# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H5 Cd3 La N6 O13' _chemical_formula_sum 'C15 H5 Cd3 La N6 O13' _chemical_formula_weight 953.36 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pa-3 _symmetry_space_group_name_Hall -P2ac2ab3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 16.8594(13) _cell_length_b 16.8594(12) _cell_length_c 16.8594(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4792.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2742 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.65 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 4.450 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8421 _exptl_absorpt_correction_T_max 0.8421 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 10247 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 30.51 _reflns_number_total 2439 _reflns_number_gt 1744 _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^)+(0.0444P)^2^+8.3123P] 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 2439 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 La1 La 0.770846(18) 0.270846(18) 0.229154(18) 0.01016(13) Uani 1 3 d S . . Cd1 Cd 0.70260(2) 0.49045(3) 0.17658(3) 0.01512(12) Uani 1 1 d . . . C1 C 0.7619(4) 0.3775(4) 0.0402(4) 0.0270(15) Uani 1 1 d . . . C2 C 0.7537(4) 0.4571(4) 0.0036(4) 0.0247(14) Uani 1 1 d . . . C3 C 0.7741(4) 0.4816(4) -0.0725(4) 0.0281(15) Uani 1 1 d . . . H3 H 0.7971 0.4520 -0.1130 0.034 Uiso 1 1 calc R . . C4 C 0.7520(4) 0.5600(4) -0.0733(4) 0.0198(13) Uani 1 1 d . . . C5 C 0.7565(4) 0.6204(4) -0.1362(4) 0.0189(12) Uani 1 1 d . . . N1 N 0.7209(3) 0.5178(3) 0.0462(3) 0.0195(11) Uani 1 1 d . . . N2 N 0.7197(3) 0.5811(3) -0.0019(3) 0.0189(11) Uani 1 1 d . . . O1 O 0.7497(3) 0.3726(2) 0.1158(2) 0.0213(9) Uani 1 1 d . . . O2 O 0.7782(4) 0.3229(3) -0.0056(3) 0.0458(16) Uani 1 1 d . . . O3 O 0.7918(2) 0.6065(3) -0.2014(2) 0.0204(9) Uani 1 1 d . . . O4 O 0.7238(3) 0.6871(3) -0.1230(3) 0.0249(10) Uani 1 1 d . . . O5 O 0.6820(3) 0.1820(3) 0.3180(3) 0.071(4) Uani 1 3 d S . . H5A H 0.7110 0.1555 0.3497 0.106 Uiso 0.33 1 d PR . . H5B H 0.6503 0.2110 0.3445 0.106 Uiso 0.33 1 d PR . . 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 La1 0.01016(13) 0.01016(13) 0.01016(13) -0.00039(11) -0.00039(11) 0.00039(11) Cd1 0.0142(2) 0.0149(2) 0.0163(2) -0.00040(16) 0.00111(16) 0.00134(16) C1 0.039(4) 0.020(3) 0.022(3) 0.004(3) 0.009(3) 0.008(3) C2 0.036(4) 0.018(3) 0.020(3) 0.001(3) 0.008(3) 0.010(3) C3 0.042(4) 0.026(4) 0.016(3) -0.001(3) 0.002(3) 0.013(3) C4 0.021(3) 0.021(3) 0.017(3) 0.004(2) 0.004(2) 0.003(2) C5 0.020(3) 0.016(3) 0.020(3) 0.002(2) -0.003(2) 0.001(2) N1 0.027(3) 0.013(2) 0.019(3) 0.003(2) 0.005(2) 0.002(2) N2 0.025(3) 0.015(2) 0.017(2) 0.000(2) 0.001(2) 0.003(2) O1 0.029(2) 0.017(2) 0.018(2) 0.0042(17) 0.0049(19) 0.0085(18) O2 0.087(5) 0.024(3) 0.027(3) 0.005(2) 0.020(3) 0.027(3) O3 0.022(2) 0.023(2) 0.016(2) 0.0030(17) 0.0004(17) 0.0078(18) O4 0.038(3) 0.019(2) 0.018(2) 0.0006(18) 0.007(2) 0.009(2) O5 0.071(4) 0.071(4) 0.071(4) 0.027(3) 0.027(3) -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 La1 O1 2.593(4) 11_556 ? La1 O1 2.593(4) . ? La1 O1 2.593(4) 8_645 ? La1 O4 2.594(4) 7_564 ? La1 O4 2.594(4) 12_654 ? La1 O4 2.594(4) 2_665 ? La1 O5 2.595(10) . ? La1 O3 2.600(4) 7_564 ? La1 O3 2.600(4) 2_665 ? La1 O3 2.600(4) 12_654 ? La1 C5 2.954(6) 7_564 ? La1 C5 2.954(6) 2_665 ? Cd1 O2 2.181(5) 11_556 ? Cd1 N2 2.183(5) 22_565 ? Cd1 N1 2.267(5) . ? Cd1 O1 2.372(4) . ? Cd1 O4 2.386(4) 22_565 ? Cd1 O3 2.629(4) 2_665 ? C1 O2 1.234(8) . ? C1 O1 1.293(7) . ? C1 C2 1.484(9) . ? C2 N1 1.367(8) . ? C2 C3 1.390(9) . ? C3 C4 1.373(9) . ? C3 H3 0.9300 . ? C4 N2 1.368(8) . ? C4 C5 1.472(8) . ? C5 O3 1.271(7) . ? C5 O4 1.272(7) . ? C5 La1 2.954(6) 2_664 ? N1 N2 1.340(7) . ? N2 Cd1 2.183(5) 19_656 ? O2 Cd1 2.181(5) 8_645 ? O3 La1 2.600(4) 2_664 ? O3 Cd1 2.629(4) 2_664 ? O4 Cd1 2.386(4) 19_656 ? O4 La1 2.594(4) 2_664 ? O5 H5A 0.8507 . ? O5 H5B 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 O1 La1 O1 72.80(16) 11_556 . ? O1 La1 O1 72.80(16) 11_556 8_645 ? O1 La1 O1 72.80(16) . 8_645 ? O1 La1 O4 130.39(14) 11_556 7_564 ? O1 La1 O4 69.12(15) . 7_564 ? O1 La1 O4 122.18(13) 8_645 7_564 ? O1 La1 O4 122.18(13) 11_556 12_654 ? O1 La1 O4 130.39(14) . 12_654 ? O1 La1 O4 69.12(15) 8_645 12_654 ? O4 La1 O4 106.65(12) 7_564 12_654 ? O1 La1 O4 69.12(15) 11_556 2_665 ? O1 La1 O4 122.18(13) . 2_665 ? O1 La1 O4 130.39(14) 8_645 2_665 ? O4 La1 O4 106.65(12) 7_564 2_665 ? O4 La1 O4 106.65(12) 12_654 2_665 ? O1 La1 O5 136.75(10) 11_556 . ? O1 La1 O5 136.75(10) . . ? O1 La1 O5 136.75(10) 8_645 . ? O4 La1 O5 67.84(11) 7_564 . ? O4 La1 O5 67.84(11) 12_654 . ? O4 La1 O5 67.84(11) 2_665 . ? O1 La1 O3 134.94(14) 11_556 7_564 ? O1 La1 O3 67.71(14) . 7_564 ? O1 La1 O3 75.52(13) 8_645 7_564 ? O4 La1 O3 50.51(13) 7_564 7_564 ? O4 La1 O3 72.84(13) 12_654 7_564 ? O4 La1 O3 153.01(15) 2_665 7_564 ? O5 La1 O3 87.98(10) . 7_564 ? O1 La1 O3 67.71(14) 11_556 2_665 ? O1 La1 O3 75.52(13) . 2_665 ? O1 La1 O3 134.94(14) 8_645 2_665 ? O4 La1 O3 72.84(13) 7_564 2_665 ? O4 La1 O3 153.01(15) 12_654 2_665 ? O4 La1 O3 50.51(13) 2_665 2_665 ? O5 La1 O3 87.98(10) . 2_665 ? O3 La1 O3 119.877(12) 7_564 2_665 ? O1 La1 O3 75.52(13) 11_556 12_654 ? O1 La1 O3 134.94(14) . 12_654 ? O1 La1 O3 67.71(14) 8_645 12_654 ? O4 La1 O3 153.01(15) 7_564 12_654 ? O4 La1 O3 50.51(13) 12_654 12_654 ? O4 La1 O3 72.84(13) 2_665 12_654 ? O5 La1 O3 87.98(10) . 12_654 ? O3 La1 O3 119.877(12) 7_564 12_654 ? O3 La1 O3 119.877(12) 2_665 12_654 ? O1 La1 C5 135.15(15) 11_556 7_564 ? O1 La1 C5 62.66(15) . 7_564 ? O1 La1 C5 97.73(15) 8_645 7_564 ? O4 La1 C5 25.47(15) 7_564 7_564 ? O4 La1 C5 92.18(15) 12_654 7_564 ? O4 La1 C5 131.76(15) 2_665 7_564 ? O5 La1 C5 79.88(12) . 7_564 ? O3 La1 C5 25.45(14) 7_564 7_564 ? O3 La1 C5 95.26(14) 2_665 7_564 ? O3 La1 C5 142.43(14) 12_654 7_564 ? O1 La1 C5 62.66(15) 11_556 2_665 ? O1 La1 C5 97.73(15) . 2_665 ? O1 La1 C5 135.15(15) 8_645 2_665 ? O4 La1 C5 92.18(15) 7_564 2_665 ? O4 La1 C5 131.76(15) 12_654 2_665 ? O4 La1 C5 25.47(15) 2_665 2_665 ? O5 La1 C5 79.88(12) . 2_665 ? O3 La1 C5 142.43(14) 7_564 2_665 ? O3 La1 C5 25.45(14) 2_665 2_665 ? O3 La1 C5 95.26(14) 12_654 2_665 ? C5 La1 C5 116.98(7) 7_564 2_665 ? O2 Cd1 N2 138.2(2) 11_556 22_565 ? O2 Cd1 N1 100.9(2) 11_556 . ? N2 Cd1 N1 115.65(19) 22_565 . ? O2 Cd1 O1 86.44(19) 11_556 . ? N2 Cd1 O1 122.17(17) 22_565 . ? N1 Cd1 O1 72.88(16) . . ? O2 Cd1 O4 82.83(19) 11_556 22_565 ? N2 Cd1 O4 72.75(17) 22_565 22_565 ? N1 Cd1 O4 98.51(17) . 22_565 ? O1 Cd1 O4 164.75(15) . 22_565 ? O2 Cd1 O3 76.47(17) 11_556 2_665 ? N2 Cd1 O3 80.10(16) 22_565 2_665 ? N1 Cd1 O3 151.66(16) . 2_665 ? O1 Cd1 O3 78.78(13) . 2_665 ? O4 Cd1 O3 108.97(15) 22_565 2_665 ? O2 C1 O1 127.3(6) . . ? O2 C1 C2 115.8(6) . . ? O1 C1 C2 116.9(6) . . ? N1 C2 C3 111.3(6) . . ? N1 C2 C1 119.7(6) . . ? C3 C2 C1 129.0(6) . . ? C4 C3 C2 103.2(6) . . ? C4 C3 H3 128.4 . . ? C2 C3 H3 128.4 . . ? N2 C4 C3 110.4(5) . . ? N2 C4 C5 118.3(5) . . ? C3 C4 C5 131.3(6) . . ? O3 C5 O4 121.2(6) . . ? O3 C5 C4 121.2(5) . . ? O4 C5 C4 117.6(5) . . ? O3 C5 La1 61.5(3) . 2_664 ? O4 C5 La1 61.2(3) . 2_664 ? C4 C5 La1 167.1(4) . 2_664 ? N2 N1 C2 106.5(5) . . ? N2 N1 Cd1 138.3(4) . . ? C2 N1 Cd1 114.4(4) . . ? N1 N2 C4 108.7(5) . . ? N1 N2 Cd1 134.3(4) . 19_656 ? C4 N2 Cd1 117.0(4) . 19_656 ? C1 O1 Cd1 115.2(4) . . ? C1 O1 La1 138.3(4) . . ? Cd1 O1 La1 106.36(15) . . ? C1 O2 Cd1 134.3(5) . 8_645 ? C5 O3 La1 93.0(3) . 2_664 ? C5 O3 Cd1 143.9(4) . 2_664 ? La1 O3 Cd1 99.01(14) 2_664 2_664 ? C5 O4 Cd1 113.9(4) . 19_656 ? C5 O4 La1 93.3(4) . 2_664 ? Cd1 O4 La1 151.89(19) 19_656 2_664 ? La1 O5 H5A 109.5 . . ? La1 O5 H5B 109.5 . . ? H5A O5 H5B 109.4 . . ? 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 O2 C1 C2 N1 167.3(7) . . . . ? O1 C1 C2 N1 -11.4(10) . . . . ? O2 C1 C2 C3 -11.5(12) . . . . ? O1 C1 C2 C3 169.8(7) . . . . ? N1 C2 C3 C4 0.1(8) . . . . ? C1 C2 C3 C4 179.0(7) . . . . ? C2 C3 C4 N2 -0.4(8) . . . . ? C2 C3 C4 C5 -179.3(7) . . . . ? N2 C4 C5 O3 174.1(6) . . . . ? C3 C4 C5 O3 -7.1(11) . . . . ? N2 C4 C5 O4 -6.0(9) . . . . ? C3 C4 C5 O4 172.8(7) . . . . ? N2 C4 C5 La1 -87(2) . . . 2_664 ? C3 C4 C5 La1 91(2) . . . 2_664 ? C3 C2 N1 N2 0.2(8) . . . . ? C1 C2 N1 N2 -178.8(6) . . . . ? C3 C2 N1 Cd1 -171.1(5) . . . . ? C1 C2 N1 Cd1 9.9(8) . . . . ? O2 Cd1 N1 N2 -89.2(6) 11_556 . . . ? N2 Cd1 N1 N2 70.0(6) 22_565 . . . ? O1 Cd1 N1 N2 -172.0(6) . . . . ? O4 Cd1 N1 N2 -4.9(6) 22_565 . . . ? O3 Cd1 N1 N2 -170.8(5) 2_665 . . . ? O2 Cd1 N1 C2 78.2(5) 11_556 . . . ? N2 Cd1 N1 C2 -122.6(5) 22_565 . . . ? O1 Cd1 N1 C2 -4.6(4) . . . . ? O4 Cd1 N1 C2 162.5(5) 22_565 . . . ? O3 Cd1 N1 C2 -3.4(7) 2_665 . . . ? C2 N1 N2 C4 -0.4(7) . . . . ? Cd1 N1 N2 C4 167.6(5) . . . . ? C2 N1 N2 Cd1 177.8(5) . . . 19_656 ? Cd1 N1 N2 Cd1 -14.1(10) . . . 19_656 ? C3 C4 N2 N1 0.6(8) . . . . ? C5 C4 N2 N1 179.6(5) . . . . ? C3 C4 N2 Cd1 -178.1(5) . . . 19_656 ? C5 C4 N2 Cd1 1.0(7) . . . 19_656 ? O2 C1 O1 Cd1 -171.9(7) . . . . ? C2 C1 O1 Cd1 6.6(8) . . . . ? O2 C1 O1 La1 13.5(13) . . . . ? C2 C1 O1 La1 -167.9(4) . . . . ? O2 Cd1 O1 C1 -103.8(5) 11_556 . . . ? N2 Cd1 O1 C1 108.6(5) 22_565 . . . ? N1 Cd1 O1 C1 -1.3(5) . . . . ? O4 Cd1 O1 C1 -58.6(8) 22_565 . . . ? O3 Cd1 O1 C1 179.3(5) 2_665 . . . ? O2 Cd1 O1 La1 72.4(2) 11_556 . . . ? N2 Cd1 O1 La1 -75.1(2) 22_565 . . . ? N1 Cd1 O1 La1 174.9(2) . . . . ? O4 Cd1 O1 La1 117.6(6) 22_565 . . . ? O3 Cd1 O1 La1 -4.52(15) 2_665 . . . ? O1 La1 O1 C1 108.8(6) 11_556 . . . ? O1 La1 O1 C1 32.0(7) 8_645 . . . ? O4 La1 O1 C1 -103.7(7) 7_564 . . . ? O4 La1 O1 C1 -9.2(7) 12_654 . . . ? O4 La1 O1 C1 159.3(6) 2_665 . . . ? O5 La1 O1 C1 -109.6(7) . . . . ? O3 La1 O1 C1 -49.1(7) 7_564 . . . ? O3 La1 O1 C1 179.5(7) 2_665 . . . ? O3 La1 O1 C1 61.5(7) 12_654 . . . ? C5 La1 O1 C1 -76.6(7) 7_564 . . . ? C5 La1 O1 C1 166.9(7) 2_665 . . . ? O1 La1 O1 Cd1 -66.1(2) 11_556 . . . ? O1 La1 O1 Cd1 -142.90(17) 8_645 . . . ? O4 La1 O1 Cd1 81.48(17) 7_564 . . . ? O4 La1 O1 Cd1 175.96(14) 12_654 . . . ? O4 La1 O1 Cd1 -15.6(2) 2_665 . . . ? O5 La1 O1 Cd1 75.5(2) . . . . ? O3 La1 O1 Cd1 136.1(2) 7_564 . . . ? O3 La1 O1 Cd1 4.63(15) 2_665 . . . ? O3 La1 O1 Cd1 -113.34(18) 12_654 . . . ? C5 La1 O1 Cd1 108.5(2) 7_564 . . . ? C5 La1 O1 Cd1 -7.9(2) 2_665 . . . ? O1 C1 O2 Cd1 -17.8(13) . . . 8_645 ? C2 C1 O2 Cd1 163.6(5) . . . 8_645 ? O4 C5 O3 La1 -14.5(6) . . . 2_664 ? C4 C5 O3 La1 165.4(5) . . . 2_664 ? O4 C5 O3 Cd1 -124.3(6) . . . 2_664 ? C4 C5 O3 Cd1 55.6(9) . . . 2_664 ? La1 C5 O3 Cd1 -109.8(6) 2_664 . . 2_664 ? O3 C5 O4 Cd1 -172.7(4) . . . 19_656 ? C4 C5 O4 Cd1 7.4(7) . . . 19_656 ? La1 C5 O4 Cd1 172.8(4) 2_664 . . 19_656 ? O3 C5 O4 La1 14.5(6) . . . 2_664 ? C4 C5 O4 La1 -165.4(5) . . . 2_664 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.112 _refine_diff_density_min -1.083 _refine_diff_density_rms 0.227 _database_code_depnum_ccdc_archive 'CCDC 968561' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H5 Cd3 Pr N6 O13' _chemical_formula_sum 'C15 H5 Cd3 N6 O13 Pr' _chemical_formula_weight 955.36 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' Cd Cd -0.8075 1.2024 '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 Cubic _symmetry_space_group_name_H-M Pa-3 _symmetry_space_group_name_Hall -P2ac2ab3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 16.8075(4) _cell_length_b 16.8075(4) _cell_length_c 16.8075(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4748.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1379 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.84 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 4.744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4822 _exptl_absorpt_correction_T_max 0.5998 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 10206 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 30.49 _reflns_number_total 2388 _reflns_number_gt 1744 _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^)+(0.0181P)^2^+6.3809P] 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 2388 _refine_ls_number_parameters 115 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0648 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.005 _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 Pr1 Pr 0.773020(16) 0.273020(16) 0.226980(16) 0.01340(10) Uani 1 3 d S . . Cd1 Cd 0.70370(2) 0.49180(2) 0.17540(2) 0.01636(9) Uani 1 1 d . . . C1 C 0.7642(3) 0.3795(3) 0.0400(3) 0.0243(12) Uani 1 1 d . . . C2 C 0.7546(3) 0.4587(3) 0.0027(3) 0.0236(11) Uani 1 1 d . . . C3 C 0.7750(3) 0.4829(3) -0.0738(3) 0.0284(13) Uani 1 1 d . . . H3 H 0.7989 0.4532 -0.1138 0.034 Uiso 1 1 calc R . . C4 C 0.7512(3) 0.5613(3) -0.0759(3) 0.0221(11) Uani 1 1 d . . . C5 C 0.7557(3) 0.6213(3) -0.1387(3) 0.0182(10) Uani 1 1 d . . . N1 N 0.7212(3) 0.5184(2) 0.0445(2) 0.0220(9) Uani 1 1 d . . . N2 N 0.7189(2) 0.5821(2) -0.0040(2) 0.0173(9) Uani 1 1 d . . . O1 O 0.7513(2) 0.3738(2) 0.1143(2) 0.0227(8) Uani 1 1 d . . . O2 O 0.7815(3) 0.3238(2) -0.0069(2) 0.0434(12) Uani 1 1 d U . . O3 O 0.7904(2) 0.6077(2) -0.20409(19) 0.0204(8) Uani 1 1 d . . . O4 O 0.7210(2) 0.68768(19) -0.1260(2) 0.0259(9) Uani 1 1 d . . . O5 O 0.6833(3) 0.1833(3) 0.3167(3) 0.062(3) Uani 1 3 d S . . H5A H 0.6383 0.1810 0.2896 0.093 Uiso 0.33 1 d PR . . H5B H 0.6760 0.2134 0.3628 0.093 Uiso 0.33 1 d PR . . 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 0.01340(10) 0.01340(10) 0.01340(10) -0.00176(10) -0.00176(10) 0.00176(10) Cd1 0.01338(18) 0.01761(19) 0.01809(19) -0.00105(14) 0.00142(14) 0.00168(13) C1 0.040(3) 0.013(3) 0.020(3) 0.009(2) 0.005(2) 0.002(2) C2 0.031(3) 0.019(3) 0.022(3) 0.000(2) 0.004(2) 0.006(2) C3 0.048(4) 0.021(3) 0.016(3) 0.003(2) 0.003(2) 0.012(3) C4 0.032(3) 0.017(3) 0.018(3) 0.002(2) 0.006(2) 0.004(2) C5 0.018(3) 0.017(3) 0.019(3) 0.0002(19) -0.003(2) -0.0008(19) N1 0.031(3) 0.022(2) 0.013(2) 0.0020(17) -0.0003(18) 0.0087(19) N2 0.027(2) 0.0111(19) 0.013(2) 0.0004(15) -0.0004(17) 0.0049(17) O1 0.031(2) 0.0188(19) 0.0183(18) 0.0029(14) 0.0031(15) 0.0052(15) O2 0.083(3) 0.019(2) 0.028(2) 0.0000(17) 0.015(2) 0.023(2) O3 0.027(2) 0.0195(18) 0.0142(17) 0.0039(14) 0.0057(14) 0.0063(15) O4 0.042(2) 0.0159(18) 0.0195(19) 0.0041(14) 0.0039(17) 0.0136(16) O5 0.062(3) 0.062(3) 0.062(3) 0.015(2) 0.015(2) -0.015(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 Pr1 O3 2.549(3) 2_665 ? Pr1 O3 2.549(3) 7_564 ? Pr1 O3 2.549(3) 12_654 ? Pr1 O4 2.560(3) 2_665 ? Pr1 O4 2.560(3) 7_564 ? Pr1 O4 2.560(3) 12_654 ? Pr1 O1 2.567(3) 11_556 ? Pr1 O1 2.567(3) 8_645 ? Pr1 O1 2.567(3) . ? Pr1 O5 2.611(7) . ? Pr1 C5 2.913(5) 2_665 ? Pr1 C5 2.913(5) 7_564 ? Cd1 O2 2.160(4) 11_556 ? Cd1 N2 2.180(4) 22_565 ? Cd1 N1 2.264(4) . ? Cd1 O1 2.372(3) . ? Cd1 O4 2.398(3) 22_565 ? Cd1 O3 2.628(3) 2_665 ? C1 O2 1.256(6) . ? C1 O1 1.272(5) . ? C1 C2 1.481(6) . ? C2 N1 1.346(6) . ? C2 C3 1.390(7) . ? C3 C4 1.378(7) . ? C3 H3 0.9300 . ? C4 N2 1.370(6) . ? C4 C5 1.461(6) . ? C5 O3 1.266(5) . ? C5 O4 1.276(5) . ? C5 Pr1 2.913(5) 2_664 ? N1 N2 1.347(5) . ? N2 Cd1 2.180(4) 19_656 ? O2 Cd1 2.160(4) 8_645 ? O3 Pr1 2.549(3) 2_664 ? O3 Cd1 2.628(3) 2_664 ? O4 Cd1 2.398(3) 19_656 ? O4 Pr1 2.560(3) 2_664 ? O5 H5A 0.8847 . ? O5 H5B 0.9333 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Pr1 O3 119.756(14) 2_665 7_564 ? O3 Pr1 O3 119.756(13) 2_665 12_654 ? O3 Pr1 O3 119.756(13) 7_564 12_654 ? O3 Pr1 O4 51.29(10) 2_665 2_665 ? O3 Pr1 O4 152.25(12) 7_564 2_665 ? O3 Pr1 O4 71.51(11) 12_654 2_665 ? O3 Pr1 O4 71.51(11) 2_665 7_564 ? O3 Pr1 O4 51.29(10) 7_564 7_564 ? O3 Pr1 O4 152.25(12) 12_654 7_564 ? O4 Pr1 O4 106.07(9) 2_665 7_564 ? O3 Pr1 O4 152.25(12) 2_665 12_654 ? O3 Pr1 O4 71.51(11) 7_564 12_654 ? O3 Pr1 O4 51.29(10) 12_654 12_654 ? O4 Pr1 O4 106.07(9) 2_665 12_654 ? O4 Pr1 O4 106.07(9) 7_564 12_654 ? O3 Pr1 O1 68.35(11) 2_665 11_556 ? O3 Pr1 O1 136.07(11) 7_564 11_556 ? O3 Pr1 O1 75.91(10) 12_654 11_556 ? O4 Pr1 O1 69.30(11) 2_665 11_556 ? O4 Pr1 O1 130.17(11) 7_564 11_556 ? O4 Pr1 O1 123.18(10) 12_654 11_556 ? O3 Pr1 O1 136.07(11) 2_665 8_645 ? O3 Pr1 O1 75.91(10) 7_564 8_645 ? O3 Pr1 O1 68.35(11) 12_654 8_645 ? O4 Pr1 O1 130.17(11) 2_665 8_645 ? O4 Pr1 O1 123.18(10) 7_564 8_645 ? O4 Pr1 O1 69.30(11) 12_654 8_645 ? O1 Pr1 O1 73.26(12) 11_556 8_645 ? O3 Pr1 O1 75.91(10) 2_665 . ? O3 Pr1 O1 68.35(11) 7_564 . ? O3 Pr1 O1 136.07(11) 12_654 . ? O4 Pr1 O1 123.18(10) 2_665 . ? O4 Pr1 O1 69.30(11) 7_564 . ? O4 Pr1 O1 130.17(11) 12_654 . ? O1 Pr1 O1 73.26(12) 11_556 . ? O1 Pr1 O1 73.26(12) 8_645 . ? O3 Pr1 O5 87.15(8) 2_665 . ? O3 Pr1 O5 87.15(8) 7_564 . ? O3 Pr1 O5 87.15(8) 12_654 . ? O4 Pr1 O5 67.31(8) 2_665 . ? O4 Pr1 O5 67.31(8) 7_564 . ? O4 Pr1 O5 67.31(8) 12_654 . ? O1 Pr1 O5 136.45(8) 11_556 . ? O1 Pr1 O5 136.45(8) 8_645 . ? O1 Pr1 O5 136.45(8) . . ? O3 Pr1 C5 25.70(11) 2_665 2_665 ? O3 Pr1 C5 142.13(11) 7_564 2_665 ? O3 Pr1 C5 94.77(11) 12_654 2_665 ? O4 Pr1 C5 25.96(11) 2_665 2_665 ? O4 Pr1 C5 90.94(12) 7_564 2_665 ? O4 Pr1 C5 131.43(12) 12_654 2_665 ? O1 Pr1 C5 63.20(12) 11_556 2_665 ? O1 Pr1 C5 136.08(12) 8_645 2_665 ? O1 Pr1 C5 98.38(12) . 2_665 ? O5 Pr1 C5 78.99(9) . 2_665 ? O3 Pr1 C5 94.77(11) 2_665 7_564 ? O3 Pr1 C5 25.70(11) 7_564 7_564 ? O3 Pr1 C5 142.13(11) 12_654 7_564 ? O4 Pr1 C5 131.43(12) 2_665 7_564 ? O4 Pr1 C5 25.96(11) 7_564 7_564 ? O4 Pr1 C5 90.94(12) 12_654 7_564 ? O1 Pr1 C5 136.08(12) 11_556 7_564 ? O1 Pr1 C5 98.38(12) 8_645 7_564 ? O1 Pr1 C5 63.20(12) . 7_564 ? O5 Pr1 C5 78.99(9) . 7_564 ? C5 Pr1 C5 116.44(6) 2_665 7_564 ? O2 Cd1 N2 138.83(17) 11_556 22_565 ? O2 Cd1 N1 100.44(17) 11_556 . ? N2 Cd1 N1 115.41(15) 22_565 . ? O2 Cd1 O1 85.86(14) 11_556 . ? N2 Cd1 O1 122.68(13) 22_565 . ? N1 Cd1 O1 72.57(13) . . ? O2 Cd1 O4 83.54(14) 11_556 22_565 ? N2 Cd1 O4 72.48(13) 22_565 22_565 ? N1 Cd1 O4 98.03(14) . 22_565 ? O1 Cd1 O4 164.32(11) . 22_565 ? O2 Cd1 O3 77.33(13) 11_556 2_665 ? N2 Cd1 O3 80.62(13) 22_565 2_665 ? N1 Cd1 O3 150.39(13) . 2_665 ? O1 Cd1 O3 77.82(11) . 2_665 ? O4 Cd1 O3 110.88(11) 22_565 2_665 ? O2 C1 O1 126.8(5) . . ? O2 C1 C2 115.5(4) . . ? O1 C1 C2 117.6(4) . . ? N1 C2 C3 111.6(5) . . ? N1 C2 C1 119.6(4) . . ? C3 C2 C1 128.8(5) . . ? C4 C3 C2 103.4(5) . . ? C4 C3 H3 128.3 . . ? C2 C3 H3 128.3 . . ? N2 C4 C3 109.6(4) . . ? N2 C4 C5 118.8(4) . . ? C3 C4 C5 131.6(5) . . ? O3 C5 O4 120.9(4) . . ? O3 C5 C4 121.7(4) . . ? O4 C5 C4 117.3(4) . . ? O3 C5 Pr1 60.9(2) . 2_664 ? O4 C5 Pr1 61.4(2) . 2_664 ? C4 C5 Pr1 166.4(3) . 2_664 ? C2 N1 N2 106.8(4) . . ? C2 N1 Cd1 114.5(3) . . ? N2 N1 Cd1 137.9(3) . . ? N1 N2 C4 108.6(4) . . ? N1 N2 Cd1 134.3(3) . 19_656 ? C4 N2 Cd1 117.1(3) . 19_656 ? C1 O1 Cd1 114.9(3) . . ? C1 O1 Pr1 138.6(3) . . ? Cd1 O1 Pr1 106.29(12) . . ? C1 O2 Cd1 134.4(3) . 8_645 ? C5 O3 Pr1 93.4(3) . 2_664 ? C5 O3 Cd1 143.3(3) . 2_664 ? Pr1 O3 Cd1 99.56(11) 2_664 2_664 ? C5 O4 Cd1 113.6(3) . 19_656 ? C5 O4 Pr1 92.7(3) . 2_664 ? Cd1 O4 Pr1 153.09(14) 19_656 2_664 ? Pr1 O5 H5A 102.9 . . ? Pr1 O5 H5B 104.0 . . ? H5A O5 H5B 109.8 . . ? 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 C1 C2 N1 167.1(5) . . . . ? O1 C1 C2 N1 -10.3(8) . . . . ? O2 C1 C2 C3 -12.1(9) . . . . ? O1 C1 C2 C3 170.5(6) . . . . ? N1 C2 C3 C4 -0.4(6) . . . . ? C1 C2 C3 C4 178.8(5) . . . . ? C2 C3 C4 N2 0.3(6) . . . . ? C2 C3 C4 C5 179.8(5) . . . . ? N2 C4 C5 O3 174.4(4) . . . . ? C3 C4 C5 O3 -5.0(9) . . . . ? N2 C4 C5 O4 -7.6(7) . . . . ? C3 C4 C5 O4 173.0(6) . . . . ? N2 C4 C5 Pr1 -88.6(15) . . . 2_664 ? C3 C4 C5 Pr1 92.0(15) . . . 2_664 ? C3 C2 N1 N2 0.4(6) . . . . ? C1 C2 N1 N2 -178.9(4) . . . . ? C3 C2 N1 Cd1 -170.7(4) . . . . ? C1 C2 N1 Cd1 10.0(6) . . . . ? O2 Cd1 N1 C2 77.0(4) 11_556 . . . ? N2 Cd1 N1 C2 -123.8(4) 22_565 . . . ? O1 Cd1 N1 C2 -5.3(4) . . . . ? O4 Cd1 N1 C2 161.8(4) 22_565 . . . ? O3 Cd1 N1 C2 -5.7(6) 2_665 . . . ? O2 Cd1 N1 N2 -90.3(5) 11_556 . . . ? N2 Cd1 N1 N2 69.0(5) 22_565 . . . ? O1 Cd1 N1 N2 -172.5(5) . . . . ? O4 Cd1 N1 N2 -5.4(5) 22_565 . . . ? O3 Cd1 N1 N2 -172.9(4) 2_665 . . . ? C2 N1 N2 C4 -0.2(6) . . . . ? Cd1 N1 N2 C4 167.7(4) . . . . ? C2 N1 N2 Cd1 179.1(4) . . . 19_656 ? Cd1 N1 N2 Cd1 -13.0(8) . . . 19_656 ? C3 C4 N2 N1 -0.1(6) . . . . ? C5 C4 N2 N1 -179.6(4) . . . . ? C3 C4 N2 Cd1 -179.5(4) . . . 19_656 ? C5 C4 N2 Cd1 1.0(6) . . . 19_656 ? O2 C1 O1 Cd1 -172.2(5) . . . . ? C2 C1 O1 Cd1 4.9(6) . . . . ? O2 C1 O1 Pr1 14.9(10) . . . . ? C2 C1 O1 Pr1 -168.0(3) . . . . ? O2 Cd1 O1 C1 -102.3(4) 11_556 . . . ? N2 Cd1 O1 C1 109.5(4) 22_565 . . . ? N1 Cd1 O1 C1 0.0(4) . . . . ? O4 Cd1 O1 C1 -54.7(6) 22_565 . . . ? O3 Cd1 O1 C1 179.8(4) 2_665 . . . ? O2 Cd1 O1 Pr1 72.82(16) 11_556 . . . ? N2 Cd1 O1 Pr1 -75.43(18) 22_565 . . . ? N1 Cd1 O1 Pr1 175.12(18) . . . . ? O4 Cd1 O1 Pr1 120.3(4) 22_565 . . . ? O3 Cd1 O1 Pr1 -5.10(12) 2_665 . . . ? O3 Pr1 O1 C1 178.6(5) 2_665 . . . ? O3 Pr1 O1 C1 -50.9(5) 7_564 . . . ? O3 Pr1 O1 C1 60.1(6) 12_654 . . . ? O4 Pr1 O1 C1 157.7(5) 2_665 . . . ? O4 Pr1 O1 C1 -106.2(5) 7_564 . . . ? O4 Pr1 O1 C1 -12.3(6) 12_654 . . . ? O1 Pr1 O1 C1 107.3(5) 11_556 . . . ? O1 Pr1 O1 C1 30.3(5) 8_645 . . . ? O5 Pr1 O1 C1 -111.2(5) . . . . ? C5 Pr1 O1 C1 166.0(5) 2_665 . . . ? C5 Pr1 O1 C1 -78.6(5) 7_564 . . . ? O3 Pr1 O1 Cd1 5.30(12) 2_665 . . . ? O3 Pr1 O1 Cd1 135.85(15) 7_564 . . . ? O3 Pr1 O1 Cd1 -113.20(15) 12_654 . . . ? O4 Pr1 O1 Cd1 -15.56(19) 2_665 . . . ? O4 Pr1 O1 Cd1 80.55(13) 7_564 . . . ? O4 Pr1 O1 Cd1 174.46(11) 12_654 . . . ? O1 Pr1 O1 Cd1 -65.93(18) 11_556 . . . ? O1 Pr1 O1 Cd1 -143.01(13) 8_645 . . . ? O5 Pr1 O1 Cd1 75.53(15) . . . . ? C5 Pr1 O1 Cd1 -7.28(15) 2_665 . . . ? C5 Pr1 O1 Cd1 108.18(17) 7_564 . . . ? O1 C1 O2 Cd1 -16.7(10) . . . 8_645 ? C2 C1 O2 Cd1 166.2(4) . . . 8_645 ? O4 C5 O3 Pr1 -13.5(5) . . . 2_664 ? C4 C5 O3 Pr1 164.5(4) . . . 2_664 ? O4 C5 O3 Cd1 -124.5(5) . . . 2_664 ? C4 C5 O3 Cd1 53.4(7) . . . 2_664 ? Pr1 C5 O3 Cd1 -111.0(5) 2_664 . . 2_664 ? O3 C5 O4 Cd1 -172.4(3) . . . 19_656 ? C4 C5 O4 Cd1 9.6(5) . . . 19_656 ? Pr1 C5 O4 Cd1 174.2(3) 2_664 . . 19_656 ? O3 C5 O4 Pr1 13.4(5) . . . 2_664 ? C4 C5 O4 Pr1 -164.6(4) . . . 2_664 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.091 _refine_diff_density_min -1.106 _refine_diff_density_rms 0.190 _database_code_depnum_ccdc_archive 'CCDC 968562' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H5 Cd3 N6 Nd O13' _chemical_formula_sum 'C15 H5 Cd3 N6 Nd O13' _chemical_formula_weight 958.69 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' Cd Cd -0.8075 1.2024 '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 Cubic _symmetry_space_group_name_H-M Pa-3 _symmetry_space_group_name_Hall -P2ac2ab3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 16.77180(10) _cell_length_b 16.77180(10) _cell_length_c 16.77180(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4717.79(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1194 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.91 _exptl_crystal_description block _exptl_crystal_colour purple _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 2.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3560 _exptl_absorpt_coefficient_mu 4.910 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5903 _exptl_absorpt_correction_T_max 0.7571 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 10180 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 30.51 _reflns_number_total 2401 _reflns_number_gt 1906 _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^)+(0.0307P)^2^+0.1081P] 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 2401 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0815 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 0.773391(16) 0.273391(16) 0.226609(16) 0.00888(11) Uani 1 3 d S . . Cd1 Cd 0.70318(2) 0.49170(2) 0.17505(2) 0.01121(10) Uani 1 1 d . . . C1 C 0.7643(4) 0.3789(3) 0.0393(3) 0.0248(13) Uani 1 1 d . . . C2 C 0.7545(4) 0.4582(3) 0.0024(3) 0.0218(12) Uani 1 1 d . . . C3 C 0.7758(4) 0.4822(3) -0.0744(3) 0.0274(14) Uani 1 1 d . . . H3 H 0.8003 0.4525 -0.1143 0.033 Uiso 1 1 calc R . . C4 C 0.7515(3) 0.5608(3) -0.0765(3) 0.0178(11) Uani 1 1 d . . . C5 C 0.7547(3) 0.6211(3) -0.1395(3) 0.0148(10) Uani 1 1 d . . . N1 N 0.7220(3) 0.5181(2) 0.0435(3) 0.0177(10) Uani 1 1 d . . . N2 N 0.7189(3) 0.5815(2) -0.0044(2) 0.0148(9) Uani 1 1 d . . . O1 O 0.7520(2) 0.3731(2) 0.1142(2) 0.0174(8) Uani 1 1 d . . . O2 O 0.7809(3) 0.3233(2) -0.0079(2) 0.0416(13) Uani 1 1 d . . . O3 O 0.7900(2) 0.6076(2) -0.2051(2) 0.0159(8) Uani 1 1 d . . . O4 O 0.7204(2) 0.6878(2) -0.1271(2) 0.0197(8) Uani 1 1 d . . . O5 O 0.6859(3) 0.1859(3) 0.3141(3) 0.057(3) Uani 1 3 d S . . H5A H 0.7150 0.1592 0.3466 0.086 Uiso 0.33 1 d PR . . H5B H 0.6538 0.2146 0.3408 0.086 Uiso 0.33 1 d PR . . 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 0.00888(11) 0.00888(11) 0.00888(11) -0.00088(10) -0.00088(10) 0.00088(10) Cd1 0.01024(17) 0.01102(17) 0.01238(18) -0.00018(14) 0.00123(14) 0.00107(13) C1 0.036(3) 0.016(3) 0.022(3) 0.006(2) 0.009(3) 0.007(3) C2 0.033(3) 0.017(3) 0.016(3) 0.002(2) 0.007(2) 0.006(2) C3 0.047(4) 0.016(3) 0.019(3) 0.004(2) 0.014(3) 0.015(3) C4 0.024(3) 0.015(3) 0.015(2) 0.005(2) 0.005(2) 0.004(2) C5 0.018(2) 0.015(2) 0.011(2) 0.000(2) -0.001(2) 0.004(2) N1 0.025(2) 0.013(2) 0.016(2) 0.0021(18) 0.0010(19) 0.0056(19) N2 0.021(2) 0.0091(19) 0.014(2) 0.0012(17) -0.0002(18) 0.0023(17) O1 0.027(2) 0.0112(17) 0.0135(17) 0.0023(15) 0.0052(16) 0.0058(16) O2 0.084(4) 0.018(2) 0.022(2) 0.0070(18) 0.019(2) 0.022(2) O3 0.0222(19) 0.0139(17) 0.0117(16) 0.0016(14) 0.0028(15) 0.0108(15) O4 0.035(2) 0.0172(19) 0.0071(16) 0.0002(14) 0.0015(16) 0.0080(17) O5 0.057(3) 0.057(3) 0.057(3) 0.018(3) 0.018(3) -0.018(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 Nd1 O3 2.535(3) 7_564 ? Nd1 O3 2.535(3) 2_665 ? Nd1 O3 2.535(3) 12_654 ? Nd1 O4 2.541(3) 7_564 ? Nd1 O4 2.541(3) 2_665 ? Nd1 O4 2.541(3) 12_654 ? Nd1 O5 2.543(8) . ? Nd1 O1 2.545(3) 11_556 ? Nd1 O1 2.545(3) 8_645 ? Nd1 O1 2.545(3) . ? Nd1 C5 2.898(5) 7_564 ? Nd1 C5 2.898(5) 2_665 ? Cd1 O2 2.163(4) 11_556 ? Cd1 N2 2.179(4) 22_565 ? Cd1 N1 2.272(4) . ? Cd1 O1 2.382(3) . ? Cd1 O4 2.408(3) 22_565 ? Cd1 O3 2.612(3) 2_665 ? C1 O2 1.254(7) . ? C1 O1 1.277(6) . ? C1 C2 1.475(7) . ? C2 N1 1.335(7) . ? C2 C3 1.396(7) . ? C3 C4 1.380(7) . ? C3 H3 0.9300 . ? C4 N2 1.373(6) . ? C4 C5 1.463(7) . ? C5 O3 1.270(6) . ? C5 O4 1.275(6) . ? C5 Nd1 2.898(5) 2_664 ? N1 N2 1.334(6) . ? N2 Cd1 2.179(4) 19_656 ? O2 Cd1 2.163(4) 8_645 ? O3 Nd1 2.535(3) 2_664 ? O3 Cd1 2.612(3) 2_664 ? O4 Cd1 2.408(3) 19_656 ? O4 Nd1 2.541(3) 2_664 ? O5 H5A 0.8575 . ? O5 H5B 0.8497 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Nd1 O3 119.769(14) 7_564 2_665 ? O3 Nd1 O3 119.769(14) 7_564 12_654 ? O3 Nd1 O3 119.769(14) 2_665 12_654 ? O3 Nd1 O4 51.63(11) 7_564 7_564 ? O3 Nd1 O4 71.24(11) 2_665 7_564 ? O3 Nd1 O4 152.44(12) 12_654 7_564 ? O3 Nd1 O4 152.44(12) 7_564 2_665 ? O3 Nd1 O4 51.63(11) 2_665 2_665 ? O3 Nd1 O4 71.24(11) 12_654 2_665 ? O4 Nd1 O4 106.06(10) 7_564 2_665 ? O3 Nd1 O4 71.24(11) 7_564 12_654 ? O3 Nd1 O4 152.44(12) 2_665 12_654 ? O3 Nd1 O4 51.63(11) 12_654 12_654 ? O4 Nd1 O4 106.06(10) 7_564 12_654 ? O4 Nd1 O4 106.06(10) 2_665 12_654 ? O3 Nd1 O5 87.24(8) 7_564 . ? O3 Nd1 O5 87.24(8) 2_665 . ? O3 Nd1 O5 87.24(8) 12_654 . ? O4 Nd1 O5 67.30(9) 7_564 . ? O4 Nd1 O5 67.30(9) 2_665 . ? O4 Nd1 O5 67.30(9) 12_654 . ? O3 Nd1 O1 135.92(12) 7_564 11_556 ? O3 Nd1 O1 68.19(12) 2_665 11_556 ? O3 Nd1 O1 76.01(11) 12_654 11_556 ? O4 Nd1 O1 129.79(11) 7_564 11_556 ? O4 Nd1 O1 69.33(12) 2_665 11_556 ? O4 Nd1 O1 123.57(11) 12_654 11_556 ? O5 Nd1 O1 136.51(8) . 11_556 ? O3 Nd1 O1 76.01(11) 7_564 8_645 ? O3 Nd1 O1 135.92(12) 2_665 8_645 ? O3 Nd1 O1 68.19(12) 12_654 8_645 ? O4 Nd1 O1 123.57(11) 7_564 8_645 ? O4 Nd1 O1 129.79(12) 2_665 8_645 ? O4 Nd1 O1 69.33(12) 12_654 8_645 ? O5 Nd1 O1 136.51(8) . 8_645 ? O1 Nd1 O1 73.17(13) 11_556 8_645 ? O3 Nd1 O1 68.19(12) 7_564 . ? O3 Nd1 O1 76.01(11) 2_665 . ? O3 Nd1 O1 135.92(12) 12_654 . ? O4 Nd1 O1 69.33(12) 7_564 . ? O4 Nd1 O1 123.57(11) 2_665 . ? O4 Nd1 O1 129.79(11) 12_654 . ? O5 Nd1 O1 136.51(8) . . ? O1 Nd1 O1 73.17(13) 11_556 . ? O1 Nd1 O1 73.17(13) 8_645 . ? O3 Nd1 C5 25.95(12) 7_564 7_564 ? O3 Nd1 C5 94.53(12) 2_665 7_564 ? O3 Nd1 C5 142.46(12) 12_654 7_564 ? O4 Nd1 C5 26.08(12) 7_564 7_564 ? O4 Nd1 C5 131.56(12) 2_665 7_564 ? O4 Nd1 C5 90.94(12) 12_654 7_564 ? O5 Nd1 C5 79.13(10) . 7_564 ? O1 Nd1 C5 135.68(13) 11_556 7_564 ? O1 Nd1 C5 98.62(12) 8_645 7_564 ? O1 Nd1 C5 62.94(13) . 7_564 ? O3 Nd1 C5 142.46(12) 7_564 2_665 ? O3 Nd1 C5 25.95(12) 2_665 2_665 ? O3 Nd1 C5 94.53(12) 12_654 2_665 ? O4 Nd1 C5 90.94(12) 7_564 2_665 ? O4 Nd1 C5 26.08(12) 2_665 2_665 ? O4 Nd1 C5 131.56(12) 12_654 2_665 ? O5 Nd1 C5 79.13(10) . 2_665 ? O1 Nd1 C5 62.94(13) 11_556 2_665 ? O1 Nd1 C5 135.68(13) 8_645 2_665 ? O1 Nd1 C5 98.62(12) . 2_665 ? C5 Nd1 C5 116.53(6) 7_564 2_665 ? O2 Cd1 N2 138.10(19) 11_556 22_565 ? O2 Cd1 N1 100.26(18) 11_556 . ? N2 Cd1 N1 116.03(16) 22_565 . ? O2 Cd1 O1 86.05(16) 11_556 . ? N2 Cd1 O1 123.23(14) 22_565 . ? N1 Cd1 O1 72.48(13) . . ? O2 Cd1 O4 82.74(15) 11_556 22_565 ? N2 Cd1 O4 72.61(14) 22_565 22_565 ? N1 Cd1 O4 97.92(14) . 22_565 ? O1 Cd1 O4 163.72(12) . 22_565 ? O2 Cd1 O3 77.08(14) 11_556 2_665 ? N2 Cd1 O3 80.99(14) 22_565 2_665 ? N1 Cd1 O3 149.88(13) . 2_665 ? O1 Cd1 O3 77.41(11) . 2_665 ? O4 Cd1 O3 111.27(12) 22_565 2_665 ? O2 C1 O1 126.8(5) . . ? O2 C1 C2 115.5(5) . . ? O1 C1 C2 117.6(5) . . ? N1 C2 C3 111.3(5) . . ? N1 C2 C1 120.5(5) . . ? C3 C2 C1 128.1(5) . . ? C4 C3 C2 102.9(5) . . ? C4 C3 H3 128.5 . . ? C2 C3 H3 128.5 . . ? N2 C4 C3 109.7(5) . . ? N2 C4 C5 118.4(4) . . ? C3 C4 C5 131.9(5) . . ? O3 C5 O4 120.6(4) . . ? O3 C5 C4 121.3(4) . . ? O4 C5 C4 118.1(4) . . ? O3 C5 Nd1 60.9(2) . 2_664 ? O4 C5 Nd1 61.2(3) . 2_664 ? C4 C5 Nd1 167.3(4) . 2_664 ? N2 N1 C2 107.8(4) . . ? N2 N1 Cd1 137.3(3) . . ? C2 N1 Cd1 114.3(3) . . ? N1 N2 C4 108.3(4) . . ? N1 N2 Cd1 134.5(3) . 19_656 ? C4 N2 Cd1 117.2(3) . 19_656 ? C1 O1 Cd1 114.4(3) . . ? C1 O1 Nd1 139.2(3) . . ? Cd1 O1 Nd1 106.24(13) . . ? C1 O2 Cd1 133.6(4) . 8_645 ? C5 O3 Nd1 93.2(3) . 2_664 ? C5 O3 Cd1 143.2(3) . 2_664 ? Nd1 O3 Cd1 99.96(12) 2_664 2_664 ? C5 O4 Cd1 113.0(3) . 19_656 ? C5 O4 Nd1 92.8(3) . 2_664 ? Cd1 O4 Nd1 153.63(16) 19_656 2_664 ? Nd1 O5 H5A 109.8 . . ? Nd1 O5 H5B 110.0 . . ? H5A O5 H5B 108.8 . . ? 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 C1 C2 N1 166.9(6) . . . . ? O1 C1 C2 N1 -10.2(9) . . . . ? O2 C1 C2 C3 -13.4(10) . . . . ? O1 C1 C2 C3 169.5(6) . . . . ? N1 C2 C3 C4 -1.4(7) . . . . ? C1 C2 C3 C4 178.8(6) . . . . ? C2 C3 C4 N2 0.8(7) . . . . ? C2 C3 C4 C5 -179.0(6) . . . . ? N2 C4 C5 O3 174.1(5) . . . . ? C3 C4 C5 O3 -6.1(10) . . . . ? N2 C4 C5 O4 -6.5(8) . . . . ? C3 C4 C5 O4 173.3(6) . . . . ? N2 C4 C5 Nd1 -89.8(17) . . . 2_664 ? C3 C4 C5 Nd1 90.1(17) . . . 2_664 ? C3 C2 N1 N2 1.5(7) . . . . ? C1 C2 N1 N2 -178.7(5) . . . . ? C3 C2 N1 Cd1 -170.8(4) . . . . ? C1 C2 N1 Cd1 9.0(7) . . . . ? O2 Cd1 N1 N2 -90.9(5) 11_556 . . . ? N2 Cd1 N1 N2 67.6(5) 22_565 . . . ? O1 Cd1 N1 N2 -173.4(5) . . . . ? O4 Cd1 N1 N2 -6.9(5) 22_565 . . . ? O3 Cd1 N1 N2 -172.8(4) 2_665 . . . ? O2 Cd1 N1 C2 78.2(4) 11_556 . . . ? N2 Cd1 N1 C2 -123.3(4) 22_565 . . . ? O1 Cd1 N1 C2 -4.3(4) . . . . ? O4 Cd1 N1 C2 162.2(4) 22_565 . . . ? O3 Cd1 N1 C2 -3.7(6) 2_665 . . . ? C2 N1 N2 C4 -0.9(6) . . . . ? Cd1 N1 N2 C4 168.7(4) . . . . ? C2 N1 N2 Cd1 178.8(4) . . . 19_656 ? Cd1 N1 N2 Cd1 -11.6(8) . . . 19_656 ? C3 C4 N2 N1 0.0(6) . . . . ? C5 C4 N2 N1 179.9(4) . . . . ? C3 C4 N2 Cd1 -179.8(4) . . . 19_656 ? C5 C4 N2 Cd1 0.1(6) . . . 19_656 ? O2 C1 O1 Cd1 -171.1(6) . . . . ? C2 C1 O1 Cd1 5.6(7) . . . . ? O2 C1 O1 Nd1 15.0(11) . . . . ? C2 C1 O1 Nd1 -168.2(4) . . . . ? O2 Cd1 O1 C1 -103.0(4) 11_556 . . . ? N2 Cd1 O1 C1 109.2(4) 22_565 . . . ? N1 Cd1 O1 C1 -0.9(4) . . . . ? O4 Cd1 O1 C1 -56.5(7) 22_565 . . . ? O3 Cd1 O1 C1 179.4(4) 2_665 . . . ? O2 Cd1 O1 Nd1 72.83(17) 11_556 . . . ? N2 Cd1 O1 Nd1 -75.03(19) 22_565 . . . ? N1 Cd1 O1 Nd1 174.90(19) . . . . ? O4 Cd1 O1 Nd1 119.4(4) 22_565 . . . ? O3 Cd1 O1 Nd1 -4.80(12) 2_665 . . . ? O3 Nd1 O1 C1 -50.2(6) 7_564 . . . ? O3 Nd1 O1 C1 179.1(6) 2_665 . . . ? O3 Nd1 O1 C1 60.6(6) 12_654 . . . ? O4 Nd1 O1 C1 -105.9(6) 7_564 . . . ? O4 Nd1 O1 C1 158.1(6) 2_665 . . . ? O4 Nd1 O1 C1 -11.9(6) 12_654 . . . ? O5 Nd1 O1 C1 -110.4(6) . . . . ? O1 Nd1 O1 C1 108.1(5) 11_556 . . . ? O1 Nd1 O1 C1 31.1(6) 8_645 . . . ? C5 Nd1 O1 C1 -78.2(6) 7_564 . . . ? C5 Nd1 O1 C1 166.3(6) 2_665 . . . ? O3 Nd1 O1 Cd1 135.58(17) 7_564 . . . ? O3 Nd1 O1 Cd1 4.98(13) 2_665 . . . ? O3 Nd1 O1 Cd1 -113.60(16) 12_654 . . . ? O4 Nd1 O1 Cd1 79.89(14) 7_564 . . . ? O4 Nd1 O1 Cd1 -16.1(2) 2_665 . . . ? O4 Nd1 O1 Cd1 173.93(11) 12_654 . . . ? O5 Nd1 O1 Cd1 75.41(16) . . . . ? O1 Nd1 O1 Cd1 -66.07(19) 11_556 . . . ? O1 Nd1 O1 Cd1 -143.10(13) 8_645 . . . ? C5 Nd1 O1 Cd1 107.60(18) 7_564 . . . ? C5 Nd1 O1 Cd1 -7.85(17) 2_665 . . . ? O1 C1 O2 Cd1 -17.6(11) . . . 8_645 ? C2 C1 O2 Cd1 165.5(4) . . . 8_645 ? O4 C5 O3 Nd1 -13.9(5) . . . 2_664 ? C4 C5 O3 Nd1 165.5(4) . . . 2_664 ? O4 C5 O3 Cd1 -125.3(5) . . . 2_664 ? C4 C5 O3 Cd1 54.2(8) . . . 2_664 ? Nd1 C5 O3 Cd1 -111.3(5) 2_664 . . 2_664 ? O3 C5 O4 Cd1 -171.8(4) . . . 19_656 ? C4 C5 O4 Cd1 8.7(6) . . . 19_656 ? Nd1 C5 O4 Cd1 174.3(3) 2_664 . . 19_656 ? O3 C5 O4 Nd1 13.9(5) . . . 2_664 ? C4 C5 O4 Nd1 -165.5(4) . . . 2_664 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.652 _refine_diff_density_min -1.009 _refine_diff_density_rms 0.206 _database_code_depnum_ccdc_archive 'CCDC 968563' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H5 Cd3 Sm N6 O13' _chemical_formula_sum 'C15 H5 Cd3 N6 O13 Sm' _chemical_formula_weight 964.80 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' Cd Cd -0.8075 1.2024 '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 Cubic _symmetry_space_group_name_H-M Pa-3 _symmetry_space_group_name_Hall -P2ac2ab3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 16.7466(2) _cell_length_b 16.7466(2) _cell_length_c 16.7466(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4696.56(10) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1273 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 27.97 _exptl_crystal_description block _exptl_crystal_colour colourless _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 2.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3576 _exptl_absorpt_coefficient_mu 5.222 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5730 _exptl_absorpt_correction_T_max 0.7447 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 10074 _diffrn_reflns_av_R_equivalents 0.0671 _diffrn_reflns_av_sigmaI/netI 0.0815 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 30.47 _reflns_number_total 2394 _reflns_number_gt 1768 _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^)+(0.0000P)^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 2394 _refine_ls_number_parameters 115 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0560 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.992 _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 Sm1 Sm 0.774834(17) 0.274834(17) 0.225166(17) 0.01203(11) Uani 1 3 d S . . Cd1 Cd 0.70370(2) 0.49230(2) 0.17443(2) 0.01208(9) Uani 1 1 d . . . C1 C 0.7643(4) 0.3806(4) 0.0389(4) 0.0225(15) Uani 1 1 d . . . C2 C 0.7547(4) 0.4585(3) 0.0022(3) 0.0214(14) Uani 1 1 d . . . C3 C 0.7752(4) 0.4822(3) -0.0745(3) 0.0256(16) Uani 1 1 d . . . H3 H 0.7989 0.4519 -0.1146 0.031 Uiso 1 1 calc R . . C4 C 0.7518(4) 0.5620(3) -0.0775(3) 0.0177(13) Uani 1 1 d . . . C5 C 0.7530(3) 0.6217(3) -0.1409(3) 0.0147(12) Uani 1 1 d . . . N1 N 0.7216(3) 0.5190(3) 0.0426(3) 0.0160(11) Uani 1 1 d . . . N2 N 0.7190(3) 0.5829(3) -0.0060(3) 0.0143(10) Uani 1 1 d . . . O1 O 0.7528(3) 0.3736(2) 0.1134(2) 0.0255(8) Uani 1 1 d U . . O2 O 0.7822(3) 0.3235(2) -0.0089(2) 0.0276(8) Uani 1 1 d U . . O3 O 0.7882(2) 0.6082(2) -0.2075(2) 0.0179(7) Uani 1 1 d U . . O4 O 0.7189(2) 0.6880(2) -0.1285(2) 0.0183(7) Uani 1 1 d U . . O5 O 0.6878(3) 0.1878(3) 0.3122(3) 0.058(3) Uani 1 3 d S . . H5B H 0.7169 0.1610 0.3449 0.087 Uiso 0.33 1 d PR . . H5A H 0.6556 0.2164 0.3390 0.087 Uiso 0.33 1 d PR . . 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 0.01203(11) 0.01203(11) 0.01203(11) -0.00192(12) -0.00192(12) 0.00192(12) Cd1 0.01040(19) 0.0122(2) 0.0136(2) -0.00028(17) 0.00109(17) 0.00149(17) C1 0.032(4) 0.016(3) 0.019(3) 0.001(3) 0.002(3) 0.007(3) C2 0.035(4) 0.015(3) 0.014(3) 0.004(3) 0.005(3) 0.009(3) C3 0.046(4) 0.017(3) 0.013(3) 0.002(3) 0.005(3) 0.018(3) C4 0.026(3) 0.016(3) 0.011(3) 0.004(2) 0.003(3) 0.005(3) C5 0.020(3) 0.011(3) 0.013(3) -0.002(2) 0.001(2) 0.001(2) N1 0.021(3) 0.013(2) 0.013(2) 0.000(2) 0.003(2) 0.003(2) N2 0.022(3) 0.007(2) 0.013(2) 0.0028(19) -0.002(2) 0.003(2) O1 0.043(2) 0.0147(16) 0.0183(17) 0.0030(14) 0.0086(16) 0.0110(15) O2 0.047(2) 0.0161(16) 0.0201(17) 0.0031(14) 0.0089(16) 0.0121(15) O3 0.0296(19) 0.0136(16) 0.0106(15) 0.0019(13) 0.0015(14) 0.0075(14) O4 0.0307(19) 0.0135(16) 0.0108(15) 0.0023(12) 0.0014(14) 0.0083(14) O5 0.058(3) 0.058(3) 0.058(3) 0.011(3) 0.011(3) -0.011(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 Sm1 O3 2.494(4) 2_665 ? Sm1 O3 2.494(4) 12_654 ? Sm1 O3 2.494(4) 7_564 ? Sm1 O1 2.525(4) 11_556 ? Sm1 O1 2.525(4) 8_645 ? Sm1 O1 2.525(4) . ? Sm1 O5 2.526(8) . ? Sm1 O4 2.531(3) 2_665 ? Sm1 O4 2.531(3) 12_654 ? Sm1 O4 2.531(3) 7_564 ? Sm1 C5 2.872(5) 2_665 ? Sm1 C5 2.872(5) 12_654 ? Cd1 O2 2.152(4) 11_556 ? Cd1 N2 2.168(4) 22_565 ? Cd1 N1 2.272(4) . ? Cd1 O1 2.380(4) . ? Cd1 O4 2.413(4) 22_565 ? Cd1 O3 2.601(4) 2_665 ? C1 O1 1.268(6) . ? C1 O2 1.283(7) . ? C1 C2 1.451(8) . ? C2 N1 1.340(6) . ? C2 C3 1.388(7) . ? C3 C4 1.394(7) . ? C3 H3 0.9300 . ? C4 N2 1.364(7) . ? C4 C5 1.458(7) . ? C5 O4 1.265(6) . ? C5 O3 1.282(6) . ? C5 Sm1 2.872(5) 2_664 ? N1 N2 1.345(6) . ? N2 Cd1 2.168(4) 19_656 ? O2 Cd1 2.152(4) 8_645 ? O3 Sm1 2.494(4) 2_664 ? O3 Cd1 2.601(4) 2_664 ? O4 Cd1 2.413(4) 19_656 ? O4 Sm1 2.531(3) 2_664 ? O5 H5B 0.8593 . ? O5 H5A 0.8494 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Sm1 O3 119.729(16) 2_665 12_654 ? O3 Sm1 O3 119.729(16) 2_665 7_564 ? O3 Sm1 O3 119.729(16) 12_654 7_564 ? O3 Sm1 O1 68.26(13) 2_665 11_556 ? O3 Sm1 O1 76.03(12) 12_654 11_556 ? O3 Sm1 O1 136.47(13) 7_564 11_556 ? O3 Sm1 O1 136.47(13) 2_665 8_645 ? O3 Sm1 O1 68.26(13) 12_654 8_645 ? O3 Sm1 O1 76.03(12) 7_564 8_645 ? O1 Sm1 O1 73.67(15) 11_556 8_645 ? O3 Sm1 O1 76.03(12) 2_665 . ? O3 Sm1 O1 136.47(13) 12_654 . ? O3 Sm1 O1 68.26(13) 7_564 . ? O1 Sm1 O1 73.67(15) 11_556 . ? O1 Sm1 O1 73.67(15) 8_645 . ? O3 Sm1 O5 87.00(9) 2_665 . ? O3 Sm1 O5 87.00(9) 12_654 . ? O3 Sm1 O5 87.00(9) 7_564 . ? O1 Sm1 O5 136.19(10) 11_556 . ? O1 Sm1 O5 136.19(10) 8_645 . ? O1 Sm1 O5 136.19(10) . . ? O3 Sm1 O4 52.15(11) 2_665 2_665 ? O3 Sm1 O4 70.67(12) 12_654 2_665 ? O3 Sm1 O4 152.01(12) 7_564 2_665 ? O1 Sm1 O4 69.44(13) 11_556 2_665 ? O1 Sm1 O4 129.80(13) 8_645 2_665 ? O1 Sm1 O4 124.22(12) . 2_665 ? O5 Sm1 O4 66.84(9) . 2_665 ? O3 Sm1 O4 152.01(12) 2_665 12_654 ? O3 Sm1 O4 52.15(11) 12_654 12_654 ? O3 Sm1 O4 70.67(12) 7_564 12_654 ? O1 Sm1 O4 124.22(12) 11_556 12_654 ? O1 Sm1 O4 69.44(13) 8_645 12_654 ? O1 Sm1 O4 129.80(13) . 12_654 ? O5 Sm1 O4 66.84(9) . 12_654 ? O4 Sm1 O4 105.55(10) 2_665 12_654 ? O3 Sm1 O4 70.67(12) 2_665 7_564 ? O3 Sm1 O4 152.01(12) 12_654 7_564 ? O3 Sm1 O4 52.15(11) 7_564 7_564 ? O1 Sm1 O4 129.80(13) 11_556 7_564 ? O1 Sm1 O4 124.22(12) 8_645 7_564 ? O1 Sm1 O4 69.44(13) . 7_564 ? O5 Sm1 O4 66.84(9) . 7_564 ? O4 Sm1 O4 105.55(10) 2_665 7_564 ? O4 Sm1 O4 105.55(10) 12_654 7_564 ? O3 Sm1 C5 26.46(13) 2_665 2_665 ? O3 Sm1 C5 93.98(13) 12_654 2_665 ? O3 Sm1 C5 142.67(13) 7_564 2_665 ? O1 Sm1 C5 62.93(15) 11_556 2_665 ? O1 Sm1 C5 136.08(14) 8_645 2_665 ? O1 Sm1 C5 99.19(14) . 2_665 ? O5 Sm1 C5 78.68(11) . 2_665 ? O4 Sm1 C5 26.10(12) 2_665 2_665 ? O4 Sm1 C5 131.01(13) 12_654 2_665 ? O4 Sm1 C5 90.59(13) 7_564 2_665 ? O3 Sm1 C5 142.67(13) 2_665 12_654 ? O3 Sm1 C5 26.46(13) 12_654 12_654 ? O3 Sm1 C5 93.98(13) 7_564 12_654 ? O1 Sm1 C5 99.19(14) 11_556 12_654 ? O1 Sm1 C5 62.93(15) 8_645 12_654 ? O1 Sm1 C5 136.08(14) . 12_654 ? O5 Sm1 C5 78.68(11) . 12_654 ? O4 Sm1 C5 90.59(13) 2_665 12_654 ? O4 Sm1 C5 26.10(12) 12_654 12_654 ? O4 Sm1 C5 131.01(13) 7_564 12_654 ? C5 Sm1 C5 116.25(7) 2_665 12_654 ? O2 Cd1 N2 137.76(17) 11_556 22_565 ? O2 Cd1 N1 100.33(16) 11_556 . ? N2 Cd1 N1 115.89(16) 22_565 . ? O2 Cd1 O1 86.01(15) 11_556 . ? N2 Cd1 O1 123.90(15) 22_565 . ? N1 Cd1 O1 72.67(15) . . ? O2 Cd1 O4 82.87(14) 11_556 22_565 ? N2 Cd1 O4 72.07(14) 22_565 22_565 ? N1 Cd1 O4 97.37(14) . 22_565 ? O1 Cd1 O4 163.51(13) . 22_565 ? O2 Cd1 O3 77.20(14) 11_556 2_665 ? N2 Cd1 O3 81.67(14) 22_565 2_665 ? N1 Cd1 O3 149.25(14) . 2_665 ? O1 Cd1 O3 76.58(12) . 2_665 ? O4 Cd1 O3 112.49(12) 22_565 2_665 ? O1 C1 O2 125.5(6) . . ? O1 C1 C2 118.9(5) . . ? O2 C1 C2 115.5(5) . . ? N1 C2 C3 110.7(5) . . ? N1 C2 C1 120.8(5) . . ? C3 C2 C1 128.5(5) . . ? C2 C3 C4 103.7(5) . . ? C2 C3 H3 128.1 . . ? C4 C3 H3 128.1 . . ? N2 C4 C3 109.2(5) . . ? N2 C4 C5 118.0(5) . . ? C3 C4 C5 132.8(5) . . ? O4 C5 O3 120.3(5) . . ? O4 C5 C4 118.4(5) . . ? O3 C5 C4 121.3(5) . . ? O4 C5 Sm1 61.7(3) . 2_664 ? O3 C5 Sm1 60.1(3) . 2_664 ? C4 C5 Sm1 168.5(4) . 2_664 ? C2 N1 N2 108.0(4) . . ? C2 N1 Cd1 113.4(4) . . ? N2 N1 Cd1 137.8(3) . . ? N1 N2 C4 108.3(4) . . ? N1 N2 Cd1 133.6(3) . 19_656 ? C4 N2 Cd1 118.1(4) . 19_656 ? C1 O1 Cd1 113.5(3) . . ? C1 O1 Sm1 140.1(4) . . ? Cd1 O1 Sm1 106.24(15) . . ? C1 O2 Cd1 133.9(4) . 8_645 ? C5 O3 Sm1 93.5(3) . 2_664 ? C5 O3 Cd1 143.1(4) . 2_664 ? Sm1 O3 Cd1 100.75(13) 2_664 2_664 ? C5 O4 Cd1 113.0(3) . 19_656 ? C5 O4 Sm1 92.2(3) . 2_664 ? Cd1 O4 Sm1 154.26(16) 19_656 2_664 ? Sm1 O5 H5B 109.9 . . ? Sm1 O5 H5A 110.2 . . ? H5B O5 H5A 108.6 . . ? 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 C1 C2 N1 -11.2(9) . . . . ? O2 C1 C2 N1 167.2(6) . . . . ? O1 C1 C2 C3 169.8(6) . . . . ? O2 C1 C2 C3 -11.8(10) . . . . ? N1 C2 C3 C4 0.0(7) . . . . ? C1 C2 C3 C4 179.2(6) . . . . ? C2 C3 C4 N2 -0.4(7) . . . . ? C2 C3 C4 C5 -177.2(6) . . . . ? N2 C4 C5 O4 -4.6(8) . . . . ? C3 C4 C5 O4 172.0(6) . . . . ? N2 C4 C5 O3 174.7(5) . . . . ? C3 C4 C5 O3 -8.8(11) . . . . ? N2 C4 C5 Sm1 -92(2) . . . 2_664 ? C3 C4 C5 Sm1 84(2) . . . 2_664 ? C3 C2 N1 N2 0.4(7) . . . . ? C1 C2 N1 N2 -178.8(5) . . . . ? C3 C2 N1 Cd1 -171.0(4) . . . . ? C1 C2 N1 Cd1 9.7(7) . . . . ? O2 Cd1 N1 C2 77.9(4) 11_556 . . . ? N2 Cd1 N1 C2 -124.5(4) 22_565 . . . ? O1 Cd1 N1 C2 -4.6(4) . . . . ? O4 Cd1 N1 C2 161.9(4) 22_565 . . . ? O3 Cd1 N1 C2 -4.4(6) 2_665 . . . ? O2 Cd1 N1 N2 -89.9(5) 11_556 . . . ? N2 Cd1 N1 N2 67.7(6) 22_565 . . . ? O1 Cd1 N1 N2 -172.4(6) . . . . ? O4 Cd1 N1 N2 -5.9(6) 22_565 . . . ? O3 Cd1 N1 N2 -172.2(4) 2_665 . . . ? C2 N1 N2 C4 -0.6(6) . . . . ? Cd1 N1 N2 C4 167.6(4) . . . . ? C2 N1 N2 Cd1 178.8(4) . . . 19_656 ? Cd1 N1 N2 Cd1 -13.0(8) . . . 19_656 ? C3 C4 N2 N1 0.7(7) . . . . ? C5 C4 N2 N1 178.0(5) . . . . ? C3 C4 N2 Cd1 -178.9(4) . . . 19_656 ? C5 C4 N2 Cd1 -1.5(7) . . . 19_656 ? O2 C1 O1 Cd1 -172.2(5) . . . . ? C2 C1 O1 Cd1 6.1(7) . . . . ? O2 C1 O1 Sm1 14.0(11) . . . . ? C2 C1 O1 Sm1 -167.7(4) . . . . ? O2 Cd1 O1 C1 -103.0(4) 11_556 . . . ? N2 Cd1 O1 C1 109.1(4) 22_565 . . . ? N1 Cd1 O1 C1 -0.9(4) . . . . ? O4 Cd1 O1 C1 -55.4(7) 22_565 . . . ? O3 Cd1 O1 C1 179.2(4) 2_665 . . . ? O2 Cd1 O1 Sm1 72.83(17) 11_556 . . . ? N2 Cd1 O1 Sm1 -75.1(2) 22_565 . . . ? N1 Cd1 O1 Sm1 175.0(2) . . . . ? O4 Cd1 O1 Sm1 120.5(4) 22_565 . . . ? O3 Cd1 O1 Sm1 -4.94(14) 2_665 . . . ? O3 Sm1 O1 C1 179.2(7) 2_665 . . . ? O3 Sm1 O1 C1 60.5(7) 12_654 . . . ? O3 Sm1 O1 C1 -50.3(6) 7_564 . . . ? O1 Sm1 O1 C1 108.2(6) 11_556 . . . ? O1 Sm1 O1 C1 30.9(6) 8_645 . . . ? O5 Sm1 O1 C1 -110.5(6) . . . . ? O4 Sm1 O1 C1 158.3(6) 2_665 . . . ? O4 Sm1 O1 C1 -13.1(7) 12_654 . . . ? O4 Sm1 O1 C1 -106.5(7) 7_564 . . . ? C5 Sm1 O1 C1 166.3(6) 2_665 . . . ? C5 Sm1 O1 C1 21.9(7) 12_654 . . . ? O3 Sm1 O1 Cd1 5.16(14) 2_665 . . . ? O3 Sm1 O1 Cd1 -113.53(18) 12_654 . . . ? O3 Sm1 O1 Cd1 135.66(19) 7_564 . . . ? O1 Sm1 O1 Cd1 -65.9(2) 11_556 . . . ? O1 Sm1 O1 Cd1 -143.20(15) 8_645 . . . ? O5 Sm1 O1 Cd1 75.46(18) . . . . ? O4 Sm1 O1 Cd1 -15.8(2) 2_665 . . . ? O4 Sm1 O1 Cd1 172.88(12) 12_654 . . . ? O4 Sm1 O1 Cd1 79.44(16) 7_564 . . . ? C5 Sm1 O1 Cd1 -7.73(18) 2_665 . . . ? C5 Sm1 O1 Cd1 -152.19(17) 12_654 . . . ? O1 C1 O2 Cd1 -15.6(10) . . . 8_645 ? C2 C1 O2 Cd1 166.1(4) . . . 8_645 ? O4 C5 O3 Sm1 -14.1(6) . . . 2_664 ? C4 C5 O3 Sm1 166.7(5) . . . 2_664 ? O4 C5 O3 Cd1 -127.1(5) . . . 2_664 ? C4 C5 O3 Cd1 53.6(9) . . . 2_664 ? Sm1 C5 O3 Cd1 -113.0(6) 2_664 . . 2_664 ? O3 C5 O4 Cd1 -171.7(4) . . . 19_656 ? C4 C5 O4 Cd1 7.6(7) . . . 19_656 ? Sm1 C5 O4 Cd1 174.4(3) 2_664 . . 19_656 ? O3 C5 O4 Sm1 13.8(6) . . . 2_664 ? C4 C5 O4 Sm1 -166.9(5) . . . 2_664 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.371 _refine_diff_density_min -2.258 _refine_diff_density_rms 0.217 _database_code_depnum_ccdc_archive 'CCDC 968564' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C15 H5 Cd3 Eu N6 O13' _chemical_formula_sum 'C15 H5 Cd3 Eu N6 O13' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colourless _diffrn_ambient_temperature 296(2) _chemical_formula_weight 966.41 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' Cd Cd -0.8075 1.2024 '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 cubic _symmetry_space_group_name_H-M 'P a -3' _symmetry_int_tables_number 205 _chemical_absolute_configuration ? _symmetry_space_group_name_Hall -P2ac2ab3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 16.7360(2) _cell_length_b 16.7360(2) _cell_length_c 16.7360(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4687.65(10) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5682 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 33.03 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 5.402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4430 _exptl_absorpt_correction_T_max 0.4430 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_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 13823 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 33.09 _reflns_number_total 2934 _reflns_number_gt 2449 _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^)+(0.0212P)^2^+6.8078P] 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 2934 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0518 _refine_ls_wR_factor_gt 0.0497 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Eu1 Eu 0.775774(7) 0.275774(7) 0.224226(7) 0.01198(5) Uani 1 3 d S . . Cd1 Cd 0.703563(11) 0.492953(11) 0.173751(11) 0.01542(5) Uani 1 1 d . . . C1 C 0.7655(2) 0.37953(17) 0.03826(16) 0.0246(6) Uani 1 1 d . . . C2 C 0.7559(2) 0.45839(16) 0.00059(17) 0.0239(6) Uani 1 1 d . . . C3 C 0.7755(2) 0.48269(17) -0.07634(18) 0.0268(6) Uani 1 1 d . . . H3 H 0.7992 0.4529 -0.1169 0.032 Uiso 1 1 calc R . . C4 C 0.75155(18) 0.56155(16) -0.07817(16) 0.0208(5) Uani 1 1 d . . . C5 C 0.75317(17) 0.62150(16) -0.14213(15) 0.0175(5) Uani 1 1 d . . . N1 N 0.72252(15) 0.51909(13) 0.04211(14) 0.0204(5) Uani 1 1 d . . . N2 N 0.71926(14) 0.58240(13) -0.00639(13) 0.0184(4) Uani 1 1 d . . . O1 O 0.75422(13) 0.37399(11) 0.11346(11) 0.0210(4) Uani 1 1 d . . . O2 O 0.78301(19) 0.32422(14) -0.00876(14) 0.0449(7) Uani 1 1 d . . . O3 O 0.78785(12) 0.60808(12) -0.20799(11) 0.0206(4) Uani 1 1 d . . . O4 O 0.71782(14) 0.68744(12) -0.12971(12) 0.0264(5) Uani 1 1 d . . . O5 O 0.68830(17) 0.18830(17) 0.31170(17) 0.0617(15) Uani 1 3 d S . . H5A H 0.6432 0.1810 0.2896 0.093 Uiso 0.33 1 d PR . . H5B H 0.6810 0.2134 0.3628 0.093 Uiso 0.33 1 d PR . . 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 0.01198(5) 0.01198(5) 0.01198(5) -0.00116(4) -0.00116(4) 0.00116(4) Cd1 0.01275(8) 0.01697(9) 0.01655(9) -0.00067(7) 0.00177(7) 0.00193(7) C1 0.0424(18) 0.0166(12) 0.0150(12) 0.0031(10) 0.0050(12) 0.0073(12) C2 0.0397(17) 0.0143(12) 0.0176(13) 0.0013(10) 0.0056(12) 0.0088(12) C3 0.0464(18) 0.0166(12) 0.0174(13) 0.0033(10) 0.0104(12) 0.0135(13) C4 0.0304(14) 0.0180(12) 0.0140(11) 0.0019(10) 0.0039(11) 0.0063(11) C5 0.0226(12) 0.0155(11) 0.0143(11) 0.0033(9) -0.0019(10) 0.0012(10) N1 0.0333(13) 0.0135(10) 0.0144(10) 0.0018(8) 0.0023(9) 0.0052(9) N2 0.0286(12) 0.0133(10) 0.0132(10) 0.0014(8) 0.0013(9) 0.0049(9) O1 0.0315(11) 0.0159(9) 0.0155(9) 0.0033(7) 0.0028(8) 0.0035(8) O2 0.089(2) 0.0198(11) 0.0261(12) 0.0053(9) 0.0163(13) 0.0260(13) O3 0.0248(10) 0.0208(9) 0.0163(9) 0.0043(7) 0.0038(7) 0.0049(8) O4 0.0444(13) 0.0174(9) 0.0173(9) 0.0022(8) 0.0030(9) 0.0109(9) O5 0.0617(15) 0.0617(15) 0.0617(15) 0.0165(14) 0.0165(14) -0.0165(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 Eu1 O3 2.4898(19) 2_665 ? Eu1 O3 2.4898(19) 12_654 ? Eu1 O3 2.4898(19) 7_564 ? Eu1 O1 2.5038(19) 11_556 ? Eu1 O1 2.5038(19) 8_645 ? Eu1 O1 2.5038(19) . ? Eu1 O4 2.523(2) 2_665 ? Eu1 O4 2.523(2) 12_654 ? Eu1 O4 2.523(2) 7_564 ? Eu1 O5 2.536(5) . ? Eu1 C5 2.862(3) 2_665 ? Eu1 C5 2.862(3) 12_654 ? Cd1 O2 2.161(2) 11_556 ? Cd1 N2 2.178(2) 22_565 ? Cd1 N1 2.268(2) . ? Cd1 O1 2.3877(19) . ? Cd1 O4 2.420(2) 22_565 ? Cd1 O3 2.607(2) 2_665 ? C1 O2 1.250(4) . ? C1 O1 1.276(3) . ? C1 C2 1.472(4) . ? C2 N1 1.352(3) . ? C2 C3 1.390(4) . ? C3 C4 1.380(4) . ? C3 H3 0.9300 . ? C4 N2 1.363(3) . ? C4 C5 1.467(4) . ? C5 O3 1.266(3) . ? C5 O4 1.269(3) . ? C5 Eu1 2.862(3) 2_664 ? N1 N2 1.336(3) . ? N2 Cd1 2.178(2) 19_656 ? O2 Cd1 2.161(2) 8_645 ? O3 Eu1 2.4898(19) 2_664 ? O3 Cd1 2.607(2) 2_664 ? O4 Cd1 2.420(2) 19_656 ? O4 Eu1 2.523(2) 2_664 ? O5 H5A 0.8490 . ? O5 H5B 0.9602 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Eu1 O3 119.653(10) 2_665 12_654 ? O3 Eu1 O3 119.653(10) 2_665 7_564 ? O3 Eu1 O3 119.653(10) 12_654 7_564 ? O3 Eu1 O1 68.72(7) 2_665 11_556 ? O3 Eu1 O1 76.30(6) 12_654 11_556 ? O3 Eu1 O1 136.74(7) 7_564 11_556 ? O3 Eu1 O1 136.74(7) 2_665 8_645 ? O3 Eu1 O1 68.72(7) 12_654 8_645 ? O3 Eu1 O1 76.30(6) 7_564 8_645 ? O1 Eu1 O1 73.45(8) 11_556 8_645 ? O3 Eu1 O1 76.30(6) 2_665 . ? O3 Eu1 O1 136.74(7) 12_654 . ? O3 Eu1 O1 68.72(7) 7_564 . ? O1 Eu1 O1 73.45(8) 11_556 . ? O1 Eu1 O1 73.45(8) 8_645 . ? O3 Eu1 O4 52.14(6) 2_665 2_665 ? O3 Eu1 O4 70.35(7) 12_654 2_665 ? O3 Eu1 O4 151.66(7) 7_564 2_665 ? O1 Eu1 O4 69.63(7) 11_556 2_665 ? O1 Eu1 O4 129.77(7) 8_645 2_665 ? O1 Eu1 O4 124.28(6) . 2_665 ? O3 Eu1 O4 151.66(7) 2_665 12_654 ? O3 Eu1 O4 52.14(6) 12_654 12_654 ? O3 Eu1 O4 70.35(7) 7_564 12_654 ? O1 Eu1 O4 124.28(6) 11_556 12_654 ? O1 Eu1 O4 69.63(7) 8_645 12_654 ? O1 Eu1 O4 129.77(7) . 12_654 ? O4 Eu1 O4 105.50(6) 2_665 12_654 ? O3 Eu1 O4 70.35(7) 2_665 7_564 ? O3 Eu1 O4 151.66(7) 12_654 7_564 ? O3 Eu1 O4 52.14(6) 7_564 7_564 ? O1 Eu1 O4 129.77(7) 11_556 7_564 ? O1 Eu1 O4 124.28(6) 8_645 7_564 ? O1 Eu1 O4 69.63(7) . 7_564 ? O4 Eu1 O4 105.50(6) 2_665 7_564 ? O4 Eu1 O4 105.50(6) 12_654 7_564 ? O3 Eu1 O5 86.61(5) 2_665 . ? O3 Eu1 O5 86.61(5) 12_654 . ? O3 Eu1 O5 86.61(5) 7_564 . ? O1 Eu1 O5 136.33(5) 11_556 . ? O1 Eu1 O5 136.33(5) 8_645 . ? O1 Eu1 O5 136.33(5) . . ? O4 Eu1 O5 66.80(5) 2_665 . ? O4 Eu1 O5 66.80(5) 12_654 . ? O4 Eu1 O5 66.80(5) 7_564 . ? O3 Eu1 C5 26.19(7) 2_665 2_665 ? O3 Eu1 C5 94.11(7) 12_654 2_665 ? O3 Eu1 C5 142.17(7) 7_564 2_665 ? O1 Eu1 C5 63.50(7) 11_556 2_665 ? O1 Eu1 C5 136.45(7) 8_645 2_665 ? O1 Eu1 C5 99.20(7) . 2_665 ? O4 Eu1 C5 26.31(7) 2_665 2_665 ? O4 Eu1 C5 131.03(7) 12_654 2_665 ? O4 Eu1 C5 90.07(7) 7_564 2_665 ? O5 Eu1 C5 78.34(5) . 2_665 ? O3 Eu1 C5 142.17(7) 2_665 12_654 ? O3 Eu1 C5 26.19(7) 12_654 12_654 ? O3 Eu1 C5 94.11(7) 7_564 12_654 ? O1 Eu1 C5 99.20(7) 11_556 12_654 ? O1 Eu1 C5 63.50(7) 8_645 12_654 ? O1 Eu1 C5 136.45(7) . 12_654 ? O4 Eu1 C5 90.07(7) 2_665 12_654 ? O4 Eu1 C5 26.31(7) 12_654 12_654 ? O4 Eu1 C5 131.03(7) 7_564 12_654 ? O5 Eu1 C5 78.34(5) . 12_654 ? C5 Eu1 C5 116.02(4) 2_665 12_654 ? O2 Cd1 N2 137.75(11) 11_556 22_565 ? O2 Cd1 N1 99.84(11) 11_556 . ? N2 Cd1 N1 116.74(9) 22_565 . ? O2 Cd1 O1 84.94(9) 11_556 . ? N2 Cd1 O1 124.37(8) 22_565 . ? N1 Cd1 O1 72.58(7) . . ? O2 Cd1 O4 83.48(9) 11_556 22_565 ? N2 Cd1 O4 72.05(7) 22_565 22_565 ? N1 Cd1 O4 97.42(8) . 22_565 ? O1 Cd1 O4 163.16(7) . 22_565 ? O2 Cd1 O3 76.92(8) 11_556 2_665 ? N2 Cd1 O3 81.54(8) 22_565 2_665 ? N1 Cd1 O3 148.72(7) . 2_665 ? O1 Cd1 O3 76.14(6) . 2_665 ? O4 Cd1 O3 112.85(7) 22_565 2_665 ? O2 C1 O1 127.0(3) . . ? O2 C1 C2 114.8(2) . . ? O1 C1 C2 118.1(2) . . ? N1 C2 C3 110.7(2) . . ? N1 C2 C1 119.9(2) . . ? C3 C2 C1 129.3(3) . . ? C4 C3 C2 103.4(2) . . ? C4 C3 H3 128.3 . . ? C2 C3 H3 128.3 . . ? N2 C4 C3 109.9(2) . . ? N2 C4 C5 118.4(2) . . ? C3 C4 C5 131.7(3) . . ? O3 C5 O4 120.7(2) . . ? O3 C5 C4 121.5(2) . . ? O4 C5 C4 117.8(2) . . ? O3 C5 Eu1 60.24(13) . 2_664 ? O4 C5 Eu1 61.76(14) . 2_664 ? C4 C5 Eu1 167.8(2) . 2_664 ? N2 N1 C2 107.5(2) . . ? N2 N1 Cd1 137.51(17) . . ? C2 N1 Cd1 114.34(17) . . ? N1 N2 C4 108.4(2) . . ? N1 N2 Cd1 133.64(17) . 19_656 ? C4 N2 Cd1 117.92(17) . 19_656 ? C1 O1 Cd1 114.13(17) . . ? C1 O1 Eu1 139.17(18) . . ? Cd1 O1 Eu1 106.60(7) . . ? C1 O2 Cd1 133.9(2) . 8_645 ? C5 O3 Eu1 93.57(16) . 2_664 ? C5 O3 Cd1 143.26(18) . 2_664 ? Eu1 O3 Cd1 100.61(7) 2_664 2_664 ? C5 O4 Cd1 113.19(17) . 19_656 ? C5 O4 Eu1 91.94(16) . 2_664 ? Cd1 O4 Eu1 154.44(9) 19_656 2_664 ? Eu1 O5 H5A 110.1 . . ? Eu1 O5 H5B 109.5 . . ? H5A O5 H5B 109.8 . . ? 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 C1 C2 N1 167.4(3) . . . . ? O1 C1 C2 N1 -11.5(5) . . . . ? O2 C1 C2 C3 -11.3(5) . . . . ? O1 C1 C2 C3 169.7(3) . . . . ? N1 C2 C3 C4 -0.2(4) . . . . ? C1 C2 C3 C4 178.7(3) . . . . ? C2 C3 C4 N2 -0.3(4) . . . . ? C2 C3 C4 C5 -178.2(3) . . . . ? N2 C4 C5 O3 174.4(3) . . . . ? C3 C4 C5 O3 -7.8(5) . . . . ? N2 C4 C5 O4 -6.3(4) . . . . ? C3 C4 C5 O4 171.5(3) . . . . ? N2 C4 C5 Eu1 -91.0(9) . . . 2_664 ? C3 C4 C5 Eu1 86.8(10) . . . 2_664 ? C3 C2 N1 N2 0.5(4) . . . . ? C1 C2 N1 N2 -178.4(3) . . . . ? C3 C2 N1 Cd1 -171.8(2) . . . . ? C1 C2 N1 Cd1 9.2(4) . . . . ? O2 Cd1 N1 N2 -91.6(3) 11_556 . . . ? N2 Cd1 N1 N2 66.6(3) 22_565 . . . ? O1 Cd1 N1 N2 -173.1(3) . . . . ? O4 Cd1 N1 N2 -7.0(3) 22_565 . . . ? O3 Cd1 N1 N2 -172.6(2) 2_665 . . . ? O2 Cd1 N1 C2 77.6(2) 11_556 . . . ? N2 Cd1 N1 C2 -124.2(2) 22_565 . . . ? O1 Cd1 N1 C2 -3.9(2) . . . . ? O4 Cd1 N1 C2 162.2(2) 22_565 . . . ? O3 Cd1 N1 C2 -3.4(3) 2_665 . . . ? C2 N1 N2 C4 -0.7(3) . . . . ? Cd1 N1 N2 C4 169.0(2) . . . . ? C2 N1 N2 Cd1 178.5(2) . . . 19_656 ? Cd1 N1 N2 Cd1 -11.8(4) . . . 19_656 ? C3 C4 N2 N1 0.6(4) . . . . ? C5 C4 N2 N1 178.8(2) . . . . ? C3 C4 N2 Cd1 -178.7(2) . . . 19_656 ? C5 C4 N2 Cd1 -0.5(4) . . . 19_656 ? O2 C1 O1 Cd1 -171.6(3) . . . . ? C2 C1 O1 Cd1 7.2(4) . . . . ? O2 C1 O1 Eu1 12.7(6) . . . . ? C2 C1 O1 Eu1 -168.5(2) . . . . ? O2 Cd1 O1 C1 -104.0(2) 11_556 . . . ? N2 Cd1 O1 C1 108.9(2) 22_565 . . . ? N1 Cd1 O1 C1 -2.0(2) . . . . ? O4 Cd1 O1 C1 -57.3(4) 22_565 . . . ? O3 Cd1 O1 C1 178.3(2) 2_665 . . . ? O2 Cd1 O1 Eu1 73.13(10) 11_556 . . . ? N2 Cd1 O1 Eu1 -73.98(11) 22_565 . . . ? N1 Cd1 O1 Eu1 175.12(11) . . . . ? O4 Cd1 O1 Eu1 119.8(2) 22_565 . . . ? O3 Cd1 O1 Eu1 -4.62(7) 2_665 . . . ? O3 Eu1 O1 C1 -179.2(3) 2_665 . . . ? O3 Eu1 O1 C1 61.8(3) 12_654 . . . ? O3 Eu1 O1 C1 -49.3(3) 7_564 . . . ? O1 Eu1 O1 C1 109.3(3) 11_556 . . . ? O1 Eu1 O1 C1 32.1(3) 8_645 . . . ? O4 Eu1 O1 C1 159.3(3) 2_665 . . . ? O4 Eu1 O1 C1 -11.9(3) 12_654 . . . ? O4 Eu1 O1 C1 -105.4(3) 7_564 . . . ? O5 Eu1 O1 C1 -109.3(3) . . . . ? C5 Eu1 O1 C1 167.9(3) 2_665 . . . ? C5 Eu1 O1 C1 23.3(4) 12_654 . . . ? O3 Eu1 O1 Cd1 4.83(7) 2_665 . . . ? O3 Eu1 O1 Cd1 -114.12(9) 12_654 . . . ? O3 Eu1 O1 Cd1 134.73(10) 7_564 . . . ? O1 Eu1 O1 Cd1 -66.67(11) 11_556 . . . ? O1 Eu1 O1 Cd1 -143.86(8) 8_645 . . . ? O4 Eu1 O1 Cd1 -16.62(12) 2_665 . . . ? O4 Eu1 O1 Cd1 172.19(7) 12_654 . . . ? O4 Eu1 O1 Cd1 78.65(8) 7_564 . . . ? O5 Eu1 O1 Cd1 74.73(9) . . . . ? C5 Eu1 O1 Cd1 -7.98(10) 2_665 . . . ? C5 Eu1 O1 Cd1 -152.62(8) 12_654 . . . ? O1 C1 O2 Cd1 -14.7(6) . . . 8_645 ? C2 C1 O2 Cd1 166.5(3) . . . 8_645 ? O4 C5 O3 Eu1 -13.3(3) . . . 2_664 ? C4 C5 O3 Eu1 166.0(2) . . . 2_664 ? O4 C5 O3 Cd1 -126.3(3) . . . 2_664 ? C4 C5 O3 Cd1 52.9(4) . . . 2_664 ? Eu1 C5 O3 Cd1 -113.1(3) 2_664 . . 2_664 ? O3 C5 O4 Cd1 -171.7(2) . . . 19_656 ? C4 C5 O4 Cd1 9.0(3) . . . 19_656 ? Eu1 C5 O4 Cd1 175.20(17) 2_664 . . 19_656 ? O3 C5 O4 Eu1 13.1(3) . . . 2_664 ? C4 C5 O4 Eu1 -166.2(2) . . . 2_664 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 33.09 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.709 _refine_diff_density_min -1.163 _refine_diff_density_rms 0.128 _database_code_depnum_ccdc_archive 'CCDC 968565'