# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1961 ############################################################################## # # # DEPOSIT MATERIAL CORRESPONDING TO MANUSCRIPT # # # # # # 9/09544F # # # # # ############################################################################## data_YCuODA _audit_creation_method SHELXL-97 _chemical_name_systematic ; Yttrium Copper Oxydiacetate ; _chemical_formula_sum 'C24 H60 Cu3 O48 Y2' _chemical_formula_weight 1485.16 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -2.7962 3.5667 '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 14.595(2) _cell_length_b 14.595(2) _cell_length_c 15.267(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2816.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 12.5 _exptl_crystal_description polyhedra _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.751 _exptl_crystal_F_000 1506 _exptl_absorpt_coefficient_mu 3.268 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'XEMP in SHELXTL/PC, Sheldrick, 1991' _exptl_absorpt_correction_T_min 0.18 _exptl_absorpt_correction_T_max 0.21 _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_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 98 _diffrn_standards_decay_% <2 _diffrn_reflns_number 3287 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 24.99 _reflns_number_total 875 _reflns_number_gt 533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 875 _refine_ls_number_parameters 86 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.081 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_ref 0.094 _refine_ls_wR_factor_gt 0.080 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max <0.001 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y Y 0.6667 0.3333 0.2500 0.0211(3) Uani 1 d S . . Cu Cu 1.0000 0.5000 0.5000 0.0237(3) Uani 1 d S . . O1 O 0.8040(2) 0.4163(2) 0.35495(18) 0.0293(8) Uani 1 d . . . O2 O 0.9464(3) 0.5569(3) 0.4105(2) 0.0399(9) Uani 1 d . . . O3 O 0.76379(15) 0.5276(3) 0.2500 0.0304(10) Uani 1 d S . . C1 C 0.8689(4) 0.5137(4) 0.3611(3) 0.0310(11) Uani 1 d . . . C2 C 0.8505(4) 0.5870(4) 0.3036(4) 0.0492(17) Uani 1 d . . . H2A H 0.8377 0.6342 0.3396 0.059 Uiso 1 calc R . . H2B H 0.9127 0.6295 0.2680 0.059 Uiso 1 calc R . . O1W O 0.4816(4) 0.3200(4) 0.0000 0.0429(14) Uani 1 d S . . H1W H 0.536(4) 0.347(4) 0.047(3) 0.09(2) Uiso 1 d . . . O2WA O 0.863(6) 0.723(5) 0.0000 0.14(2) Uiso 0.18 d SP . . O2WB O 0.977(3) 0.842(2) 0.1790(14) 0.13(1) Uiso 0.22 d P . . O2WC O 0.942(6) 0.848(4) 0.370(3) 0.14(2) Uiso 0.11 d P . . O2WD O 0.953(3) 0.757(3) 0.054(2) 0.14(2) Uiso 0.19 d P . . O2WE O 1.022(4) 0.792(3) 0.0000 0.14(1) Uiso 0.28 d SP . . O2WF O 0.919(3) 0.734(3) 0.0000 0.12(1) Uiso 0.36 d SP . . O2WG O 1.0000 0.845(4) 0.2500 0.13(2) Uiso 0.14 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 Y 0.0209(3) 0.0209(3) 0.0215(4) 0.000 0.000 0.01044(17) Cu 0.0184(5) 0.0305(7) 0.0223(5) 0.000 0.000 0.0123(7) O1 0.0310(15) 0.0216(18) 0.0319(15) 0.0007(15) -0.0088(13) 0.0105(16) O2 0.0340(18) 0.033(2) 0.0446(19) 0.0001(18) -0.0209(18) 0.0106(17) O3 0.0303(17) 0.027(2) 0.033(2) 0.000 -0.012(2) 0.0136(11) C1 0.024(2) 0.038(3) 0.035(2) -0.002(2) -0.008(2) 0.019(2) C2 0.044(3) 0.030(3) 0.061(4) 0.002(3) -0.031(3) 0.009(3) O1W 0.043(3) 0.051(4) 0.041(3) 0.000 0.000 0.028(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 Y O1 2.371(3) 3_665 ? Y O1 2.371(3) 24_556 ? Y O1 2.371(3) 22_666 ? Y O1 2.371(3) . ? Y O1 2.371(3) 2_655 ? Y O1 2.371(3) 23_656 ? Y O3 2.455(4) 3_665 ? Y O3 2.455(4) 2_655 ? Y O3 2.455(4) . ? Cu O2 1.954(3) 13_766 ? Cu O2 1.954(3) 16_556 ? Cu O2 1.954(3) 4_765 ? Cu O2 1.954(3) . ? Cu O1W 2.504(6) 8_655 ? Cu O1W 2.504(6) 20_666 ? O1 C1 1.257(5) . ? O2 C1 1.237(5) . ? O3 C2 1.387(5) . ? O3 C2 1.387(5) 23_656 ? C1 C2 1.510(6) . ? O1W Cu 2.504(5) 8_654 ? 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 Y O1 127.50(14) 3_665 24_556 ? O1 Y O1 85.91(14) 3_665 22_666 ? O1 Y O1 79.34(10) 24_556 22_666 ? O1 Y O1 79.34(10) 3_665 . ? O1 Y O1 85.91(14) 24_556 . ? O1 Y O1 146.33(15) 22_666 . ? O1 Y O1 79.34(10) 3_665 2_655 ? O1 Y O1 146.33(15) 24_556 2_655 ? O1 Y O1 127.50(14) 22_666 2_655 ? O1 Y O1 79.34(10) . 2_655 ? O1 Y O1 146.33(15) 3_665 23_656 ? O1 Y O1 79.34(10) 24_556 23_656 ? O1 Y O1 79.34(10) 22_666 23_656 ? O1 Y O1 127.50(14) . 23_656 ? O1 Y O1 85.91(14) 2_655 23_656 ? O1 Y O3 63.75(7) 3_665 3_665 ? O1 Y O3 63.75(7) 24_556 3_665 ? O1 Y O3 73.17(7) 22_666 3_665 ? O1 Y O3 73.17(7) . 3_665 ? O1 Y O3 137.04(7) 2_655 3_665 ? O1 Y O3 137.04(7) 23_656 3_665 ? O1 Y O3 73.17(7) 3_665 2_655 ? O1 Y O3 137.04(7) 24_556 2_655 ? O1 Y O3 63.75(7) 22_666 2_655 ? O1 Y O3 137.04(7) . 2_655 ? O1 Y O3 63.75(7) 2_655 2_655 ? O1 Y O3 73.17(7) 23_656 2_655 ? O3 Y O3 120.0 3_665 2_655 ? O1 Y O3 137.04(7) 3_665 . ? O1 Y O3 73.17(7) 24_556 . ? O1 Y O3 137.04(7) 22_666 . ? O1 Y O3 63.75(7) . . ? O1 Y O3 73.17(7) 2_655 . ? O1 Y O3 63.75(7) 23_656 . ? O3 Y O3 120.0 3_665 . ? O3 Y O3 120.0 2_655 . ? O2 Cu O2 91.3(2) 13_766 16_556 ? O2 Cu O2 88.7(2) 13_766 4_765 ? O2 Cu O2 180.0 16_556 4_765 ? O2 Cu O2 180.0 13_766 . ? O2 Cu O2 88.7(2) 16_556 . ? O2 Cu O2 91.3(2) 4_765 . ? O2 Cu O1W 85.49(13) 13_766 8_655 ? O2 Cu O1W 94.51(13) 16_556 8_655 ? O2 Cu O1W 85.49(13) 4_765 8_655 ? O2 Cu O1W 94.51(13) . 8_655 ? O2 Cu O1W 94.51(13) 13_766 20_666 ? O2 Cu O1W 85.49(13) 16_556 20_666 ? O2 Cu O1W 94.51(13) 4_765 20_666 ? O2 Cu O1W 85.49(13) . 20_666 ? O1W Cu O1W 180.0 8_655 20_666 ? C1 O1 Y 126.5(3) . . ? C1 O2 Cu 131.8(3) . . ? C2 O3 C2 114.5(5) . 23_656 ? C2 O3 Y 122.8(3) . . ? C2 O3 Y 122.8(3) 23_656 . ? O2 C1 O1 127.1(5) . . ? O2 C1 C2 115.8(4) . . ? O1 C1 C2 117.2(4) . . ? O3 C2 C1 109.3(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 Y O1 C1 -164.0(4) 3_665 . . . ? O1 Y O1 C1 66.6(4) 24_556 . . . ? O1 Y O1 C1 130.4(4) 22_666 . . . ? O1 Y O1 C1 -83.0(4) 2_655 . . . ? O1 Y O1 C1 -6.7(3) 23_656 . . . ? O3 Y O1 C1 130.4(4) 3_665 . . . ? O3 Y O1 C1 -113.4(4) 2_655 . . . ? O3 Y O1 C1 -6.7(3) . . . . ? O2 Cu O2 C1 -145(100) 13_766 . . . ? O2 Cu O2 C1 -105.6(4) 16_556 . . . ? O2 Cu O2 C1 74.4(4) 4_765 . . . ? O1W Cu O2 C1 -11.2(5) 8_655 . . . ? O1W Cu O2 C1 168.8(5) 20_666 . . . ? O1 Y O3 C2 38.1(3) 3_665 . . . ? O1 Y O3 C2 -89.4(3) 24_556 . . . ? O1 Y O3 C2 -141.9(3) 22_666 . . . ? O1 Y O3 C2 4.4(3) . . . . ? O1 Y O3 C2 90.6(3) 2_655 . . . ? O1 Y O3 C2 -175.6(3) 23_656 . . . ? O3 Y O3 C2 -44.5(3) 3_665 . . . ? O3 Y O3 C2 135.5(3) 2_655 . . . ? O1 Y O3 C2 -141.9(3) 3_665 . . 23_656 ? O1 Y O3 C2 90.6(3) 24_556 . . 23_656 ? O1 Y O3 C2 38.1(3) 22_666 . . 23_656 ? O1 Y O3 C2 -175.6(3) . . . 23_656 ? O1 Y O3 C2 -89.4(3) 2_655 . . 23_656 ? O1 Y O3 C2 4.4(3) 23_656 . . 23_656 ? O3 Y O3 C2 135.5(3) 3_665 . . 23_656 ? O3 Y O3 C2 -44.5(3) 2_655 . . 23_656 ? Cu O2 C1 O1 -2.1(8) . . . . ? Cu O2 C1 C2 176.7(4) . . . . ? Y O1 C1 O2 -173.2(4) . . . . ? Y O1 C1 C2 7.9(6) . . . . ? C2 O3 C2 C1 177.5(5) 23_656 . . . ? Y O3 C2 C1 -2.5(5) . . . . ? O2 C1 C2 O3 178.0(4) . . . . ? O1 C1 C2 O3 -3.0(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.373 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.082 ############################################################################ data_GdCuODA _audit_creation_method SHELXL-97 _chemical_name_systematic ; Gadolinium Copper Oxydiacetate ; _chemical_formula_sum 'C24 H60 Cu3 Gd2 O48' _chemical_formula_weight 1621.84 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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' _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 14.717(2) _cell_length_b 14.717(2) _cell_length_c 15.169(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2845.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedra _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.893 _exptl_crystal_F_000 1606 _exptl_absorpt_coefficient_mu 3.515 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'XEMP in SHELXTL/PC, Sheldrick, 1991' _exptl_absorpt_correction_T_min 0.14 _exptl_absorpt_correction_T_max 0.20 _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_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 98 _diffrn_standards_decay_% <2 _diffrn_reflns_number 3351 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.019 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.05 _reflns_number_total 890 _reflns_number_gt 684 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens XDISK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.028P)^2^+4.247P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 890 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.037 _refine_ls_R_factor_gt 0.024 _refine_ls_wR_factor_ref 0.060 _refine_ls_wR_factor_gt 0.054 _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_restrained_S_all 1.06 _refine_ls_shift/su_max <0.01 _refine_ls_shift/su_mean <0.01 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd Gd 0.6667 0.3333 0.2500 0.02305(15) Uani 1 d S . . Cu Cu 1.0000 0.5000 0.5000 0.0263(2) Uani 1 d S . . O1 O 0.8059(2) 0.41894(19) 0.35658(17) 0.0341(7) Uani 1 d . . . O2 O 0.9489(2) 0.5586(2) 0.4100(2) 0.0441(8) Uani 1 d . . . O3 O 0.76409(13) 0.5282(3) 0.2500 0.0326(8) Uani 1 d S . . C1 C 0.8704(3) 0.5151(3) 0.3610(3) 0.0315(9) Uani 1 d . . . C2 C 0.8524(3) 0.5877(3) 0.3033(3) 0.0531(14) Uani 1 d . . . H2A H 0.8412 0.6355 0.3396 0.064 Uiso 1 calc R . . H2B H 0.9136 0.6288 0.2667 0.064 Uiso 1 calc R . . O1W O 0.4796(4) 0.3202(4) 0.0000 0.0482(12) Uani 1 d S . . H1W H 0.528(4) 0.346(4) 0.044(3) 0.10(2) Uiso 1 d . . . O2WA O 0.272(3) 0.149(4) 0.0000 0.130(14) Uiso 0.22 d SP . . O2WB O 0.2567(17) 0.1969(16) 0.0315(12) 0.129(8) Uiso 0.29 d P . . O2WC O 0.208(3) 0.224(3) 0.0000 0.130(13) Uiso 0.24 d SP . . O2WD O 0.136(3) 0.156(3) 0.324(2) 0.127(11) Uiso 0.17 d P . . O2WE O 0.151(5) 0.151(5) 0.2500 0.12(2) Uiso 0.12 d SP . . O2WF O 0.150(5) 0.101(5) 0.379(3) 0.12(2) Uiso 0.09 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 Gd 0.02335(17) 0.02335(17) 0.0224(2) 0.000 0.000 0.01168(9) Cu 0.0214(4) 0.0352(6) 0.0243(4) 0.000 0.000 0.0155(5) O1 0.0350(14) 0.0296(16) 0.0345(14) 0.0028(12) -0.0080(12) 0.0137(12) O2 0.0360(16) 0.0342(16) 0.0524(17) 0.0002(15) -0.0219(15) 0.0103(14) O3 0.0328(13) 0.0282(18) 0.0353(18) 0.000 -0.0138(19) 0.0141(9) C1 0.027(2) 0.035(2) 0.031(2) -0.0008(19) -0.0048(18) 0.0148(18) C2 0.043(3) 0.033(2) 0.068(3) 0.005(2) -0.032(3) 0.007(2) O1W 0.045(3) 0.059(3) 0.042(3) 0.000 0.000 0.027(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 Gd O1 2.412(3) 24_556 ? Gd O1 2.412(3) 3_665 ? Gd O1 2.412(3) 22_666 ? Gd O1 2.412(3) . ? Gd O1 2.412(3) 2_655 ? Gd O1 2.412(3) 23_656 ? Gd O3 2.483(3) 3_665 ? Gd O3 2.483(3) . ? Gd O3 2.483(3) 2_655 ? Cu O2 1.955(3) 4_765 ? Cu O2 1.955(3) 13_766 ? Cu O2 1.955(3) . ? Cu O2 1.955(3) 16_556 ? Cu O1W 2.510(5) 8_655 ? Cu O1W 2.510(5) 20_666 ? O1 C1 1.251(5) . ? O2 C1 1.247(5) . ? O3 C2 1.405(4) . ? O3 C2 1.405(4) 23_656 ? C1 C2 1.503(5) . ? O1W Cu 2.510(5) 8_654 ? 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 Gd O1 126.21(12) 24_556 3_665 ? O1 Gd O1 79.99(10) 24_556 22_666 ? O1 Gd O1 85.26(13) 3_665 22_666 ? O1 Gd O1 85.26(13) 24_556 . ? O1 Gd O1 79.99(10) 3_665 . ? O1 Gd O1 147.07(12) 22_666 . ? O1 Gd O1 147.07(12) 24_556 2_655 ? O1 Gd O1 79.99(9) 3_665 2_655 ? O1 Gd O1 126.21(12) 22_666 2_655 ? O1 Gd O1 79.99(10) . 2_655 ? O1 Gd O1 79.99(10) 24_556 23_656 ? O1 Gd O1 147.07(12) 3_665 23_656 ? O1 Gd O1 79.99(10) 22_666 23_656 ? O1 Gd O1 126.21(12) . 23_656 ? O1 Gd O1 85.26(13) 2_655 23_656 ? O1 Gd O3 63.11(6) 24_556 3_665 ? O1 Gd O3 63.11(6) 3_665 3_665 ? O1 Gd O3 73.54(6) 22_666 3_665 ? O1 Gd O3 73.54(6) . 3_665 ? O1 Gd O3 137.37(6) 2_655 3_665 ? O1 Gd O3 137.37(6) 23_656 3_665 ? O1 Gd O3 73.54(6) 24_556 . ? O1 Gd O3 137.37(6) 3_665 . ? O1 Gd O3 137.37(6) 22_666 . ? O1 Gd O3 63.11(6) . . ? O1 Gd O3 73.54(6) 2_655 . ? O1 Gd O3 63.11(6) 23_656 . ? O3 Gd O3 120.0 3_665 . ? O1 Gd O3 137.37(6) 24_556 2_655 ? O1 Gd O3 73.54(6) 3_665 2_655 ? O1 Gd O3 63.11(6) 22_666 2_655 ? O1 Gd O3 137.37(6) . 2_655 ? O1 Gd O3 63.11(6) 2_655 2_655 ? O1 Gd O3 73.54(6) 23_656 2_655 ? O3 Gd O3 120.0 3_665 2_655 ? O3 Gd O3 120.0 . 2_655 ? O2 Cu O2 88.62(19) 4_765 13_766 ? O2 Cu O2 91.38(19) 4_765 . ? O2 Cu O2 180.0 13_766 . ? O2 Cu O2 180.0 4_765 16_556 ? O2 Cu O2 91.38(19) 13_766 16_556 ? O2 Cu O2 88.62(19) . 16_556 ? O2 Cu O1W 84.14(11) 4_765 8_655 ? O2 Cu O1W 84.14(11) 13_766 8_655 ? O2 Cu O1W 95.86(12) . 8_655 ? O2 Cu O1W 95.86(12) 16_556 8_655 ? O2 Cu O1W 95.86(11) 4_765 20_666 ? O2 Cu O1W 95.86(11) 13_766 20_666 ? O2 Cu O1W 84.14(11) . 20_666 ? O2 Cu O1W 84.14(11) 16_556 20_666 ? O1W Cu O1W 180.0 8_655 20_666 ? C1 O1 Gd 126.4(2) . . ? C1 O2 Cu 130.6(3) . . ? C2 O3 C2 114.7(4) . 23_656 ? C2 O3 Gd 122.7(2) . . ? C2 O3 Gd 122.7(2) 23_656 . ? O2 C1 O1 126.7(4) . . ? O2 C1 C2 115.4(4) . . ? O1 C1 C2 118.0(3) . . ? O3 C2 C1 109.2(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 Gd O1 C1 66.1(3) 24_556 . . . ? O1 Gd O1 C1 -165.8(3) 3_665 . . . ? O1 Gd O1 C1 129.4(3) 22_666 . . . ? O1 Gd O1 C1 -84.3(4) 2_655 . . . ? O1 Gd O1 C1 -7.8(3) 23_656 . . . ? O3 Gd O1 C1 129.4(3) 3_665 . . . ? O3 Gd O1 C1 -7.8(3) . . . . ? O3 Gd O1 C1 -113.9(3) 2_655 . . . ? O2 Cu O2 C1 75.0(4) 4_765 . . . ? O2 Cu O2 C1 -63(100) 13_766 . . . ? O2 Cu O2 C1 -105.0(4) 16_556 . . . ? O1W Cu O2 C1 -9.2(4) 8_655 . . . ? O1W Cu O2 C1 170.8(4) 20_666 . . . ? O1 Gd O3 C2 -87.5(3) 24_556 . . . ? O1 Gd O3 C2 38.5(3) 3_665 . . . ? O1 Gd O3 C2 -141.5(3) 22_666 . . . ? O1 Gd O3 C2 5.5(3) . . . . ? O1 Gd O3 C2 92.5(3) 2_655 . . . ? O1 Gd O3 C2 -174.5(3) 23_656 . . . ? O3 Gd O3 C2 -43.2(3) 3_665 . . . ? O3 Gd O3 C2 136.8(3) 2_655 . . . ? O1 Gd O3 C2 92.5(3) 24_556 . . 23_656 ? O1 Gd O3 C2 -141.5(3) 3_665 . . 23_656 ? O1 Gd O3 C2 38.5(3) 22_666 . . 23_656 ? O1 Gd O3 C2 -174.5(3) . . . 23_656 ? O1 Gd O3 C2 -87.5(3) 2_655 . . 23_656 ? O1 Gd O3 C2 5.5(3) 23_656 . . 23_656 ? O3 Gd O3 C2 136.8(3) 3_665 . . 23_656 ? O3 Gd O3 C2 -43.2(3) 2_655 . . 23_656 ? Cu O2 C1 O1 -2.8(7) . . . . ? Cu O2 C1 C2 176.1(3) . . . . ? Gd O1 C1 O2 -172.1(3) . . . . ? Gd O1 C1 C2 9.0(6) . . . . ? C2 O3 C2 C1 176.3(5) 23_656 . . . ? Gd O3 C2 C1 -3.7(5) . . . . ? O2 C1 C2 O3 178.0(4) . . . . ? O1 C1 C2 O3 -3.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.301 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.073 ############################################################################ data_EuCuODA _audit_creation_method SHELXL-97 _chemical_name_systematic ; Europium Copper Oxydiacetate ; _chemical_formula_sum 'C24 H60 Cu3 Eu2 O48' _chemical_formula_weight 1611.26 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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 14.872(1) _cell_length_b 14.872(1) _cell_length_c 15.019(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2876.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedra _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1602 _exptl_absorpt_coefficient_mu 3.352 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'XEMP in SHELXTL/PC, Sheldrick, 1991' _exptl_absorpt_correction_T_min 0.18 _exptl_absorpt_correction_T_max 0.29 _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_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 98 _diffrn_standards_decay_% <2 _diffrn_reflns_number 3327 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.019 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.06 _reflns_number_total 896 _reflns_number_gt 730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.067P)^2^+13.29P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_number_reflns 896 _refine_ls_number_parameters 70 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.042 _refine_ls_R_factor_gt 0.035 _refine_ls_wR_factor_ref 0.106 _refine_ls_wR_factor_gt 0.100 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max <0.01 _refine_ls_shift/su_mean <0.01 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu Eu 0.6667 0.3333 0.2500 0.0197(3) Uani 1 d S . . Cu Cu 1.0000 0.5000 0.5000 0.0230(4) Uani 1 d S . . O1 O 0.8060(3) 0.4196(3) 0.3572(3) 0.0315(9) Uani 1 d . . . O2 O 0.9491(3) 0.5571(3) 0.4091(3) 0.0413(10) Uani 1 d . . . O3 O 0.76342(19) 0.5268(4) 0.2500 0.0285(11) Uani 1 d S . . C1 C 0.8701(4) 0.5145(4) 0.3603(4) 0.0284(12) Uani 1 d . . . C2 C 0.8518(5) 0.5861(5) 0.3022(5) 0.0491(18) Uani 1 d . . . H2A H 0.8419 0.6341 0.3389 0.059 Uiso 1 calc R . . H2B H 0.9116 0.6260 0.2642 0.059 Uiso 1 calc R . . O1W O 0.4793(5) 0.3217(5) 0.0000 0.0458(16) Uani 1 d S . . H1W H 0.540(5) 0.361(6) 0.046(5) 0.07(2) Uiso 1 d . . . O2WA O 0.256(3) 0.192(3) 0.0000 0.13(1) Uiso 0.40 d SP . . O2WB O 0.849(3) 0.834(3) 0.320(3) 0.13(1) Uiso 0.24 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 Eu 0.0198(3) 0.0198(3) 0.0193(4) 0.000 0.000 0.00992(15) Cu 0.0181(6) 0.0320(7) 0.0208(6) 0.000 0.000 0.0140(6) O1 0.032(2) 0.027(2) 0.0323(19) 0.0015(16) -0.0090(18) 0.0129(16) O2 0.032(2) 0.033(2) 0.050(2) 0.002(2) -0.022(2) 0.0095(18) O3 0.0272(19) 0.024(3) 0.033(3) 0.000 -0.013(2) 0.0119(13) C1 0.025(3) 0.028(3) 0.031(3) 0.001(3) -0.004(2) 0.012(2) C2 0.038(3) 0.031(3) 0.063(5) 0.003(3) -0.031(3) 0.006(3) O1W 0.042(4) 0.057(4) 0.041(3) 0.000 0.000 0.026(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 Eu O1 2.424(4) 24_556 ? Eu O1 2.424(4) 3_665 ? Eu O1 2.424(4) . ? Eu O1 2.424(4) 22_666 ? Eu O1 2.424(4) 23_656 ? Eu O1 2.424(4) 2_655 ? Eu O3 2.492(5) 3_665 ? Eu O3 2.492(5) 2_655 ? Eu O3 2.492(5) . ? Cu O2 1.951(4) . ? Cu O2 1.951(4) 16_556 ? Cu O2 1.951(4) 4_765 ? Cu O2 1.951(4) 13_766 ? Cu O1W 2.512(7) 20_666 ? Cu O1W 2.512(7) 8_655 ? O1 C1 1.248(6) . ? O2 C1 1.254(6) . ? O3 C2 1.401(6) . ? O3 C2 1.401(6) 23_656 ? C1 C2 1.502(8) . ? O1W Cu 2.512(7) 8_654 ? 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 Eu O1 125.42(17) 24_556 3_665 ? O1 Eu O1 84.50(19) 24_556 . ? O1 Eu O1 80.65(14) 3_665 . ? O1 Eu O1 80.65(14) 24_556 22_666 ? O1 Eu O1 84.50(19) 3_665 22_666 ? O1 Eu O1 147.27(17) . 22_666 ? O1 Eu O1 80.65(14) 24_556 23_656 ? O1 Eu O1 147.27(17) 3_665 23_656 ? O1 Eu O1 125.42(17) . 23_656 ? O1 Eu O1 80.65(14) 22_666 23_656 ? O1 Eu O1 147.27(17) 24_556 2_655 ? O1 Eu O1 80.65(14) 3_665 2_655 ? O1 Eu O1 80.65(14) . 2_655 ? O1 Eu O1 125.42(17) 22_666 2_655 ? O1 Eu O1 84.50(19) 23_656 2_655 ? O1 Eu O3 62.71(8) 24_556 3_665 ? O1 Eu O3 62.71(8) 3_665 3_665 ? O1 Eu O3 73.63(9) . 3_665 ? O1 Eu O3 73.63(9) 22_666 3_665 ? O1 Eu O3 137.75(9) 23_656 3_665 ? O1 Eu O3 137.75(9) 2_655 3_665 ? O1 Eu O3 137.75(9) 24_556 2_655 ? O1 Eu O3 73.63(9) 3_665 2_655 ? O1 Eu O3 137.75(9) . 2_655 ? O1 Eu O3 62.71(8) 22_666 2_655 ? O1 Eu O3 73.63(9) 23_656 2_655 ? O1 Eu O3 62.71(8) 2_655 2_655 ? O3 Eu O3 120.0 3_665 2_655 ? O1 Eu O3 73.63(9) 24_556 . ? O1 Eu O3 137.75(9) 3_665 . ? O1 Eu O3 62.71(8) . . ? O1 Eu O3 137.75(9) 22_666 . ? O1 Eu O3 62.71(8) 23_656 . ? O1 Eu O3 73.63(9) 2_655 . ? O3 Eu O3 120.000(1) 3_665 . ? O3 Eu O3 120.0 2_655 . ? O2 Cu O2 88.9(3) . 16_556 ? O2 Cu O2 91.1(3) . 4_765 ? O2 Cu O2 180.0 16_556 4_765 ? O2 Cu O2 180.0 . 13_766 ? O2 Cu O2 91.1(3) 16_556 13_766 ? O2 Cu O2 88.9(3) 4_765 13_766 ? O2 Cu O1W 84.30(16) . 20_666 ? O2 Cu O1W 84.30(16) 16_556 20_666 ? O2 Cu O1W 95.70(16) 4_765 20_666 ? O2 Cu O1W 95.70(16) 13_766 20_666 ? O2 Cu O1W 95.70(16) . 8_655 ? O2 Cu O1W 95.70(16) 16_556 8_655 ? O2 Cu O1W 84.30(16) 4_765 8_655 ? O2 Cu O1W 84.30(16) 13_766 8_655 ? O1W Cu O1W 180.0 20_666 8_655 ? C1 O1 Eu 126.2(3) . . ? C1 O2 Cu 131.1(4) . . ? C2 O3 C2 114.0(6) . 23_656 ? C2 O3 Eu 123.0(3) . . ? C2 O3 Eu 123.0(3) 23_656 . ? O1 C1 O2 125.9(5) . . ? O1 C1 C2 118.2(5) . . ? O2 C1 C2 115.9(5) . . ? O3 C2 C1 109.0(5) . . ? 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 Eu O1 C1 65.6(4) 24_556 . . . ? O1 Eu O1 C1 -167.1(4) 3_665 . . . ? O1 Eu O1 C1 128.7(5) 22_666 . . . ? O1 Eu O1 C1 -8.9(4) 23_656 . . . ? O1 Eu O1 C1 -85.2(5) 2_655 . . . ? O3 Eu O1 C1 128.7(5) 3_665 . . . ? O3 Eu O1 C1 -114.4(4) 2_655 . . . ? O3 Eu O1 C1 -8.9(4) . . . . ? O2 Cu O2 C1 -103.2(5) 16_556 . . . ? O2 Cu O2 C1 76.8(5) 4_765 . . . ? O2 Cu O2 C1 -35(100) 13_766 . . . ? O1W Cu O2 C1 172.4(6) 20_666 . . . ? O1W Cu O2 C1 -7.6(6) 8_655 . . . ? O1 Eu O3 C2 -85.7(4) 24_556 . . . ? O1 Eu O3 C2 39.4(4) 3_665 . . . ? O1 Eu O3 C2 6.5(4) . . . . ? O1 Eu O3 C2 -140.6(4) 22_666 . . . ? O1 Eu O3 C2 -173.5(4) 23_656 . . . ? O1 Eu O3 C2 94.3(4) 2_655 . . . ? O3 Eu O3 C2 -41.9(4) 3_665 . . . ? O3 Eu O3 C2 138.1(4) 2_655 . . . ? O1 Eu O3 C2 94.3(4) 24_556 . . 23_656 ? O1 Eu O3 C2 -140.6(4) 3_665 . . 23_656 ? O1 Eu O3 C2 -173.5(4) . . . 23_656 ? O1 Eu O3 C2 39.4(4) 22_666 . . 23_656 ? O1 Eu O3 C2 6.5(4) 23_656 . . 23_656 ? O1 Eu O3 C2 -85.7(4) 2_655 . . 23_656 ? O3 Eu O3 C2 138.1(4) 3_665 . . 23_656 ? O3 Eu O3 C2 -41.9(4) 2_655 . . 23_656 ? Eu O1 C1 O2 -171.1(4) . . . . ? Eu O1 C1 C2 10.1(8) . . . . ? Cu O2 C1 O1 -3.5(9) . . . . ? Cu O2 C1 C2 175.4(4) . . . . ? C2 O3 C2 C1 175.5(7) 23_656 . . . ? Eu O3 C2 C1 -4.5(7) . . . . ? O1 C1 C2 O3 -3.1(8) . . . . ? O2 C1 C2 O3 178.0(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.967 _refine_diff_density_min -1.272 _refine_diff_density_rms 0.160 ########################################################################## data_NdCuODA _audit_creation_method SHELXL-97 _chemical_name_systematic ; Neodimium Copper Oxydiacetate ; _chemical_formula_sum 'C24 H60 Cu3 Nd2 O48' _chemical_formula_weight 1595.82 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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' _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 15.0645(16) _cell_length_b 15.0645(16) _cell_length_c 14.751(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2899.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedra _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.828 _exptl_crystal_F_000 1590 _exptl_absorpt_coefficient_mu 2.954 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'XEMP in SHELXTL/PC, Sheldrick, 1991' _exptl_absorpt_correction_T_min 0.36 _exptl_absorpt_correction_T_max 0.28 _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_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 98 _diffrn_standards_decay_% <2 _diffrn_reflns_number 3353 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.05 _reflns_number_total 902 _reflns_number_gt 722 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens XDISK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0773P)^2^+19.0529P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 902 _refine_ls_number_parameters 80 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.903 _refine_ls_shift/su_max <0.001 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd Nd 0.6667 0.3333 0.2500 0.0201(3) Uani 1 d S . . Cu Cu 1.0000 0.5000 0.5000 0.0236(3) Uani 1 d S . . O1 O 0.8075(3) 0.4219(3) 0.3589(3) 0.0322(9) Uani 1 d . . . O2 O 0.9510(3) 0.5581(3) 0.4076(3) 0.0407(10) Uani 1 d . . . O3 O 0.76374(19) 0.5275(4) 0.2500 0.0296(12) Uani 1 d S . . C1 C 0.8722(4) 0.5158(4) 0.3601(4) 0.0291(12) Uani 1 d . . . C2 C 0.8540(5) 0.5859(4) 0.3004(5) 0.0486(18) Uani 1 d . . . H2A H 0.8474 0.6356 0.3373 0.058 Uiso 1 calc R . . H2B H 0.9117 0.6227 0.2597 0.058 Uiso 1 calc R . . O1W O 0.4765(5) 0.3207(6) 0.0000 0.0470(17) Uani 1 d S . . H1W H 0.519(6) 0.341(6) 0.048(4) 0.07(2) Uiso 1 d . . . O2WA O 0.276(4) 0.164(4) 0.0000 0.12(2) Uiso 0.30 d SP . . O2WB O 0.203(7) 0.225(7) 0.0000 0.12(3) Uiso 0.16 d SP . . O2WC O 0.846(8) 0.858(7) 0.283(6) 0.13(3) Uiso 0.10 d P . . O2WD O 0.845(6) 0.891(7) 0.387(5) 0.13(3) Uiso 0.12 d P . . O2WE O 0.253(2) 0.208(2) -0.032(2) 0.12(1) Uiso 0.27 d P . . O2WF O 0.829(5) 0.972(5) 0.330(4) 0.12(2) Uiso 0.16 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 Nd 0.0210(3) 0.0210(3) 0.0184(4) 0.000 0.000 0.01048(15) Cu 0.0209(6) 0.0356(8) 0.0175(6) 0.000 0.000 0.0164(6) O1 0.032(2) 0.030(2) 0.0324(19) 0.0034(17) -0.0097(18) 0.0129(16) O2 0.033(2) 0.037(2) 0.045(2) 0.004(2) -0.021(2) 0.0118(19) O3 0.0273(19) 0.026(3) 0.035(3) 0.000 -0.014(2) 0.0130(13) C1 0.026(3) 0.034(3) 0.027(3) 0.002(3) -0.004(2) 0.014(2) C2 0.041(4) 0.028(3) 0.063(5) 0.003(3) -0.033(3) 0.007(3) O1W 0.045(4) 0.065(5) 0.032(3) 0.000 0.000 0.029(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd O1 2.456(4) 24_556 ? Nd O1 2.456(4) 3_665 ? Nd O1 2.456(4) 22_666 ? Nd O1 2.456(4) . ? Nd O1 2.456(4) 23_656 ? Nd O1 2.456(4) 2_655 ? Nd O3 2.533(5) 3_665 ? Nd O3 2.533(5) 2_655 ? Nd O3 2.533(5) . ? Cu O2 1.954(4) 4_765 ? Cu O2 1.954(4) . ? Cu O2 1.954(4) 13_766 ? Cu O2 1.954(4) 16_556 ? Cu O1W 2.542(8) 20_666 ? Cu O1W 2.542(7) 8_655 ? O1 C1 1.254(6) . ? O2 C1 1.245(7) . ? O3 C2 1.407(6) . ? O3 C2 1.407(6) 23_656 ? C1 C2 1.501(8) . ? O1W Cu 2.542(7) 8_654 ? 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 Nd O1 123.87(16) 24_556 3_665 ? O1 Nd O1 81.83(14) 24_556 22_666 ? O1 Nd O1 83.17(18) 3_665 22_666 ? O1 Nd O1 83.17(18) 24_556 . ? O1 Nd O1 81.83(14) 3_665 . ? O1 Nd O1 147.78(17) 22_666 . ? O1 Nd O1 81.83(13) 24_556 23_656 ? O1 Nd O1 147.78(17) 3_665 23_656 ? O1 Nd O1 81.83(13) 22_666 23_656 ? O1 Nd O1 123.87(16) . 23_656 ? O1 Nd O1 147.78(17) 24_556 2_655 ? O1 Nd O1 81.83(13) 3_665 2_655 ? O1 Nd O1 123.87(16) 22_666 2_655 ? O1 Nd O1 81.83(13) . 2_655 ? O1 Nd O1 83.17(18) 23_656 2_655 ? O1 Nd O3 61.93(8) 24_556 3_665 ? O1 Nd O3 61.93(8) 3_665 3_665 ? O1 Nd O3 73.89(9) 22_666 3_665 ? O1 Nd O3 73.89(9) . 3_665 ? O1 Nd O3 138.42(9) 23_656 3_665 ? O1 Nd O3 138.42(9) 2_655 3_665 ? O1 Nd O3 138.42(9) 24_556 2_655 ? O1 Nd O3 73.89(9) 3_665 2_655 ? O1 Nd O3 61.93(8) 22_666 2_655 ? O1 Nd O3 138.42(9) . 2_655 ? O1 Nd O3 73.89(9) 23_656 2_655 ? O1 Nd O3 61.93(8) 2_655 2_655 ? O3 Nd O3 120.0 3_665 2_655 ? O1 Nd O3 73.89(9) 24_556 . ? O1 Nd O3 138.42(9) 3_665 . ? O1 Nd O3 138.42(9) 22_666 . ? O1 Nd O3 61.93(8) . . ? O1 Nd O3 61.93(8) 23_656 . ? O1 Nd O3 73.89(9) 2_655 . ? O3 Nd O3 120.0 3_665 . ? O3 Nd O3 120.0 2_655 . ? O2 Cu O2 91.5(3) 4_765 . ? O2 Cu O2 88.5(3) 4_765 13_766 ? O2 Cu O2 180.000(1) . 13_766 ? O2 Cu O2 180.0 4_765 16_556 ? O2 Cu O2 88.5(3) . 16_556 ? O2 Cu O2 91.5(3) 13_766 16_556 ? O2 Cu O1W 96.96(16) 4_765 20_666 ? O2 Cu O1W 83.04(16) . 20_666 ? O2 Cu O1W 96.96(16) 13_766 20_666 ? O2 Cu O1W 83.04(16) 16_556 20_666 ? O2 Cu O1W 83.04(16) 4_765 8_655 ? O2 Cu O1W 96.96(16) . 8_655 ? O2 Cu O1W 83.04(16) 13_766 8_655 ? O2 Cu O1W 96.96(16) 16_556 8_655 ? O1W Cu O1W 180.0 20_666 8_655 ? C1 O1 Nd 126.5(3) . . ? C1 O2 Cu 129.8(4) . . ? C2 O3 C2 114.5(6) . 23_656 ? C2 O3 Nd 122.8(3) . . ? C2 O3 Nd 122.8(3) 23_656 . ? O2 C1 O1 126.1(5) . . ? O2 C1 C2 115.6(5) . . ? O1 C1 C2 118.2(5) . . ? O3 C2 C1 109.2(5) . . ? 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 Nd O1 C1 64.7(4) 24_556 . . . ? O1 Nd O1 C1 -169.6(4) 3_665 . . . ? O1 Nd O1 C1 127.4(5) 22_666 . . . ? O1 Nd O1 C1 -10.7(4) 23_656 . . . ? O1 Nd O1 C1 -86.7(5) 2_655 . . . ? O3 Nd O1 C1 127.4(5) 3_665 . . . ? O3 Nd O1 C1 -115.3(4) 2_655 . . . ? O3 Nd O1 C1 -10.7(4) . . . . ? O2 Cu O2 C1 77.9(5) 4_765 . . . ? O2 Cu O2 C1 -87(100) 13_766 . . . ? O2 Cu O2 C1 -102.1(5) 16_556 . . . ? O1W Cu O2 C1 174.7(5) 20_666 . . . ? O1W Cu O2 C1 -5.3(5) 8_655 . . . ? O1 Nd O3 C2 -81.9(4) 24_556 . . . ? O1 Nd O3 C2 41.4(4) 3_665 . . . ? O1 Nd O3 C2 -138.6(4) 22_666 . . . ? O1 Nd O3 C2 8.9(4) . . . . ? O1 Nd O3 C2 -171.1(4) 23_656 . . . ? O1 Nd O3 C2 98.1(4) 2_655 . . . ? O3 Nd O3 C2 -39.0(4) 3_665 . . . ? O3 Nd O3 C2 141.0(4) 2_655 . . . ? O1 Nd O3 C2 98.1(4) 24_556 . . 23_656 ? O1 Nd O3 C2 -138.6(4) 3_665 . . 23_656 ? O1 Nd O3 C2 41.4(4) 22_666 . . 23_656 ? O1 Nd O3 C2 -171.1(4) . . . 23_656 ? O1 Nd O3 C2 8.9(4) 23_656 . . 23_656 ? O1 Nd O3 C2 -81.9(4) 2_655 . . 23_656 ? O3 Nd O3 C2 141.0(4) 3_665 . . 23_656 ? O3 Nd O3 C2 -39.0(4) 2_655 . . 23_656 ? Cu O2 C1 O1 -3.7(9) . . . . ? Cu O2 C1 C2 175.3(4) . . . . ? Nd O1 C1 O2 -169.9(4) . . . . ? Nd O1 C1 C2 11.2(8) . . . . ? C2 O3 C2 C1 172.7(7) 23_656 . . . ? Nd O3 C2 C1 -7.3(7) . . . . ? O2 C1 C2 O3 179.0(5) . . . . ? O1 C1 C2 O3 -2.0(8) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.784 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.236 ############################################################################ data_PrCuODA _audit_creation_method SHELXL-97 _chemical_name_systematic ; Praseodimium Copper Oxydiacetate ; _chemical_formula_sum 'C24 H60 Cu3 O48 Pr2 ' _chemical_formula_weight 1589.16 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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 15.199(2) _cell_length_b 15.199(2) _cell_length_c 14.584(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2917.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedra _exptl_crystal_colour blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.809 _exptl_crystal_F_000 1586 _exptl_absorpt_coefficient_mu 2.825 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'XEMP in SHELXTL/PC, Sheldrick, 1991' _exptl_absorpt_correction_T_min 0.33 _exptl_absorpt_correction_T_max 0.38 _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_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 98 _diffrn_standards_decay_% <2 _diffrn_reflns_number 6666 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0123 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.03 _reflns_number_total 906 _reflns_number_gt 773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens XDISK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.077P)^2^+19.053P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 906 _refine_ls_number_parameters 81 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_shift/su_max <0.001 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr Pr 0.6667 0.3333 0.2500 0.0212(3) Uani 1 d S . . Cu Cu 1.0000 0.5000 0.5000 0.0243(3) Uani 1 d S . . O1 O 0.8080(3) 0.4229(2) 0.3593(2) 0.0318(8) Uani 1 d . . . O2 O 0.9517(3) 0.5580(3) 0.4064(3) 0.0408(9) Uani 1 d . . . O3 O 0.76381(17) 0.5276(3) 0.2500 0.0295(11) Uani 1 d S . . C1 C 0.8725(4) 0.5155(4) 0.3598(3) 0.0292(11) Uani 1 d . . . C2 C 0.8544(4) 0.5853(4) 0.2995(4) 0.0460(15) Uani 1 d . . . H2A H 0.8493 0.6354 0.3368 0.055 Uiso 1 calc R . . H2B H 0.9108 0.6208 0.2574 0.055 Uiso 1 calc R . . O1W O 0.4755(5) 0.3202(5) 0.0000 0.0489(15) Uani 1 d S . . H1W H 0.524(7) 0.345(7) 0.046(5) 0.12(4) Uiso 1 d . . . O2WA O 0.275(4) 0.158(4) 0.0000 0.13(2) Uiso 0.28 d SP . . O2WB O 0.844(7) 0.856(7) 0.284(5) 0.14(3) Uiso 0.11 d P . . O2WC O 0.840(5) 0.890(6) 0.385(4) 0.14(2) Uiso 0.14 d P . . O2WD O 0.260(2) 0.205(2) -0.0350(18) 0.13(1) Uiso 0.31 d P . . O2WE O 0.223(5) 0.231(5) 0.0000 0.14(2) Uiso 0.22 d SP . . O2WF O 0.828(4) 0.969(4) 0.328(3) 0.13(2) Uiso 0.18 d P . . O2WG O 1.0000 1.0000 0.5000 0.14(12) Uiso 0.10 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 Pr 0.0207(3) 0.0207(3) 0.0221(4) 0.000 0.000 0.01034(15) Cu 0.0213(6) 0.0377(7) 0.0183(6) 0.000 0.000 0.0180(5) O1 0.0321(18) 0.0274(18) 0.0327(17) 0.0016(15) -0.0128(16) 0.0126(14) O2 0.035(2) 0.036(2) 0.044(2) 0.0025(18) -0.0221(18) 0.0120(16) O3 0.0283(18) 0.025(2) 0.034(2) 0.000 -0.0138(18) 0.0125(12) C1 0.025(2) 0.034(3) 0.026(2) 0.002(2) -0.005(2) 0.014(2) C2 0.035(3) 0.028(3) 0.060(4) 0.005(3) -0.030(3) 0.005(2) O1W 0.045(4) 0.065(4) 0.038(3) 0.000 0.000 0.028(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 Pr O1 2.467(3) 3_665 ? Pr O1 2.467(3) 24_556 ? Pr O1 2.467(3) . ? Pr O1 2.467(3) 22_666 ? Pr O1 2.467(3) 2_655 ? Pr O1 2.467(3) 23_656 ? Pr O3 2.557(5) 3_665 ? Pr O3 2.557(5) 2_655 ? Pr O3 2.557(5) . ? Cu O2 1.955(3) 16_556 ? Cu O2 1.955(3) . ? Cu O2 1.955(3) 13_766 ? Cu O2 1.955(3) 4_765 ? Cu O1W 2.566(7) 8_655 ? Cu O1W 2.566(7) 20_666 ? O1 C1 1.250(6) . ? O2 C1 1.246(6) . ? O3 C2 1.406(5) . ? O3 C2 1.406(5) 23_656 ? C1 C2 1.505(7) . ? O1W Cu 2.566(7) 8_654 ? 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 Pr O1 122.88(15) 3_665 24_556 ? O1 Pr O1 82.77(12) 3_665 . ? O1 Pr O1 82.05(17) 24_556 . ? O1 Pr O1 82.05(17) 3_665 22_666 ? O1 Pr O1 82.77(12) 24_556 22_666 ? O1 Pr O1 147.91(15) . 22_666 ? O1 Pr O1 82.77(12) 3_665 2_655 ? O1 Pr O1 147.91(15) 24_556 2_655 ? O1 Pr O1 82.77(12) . 2_655 ? O1 Pr O1 122.88(15) 22_666 2_655 ? O1 Pr O1 147.91(16) 3_665 23_656 ? O1 Pr O1 82.77(12) 24_556 23_656 ? O1 Pr O1 122.88(15) . 23_656 ? O1 Pr O1 82.77(12) 22_666 23_656 ? O1 Pr O1 82.05(17) 2_655 23_656 ? O1 Pr O3 61.44(7) 3_665 3_665 ? O1 Pr O3 61.44(7) 24_556 3_665 ? O1 Pr O3 73.96(8) . 3_665 ? O1 Pr O3 73.96(8) 22_666 3_665 ? O1 Pr O3 138.98(8) 2_655 3_665 ? O1 Pr O3 138.98(8) 23_656 3_665 ? O1 Pr O3 73.96(8) 3_665 2_655 ? O1 Pr O3 138.98(8) 24_556 2_655 ? O1 Pr O3 138.98(8) . 2_655 ? O1 Pr O3 61.44(7) 22_666 2_655 ? O1 Pr O3 61.44(7) 2_655 2_655 ? O1 Pr O3 73.96(8) 23_656 2_655 ? O3 Pr O3 120.0 3_665 2_655 ? O1 Pr O3 138.98(8) 3_665 . ? O1 Pr O3 73.96(8) 24_556 . ? O1 Pr O3 61.44(7) . . ? O1 Pr O3 138.98(8) 22_666 . ? O1 Pr O3 73.96(8) 2_655 . ? O1 Pr O3 61.44(7) 23_656 . ? O3 Pr O3 120.0 3_665 . ? O3 Pr O3 120.0 2_655 . ? O2 Cu O2 88.5(2) 16_556 . ? O2 Cu O2 91.5(2) 16_556 13_766 ? O2 Cu O2 180.0 . 13_766 ? O2 Cu O2 180.0 16_556 4_765 ? O2 Cu O2 91.5(2) . 4_765 ? O2 Cu O2 88.5(2) 13_766 4_765 ? O2 Cu O1W 97.32(14) 16_556 8_655 ? O2 Cu O1W 97.32(14) . 8_655 ? O2 Cu O1W 82.68(14) 13_766 8_655 ? O2 Cu O1W 82.68(14) 4_765 8_655 ? O2 Cu O1W 82.68(14) 16_556 20_666 ? O2 Cu O1W 82.68(14) . 20_666 ? O2 Cu O1W 97.32(14) 13_766 20_666 ? O2 Cu O1W 97.32(14) 4_765 20_666 ? O1W Cu O1W 180.0 8_655 20_666 ? C1 O1 Pr 127.0(3) . . ? C1 O2 Cu 129.2(3) . . ? C2 O3 C2 114.7(5) . 23_656 ? C2 O3 Pr 122.7(3) . . ? C2 O3 Pr 122.7(3) 23_656 . ? O2 C1 O1 126.6(5) . . ? O2 C1 C2 115.1(4) . . ? O1 C1 C2 118.2(4) . . ? O3 C2 C1 109.1(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 Pr O1 C1 -170.6(4) 3_665 . . . ? O1 Pr O1 C1 64.6(4) 24_556 . . . ? O1 Pr O1 C1 127.1(4) 22_666 . . . ? O1 Pr O1 C1 -87.1(5) 2_655 . . . ? O1 Pr O1 C1 -11.4(4) 23_656 . . . ? O3 Pr O1 C1 127.1(4) 3_665 . . . ? O3 Pr O1 C1 -115.4(4) 2_655 . . . ? O3 Pr O1 C1 -11.4(4) . . . . ? O2 Cu O2 C1 -101.0(5) 16_556 . . . ? O2 Cu O2 C1 58(100) 13_766 . . . ? O2 Cu O2 C1 79.0(5) 4_765 . . . ? O1W Cu O2 C1 -3.8(5) 8_655 . . . ? O1W Cu O2 C1 176.2(5) 20_666 . . . ? O1 Pr O3 C2 42.2(4) 3_665 . . . ? O1 Pr O3 C2 -79.8(4) 24_556 . . . ? O1 Pr O3 C2 9.8(3) . . . . ? O1 Pr O3 C2 -137.8(4) 22_666 . . . ? O1 Pr O3 C2 100.2(4) 2_655 . . . ? O1 Pr O3 C2 -170.2(3) 23_656 . . . ? O3 Pr O3 C2 -37.6(3) 3_665 . . . ? O3 Pr O3 C2 142.4(3) 2_655 . . . ? O1 Pr O3 C2 -137.8(4) 3_665 . . 23_656 ? O1 Pr O3 C2 100.2(4) 24_556 . . 23_656 ? O1 Pr O3 C2 -170.2(3) . . . 23_656 ? O1 Pr O3 C2 42.2(4) 22_666 . . 23_656 ? O1 Pr O3 C2 -79.8(4) 2_655 . . 23_656 ? O1 Pr O3 C2 9.8(3) 23_656 . . 23_656 ? O3 Pr O3 C2 142.4(3) 3_665 . . 23_656 ? O3 Pr O3 C2 -37.6(3) 2_655 . . 23_656 ? Cu O2 C1 O1 -4.5(8) . . . . ? Cu O2 C1 C2 174.7(4) . . . . ? Pr O1 C1 O2 -169.0(4) . . . . ? Pr O1 C1 C2 11.7(7) . . . . ? C2 O3 C2 C1 171.7(6) 23_656 . . . ? Pr O3 C2 C1 -8.3(6) . . . . ? O2 C1 C2 O3 179.1(4) . . . . ? O1 C1 C2 O3 -1.6(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.663 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.211 ############################################################################