(2) 0.010(2) 0.037(3) -0.003(2) 0.011(2) -0.0010(19) O9 0.099(6) 0.025(3) 0.062(4) -0.013(3) 0.068(4) -0.015(3) O10 0.015(2) 0.014(2) 0.014(2) 0.0001(18) 0.0071(18) -0.0022(18) O11 0.013(2) 0.022(3) 0.016(2) 0.0105(19) 0.0008(19) -0.0028(19) O12 0.015(2) 0.023(3) 0.018(2) 0.004(2) 0.002(2) -0.004(2) O13 0.014(2) 0.016(3) 0.032(3) 0.012(2) 0.001(2) -0.0038(19) O14 0.015(2) 0.014(2) 0.018(2) 0.0015(19) 0.0041(18) -0.0038(18) O15 0.011(2) 0.015(2) 0.031(3) 0.007(2) 0.001(2) -0.0015(19) O16 0.017(4) 0.017(4) 0.018(4) 0.003(3) 0.006(4) 0.000(3) O16' 0.019(5) 0.021(5) 0.019(5) 0.000(4) 0.008(4) 0.000(4) O17 0.012(5) 0.015(6) 0.015(5) -0.001(4) 0.003(4) 0.002(4) O17' 0.019(3) 0.020(4) 0.018(3) 0.000(3) 0.005(2) 0.005(3) O19 0.029(4) 0.035(5) 0.032(5) 0.001(4) 0.009(3) -0.003(4) O19' 0.037(4) 0.033(5) 0.039(5) 0.004(4) 0.006(3) -0.001(4) O22 0.022(4) 0.023(5) 0.025(5) -0.003(4) 0.005(3) -0.001(4) O22' 0.019(4) 0.021(5) 0.021(4) -0.006(3) 0.005(3) 0.001(3) O18 0.030(3) 0.019(2) 0.036(3) -0.001(2) 0.015(2) -0.003(2) O20 0.051(3) 0.040(3) 0.063(3) -0.018(3) 0.007(3) 0.007(3) O21 0.016(2) 0.026(2) 0.019(2) -0.0011(19) 0.0045(18) -0.0006(19) O23 0.050(4) 0.069(5) 0.062(5) 0.018(4) 0.016(4) -0.014(4) O24 0.070(5) 0.043(4) 0.038(4) 0.003(3) -0.003(3) -0.010(3) O25 0.070(5) 0.047(4) 0.038(4) 0.004(3) 0.023(3) 0.002(3) O26 0.150(10) 0.083(7) 0.119(9) -0.014(6) -0.011(7) 0.082(7) O27 0.156(12) 0.158(12) 0.121(10) 0.028(9) 0.043(9) 0.040(10) O28 0.065(6) 0.273(17) 0.095(8) 0.090(9) 0.022(6) 0.039(8) O29 0.068(9) 0.046(8) 0.040(7) 0.013(6) 0.015(7) 0.005(7) O30 0.067(10) 0.037(8) 0.057(9) 0.016(7) -0.014(7) -0.014(7) O31 0.096(6) 0.101(6) 0.100(6) -0.003(4) 0.034(4) -0.003(4) O31' 0.097(6) 0.101(6) 0.101(6) 0.003(4) 0.037(4) -0.001(4) O32 0.18(2) 0.039(9) 0.036(8) -0.002(7) -0.026(10) -0.003(11) O33 0.062(10) 0.065(10) 0.062(9) 0.005(8) 0.001(8) -0.018(8) _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 Tm1 O6 2.340(4) . ? Tm1 O2 2.348(4) . ? Tm1 O11 2.365(4) . ? Tm1 O10 2.373(4) . ? Tm1 O14 2.385(4) . ? Tm1 O5 2.389(4) . ? Tm1 N3 2.431(5) . ? Tm1 N2 2.448(5) . ? Tm1 N1 2.456(5) . ? Co1 O18 2.041(5) . ? Co1 O13 2.048(5) 4_475 ? Co1 O16' 2.057(14) . ? Co1 O16 2.079(9) . ? Co1 O17' 2.096(7) . ? Co1 O7 2.161(4) 1_455 ? Co1 O4 2.206(4) . ? Co1 O17 2.240(19) . ? Co2 O22 1.947(14) . ? Co2 O19 2.056(13) . ? Co2 O20 2.069(6) . ? Co2 O19' 2.093(13) . ? Co2 O21 2.116(5) . ? Co2 O1 2.122(4) . ? Co2 O15 2.139(5) 1_655 ? Co2 O22' 2.141(11) . ? C1 O1 1.242(8) . ? C1 O2 1.263(8) . ? C1 C2 1.509(8) . ? C2 N1 1.332(8) . ? C2 C3 1.385(9) . ? C3 C4 1.387(9) . ? C3 H3 0.9300 . ? C4 O3 1.341(7) . ? C4 C5 1.387(9) . ? C5 C6 1.384(8) . ? C5 H5 0.9300 . ? C6 N1 1.336(8) . ? C6 C7 1.494(8) . ? C7 O4 1.254(7) . ? C7 O5 1.258(7) . ? C8 O7 1.251(8) . ? C8 O6 1.256(8) . ? C8 C9 1.506(9) . ? C9 N2 1.341(8) . ? C9 C10 1.374(9) . ? C10 C11 1.377(9) . ? C10 H10 0.9300 . ? C11 O8 1.348(8) . ? C11 C12 1.390(9) . ? C12 C13 1.381(9) . ? C12 H12 0.9300 . ? C13 N2 1.335(8) . ? C13 C14 1.487(9) . ? C14 O9 1.217(8) . ? C14 O10 1.281(8) . ? C15 O12 1.248(8) . ? C15 O11 1.268(8) . ? C15 C16 1.493(9) . ? C16 N3 1.340(8) . ? C16 C17 1.380(9) . ? C17 C18 1.409(9) . ? C17 H17 0.9300 . ? C18 O13 1.303(8) . ? C18 C19 1.412(9) . ? C19 C20 1.378(9) . ? C19 H19 0.9300 . ? C20 N3 1.322(8) . ? C20 C21 1.509(9) . ? C21 O15 1.242(8) . ? C21 O14 1.264(8) . ? O3 H3A 0.8122 . ? O7 Co1 2.161(4) 1_655 ? O8 H8A 0.8484 . ? O13 Co1 2.048(5) 4_676 ? O15 Co2 2.139(4) 1_455 ? 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 O6 Tm1 O2 75.84(16) . . ? O6 Tm1 O11 76.82(15) . . ? O2 Tm1 O11 79.51(16) . . ? O6 Tm1 O10 128.64(15) . . ? O2 Tm1 O10 147.69(15) . . ? O11 Tm1 O10 86.00(15) . . ? O6 Tm1 O14 145.21(15) . . ? O2 Tm1 O14 86.82(16) . . ? O11 Tm1 O14 129.85(15) . . ? O10 Tm1 O14 80.55(15) . . ? O6 Tm1 O5 89.62(15) . . ? O2 Tm1 O5 128.84(14) . . ? O11 Tm1 O5 144.83(15) . . ? O10 Tm1 O5 77.39(14) . . ? O14 Tm1 O5 77.99(15) . . ? O6 Tm1 N3 134.55(16) . . ? O2 Tm1 N3 73.06(16) . . ? O11 Tm1 N3 65.62(16) . . ? O10 Tm1 N3 74.66(16) . . ? O14 Tm1 N3 64.24(16) . . ? O5 Tm1 N3 135.81(16) . . ? O6 Tm1 N2 64.22(16) . . ? O2 Tm1 N2 135.84(16) . . ? O11 Tm1 N2 73.93(16) . . ? O10 Tm1 N2 64.56(16) . . ? O14 Tm1 N2 137.11(16) . . ? O5 Tm1 N2 70.95(16) . . ? N3 Tm1 N2 123.54(17) . . ? O6 Tm1 N1 73.83(16) . . ? O2 Tm1 N1 64.68(16) . . ? O11 Tm1 N1 137.99(17) . . ? O10 Tm1 N1 135.97(16) . . ? O14 Tm1 N1 71.50(16) . . ? O5 Tm1 N1 64.17(15) . . ? N3 Tm1 N1 119.15(17) . . ? N2 Tm1 N1 117.30(17) . . ? O18 Co1 O13 91.1(2) . 4_475 ? O18 Co1 O16' 166.5(7) . . ? O13 Co1 O16' 102.4(7) 4_475 . ? O18 Co1 O16 176.7(5) . . ? O13 Co1 O16 85.8(5) 4_475 . ? O16' Co1 O16 16.6(4) . . ? O18 Co1 O17' 93.7(4) . . ? O13 Co1 O17' 168.8(3) 4_475 . ? O16' Co1 O17' 73.0(8) . . ? O16 Co1 O17' 89.6(6) . . ? O18 Co1 O7 87.97(19) . 1_455 ? O13 Co1 O7 90.84(19) 4_475 1_455 ? O16' Co1 O7 91.6(4) . 1_455 ? O16 Co1 O7 93.2(3) . 1_455 ? O17' Co1 O7 79.2(3) . 1_455 ? O18 Co1 O4 91.78(19) . . ? O13 Co1 O4 101.23(17) 4_475 . ? O16' Co1 O4 85.9(4) . . ? O16 Co1 O4 87.7(3) . . ? O17' Co1 O4 88.8(2) . . ? O7 Co1 O4 167.93(17) 1_455 . ? O18 Co1 O17 76.9(7) . . ? O13 Co1 O17 167.4(7) 4_475 . ? O16' Co1 O17 89.6(10) . . ? O16 Co1 O17 106.3(9) . . ? O17' Co1 O17 17.9(5) . . ? O7 Co1 O17 84.9(5) 1_455 . ? O4 Co1 O17 83.3(5) . . ? O22 Co2 O19 67.6(9) . . ? O22 Co2 O20 165.6(7) . . ? O19 Co2 O20 98.2(6) . . ? O22 Co2 O19' 86.2(9) . . ? O19 Co2 O19' 19.7(4) . . ? O20 Co2 O19' 79.4(6) . . ? O22 Co2 O21 100.9(7) . . ? O19 Co2 O21 167.3(6) . . ? O20 Co2 O21 93.5(3) . . ? O19' Co2 O21 172.9(6) . . ? O22 Co2 O1 92.9(4) . . ? O19 Co2 O1 89.4(4) . . ? O20 Co2 O1 89.6(2) . . ? O19' Co2 O1 95.0(4) . . ? O21 Co2 O1 85.71(18) . . ? O22 Co2 O15 83.7(4) . 1_655 ? O19 Co2 O15 94.3(4) . 1_655 ? O20 Co2 O15 95.0(2) . 1_655 ? O19' Co2 O15 90.2(4) . 1_655 ? O21 Co2 O15 89.59(18) . 1_655 ? O1 Co2 O15 173.59(18) . 1_655 ? O22 Co2 O22' 18.5(4) . . ? O19 Co2 O22' 85.5(7) . . ? O20 Co2 O22' 175.8(5) . . ? O19' Co2 O22' 104.4(7) . . ? O21 Co2 O22' 82.6(4) . . ? O1 Co2 O22' 88.5(3) . . ? O15 Co2 O22' 86.6(3) 1_655 . ? O1 C1 O2 126.2(6) . . ? O1 C1 C2 118.5(5) . . ? O2 C1 C2 115.2(5) . . ? N1 C2 C3 123.5(6) . . ? N1 C2 C1 113.1(5) . . ? C3 C2 C1 123.4(6) . . ? C2 C3 C4 117.5(6) . . ? C2 C3 H3 121.2 . . ? C4 C3 H3 121.2 . . ? O3 C4 C3 121.1(6) . . ? O3 C4 C5 119.2(6) . . ? C3 C4 C5 119.6(6) . . ? C6 C5 C4 118.4(6) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? N1 C6 C5 122.6(6) . . ? N1 C6 C7 113.7(5) . . ? C5 C6 C7 123.7(6) . . ? O4 C7 O5 124.9(6) . . ? O4 C7 C6 119.6(5) . . ? O5 C7 C6 115.5(5) . . ? O7 C8 O6 125.1(6) . . ? O7 C8 C9 119.5(6) . . ? O6 C8 C9 115.4(5) . . ? N2 C9 C10 123.4(6) . . ? N2 C9 C8 111.8(5) . . ? C10 C9 C8 124.8(6) . . ? C9 C10 C11 118.2(6) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? O8 C11 C10 119.1(6) . . ? O8 C11 C12 121.7(6) . . ? C10 C11 C12 119.2(6) . . ? C13 C12 C11 118.4(6) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? N2 C13 C12 122.8(6) . . ? N2 C13 C14 113.9(6) . . ? C12 C13 C14 123.3(6) . . ? O9 C14 O10 124.0(7) . . ? O9 C14 C13 121.1(6) . . ? O10 C14 C13 114.9(6) . . ? O12 C15 O11 124.0(6) . . ? O12 C15 C16 120.1(6) . . ? O11 C15 C16 116.0(6) . . ? N3 C16 C17 123.0(6) . . ? N3 C16 C15 114.1(6) . . ? C17 C16 C15 122.9(6) . . ? C16 C17 C18 119.7(6) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? O13 C18 C17 122.8(6) . . ? O13 C18 C19 120.8(6) . . ? C17 C18 C19 116.4(6) . . ? C20 C19 C18 118.9(6) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? N3 C20 C19 124.4(6) . . ? N3 C20 C21 112.9(5) . . ? C19 C20 C21 122.7(6) . . ? O15 C21 O14 125.2(6) . . ? O15 C21 C20 119.8(6) . . ? O14 C21 C20 115.1(5) . . ? C2 N1 C6 118.3(5) . . ? C2 N1 Tm1 120.6(4) . . ? C6 N1 Tm1 120.9(4) . . ? C13 N2 C9 117.7(5) . . ? C13 N2 Tm1 120.6(4) . . ? C9 N2 Tm1 121.2(4) . . ? C20 N3 C16 117.6(6) . . ? C20 N3 Tm1 122.4(4) . . ? C16 N3 Tm1 119.9(4) . . ? C1 O1 Co2 126.1(4) . . ? C1 O2 Tm1 126.3(4) . . ? C4 O3 H3A 110.3 . . ? C7 O4 Co1 125.3(4) . . ? C7 O5 Tm1 125.6(4) . . ? C8 O6 Tm1 126.8(4) . . ? C8 O7 Co1 124.3(4) . 1_655 ? C11 O8 H8A 109.4 . . ? C14 O10 Tm1 125.2(4) . . ? C15 O11 Tm1 124.1(4) . . ? C18 O13 Co1 129.1(4) . 4_676 ? C21 O14 Tm1 125.3(4) . . ? C21 O15 Co2 125.6(4) . 1_455 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.823 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.156 # Attachment '772815.cif' data_25 _database_code_depnum_ccdc_archive 'CCDC 772815' #TrackingRef '772815.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H40 Co2 N3 O31 Yb' _chemical_formula_weight 1121.46 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' Co Co 0.3494 0.9721 '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' Yb Yb -0.3850 5.5486 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8997(18) _cell_length_b 23.845(5) _cell_length_c 18.414(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.70(3) _cell_angle_gamma 90.00 _cell_volume 3655.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 9415 _cell_measurement_theta_min 1.7079 _cell_measurement_theta_max 27.8326 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.038 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2236 _exptl_absorpt_coefficient_mu 3.551 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8152 _exptl_absorpt_correction_T_max 0.9324 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27291 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6393 _reflns_number_gt 6211 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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. ISOR: the parameter to go anisotropic restraint to appointed atoms. SIMU: the parameter to set some atoms in limited range having the save shift parameters, and this parameter always is used with ISOR. Isor and Simu are applied for water molecule O16, O17, O18, O18', O19, O20, O21 and O22. ; _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^)+(0.0155P)^2^+41.8075P] 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 6393 _refine_ls_number_parameters 571 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.0975 _refine_ls_wR_factor_gt 0.0965 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.001 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 -0.00075(11) 0.83170(4) 0.02203(6) 0.0232(2) Uani 1 1 d . . . Co2 Co 0.92501(11) 0.90580(4) 0.42916(6) 0.0161(2) Uani 1 1 d . . . Yb1 Yb 0.54307(3) 0.691129(11) 0.078653(16) 0.01143(9) Uani 1 1 d . A . C1 C 0.6711(8) 0.7772(3) -0.0238(4) 0.0159(15) Uani 1 1 d . A . C2 C 0.5219(8) 0.7549(3) -0.0848(4) 0.0134(14) Uani 1 1 d . . . C3 C 0.4685(8) 0.7732(3) -0.1610(4) 0.0154(14) Uani 1 1 d . . . H3 H 0.5254 0.8001 -0.1774 0.018 Uiso 1 1 d R . . C4 C 0.3280(8) 0.7508(3) -0.2117(4) 0.0149(14) Uani 1 1 d . . . C5 C 0.2484(8) 0.7092(3) -0.1861(4) 0.0160(14) Uani 1 1 d . . . H5 H 0.1553 0.6925 -0.2197 0.019 Uiso 1 1 d R . . C6 C 0.3131(8) 0.6937(3) -0.1088(4) 0.0111(13) Uani 1 1 d . . . C7 C 0.2357(7) 0.6515(3) -0.0726(4) 0.0116(13) Uani 1 1 d . A . C8 C 0.7133(8) 0.5857(3) 0.0268(4) 0.0135(14) Uani 1 1 d . A . C9 C 0.6384(8) 0.5561(3) 0.0779(4) 0.0158(14) Uani 1 1 d . . . C10 C 0.6371(8) 0.4984(3) 0.0865(4) 0.0151(14) Uani 1 1 d . . . H10 H 0.6912 0.4750 0.0636 0.018 Uiso 1 1 d R . . C11 C 0.5510(8) 0.4767(3) 0.1298(4) 0.0183(15) Uani 1 1 d . . . C12 C 0.4807(9) 0.5128(3) 0.1674(4) 0.0220(16) Uani 1 1 d . . . H12 H 0.4258 0.4992 0.1983 0.026 Uiso 1 1 d R . . C13 C 0.4933(8) 0.5697(3) 0.1568(4) 0.0172(15) Uani 1 1 d . . . C14 C 0.4235(9) 0.6131(3) 0.1941(4) 0.0229(16) Uani 1 1 d . A . C15 C 0.3540(8) 0.8046(3) 0.0985(4) 0.0158(14) Uani 1 1 d . . . C16 C 0.5070(8) 0.8088(3) 0.1684(4) 0.0161(14) Uani 1 1 d . A . C17 C 0.5410(8) 0.8519(3) 0.2206(4) 0.0195(15) Uani 1 1 d . . . H17 H 0.4681 0.8811 0.2136 0.023 Uiso 1 1 d R A . C18 C 0.6859(8) 0.8521(3) 0.2843(4) 0.0194(15) Uani 1 1 d . A . C19 C 0.7891(8) 0.8065(3) 0.2892(4) 0.0188(15) Uani 1 1 d . . . H19 H 0.8886 0.8048 0.3291 0.023 Uiso 1 1 d R A . C20 C 0.7432(8) 0.7641(3) 0.2355(4) 0.0170(15) Uani 1 1 d . A . C21 C 0.8422(8) 0.7127(3) 0.2385(4) 0.0178(15) Uani 1 1 d . . . N1 N 0.4472(6) 0.7162(2) -0.0588(3) 0.0128(12) Uani 1 1 d . . . N2 N 0.5677(6) 0.5915(2) 0.1117(3) 0.0128(12) Uani 1 1 d . . . N3 N 0.6039(6) 0.7649(2) 0.1746(3) 0.0129(12) Uani 1 1 d . . . O1 O 0.7561(6) 0.8118(2) -0.0419(3) 0.0204(11) Uani 1 1 d . . . O2 O 0.7005(5) 0.75716(19) 0.0440(3) 0.0152(10) Uani 1 1 d . . . O3 O 0.1081(5) 0.62817(19) -0.1139(3) 0.0153(10) Uani 1 1 d . . . O4 O 0.3067(5) 0.64385(19) -0.0011(3) 0.0143(10) Uani 1 1 d . . . O5 O 0.2637(6) 0.7666(2) -0.2863(3) 0.0199(11) Uani 1 1 d . . . H5A H 0.3206 0.7906 -0.2955 0.030 Uiso 1 1 d R . . O6 O 0.6937(6) 0.63775(19) 0.0231(3) 0.0175(10) Uani 1 1 d . . . O7 O 0.7865(6) 0.5577(2) -0.0070(3) 0.0220(11) Uani 1 1 d . . . O8 O 0.4230(5) 0.66310(18) 0.1685(3) 0.0138(10) Uani 1 1 d . . . O9 O 0.3706(10) 0.6000(3) 0.2448(4) 0.054(2) Uani 1 1 d . . . O10 O 0.5399(6) 0.4208(2) 0.1347(3) 0.0249(12) Uani 1 1 d . . . H10A H 0.4613 0.4130 0.1460 0.037 Uiso 1 1 d R . . O11 O 0.3440(5) 0.76222(19) 0.0560(3) 0.0170(10) Uani 1 1 d . A . O12 O 0.2497(6) 0.8419(2) 0.0866(3) 0.0224(11) Uani 1 1 d . A . O13 O 0.7914(5) 0.68040(19) 0.1810(3) 0.0170(10) Uani 1 1 d . A . O14 O 0.9675(6) 0.7051(2) 0.2957(3) 0.0209(11) Uani 1 1 d . A . O15 O 0.7192(6) 0.8926(2) 0.3351(3) 0.0250(12) Uani 1 1 d . . . O16 O 0.0559(6) 0.7729(2) -0.0495(3) 0.0228(11) Uani 1 1 d U A . H16A H 0.0357 0.7789 -0.0980 0.027 Uiso 1 1 d R . . H16B H 0.1582 0.7698 -0.0280 0.027 Uiso 1 1 d R . . O17 O -0.0139(9) 0.8982(3) -0.0509(4) 0.059(2) Uani 1 1 d U A . H17A H -0.1067 0.9133 -0.0770 0.071 Uiso 1 1 d R . . H17B H 0.0335 0.8850 -0.0821 0.071 Uiso 1 1 d R . . O18 O -0.0560(17) 0.8979(8) 0.0827(9) 0.044(4) Uani 0.54(3) 1 d PU A 1 O18' O -0.0730(18) 0.8732(9) 0.1013(10) 0.040(4) Uani 0.46(3) 1 d PU A 2 O19 O 0.0063(8) 0.7685(4) 0.0989(4) 0.064(2) Uani 1 1 d U A . O20 O 0.9491(7) 0.9841(2) 0.3911(3) 0.0313(13) Uani 1 1 d U . . H20A H 0.9084 0.9923 0.3433 0.038 Uiso 1 1 d R A . H20B H 1.0135 1.0070 0.4223 0.038 Uiso 1 1 d R . . O21 O 1.1127(8) 0.9223(3) 0.5360(4) 0.0523(18) Uani 1 1 d U . . O22 O 0.9131(8) 0.8273(3) 0.4719(4) 0.0508(17) Uani 1 1 d U . . H22A H 0.9860 0.8020 0.4842 0.061 Uiso 1 1 d R A . H22B H 0.8555 0.8300 0.5004 0.061 Uiso 1 1 d R . . O23 O 0.0919(10) 0.9228(3) 0.2398(4) 0.067(2) Uani 1 1 d . . . H23A H 0.1536 0.9320 0.2153 0.080 Uiso 1 1 d R . . H23B H 0.0305 0.9485 0.2458 0.080 Uiso 1 1 d R . . O24 O 0.0268(9) 0.6137(4) 0.1605(5) 0.072(2) Uani 1 1 d . . . H24A H -0.0422 0.6407 0.1580 0.087 Uiso 1 1 d R . . H24B H 0.0164 0.5990 0.1157 0.087 Uiso 1 1 d R . . O25 O 0.1143(10) 0.5042(3) 0.2623(4) 0.067(2) Uani 1 1 d . . . H25A H 0.0790 0.5336 0.2773 0.080 Uiso 1 1 d R . . H25B H 0.2108 0.4948 0.2893 0.080 Uiso 1 1 d R . . O26 O 0.1380(16) 0.8905(5) 0.8342(8) 0.151(6) Uani 1 1 d . . . O27 O 0.4275(19) 0.4860(6) 0.3550(9) 0.087(6) Uani 0.64(2) 1 d P B 1 O27' O 0.635(4) 0.4521(12) 0.439(2) 0.126(16) Uani 0.36(2) 1 d P B 2 O28 O 0.2771(14) 0.9682(8) 0.1631(8) 0.168(7) Uani 1 1 d . C 1 O29 O 0.751(2) 0.9023(7) 0.8075(10) 0.085(6) Uani 0.50 1 d P D 1 O30 O 0.455(2) 0.5942(6) 0.4036(10) 0.104(7) Uani 0.64(2) 1 d P E 1 O30' O 0.714(4) 0.4248(13) 0.5415(19) 0.108(13) Uani 0.36(2) 1 d P E 2 O31 O 0.6624(19) 0.9432(7) 0.8839(10) 0.077(5) Uani 0.50 1 d P . . O32 O 0.652(2) 0.9332(11) 0.0399(10) 0.121(10) Uani 0.50 1 d P . . O33 O 0.875(3) 0.0006(7) 0.9834(11) 0.105(8) Uani 0.50 1 d P . . 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 0.0127(5) 0.0280(6) 0.0246(6) -0.0042(4) 0.0013(4) -0.0011(4) Co2 0.0133(5) 0.0159(5) 0.0200(5) -0.0037(4) 0.0071(4) 0.0009(4) Yb1 0.01007(15) 0.01134(15) 0.01269(16) -0.00101(11) 0.00378(11) -0.00076(11) C1 0.013(3) 0.014(3) 0.020(4) 0.002(3) 0.006(3) 0.002(3) C2 0.013(3) 0.013(3) 0.012(3) 0.000(3) 0.003(3) 0.001(3) C3 0.017(3) 0.010(3) 0.021(4) 0.001(3) 0.009(3) 0.000(3) C4 0.018(4) 0.018(3) 0.009(3) 0.000(3) 0.006(3) 0.001(3) C5 0.013(3) 0.017(3) 0.019(4) -0.003(3) 0.007(3) -0.001(3) C6 0.014(3) 0.008(3) 0.010(3) -0.001(3) 0.003(3) 0.000(3) C7 0.011(3) 0.007(3) 0.020(4) -0.004(3) 0.008(3) -0.003(2) C8 0.012(3) 0.012(3) 0.014(3) -0.006(3) 0.001(3) -0.004(3) C9 0.014(3) 0.017(3) 0.016(4) 0.001(3) 0.006(3) 0.001(3) C10 0.010(3) 0.014(3) 0.021(4) 0.000(3) 0.005(3) -0.001(3) C11 0.009(3) 0.015(3) 0.028(4) 0.001(3) 0.004(3) -0.001(3) C12 0.022(4) 0.023(4) 0.023(4) 0.004(3) 0.011(3) 0.004(3) C13 0.015(3) 0.017(4) 0.020(4) 0.000(3) 0.007(3) -0.001(3) C14 0.026(4) 0.026(4) 0.022(4) 0.000(3) 0.015(3) 0.002(3) C15 0.014(3) 0.012(3) 0.020(4) -0.002(3) 0.003(3) 0.000(3) C16 0.011(3) 0.016(3) 0.021(4) -0.001(3) 0.006(3) -0.003(3) C17 0.015(4) 0.015(3) 0.028(4) -0.004(3) 0.007(3) 0.000(3) C18 0.012(3) 0.021(4) 0.024(4) -0.008(3) 0.005(3) -0.002(3) C19 0.011(3) 0.021(4) 0.024(4) -0.009(3) 0.006(3) -0.004(3) C20 0.013(3) 0.017(4) 0.018(4) 0.000(3) 0.001(3) -0.001(3) C21 0.011(3) 0.016(3) 0.025(4) 0.001(3) 0.005(3) -0.001(3) N1 0.013(3) 0.012(3) 0.012(3) 0.002(2) 0.003(2) -0.001(2) N2 0.011(3) 0.011(3) 0.016(3) -0.001(2) 0.005(2) 0.001(2) N3 0.008(3) 0.011(3) 0.017(3) -0.004(2) 0.002(2) 0.001(2) O1 0.015(2) 0.019(3) 0.023(3) 0.002(2) 0.002(2) -0.007(2) O2 0.015(2) 0.015(2) 0.013(2) 0.0049(19) 0.003(2) -0.0032(19) O3 0.013(2) 0.018(2) 0.016(2) 0.003(2) 0.005(2) -0.0013(19) O4 0.012(2) 0.018(2) 0.010(2) -0.0012(19) 0.0000(19) -0.0028(19) O5 0.021(3) 0.025(3) 0.013(3) 0.007(2) 0.005(2) -0.007(2) O6 0.021(3) 0.013(2) 0.021(3) 0.004(2) 0.010(2) 0.0013(19) O7 0.025(3) 0.016(3) 0.031(3) -0.003(2) 0.019(2) -0.002(2) O8 0.016(2) 0.011(2) 0.015(2) 0.0007(19) 0.007(2) 0.0015(18) O9 0.100(6) 0.030(3) 0.065(5) 0.011(3) 0.071(5) 0.015(4) O10 0.020(3) 0.013(2) 0.045(3) 0.004(2) 0.015(3) 0.000(2) O11 0.012(2) 0.017(2) 0.021(3) 0.000(2) 0.005(2) 0.0023(19) O12 0.015(3) 0.017(3) 0.032(3) -0.006(2) 0.004(2) 0.004(2) O13 0.011(2) 0.019(3) 0.017(3) -0.010(2) 0.000(2) 0.0018(19) O14 0.014(2) 0.023(3) 0.022(3) -0.003(2) 0.002(2) 0.006(2) O15 0.016(3) 0.017(3) 0.034(3) -0.016(2) -0.001(2) 0.002(2) O16 0.017(2) 0.029(3) 0.019(2) 0.001(2) 0.002(2) 0.002(2) O17 0.053(4) 0.046(3) 0.071(4) 0.019(3) 0.012(3) -0.005(3) O18 0.041(5) 0.040(5) 0.046(5) -0.005(4) 0.009(4) 0.002(4) O18' 0.036(5) 0.041(6) 0.041(5) -0.002(4) 0.013(4) 0.004(4) O19 0.040(3) 0.094(4) 0.054(4) 0.038(3) 0.011(3) -0.008(3) O20 0.033(3) 0.021(2) 0.041(3) -0.006(2) 0.014(2) -0.006(2) O21 0.040(3) 0.065(4) 0.041(3) -0.022(3) 0.001(3) 0.021(3) O22 0.063(4) 0.043(3) 0.070(4) 0.018(3) 0.053(3) 0.020(3) O23 0.088(6) 0.045(4) 0.053(5) -0.005(4) 0.007(4) 0.018(4) O24 0.057(5) 0.080(6) 0.083(6) -0.015(5) 0.028(5) 0.023(4) O25 0.090(6) 0.057(5) 0.062(5) -0.002(4) 0.037(5) 0.000(4) O26 0.164(12) 0.080(8) 0.145(11) 0.028(7) -0.024(9) -0.076(8) O27 0.100(12) 0.079(11) 0.087(11) 0.023(8) 0.041(9) 0.027(8) O27' 0.12(3) 0.07(2) 0.18(4) -0.02(2) 0.04(3) -0.005(18) O28 0.081(8) 0.29(2) 0.132(11) 0.112(12) 0.039(8) 0.053(10) O29 0.098(13) 0.060(11) 0.058(10) -0.015(8) -0.019(10) 0.026(10) O30 0.129(15) 0.071(11) 0.101(13) 0.010(9) 0.027(11) -0.002(10) O30' 0.13(3) 0.11(2) 0.11(3) 0.008(19) 0.07(2) 0.01(2) O31 0.059(10) 0.067(11) 0.082(12) -0.015(9) -0.006(9) 0.022(8) O32 0.048(10) 0.24(3) 0.056(11) 0.003(14) 0.002(8) 0.100(14) O33 0.16(2) 0.047(10) 0.073(13) 0.007(9) -0.009(13) 0.003(12) _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 O18' 2.046(15) . ? Co1 O19 2.052(7) . ? Co1 O17 2.053(7) . ? Co1 O18 2.090(14) . ? Co1 O16 2.103(5) . ? Co1 O1 2.120(5) 1_455 ? Co1 O12 2.137(5) . ? Co2 O20 2.032(5) . ? Co2 O22 2.049(6) . ? Co2 O15 2.052(5) . ? Co2 O21 2.119(6) . ? Co2 O7 2.164(5) 4_576 ? Co2 O3 2.202(5) 4_676 ? Yb1 O6 2.331(5) . ? Yb1 O2 2.341(4) . ? Yb1 O13 2.357(5) . ? Yb1 O8 2.360(4) . ? Yb1 O11 2.380(4) . ? Yb1 O4 2.381(4) . ? Yb1 N3 2.415(5) . ? Yb1 N1 2.442(5) . ? Yb1 N2 2.444(5) . ? C1 O1 1.242(8) . ? C1 O2 1.274(8) . ? C1 C2 1.501(9) . ? C2 N1 1.322(8) . ? C2 C3 1.384(9) . ? C3 C4 1.378(9) . ? C3 H3 0.9301 . ? C4 O5 1.342(8) . ? C4 C5 1.393(9) . ? C5 C6 1.384(9) . ? C5 H5 0.9301 . ? C6 N1 1.335(8) . ? C6 C7 1.502(9) . ? C7 O3 1.251(8) . ? C7 O4 1.257(8) . ? C8 O7 1.243(8) . ? C8 O6 1.252(8) . ? C8 C9 1.507(9) . ? C9 N2 1.330(9) . ? C9 C10 1.386(9) . ? C10 C11 1.386(10) . ? C10 H10 0.9298 . ? C11 O10 1.343(8) . ? C11 C12 1.383(10) . ? C12 C13 1.380(10) . ? C12 H12 0.9299 . ? C13 N2 1.338(9) . ? C13 C14 1.494(10) . ? C14 O9 1.225(9) . ? C14 O8 1.282(9) . ? C15 O12 1.248(8) . ? C15 O11 1.262(8) . ? C15 C16 1.511(9) . ? C16 N3 1.335(9) . ? C16 C17 1.365(10) . ? C17 C18 1.404(10) . ? C17 H17 0.9300 . ? C18 O15 1.303(8) . ? C18 C19 1.405(10) . ? C19 C20 1.373(10) . ? C19 H19 0.9301 . ? C20 N3 1.346(8) . ? C20 C21 1.498(9) . ? C21 O14 1.247(8) . ? C21 O13 1.257(8) . ? O1 Co1 2.120(5) 1_655 ? O3 Co2 2.202(5) 4_475 ? O5 H5A 0.8200 . ? O7 Co2 2.164(5) 4_575 ? O10 H10A 0.8201 . ? O16 H16A 0.8597 . ? O16 H16B 0.8583 . ? O17 H17A 0.8734 . ? O17 H17B 0.8821 . ? O20 H20A 0.8474 . ? O20 H20B 0.8514 . ? O22 H22A 0.8557 . ? O22 H22B 0.8565 . ? O23 H23A 0.8533 . ? O23 H23B 0.8520 . ? O24 H24A 0.8782 . ? O24 H24B 0.8713 . ? O25 H25A 0.8538 . ? O25 H25B 0.8561 . ? 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 O18' Co1 O19 78.7(7) . . ? O18' Co1 O17 97.7(7) . . ? O19 Co1 O17 176.3(3) . . ? O18' Co1 O18 20.1(5) . . ? O19 Co1 O18 98.1(7) . . ? O17 Co1 O18 78.3(6) . . ? O18' Co1 O16 167.0(7) . . ? O19 Co1 O16 89.2(3) . . ? O17 Co1 O16 94.4(3) . . ? O18 Co1 O16 172.6(6) . . ? O18' Co1 O1 89.3(5) . 1_455 ? O19 Co1 O1 89.7(2) . 1_455 ? O17 Co1 O1 89.9(2) . 1_455 ? O18 Co1 O1 94.5(4) . 1_455 ? O16 Co1 O1 85.8(2) . 1_455 ? O18' Co1 O12 94.4(5) . . ? O19 Co1 O12 85.9(2) . . ? O17 Co1 O12 94.8(2) . . ? O18 Co1 O12 90.7(4) . . ? O16 Co1 O12 89.48(19) . . ? O1 Co1 O12 173.58(19) 1_455 . ? O20 Co2 O22 176.9(3) . . ? O20 Co2 O15 91.2(2) . . ? O22 Co2 O15 91.8(3) . . ? O20 Co2 O21 90.3(3) . . ? O22 Co2 O21 86.8(3) . . ? O15 Co2 O21 170.9(2) . . ? O20 Co2 O7 88.2(2) . 4_576 ? O22 Co2 O7 92.4(2) . 4_576 ? O15 Co2 O7 90.6(2) . 4_576 ? O21 Co2 O7 80.5(2) . 4_576 ? O20 Co2 O3 91.9(2) . 4_676 ? O22 Co2 O3 87.0(2) . 4_676 ? O15 Co2 O3 101.13(19) . 4_676 ? O21 Co2 O3 87.8(2) . 4_676 ? O7 Co2 O3 168.27(19) 4_576 4_676 ? O6 Yb1 O2 75.84(16) . . ? O6 Yb1 O13 76.68(16) . . ? O2 Yb1 O13 78.97(16) . . ? O6 Yb1 O8 128.74(15) . . ? O2 Yb1 O8 147.57(16) . . ? O13 Yb1 O8 86.43(16) . . ? O6 Yb1 O11 145.08(16) . . ? O2 Yb1 O11 87.32(16) . . ? O13 Yb1 O11 130.30(16) . . ? O8 Yb1 O11 80.29(16) . . ? O6 Yb1 O4 89.46(16) . . ? O2 Yb1 O4 129.34(15) . . ? O13 Yb1 O4 144.68(16) . . ? O8 Yb1 O4 77.16(16) . . ? O11 Yb1 O4 77.78(16) . . ? O6 Yb1 N3 134.73(17) . . ? O2 Yb1 N3 73.02(18) . . ? O13 Yb1 N3 65.78(16) . . ? O8 Yb1 N3 74.58(17) . . ? O11 Yb1 N3 64.52(17) . . ? O4 Yb1 N3 135.79(17) . . ? O6 Yb1 N1 73.93(17) . . ? O2 Yb1 N1 64.95(17) . . ? O13 Yb1 N1 137.78(18) . . ? O8 Yb1 N1 135.76(17) . . ? O11 Yb1 N1 71.23(17) . . ? O4 Yb1 N1 64.40(17) . . ? N3 Yb1 N1 119.04(18) . . ? O6 Yb1 N2 64.10(17) . . ? O2 Yb1 N2 135.41(17) . . ? O13 Yb1 N2 73.70(17) . . ? O8 Yb1 N2 64.74(16) . . ? O11 Yb1 N2 137.07(17) . . ? O4 Yb1 N2 71.03(17) . . ? N3 Yb1 N2 123.33(19) . . ? N1 Yb1 N2 117.62(18) . . ? O1 C1 O2 125.4(6) . . ? O1 C1 C2 119.7(6) . . ? O2 C1 C2 114.9(6) . . ? N1 C2 C3 123.4(6) . . ? N1 C2 C1 113.7(6) . . ? C3 C2 C1 122.9(6) . . ? C4 C3 C2 117.9(6) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? O5 C4 C3 122.7(6) . . ? O5 C4 C5 117.6(6) . . ? C3 C4 C5 119.7(6) . . ? C6 C5 C4 117.5(6) . . ? C6 C5 H5 121.1 . . ? C4 C5 H5 121.3 . . ? N1 C6 C5 123.1(6) . . ? N1 C6 C7 113.7(5) . . ? C5 C6 C7 123.1(6) . . ? O3 C7 O4 125.7(6) . . ? O3 C7 C6 119.2(6) . . ? O4 C7 C6 115.0(5) . . ? O7 C8 O6 126.3(6) . . ? O7 C8 C9 119.2(6) . . ? O6 C8 C9 114.5(6) . . ? N2 C9 C10 123.5(6) . . ? N2 C9 C8 112.4(6) . . ? C10 C9 C8 124.1(6) . . ? C9 C10 C11 117.7(6) . . ? C9 C10 H10 121.2 . . ? C11 C10 H10 121.1 . . ? O10 C11 C12 121.8(7) . . ? O10 C11 C10 118.5(6) . . ? C12 C11 C10 119.7(6) . . ? C13 C12 C11 117.8(7) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 121.3 . . ? N2 C13 C12 123.5(6) . . ? N2 C13 C14 113.2(6) . . ? C12 C13 C14 123.3(6) . . ? O9 C14 O8 124.4(7) . . ? O9 C14 C13 120.5(7) . . ? O8 C14 C13 115.1(6) . . ? O12 C15 O11 125.2(6) . . ? O12 C15 C16 119.5(6) . . ? O11 C15 C16 115.2(6) . . ? N3 C16 C17 123.6(6) . . ? N3 C16 C15 112.4(6) . . ? C17 C16 C15 124.0(6) . . ? C16 C17 C18 120.0(6) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 120.2 . . ? O15 C18 C17 120.7(6) . . ? O15 C18 C19 123.3(6) . . ? C17 C18 C19 116.0(6) . . ? C20 C19 C18 120.2(6) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 120.2 . . ? N3 C20 C19 122.8(6) . . ? N3 C20 C21 113.5(6) . . ? C19 C20 C21 123.7(6) . . ? O14 C21 O13 124.7(6) . . ? O14 C21 C20 119.3(6) . . ? O13 C21 C20 116.0(6) . . ? C2 N1 C6 118.2(6) . . ? C2 N1 Yb1 120.6(4) . . ? C6 N1 Yb1 121.1(4) . . ? C9 N2 C13 117.7(6) . . ? C9 N2 Yb1 121.0(4) . . ? C13 N2 Yb1 120.8(4) . . ? C16 N3 C20 117.3(6) . . ? C16 N3 Yb1 122.5(4) . . ? C20 N3 Yb1 120.1(4) . . ? C1 O1 Co1 126.7(5) . 1_655 ? C1 O2 Yb1 125.7(4) . . ? C7 O3 Co2 125.0(4) . 4_475 ? C7 O4 Yb1 125.8(4) . . ? C4 O5 H5A 109.6 . . ? C8 O6 Yb1 127.4(4) . . ? C8 O7 Co2 123.9(4) . 4_575 ? C14 O8 Yb1 125.3(4) . . ? C11 O10 H10A 109.4 . . ? C15 O11 Yb1 125.2(4) . . ? C15 O12 Co1 125.5(4) . . ? C21 O13 Yb1 124.3(4) . . ? C18 O15 Co2 128.9(4) . . ? Co1 O16 H16A 122.1 . . ? Co1 O16 H16B 102.6 . . ? H16A O16 H16B 106.9 . . ? Co1 O17 H17A 120.3 . . ? Co1 O17 H17B 102.8 . . ? H17A O17 H17B 111.4 . . ? Co2 O20 H20A 120.8 . . ? Co2 O20 H20B 119.0 . . ? H20A O20 H20B 119.4 . . ? Co2 O22 H22A 127.5 . . ? Co2 O22 H22B 106.8 . . ? H22A O22 H22B 117.0 . . ? H23A O23 H23B 116.5 . . ? H24A O24 H24B 114.0 . . ? H25A O25 H25B 115.9 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.797 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.152