# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Zhong-Min Su' _publ_contact_author_email ZMSU@NENU.EDU.CN _publ_section_title ; A Series of Novel Chiral Lanthanide Coordination Polymers with Channels Constructed from 16Ln-Based Cage-like Building Units ; loop_ _publ_author_name 'Zhong-Min Su' 'Dong-Ying Du' 'Ya-Qian Lan' 'Kui-Zhan Shao' ; Xin-Long Wang ; 'Gang Yuan' # Attachment 'data1-7.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 736139' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H6 La N3 O7' _chemical_formula_sum 'C4 H6 La N3 O7' _chemical_formula_weight 343.00 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M p3221 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' 'y, x, -z' _cell_length_a 8.9410(5) _cell_length_b 8.9410(4) _cell_length_c 10.0260(4) _cell_angle_alpha 90.0000(10) _cell_angle_beta 90.0000(10) _cell_angle_gamma 120.000(5) _cell_volume 694.11(6) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3900 _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 4.639 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.257 _exptl_absorpt_correction_T_max 0.362 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4284 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 28.27 _reflns_number_total 1112 _reflns_number_gt 1100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _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^)+(0.0602P)^2^+1.8101P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(5) _refine_ls_number_reflns 1112 _refine_ls_number_parameters 54 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.77447(4) 0.0000 0.1667 0.00790(14) Uani 1 2 d S . . O2 O 0.5343(5) -0.2874(6) 0.2410(4) 0.0202(9) Uani 1 1 d . . . O1W O 1.0000 0.2491(3) 0.3333 0.0230(13) Uani 1 2 d SD . . H1W H 0.9345 0.2771 0.3746 0.035 Uiso 1 1 d RD . . C1 C 0.5271 -0.3742(3) 0.3417 0.0122(10) Uani 1 1 d R . . N1 N 0.8060 -0.1305(3) 0.4026 0.0147(9) Uani 1 1 d R . . C2 C 0.6741 -0.2859(3) 0.4376 0.0140(10) Uani 1 1 d R . . O2W O 0.1848 -0.4750(3) 0.1739 0.126(4) Uani 1 1 d RU . . N2 N 0.9238 -0.0761(3) 0.5000 0.0165(12) Uani 1 2 d SR . . O1 O 0.4084 -0.5252(3) 0.3631 0.0205(8) Uani 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.00684(16) 0.0092(2) 0.0085(2) 0.00124(13) 0.00062(7) 0.00458(11) O2 0.0158(18) 0.018(2) 0.0177(19) 0.0074(17) -0.0044(15) 0.0020(18) O1W 0.027(3) 0.017(2) 0.029(3) -0.0056(13) -0.011(3) 0.0133(16) C1 0.009(2) 0.014(3) 0.010(2) 0.0012(19) 0.0001(19) 0.003(2) N1 0.010(2) 0.013(2) 0.015(2) 0.0024(18) -0.0031(16) 0.0017(19) C2 0.014(2) 0.012(2) 0.012(2) -0.0006(19) 0.0008(19) 0.003(2) O2W 0.126(4) 0.126(4) 0.126(4) 0.0022(10) -0.0019(10) 0.063(2) N2 0.013(2) 0.013(2) 0.013(3) 0.0016(15) -0.0016(15) -0.001(3) O1 0.0184(19) 0.0139(19) 0.0186(19) 0.0055(17) -0.0003(15) 0.0000(16) _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 2.4246(15) 5_665 ? La1 O1 2.4246(15) 2_544 ? La1 O2 2.500(4) . ? La1 O2 2.500(4) 4 ? La1 N2 2.6971(13) 2_644 ? La1 O1W 2.7070(11) . ? La1 O1W 2.7070(11) 2_644 ? La1 N1 2.7139(12) . ? La1 N1 2.7139(12) 4 ? O2 C1 1.255(4) . ? O1W La1 2.7070(11) 3_765 ? O1W H1W 0.8500 . ? C1 O1 1.2501 . ? C1 C2 1.4959 . ? N1 N2 1.3370 . ? N1 C2 1.3437 . ? C2 C2 1.3958(19) 6_646 ? N2 N1 1.3378(16) 6_646 ? N2 La1 2.6971(13) 3_765 ? O1 La1 2.4246(15) 3_655 ? 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 74.4 5_665 2_544 ? O1 La1 O2 75.22(13) 5_665 . ? O1 La1 O2 72.86(10) 2_544 . ? O1 La1 O2 72.86(10) 5_665 4 ? O1 La1 O2 75.22(13) 2_544 4 ? O2 La1 O2 139.6(2) . 4 ? O1 La1 N2 142.8 5_665 2_644 ? O1 La1 N2 142.8 2_544 2_644 ? O2 La1 N2 110.16(12) . 2_644 ? O2 La1 N2 110.20(12) 4 2_644 ? O1 La1 O1W 76.43(4) 5_665 . ? O1 La1 O1W 140.004(18) 2_544 . ? O2 La1 O1W 124.41(10) . . ? O2 La1 O1W 70.43(12) 4 . ? N2 La1 O1W 70.53(7) 2_644 . ? O1 La1 O1W 140.004(18) 5_665 2_644 ? O1 La1 O1W 76.43(4) 2_544 2_644 ? O2 La1 O1W 70.43(12) . 2_644 ? O2 La1 O1W 124.41(10) 4 2_644 ? N2 La1 O1W 70.502(7) 2_644 2_644 ? O1W La1 O1W 141.04(7) . 2_644 ? O1 La1 N1 80.8 5_665 . ? O1 La1 N1 131.9 2_544 . ? O2 La1 N1 61.23(9) . . ? O2 La1 N1 134.53(11) 4 . ? N2 La1 N1 71.4 2_644 . ? O1W La1 N1 67.724(5) . . ? O1W La1 N1 99.58(3) 2_644 . ? O1 La1 N1 131.9 5_665 4 ? O1 La1 N1 80.8 2_544 4 ? O2 La1 N1 134.53(11) . 4 ? O2 La1 N1 61.23(9) 4 4 ? N2 La1 N1 71.4 2_644 4 ? O1W La1 N1 99.58(3) . 4 ? O1W La1 N1 67.724(5) 2_644 4 ? N1 La1 N1 142.8 . 4 ? C1 O2 La1 128.9(3) . . ? La1 O1W La1 126.47(9) . 3_765 ? La1 O1W H1W 101.7 . . ? La1 O1W H1W 111.9 3_765 . ? O1 C1 O2 124.0(2) . . ? O1 C1 C2 120.5 . . ? O2 C1 C2 115.5(2) . . ? N2 N1 C2 108.1 . . ? N2 N1 La1 135.4 . . ? C2 N1 La1 116.5 . . ? N1 C2 C2 107.1 . 6_646 ? N1 C2 C1 117.6 . . ? C2 C2 C1 135.3 6_646 . ? N1 N2 N1 109.7 6_646 . ? N1 N2 La1 125.14(7) 6_646 3_765 ? N1 N2 La1 125.2 . 3_765 ? C1 O1 La1 155.3 . 3_655 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.220 _refine_diff_density_min -1.858 _refine_diff_density_rms 0.231 data_2 _database_code_depnum_ccdc_archive 'CCDC 736140' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H6 Ce N3 O7' _chemical_formula_sum 'C4 H6 Ce N3 O7' _chemical_formula_weight 344.21 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M p3221 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' 'y, x, -z' _cell_length_a 8.888(5) _cell_length_b 8.888(8) _cell_length_c 9.973(6) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 120.000(5) _cell_volume 682.3(6) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3700 _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 483 _exptl_absorpt_coefficient_mu 5.027 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.2227 _exptl_absorpt_correction_T_max 0.340 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4169 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 28.30 _reflns_number_total 1076 _reflns_number_gt 1066 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _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^)+(0.0435P)^2^+2.0289P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.031(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 1076 _refine_ls_number_parameters 71 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.22572(4) 0.0000 0.6667 0.00876(15) Uani 1 2 d S . . O1 O 0.5927(5) 0.5259(6) 0.8623(4) 0.0210(8) Uani 1 1 d . . . C2 C 0.3262(7) 0.2859(7) 0.9374(5) 0.0156(10) Uani 1 1 d . . . O2 O 0.4660(5) 0.2878(6) 0.7394(4) 0.0203(8) Uani 1 1 d . . . O1W O 0.2476(6) 0.2476(6) 0.5000 0.0235(13) Uani 1 2 d SD . . H1W H 0.3382 0.2671 0.4571 0.035 Uiso 1 1 d RD . . C1 C 0.4741(6) 0.3749(7) 0.8409(5) 0.0130(10) Uani 1 1 d . . . N1 N 0.1935(5) 0.1295(6) 0.9019(4) 0.0154(9) Uani 1 1 d . . . N2 N 0.0745(7) 0.0745(7) 1.0000 0.0168(12) Uani 1 2 d S . . O2W O 0.8180(19) 0.472(2) 0.6728(14) 0.139(4) Uani 1 1 d U . . 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 Ce1 0.00799(17) 0.0102(2) 0.00885(19) -0.00136(12) -0.00068(6) 0.00508(11) O1 0.0183(18) 0.0147(19) 0.0190(18) -0.0039(16) 0.0016(14) 0.0000(15) C2 0.018(3) 0.012(2) 0.013(2) -0.0008(18) -0.0019(18) 0.005(2) O2 0.0174(17) 0.018(2) 0.0164(17) -0.0060(16) 0.0037(14) 0.0017(17) O1W 0.016(2) 0.016(2) 0.033(3) 0.0066(12) -0.0066(12) 0.005(2) C1 0.010(2) 0.014(2) 0.011(2) -0.0014(17) -0.0010(18) 0.002(2) N1 0.0121(19) 0.014(2) 0.014(2) -0.0003(17) 0.0028(15) 0.0024(17) N2 0.015(2) 0.015(2) 0.014(3) -0.0026(13) 0.0026(13) 0.002(3) O2W 0.139(4) 0.139(4) 0.139(4) -0.0023(10) 0.0019(10) 0.069(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 Ce1 O1 2.408(4) 5_656 ? Ce1 O1 2.408(4) 2_654 ? Ce1 O2 2.483(4) . ? Ce1 O2 2.483(4) 4_556 ? Ce1 N2 2.669(6) 2_554 ? Ce1 O1W 2.686(3) 3 ? Ce1 O1W 2.686(3) . ? Ce1 N1 2.691(5) . ? Ce1 N1 2.691(5) 4_556 ? O1 C1 1.242(7) . ? O1 Ce1 2.408(4) 3_665 ? C2 N1 1.345(7) . ? C2 C2 1.394(10) 6_557 ? C2 C1 1.497(7) . ? O2 C1 1.255(7) . ? O1W Ce1 2.686(3) 2_554 ? O1W H1W 0.8496 . ? N1 N2 1.340(5) . ? N2 N1 1.340(5) 6_557 ? N2 Ce1 2.669(6) 3 ? 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 Ce1 O1 75.00(18) 5_656 2_654 ? O1 Ce1 O2 75.54(16) 5_656 . ? O1 Ce1 O2 72.69(14) 2_654 . ? O1 Ce1 O2 72.69(14) 5_656 4_556 ? O1 Ce1 O2 75.54(16) 2_654 4_556 ? O2 Ce1 O2 139.7(2) . 4_556 ? O1 Ce1 N2 142.50(9) 5_656 2_554 ? O1 Ce1 N2 142.50(9) 2_654 2_554 ? O2 Ce1 N2 110.17(11) . 2_554 ? O2 Ce1 N2 110.17(11) 4_556 2_554 ? O1 Ce1 O1W 76.31(12) 5_656 3 ? O1 Ce1 O1W 140.51(14) 2_654 3 ? O2 Ce1 O1W 124.64(11) . 3 ? O2 Ce1 O1W 70.37(15) 4_556 3 ? N2 Ce1 O1W 70.29(8) 2_554 3 ? O1 Ce1 O1W 140.51(14) 5_656 . ? O1 Ce1 O1W 76.31(12) 2_654 . ? O2 Ce1 O1W 70.37(15) . . ? O2 Ce1 O1W 124.64(11) 4_556 . ? N2 Ce1 O1W 70.29(8) 2_554 . ? O1W Ce1 O1W 140.58(17) 3 . ? O1 Ce1 N1 80.56(15) 5_656 . ? O1 Ce1 N1 132.23(14) 2_654 . ? O2 Ce1 N1 61.66(13) . . ? O2 Ce1 N1 134.07(15) 4_556 . ? N2 Ce1 N1 71.32(10) 2_554 . ? O1W Ce1 N1 67.37(13) 3 . ? O1W Ce1 N1 99.71(11) . . ? O1 Ce1 N1 132.23(14) 5_656 4_556 ? O1 Ce1 N1 80.56(15) 2_654 4_556 ? O2 Ce1 N1 134.07(15) . 4_556 ? O2 Ce1 N1 61.66(13) 4_556 4_556 ? N2 Ce1 N1 71.32(10) 2_554 4_556 ? O1W Ce1 N1 99.71(11) 3 4_556 ? O1W Ce1 N1 67.37(13) . 4_556 ? N1 Ce1 N1 142.64(19) . 4_556 ? C1 O1 Ce1 154.9(4) . 3_665 ? N1 C2 C2 107.2(3) . 6_557 ? N1 C2 C1 117.5(4) . . ? C2 C2 C1 135.3(3) 6_557 . ? C1 O2 Ce1 128.7(3) . . ? Ce1 O1W Ce1 127.1(2) 2_554 . ? Ce1 O1W H1W 111.2 2_554 . ? Ce1 O1W H1W 98.7 . . ? O1 C1 O2 124.1(5) . . ? O1 C1 C2 120.5(5) . . ? O2 C1 C2 115.4(5) . . ? C2 N1 N2 108.0(4) . . ? C2 N1 Ce1 116.5(3) . . ? N2 N1 Ce1 135.5(3) . . ? N1 N2 N1 109.6(6) 6_557 . ? N1 N2 Ce1 125.2(3) 6_557 3 ? N1 N2 Ce1 125.2(3) . 3 ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.135 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.160 data_3 _database_code_depnum_ccdc_archive 'CCDC 736141' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H6 N3 O7 Pr' _chemical_formula_sum 'C4 H6 N3 O7 Pr' _chemical_formula_weight 345.00 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' 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 p3221 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' 'y, x, -z' _cell_length_a 8.841(4) _cell_length_b 8.841(4) _cell_length_c 9.922(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 120.000(5) _cell_volume 671.6(6) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4000 _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 486 _exptl_absorpt_coefficient_mu 5.464 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.265 _exptl_absorpt_correction_T_max 0.342 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4114 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 28.19 _reflns_number_total 1072 _reflns_number_gt 1056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _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^)+(0.0551P)^2^+1.9576P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_number_reflns 1072 _refine_ls_number_parameters 51 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0775 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.22550(4) 0.0000 0.6667 0.00827(14) Uani 1 2 d S . . O1W O 0.0000 -0.2462(3) 0.8333 0.0229(14) Uani 1 2 d SD . . H1W H -0.0795 -0.3412 0.7995 0.034 Uiso 1 1 d RD . . N1 N 0.1939 0.1291(3) 0.9018 0.0156(10) Uani 1 1 d R . . N2 N 0.0732 0.0731(3) 1.0000 0.0163(14) Uani 1 2 d SR . . C2 C 0.3263 0.2855(3) 0.9374 0.0159(12) Uani 1 1 d R . . O1 O 0.5942 0.5275(3) 0.8617 0.0203(9) Uani 1 1 d R . . O2 O 0.4659 0.2880(3) 0.7375 0.0196(9) Uani 1 1 d R . . C1 C 0.4744 0.3758(3) 0.8397 0.0125(11) Uani 1 1 d R . . O2W O 0.8153 0.4700(3) 0.6731 0.160(6) Uani 1 1 d RU . . 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 0.00743(17) 0.0097(2) 0.00843(19) -0.00125(14) -0.00062(7) 0.00484(11) O1W 0.024(3) 0.014(2) 0.034(4) 0.0064(14) 0.013(3) 0.0118(17) N1 0.012(2) 0.014(2) 0.017(2) -0.0001(19) 0.0035(18) 0.004(2) N2 0.017(2) 0.017(2) 0.010(3) -0.0021(14) 0.0021(14) 0.005(3) C2 0.018(3) 0.013(3) 0.014(3) 0.002(2) 0.001(2) 0.005(2) O1 0.018(2) 0.015(2) 0.017(2) -0.0030(18) 0.0011(16) 0.0005(18) O2 0.015(2) 0.018(2) 0.0145(19) -0.0075(18) 0.0019(16) -0.0002(19) C1 0.010(3) 0.016(3) 0.009(2) -0.001(2) -0.001(2) 0.005(2) O2W 0.160(6) 0.160(6) 0.160(6) -0.0014(10) 0.0012(10) 0.079(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 Pr1 O1 2.3898(17) 5_656 ? Pr1 O1 2.3898(17) 2_654 ? Pr1 O2 2.4665(19) . ? Pr1 O2 2.4665(19) 4_556 ? Pr1 N2 2.6404(19) 2_554 ? Pr1 O1W 2.6659(15) . ? Pr1 O1W 2.6659(15) 2_554 ? Pr1 N1 2.6723(15) . ? Pr1 N1 2.6723(15) 4_556 ? O1W Pr1 2.6659(15) 3 ? O1W H1W 0.8500 . ? N1 C2 1.3378 . ? N1 N2 1.3435 . ? N2 N1 1.3439(15) 6_557 ? N2 Pr1 2.6404(19) 3 ? C2 C2 1.3904(18) 6_557 ? C2 C1 1.4987 . ? O1 C1 1.2437 . ? O1 Pr1 2.3898(17) 3_665 ? O2 C1 1.2563 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pr1 O1 75.5 5_656 2_654 ? O1 Pr1 O2 75.8 5_656 . ? O1 Pr1 O2 72.51(7) 2_654 . ? O1 Pr1 O2 72.51(7) 5_656 4_556 ? O1 Pr1 O2 75.8 2_654 4_556 ? O2 Pr1 O2 139.59(8) . 4_556 ? O1 Pr1 N2 142.2 5_656 2_554 ? O1 Pr1 N2 142.2 2_654 2_554 ? O2 Pr1 N2 110.2 . 2_554 ? O2 Pr1 N2 110.22(8) 4_556 2_554 ? O1 Pr1 O1W 76.20(5) 5_656 . ? O1 Pr1 O1W 140.86(2) 2_654 . ? O2 Pr1 O1W 124.94(4) . . ? O2 Pr1 O1W 70.24(3) 4_556 . ? N2 Pr1 O1W 70.15(7) 2_554 . ? O1 Pr1 O1W 140.86(2) 5_656 2_554 ? O1 Pr1 O1W 76.20(5) 2_654 2_554 ? O2 Pr1 O1W 70.24(3) . 2_554 ? O2 Pr1 O1W 124.94(4) 4_556 2_554 ? N2 Pr1 O1W 70.136(10) 2_554 2_554 ? O1W Pr1 O1W 140.29(7) . 2_554 ? O1 Pr1 N1 80.2 5_656 . ? O1 Pr1 N1 132.3 2_654 . ? O2 Pr1 N1 62.0 . . ? O2 Pr1 N1 133.6 4_556 . ? N2 Pr1 N1 71.4 2_554 . ? O1W Pr1 N1 67.16(3) . . ? O1W Pr1 N1 99.90(5) 2_554 . ? O1 Pr1 N1 132.3 5_656 4_556 ? O1 Pr1 N1 80.2 2_654 4_556 ? O2 Pr1 N1 133.6 . 4_556 ? O2 Pr1 N1 62.0 4_556 4_556 ? N2 Pr1 N1 71.5 2_554 4_556 ? O1W Pr1 N1 99.90(5) . 4_556 ? O1W Pr1 N1 67.16(3) 2_554 4_556 ? N1 Pr1 N1 142.9 . 4_556 ? Pr1 O1W Pr1 127.48(9) . 3 ? Pr1 O1W H1W 118.2 . . ? Pr1 O1W H1W 92.0 3 . ? C2 N1 N2 108.2 . . ? C2 N1 Pr1 116.6 . . ? N2 N1 Pr1 135.2 . . ? N1 N2 N1 109.0 6_557 . ? N1 N2 Pr1 125.51(7) 6_557 3 ? N1 N2 Pr1 125.5 . 3 ? N1 C2 C2 107.3 . 6_557 ? N1 C2 C1 117.4 . . ? C2 C2 C1 135.3 6_557 . ? C1 O1 Pr1 154.9 . 3_665 ? C1 O2 Pr1 128.5 . . ? O1 C1 O2 124.3 . . ? O1 C1 C2 120.4 . . ? O2 C1 C2 115.2 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.395 _refine_diff_density_min -1.047 _refine_diff_density_rms 0.217 data_4 _database_code_depnum_ccdc_archive 'CCDC 736142' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H6 N3 Nd O7' _chemical_formula_sum 'C4 H6 N3 Nd O7' _chemical_formula_weight 352.36 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' 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 p3221 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' 'y, x, -z' _cell_length_a 8.8050(9) _cell_length_b 8.8050(9) _cell_length_c 9.8830(10) _cell_angle_alpha 90.0000(12) _cell_angle_beta 90.0000(10) _cell_angle_gamma 120.000(10) _cell_volume 663.56(10) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'total reflection' _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 501 _exptl_absorpt_coefficient_mu 5.894 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.184 _exptl_absorpt_correction_T_max 0.302 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area-detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4042 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 28.32 _reflns_number_total 1063 _reflns_number_gt 1042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _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^)+(0.0350P)^2^+2.1989P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(6) _refine_ls_number_reflns 1063 _refine_ls_number_parameters 70 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0224 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.664 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.77471(6) 0.0000 0.6667 0.00858(17) Uani 1 2 d S . . O1W O 1.0000 0.2457(10) 0.8333 0.025(2) Uani 1 2 d SD . . H1W H 1.0677 0.3371 0.7881 0.037 Uiso 1 1 d RD . . O2 O 0.2885(9) -0.1777(10) 0.4025(6) 0.0194(12) Uani 1 1 d . . . O1 O 0.5286(9) -0.0672(10) 0.5274(6) 0.0207(12) Uani 1 1 d . . . C1 C 0.3770(12) -0.0983(11) 0.5058(8) 0.0141(16) Uani 1 1 d . . . C2 C 0.2858(11) -0.0403(11) 0.6038(8) 0.0151(16) Uani 1 1 d . . . N2 N 0.0728(11) 0.0000 0.6667 0.0164(19) Uani 1 2 d S . . N1 N 0.1291(9) -0.0644(10) 0.5688(7) 0.0149(14) Uani 1 1 d . . . O2W O 1.182(3) 0.534(4) 0.671(3) 0.184(10) Uani 1 1 d DU . . H1 H 1.2261 0.4837 0.6256 0.276 Uiso 1 1 d RD . . H2 H 1.1578 0.5807 0.7367 0.276 Uiso 1 1 d RD . . 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 0.0081(2) 0.0102(3) 0.0081(2) 0.0012(2) 0.00061(10) 0.00508(14) O1W 0.026(5) 0.016(3) 0.036(5) -0.007(2) -0.013(4) 0.013(2) O2 0.018(3) 0.034(4) 0.012(3) -0.010(3) -0.006(2) 0.018(3) O1 0.016(3) 0.032(3) 0.017(3) -0.004(3) -0.004(3) 0.015(3) C1 0.016(4) 0.017(4) 0.011(3) -0.002(3) -0.004(3) 0.009(3) C2 0.014(4) 0.019(4) 0.011(3) 0.001(3) -0.001(3) 0.007(3) N2 0.015(3) 0.024(6) 0.013(4) -0.005(4) -0.003(2) 0.012(3) N1 0.014(3) 0.020(4) 0.014(3) -0.007(3) -0.001(3) 0.011(3) O2W 0.184(10) 0.184(10) 0.184(10) 0.0009(16) -0.0004(16) 0.092(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O1 2.378(6) 4_556 ? Nd1 O1 2.378(6) . ? Nd1 O2 2.456(6) 3_655 ? Nd1 O2 2.456(6) 6_656 ? Nd1 N2 2.625(10) 1_655 ? Nd1 O1W 2.653(4) . ? Nd1 O1W 2.653(4) 2_644 ? Nd1 N1 2.666(7) 3_655 ? Nd1 N1 2.666(7) 6_656 ? O1W Nd1 2.653(4) 3_765 ? O1W H1W 0.8500 . ? O2 C1 1.262(10) . ? O2 Nd1 2.456(6) 2_544 ? O1 C1 1.240(11) . ? C1 C2 1.501(11) . ? C2 N1 1.333(11) . ? C2 C2 1.385(16) 4_556 ? N2 N1 1.335(9) 4_556 ? N2 N1 1.335(8) . ? N2 Nd1 2.625(10) 1_455 ? N1 Nd1 2.666(7) 2_544 ? O2W H1 0.8500 . ? O2W H2 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nd1 O1 76.3(3) 4_556 . ? O1 Nd1 O2 76.1(3) 4_556 3_655 ? O1 Nd1 O2 72.3(2) . 3_655 ? O1 Nd1 O2 72.3(2) 4_556 6_656 ? O1 Nd1 O2 76.1(3) . 6_656 ? O2 Nd1 O2 139.5(3) 3_655 6_656 ? O1 Nd1 N2 141.86(14) 4_556 1_655 ? O1 Nd1 N2 141.86(14) . 1_655 ? O2 Nd1 N2 110.27(17) 3_655 1_655 ? O2 Nd1 N2 110.27(17) 6_656 1_655 ? O1 Nd1 O1W 75.86(18) 4_556 . ? O1 Nd1 O1W 141.2(2) . . ? O2 Nd1 O1W 125.28(16) 3_655 . ? O2 Nd1 O1W 70.0(2) 6_656 . ? N2 Nd1 O1W 70.12(13) 1_655 . ? O1 Nd1 O1W 141.2(2) 4_556 2_644 ? O1 Nd1 O1W 75.86(18) . 2_644 ? O2 Nd1 O1W 70.0(2) 3_655 2_644 ? O2 Nd1 O1W 125.28(16) 6_656 2_644 ? N2 Nd1 O1W 70.12(13) 1_655 2_644 ? O1W Nd1 O1W 140.2(3) . 2_644 ? O1 Nd1 N1 79.9(2) 4_556 3_655 ? O1 Nd1 N1 132.5(2) . 3_655 ? O2 Nd1 N1 62.4(2) 3_655 3_655 ? O2 Nd1 N1 133.2(2) 6_656 3_655 ? N2 Nd1 N1 71.44(15) 1_655 3_655 ? O1W Nd1 N1 67.1(2) . 3_655 ? O1W Nd1 N1 99.97(17) 2_644 3_655 ? O1 Nd1 N1 132.5(2) 4_556 6_656 ? O1 Nd1 N1 79.9(2) . 6_656 ? O2 Nd1 N1 133.2(2) 3_655 6_656 ? O2 Nd1 N1 62.4(2) 6_656 6_656 ? N2 Nd1 N1 71.44(15) 1_655 6_656 ? O1W Nd1 N1 99.97(17) . 6_656 ? O1W Nd1 N1 67.1(2) 2_644 6_656 ? N1 Nd1 N1 142.9(3) 3_655 6_656 ? Nd1 O1W Nd1 127.6(3) . 3_765 ? Nd1 O1W H1W 109.3 . . ? Nd1 O1W H1W 101.3 3_765 . ? C1 O2 Nd1 128.2(5) . 2_544 ? C1 O1 Nd1 154.2(6) . . ? O2 C1 O1 124.0(8) . . ? O2 C1 C2 115.1(8) . . ? O1 C1 C2 120.9(7) . . ? N1 C2 C2 107.1(4) . 4_556 ? N1 C2 C1 117.7(7) . . ? C2 C2 C1 135.2(5) 4_556 . ? N1 N2 N1 108.6(9) 4_556 . ? N1 N2 Nd1 125.7(4) 4_556 1_455 ? N1 N2 Nd1 125.7(4) . 1_455 ? C2 N1 N2 108.6(7) . . ? C2 N1 Nd1 116.3(5) . 2_544 ? N2 N1 Nd1 135.1(5) . 2_544 ? H1 O2W H2 161.0 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.179 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.180 data_5 _database_code_depnum_ccdc_archive 'CCDC 736143' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H6 N3 O7 Sm' _chemical_formula_sum 'C4 H6 N3 O7 Sm' _chemical_formula_weight 354.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M p3221 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' 'y, x, -z' _cell_length_a 8.712(4) _cell_length_b 8.712(4) _cell_length_c 9.818(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 120.000(5) _cell_volume 645.3(6) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 495 _exptl_absorpt_coefficient_mu 6.849 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.247 _exptl_absorpt_correction_T_max 0.332 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3961 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 28.19 _reflns_number_total 1036 _reflns_number_gt 1021 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _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^)+(0.0364P)^2^+3.0185P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_number_reflns 1036 _refine_ls_number_parameters 71 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0609 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.070 _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 Sm1 Sm 0.77511(4) 0.0000 0.6667 0.00784(12) Uani 1 2 d S . . O1W O 1.0000 0.2461(8) 0.8333 0.0310(18) Uani 1 2 d SD . . H1W H 1.0689 0.3377 0.7873 0.047 Uiso 1 1 d RD . . C2 C 0.6714(8) -0.2878(8) 0.9364(6) 0.0137(12) Uani 1 1 d . . . O1 O 0.4013(6) -0.5335(6) 0.8583(4) 0.0196(9) Uani 1 1 d . . . O2 O 0.5345(6) -0.2897(7) 0.7332(5) 0.0230(10) Uani 1 1 d . . . C1 C 0.5237(9) -0.3794(9) 0.8376(6) 0.0153(12) Uani 1 1 d . . . N1 N 0.8070(6) -0.1278(7) 0.9002(5) 0.0138(10) Uani 1 1 d . . . N2 N 0.9290(8) -0.0710(8) 1.0000 0.0150(14) Uani 1 2 d S . . O2W O 1.243(4) 0.482(4) 0.612(3) 0.332(15) Uani 1 1 d U . . 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 0.00710(15) 0.0093(2) 0.00781(17) 0.00103(14) 0.00051(7) 0.00467(10) O1W 0.030(4) 0.019(3) 0.048(5) -0.0122(18) -0.024(4) 0.0149(19) C2 0.015(3) 0.014(3) 0.009(2) 0.000(2) -0.002(2) 0.005(2) O1 0.017(2) 0.015(2) 0.015(2) 0.0062(18) -0.0002(16) -0.0010(18) O2 0.019(2) 0.018(2) 0.016(2) 0.0075(19) -0.0077(17) -0.0029(19) C1 0.013(3) 0.015(3) 0.013(2) -0.001(2) -0.002(2) 0.004(3) N1 0.011(2) 0.013(2) 0.012(2) 0.0006(19) -0.0022(18) 0.002(2) N2 0.012(2) 0.012(2) 0.014(3) 0.0021(15) -0.0021(15) 0.001(3) O2W 0.33(2) 0.29(2) 0.295(18) 0.091(15) -0.191(15) 0.093(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O1 2.344(4) 5_666 ? Sm1 O1 2.344(4) 2_544 ? Sm1 O2 2.429(5) . ? Sm1 O2 2.429(5) 4_556 ? Sm1 N2 2.578(7) 2_644 ? Sm1 N1 2.623(5) . ? Sm1 N1 2.623(5) 4_556 ? Sm1 O1W 2.629(3) . ? Sm1 O1W 2.629(3) 2_644 ? O1W Sm1 2.629(3) 3_765 ? O1W H1W 0.8500 . ? C2 N1 1.348(8) . ? C2 C2 1.392(11) 6_647 ? C2 C1 1.486(8) . ? O1 C1 1.245(8) . ? O1 Sm1 2.344(4) 3_655 ? O2 C1 1.263(8) . ? N1 N2 1.345(6) . ? N2 N1 1.345(6) 6_647 ? N2 Sm1 2.578(7) 3_765 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sm1 O1 78.0(2) 5_666 2_544 ? O1 Sm1 O2 76.3(2) 5_666 . ? O1 Sm1 O2 72.78(17) 2_544 . ? O1 Sm1 O2 72.78(17) 5_666 4_556 ? O1 Sm1 O2 76.3(2) 2_544 4_556 ? O2 Sm1 O2 139.8(3) . 4_556 ? O1 Sm1 N2 140.98(10) 5_666 2_644 ? O1 Sm1 N2 140.98(10) 2_544 2_644 ? O2 Sm1 N2 110.08(14) . 2_644 ? O2 Sm1 N2 110.08(14) 4_556 2_644 ? O1 Sm1 N1 78.80(17) 5_666 . ? O1 Sm1 N1 133.52(17) 2_544 . ? O2 Sm1 N1 62.83(15) . . ? O2 Sm1 N1 132.46(17) 4_556 . ? N2 Sm1 N1 71.45(11) 2_644 . ? O1 Sm1 N1 133.52(17) 5_666 4_556 ? O1 Sm1 N1 78.80(17) 2_544 4_556 ? O2 Sm1 N1 132.46(17) . 4_556 ? O2 Sm1 N1 62.83(15) 4_556 4_556 ? N2 Sm1 N1 71.45(11) 2_644 4_556 ? N1 Sm1 N1 142.9(2) . 4_556 ? O1 Sm1 O1W 75.20(14) 5_666 . ? O1 Sm1 O1W 141.26(17) 2_544 . ? O2 Sm1 O1W 125.72(13) . . ? O2 Sm1 O1W 69.39(19) 4_556 . ? N2 Sm1 O1W 70.27(11) 2_644 . ? N1 Sm1 O1W 66.94(15) . . ? N1 Sm1 O1W 100.19(13) 4_556 . ? O1 Sm1 O1W 141.26(18) 5_666 2_644 ? O1 Sm1 O1W 75.20(13) 2_544 2_644 ? O2 Sm1 O1W 69.39(19) . 2_644 ? O2 Sm1 O1W 125.72(13) 4_556 2_644 ? N2 Sm1 O1W 70.27(11) 2_644 2_644 ? N1 Sm1 O1W 100.19(13) . 2_644 ? N1 Sm1 O1W 66.94(15) 4_556 2_644 ? O1W Sm1 O1W 140.5(2) . 2_644 ? Sm1 O1W Sm1 127.4(3) . 3_765 ? Sm1 O1W H1W 108.9 . . ? Sm1 O1W H1W 101.3 3_765 . ? N1 C2 C2 107.3(3) . 6_647 ? N1 C2 C1 117.3(5) . . ? C2 C2 C1 135.4(4) 6_647 . ? C1 O1 Sm1 152.8(4) . 3_655 ? C1 O2 Sm1 128.3(4) . . ? O1 C1 O2 124.0(6) . . ? O1 C1 C2 121.2(6) . . ? O2 C1 C2 114.9(6) . . ? C2 N1 N2 108.1(5) . . ? C2 N1 Sm1 116.5(4) . . ? N2 N1 Sm1 135.4(4) . . ? N1 N2 N1 109.2(7) . 6_647 ? N1 N2 Sm1 125.4(3) . 3_765 ? N1 N2 Sm1 125.4(3) 6_647 3_765 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.354 _refine_diff_density_min -1.789 _refine_diff_density_rms 0.181 data_6 _database_code_depnum_ccdc_archive 'CCDC 736144' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H6 Eu N3 O7' _chemical_formula_sum 'C4 H6 Eu N3 O7' _chemical_formula_weight 360.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 p3221 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' 'y, x, -z' _cell_length_a 8.674(5) _cell_length_b 8.674(5) _cell_length_c 9.796(6) _cell_angle_alpha 90.000(7) _cell_angle_beta 90.000(7) _cell_angle_gamma 120.000(6) _cell_volume 638.3(6) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'total reflection' _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.810 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 510 _exptl_absorpt_coefficient_mu 7.396 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.296 _exptl_absorpt_correction_T_max 0.421 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area-detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3919 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 28.33 _reflns_number_total 1024 _reflns_number_gt 1009 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _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^)+(0.0441P)^2^+3.5201P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(4) _refine_ls_number_reflns 1024 _refine_ls_number_parameters 51 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0717 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.048 _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 Eu1 Eu 0.77540(4) 0.0000 0.1667 0.00778(13) Uani 1 2 d S . . O1W O 1.0000 0.2443(3) 0.3333 0.036(2) Uani 1 2 d SD . . H1W H 0.9281 0.2825 0.3466 0.055 Uiso 1 1 d RD . . O2 O 0.5357 -0.2909(3) 0.2314 0.0236(11) Uani 1 1 d R . . N1 N 0.8077 -0.1278(3) 0.4005 0.0142(11) Uani 1 1 d R . . O1 O 0.3996 -0.5343(3) 0.3583 0.0195(10) Uani 1 1 d R . . N2 N 0.9283 -0.0717(3) 0.5000 0.0127(14) Uani 1 2 d SR . . C1 C 0.5220 -0.3811(3) 0.3369 0.0155(12) Uani 1 1 d R . . C2 C 0.6719 -0.2872(3) 0.4363 0.0143(13) Uani 1 1 d R . . O2W O 0.2983 -0.5131(3) 0.0761 0.357(18) Uani 1 1 d RU . . H1 H 0.3839 -0.4709 0.1330 0.536 Uiso 1 1 d R . . H2 H 0.2527 -0.4462 0.0769 0.536 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.00718(16) 0.0094(2) 0.00747(19) 0.00096(14) 0.00048(7) 0.00472(11) O1W 0.037(5) 0.018(3) 0.060(6) -0.019(2) -0.039(4) 0.019(2) O2 0.022(2) 0.017(2) 0.013(2) 0.007(2) -0.0075(19) -0.004(2) N1 0.013(2) 0.013(3) 0.013(3) 0.000(2) -0.002(2) 0.004(2) O1 0.018(2) 0.014(2) 0.015(2) 0.0039(19) 0.0002(17) -0.0008(19) N2 0.008(2) 0.008(2) 0.015(3) 0.0040(16) -0.0040(16) -0.001(3) C1 0.019(3) 0.017(3) 0.011(3) 0.000(2) -0.001(2) 0.009(3) C2 0.016(3) 0.014(3) 0.011(3) -0.001(2) -0.001(2) 0.006(3) O2W 0.357(18) 0.357(18) 0.357(18) 0.0002(10) -0.0004(10) 0.179(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O1 2.3305(17) 5_665 ? Eu1 O1 2.3305(17) 2_544 ? Eu1 O2 2.418(2) . ? Eu1 O2 2.418(2) 4 ? Eu1 N2 2.570(2) 2_644 ? Eu1 O1W 2.6122(15) . ? Eu1 O1W 2.6122(15) 2_644 ? Eu1 N1 2.6204(16) . ? Eu1 N1 2.6204(16) 4 ? Eu1 H1W 2.7604 . ? O1W Eu1 2.6122(15) 3_765 ? O1W H1W 0.8500 . ? O2 C1 1.2650 . ? N1 N2 1.3309 . ? N1 C2 1.3390 . ? O1 C1 1.2354 . ? O1 Eu1 2.3305(17) 3_655 ? N2 N1 1.3309(16) 6_646 ? N2 Eu1 2.570(2) 3_765 ? C1 C2 1.4978 . ? C2 C2 1.392(2) 6_646 ? O2W H1 0.8500 . ? O2W H2 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Eu1 O1 78.5 5_665 2_544 ? O1 Eu1 O2 77.0 5_665 . ? O1 Eu1 O2 72.65(8) 2_544 . ? O1 Eu1 O2 72.65(8) 5_665 4 ? O1 Eu1 O2 77.0 2_544 4 ? O2 Eu1 O2 140.48(9) . 4 ? O1 Eu1 N2 140.7 5_665 2_644 ? O1 Eu1 N2 140.7 2_544 2_644 ? O2 Eu1 N2 109.8 . 2_644 ? O2 Eu1 N2 109.76(9) 4 2_644 ? O1 Eu1 O1W 75.00(5) 5_665 . ? O1 Eu1 O1W 141.77(2) 2_544 . ? O2 Eu1 O1W 125.88(4) . . ? O2 Eu1 O1W 69.14(3) 4 . ? N2 Eu1 O1W 70.11(7) 2_644 . ? O1 Eu1 O1W 141.77(2) 5_665 2_644 ? O1 Eu1 O1W 75.00(5) 2_544 2_644 ? O2 Eu1 O1W 69.14(3) . 2_644 ? O2 Eu1 O1W 125.88(4) 4 2_644 ? N2 Eu1 O1W 70.118(10) 2_644 2_644 ? O1W Eu1 O1W 140.23(8) . 2_644 ? O1 Eu1 N1 78.7 5_665 . ? O1 Eu1 N1 133.6 2_544 . ? O2 Eu1 N1 63.1 . . ? O2 Eu1 N1 131.9 4 . ? N2 Eu1 N1 71.4 2_644 . ? O1W Eu1 N1 66.59(3) . . ? O1W Eu1 N1 100.41(5) 2_644 . ? O1 Eu1 N1 133.6 5_665 4 ? O1 Eu1 N1 78.7 2_544 4 ? O2 Eu1 N1 131.9 . 4 ? O2 Eu1 N1 63.1 4 4 ? N2 Eu1 N1 71.4 2_644 4 ? O1W Eu1 N1 100.41(5) . 4 ? O1W Eu1 N1 66.59(3) 2_644 4 ? N1 Eu1 N1 142.9 . 4 ? O1 Eu1 H1W 58.9 5_665 . ? O1 Eu1 H1W 124.9 2_544 . ? O2 Eu1 H1W 122.6 . . ? O2 Eu1 H1W 59.0 4 . ? N2 Eu1 H1W 87.9 2_644 . ? O1W Eu1 H1W 17.9 . . ? O1W Eu1 H1W 158.0 2_644 . ? N1 Eu1 H1W 73.3 . . ? N1 Eu1 H1W 105.4 4 . ? Eu1 O1W Eu1 127.99(10) . 3_765 ? Eu1 O1W H1W 90.9 . . ? Eu1 O1W H1W 130.3 3_765 . ? C1 O2 Eu1 128.7 . . ? N2 N1 C2 108.1 . . ? N2 N1 Eu1 135.7 . . ? C2 N1 Eu1 116.1 . . ? C1 O1 Eu1 152.9 . 3_655 ? N1 N2 N1 109.7 6_646 . ? N1 N2 Eu1 125.15(7) 6_646 3_765 ? N1 N2 Eu1 125.2 . 3_765 ? O1 C1 O2 124.6 . . ? O1 C1 C2 121.4 . . ? O2 C1 C2 114.0 . . ? N1 C2 C2 107.0 . 6_646 ? N1 C2 C1 117.9 . . ? C2 C2 C1 135.0 6_646 . ? H1 O2W H2 107.7 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.656 _refine_diff_density_min -1.804 _refine_diff_density_rms 0.212 data_7 _database_code_depnum_ccdc_archive 'CCDC 736145' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H6 Gd N3 O7' _chemical_formula_sum 'C4 H6 Gd N3 O7' _chemical_formula_weight 365.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 p3221 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' 'y, x, -z' _cell_length_a 8.639(7) _cell_length_b 8.639(5) _cell_length_c 9.772(6) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 120.000(5) _cell_volume 631.6(6) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'total reflection' _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.882 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 513 _exptl_absorpt_coefficient_mu 7.902 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.148 _exptl_absorpt_correction_T_max 0.245 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area-detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3820 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 28.28 _reflns_number_total 992 _reflns_number_gt 979 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _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^)+(0.0606P)^2^+3.7295P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(5) _refine_ls_number_reflns 992 _refine_ls_number_parameters 51 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.22438(5) 0.0000 0.1667 0.00704(16) Uani 1 2 d S . . O1W O 0.2434(3) 0.2434(3) 0.0000 0.0312(15) Uani 1 2 d SDU . . H1W H 0.3003 0.3576 0.0033 0.047 Uiso 1 1 d RD . . N1 N 0.0646(3) -0.1280(3) -0.0664 0.0137(12) Uani 1 1 d R . . N2 N -0.0004(3) -0.0709(3) -0.1667 0.0126(16) Uani 1 2 d SRU . . C2 C 0.0411(3) -0.2879(3) -0.1036 0.0136(14) Uani 1 1 d R . . O1 O 0.4641(3) 0.0673(3) 0.0243 0.0179(11) Uani 1 1 d R . . O2 O 0.1719(3) -0.2925(3) 0.1025 0.0230(13) Uani 1 1 d R . . C1 C 0.0960(3) -0.3803(3) -0.0024 0.0136(13) Uani 1 1 d R . . O2W O 0.1824(3) -0.5259(3) 0.2717 0.36(2) Uani 1 1 d RU . . H1 H 0.1328 -0.5035 0.3378 0.538 Uiso 1 1 d R . . H2 H 0.2050 -0.5909 0.2195 0.538 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.00606(19) 0.0080(2) 0.0077(2) -0.00093(16) -0.00047(8) 0.00398(12) O1W 0.0308(15) 0.0308(15) 0.0321(18) 0.0020(7) -0.0020(7) 0.0155(11) N1 0.017(3) 0.013(3) 0.014(3) 0.001(2) 0.000(3) 0.009(3) N2 0.015(4) 0.008(3) 0.018(4) -0.0034(17) -0.007(3) 0.008(2) C2 0.015(3) 0.011(3) 0.014(3) 0.002(3) -0.001(3) 0.006(3) O1 0.012(3) 0.030(3) 0.017(3) 0.001(2) 0.002(2) 0.013(2) O2 0.048(4) 0.011(3) 0.014(2) -0.006(2) -0.015(3) 0.018(3) C1 0.016(3) 0.014(3) 0.013(3) 0.002(3) -0.003(3) 0.009(3) O2W 0.36(2) 0.36(2) 0.36(2) 0.0001(10) -0.0001(10) 0.179(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.3147(19) 4 ? Gd1 O1 2.3147(19) . ? Gd1 O2 2.416(2) 4 ? Gd1 O2 2.416(2) . ? Gd1 N2 2.549(2) 3 ? Gd1 O1W 2.5992(16) 3 ? Gd1 O1W 2.5992(16) . ? Gd1 N1 2.6056(18) 4 ? Gd1 N1 2.6056(18) . ? O1W Gd1 2.5992(16) 2_554 ? O1W H1W 0.8552 . ? N1 N2 1.3399 . ? N1 C2 1.3424 . ? N2 N1 1.3376(19) 5_554 ? N2 Gd1 2.549(2) 2_554 ? C2 C2 1.378(2) 5_554 ? C2 C1 1.4891 . ? O1 C1 1.2574 6_655 ? O2 C1 1.2489 . ? C1 O1 1.2574 6_545 ? O2W H1 0.8500 . ? O2W H2 0.8500 . ? 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 Gd1 O1 79.4 4 . ? O1 Gd1 O2 77.5 4 4 ? O1 Gd1 O2 72.60(9) . 4 ? O1 Gd1 O2 72.60(9) 4 . ? O1 Gd1 O2 77.5 . . ? O2 Gd1 O2 140.81(10) 4 . ? O1 Gd1 N2 140.3 4 3 ? O1 Gd1 N2 140.3 . 3 ? O2 Gd1 N2 109.53(11) 4 3 ? O2 Gd1 N2 109.7 . 3 ? O1 Gd1 O1W 74.55(6) 4 3 ? O1 Gd1 O1W 142.31(2) . 3 ? O2 Gd1 O1W 125.91(4) 4 3 ? O2 Gd1 O1W 69.04(3) . 3 ? N2 Gd1 O1W 70.101(11) 3 3 ? O1 Gd1 O1W 142.31(2) 4 . ? O1 Gd1 O1W 74.55(6) . . ? O2 Gd1 O1W 69.04(3) 4 . ? O2 Gd1 O1W 125.91(4) . . ? N2 Gd1 O1W 69.99(9) 3 . ? O1W Gd1 O1W 140.10(9) 3 . ? O1 Gd1 N1 78.4 4 4 ? O1 Gd1 N1 133.6 . 4 ? O2 Gd1 N1 63.1 4 4 ? O2 Gd1 N1 131.8 . 4 ? N2 Gd1 N1 71.5 3 4 ? O1W Gd1 N1 66.51(3) 3 4 ? O1W Gd1 N1 100.48(6) . 4 ? O1 Gd1 N1 133.6 4 . ? O1 Gd1 N1 78.4 . . ? O2 Gd1 N1 131.8 4 . ? O2 Gd1 N1 63.1 . . ? N2 Gd1 N1 71.5 3 . ? O1W Gd1 N1 100.48(6) 3 . ? O1W Gd1 N1 66.51(3) . . ? N1 Gd1 N1 143.0 4 . ? Gd1 O1W Gd1 128.28(12) 2_554 . ? Gd1 O1W H1W 94.4 2_554 . ? Gd1 O1W H1W 132.6 . . ? N2 N1 C2 107.8 . . ? N2 N1 Gd1 135.5 . . ? C2 N1 Gd1 116.7 . . ? N1 N2 N1 109.37(6) 5_554 . ? N1 N2 Gd1 125.38(8) 5_554 2_554 ? N1 N2 Gd1 125.2 . 2_554 ? N1 C2 C2 107.5 . 5_554 ? N1 C2 C1 116.6 . . ? C2 C2 C1 135.8 5_554 . ? C1 O1 Gd1 152.4 6_655 . ? C1 O2 Gd1 127.9 . . ? O2 C1 O1 123.5 . 6_545 ? O2 C1 C2 115.5 . . ? O1 C1 C2 120.9 6_545 . ? H1 O2W H2 156.2 . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.988 _refine_diff_density_min -1.886 _refine_diff_density_rms 0.231