# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Linpei Jin' _publ_contact_author_email LPJIN@BNU.EDU.CN _publ_section_title ; Water chain supported architecture of lanthanide coordination polymers with pyrazinetricarboxylic acid ; loop_ _publ_author_name 'Linpei Jin.' 'Yonghong Wan.' 'Feng-Qin Wang.' 'Kezhi Wang.' ; Xiang-Jun Zheng ; 'Xiao-Yu Zhou.' # Attachment '1-eu.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 291610' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H13 Eu N2 O12' _chemical_formula_weight 469.15 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 Monoclinic _symmetry_space_group_name_H-M P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.571(4) _cell_length_b 6.751(2) _cell_length_c 11.093(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.300(5) _cell_angle_gamma 90.00 _cell_volume 658.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3035 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 26.33 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 4.836 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.452 _exptl_absorpt_correction_T_max 0.608 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 3768 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.35 _reflns_number_total 1454 _reflns_number_gt 1355 _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^)+(0.0810P)^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 1454 _refine_ls_number_parameters 125 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1073 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.38518(3) 0.7500 0.23011(3) 0.01358(18) Uani 1 2 d S . . O1 O 0.2424(5) 0.7500 -0.0031(5) 0.0232(12) Uani 1 2 d S . . O2 O 0.0296(6) 0.7500 -0.1830(6) 0.0310(14) Uani 1 2 d S . . O3 O -0.2970(4) 0.9141(5) -0.2196(4) 0.0273(9) Uani 1 1 d . . . O4 O 0.2816(6) 0.7500 0.3988(5) 0.0222(11) Uani 1 2 d S . . O5 O 0.0903(6) 0.7500 0.4666(6) 0.0368(16) Uani 1 2 d S . . N1 N 0.0964(7) 0.7500 0.1519(7) 0.0166(13) Uani 1 2 d S . . N2 N -0.2158(7) 0.7500 0.0650(7) 0.0244(14) Uani 1 2 d S . . C1 C 0.0984(7) 0.7500 -0.0639(7) 0.0168(14) Uani 1 2 d S . . C2 C 0.0092(8) 0.7500 0.0234(7) 0.0152(14) Uani 1 2 d S . . C3 C -0.1496(8) 0.7500 -0.0204(8) 0.0182(15) Uani 1 2 d S . . C4 C -0.2562(7) 0.7500 -0.1649(8) 0.0170(14) Uani 1 2 d S . . C5 C -0.1268(8) 0.7500 0.1915(10) 0.0292(18) Uani 1 2 d S . . H5A H -0.1715 0.7500 0.2522 0.035 Uiso 1 2 calc SR . . C6 C 0.0323(8) 0.7500 0.2376(7) 0.0162(14) Uani 1 2 d S . . C7 C 0.1434(10) 0.7500 0.3813(8) 0.0213(16) Uani 1 2 d S . . O6 O 0.5765(4) 0.5520(6) 0.4049(4) 0.0348(10) Uani 1 1 d . . . H6A H 0.5507 0.4344 0.4143 0.042 Uiso 1 1 d R . . H6B H 0.6263 0.5926 0.4828 0.042 Uiso 1 1 d R . . O7 O 0.5331(5) 0.5422(7) 0.1369(5) 0.0409(11) Uani 1 1 d . . . H7A H 0.5737 0.5912 0.0880 0.049 Uiso 1 1 d R . . H7B H 0.6030 0.4668 0.1872 0.049 Uiso 1 1 d R . . O8 O 0.7312(6) 1.2500 0.2679(6) 0.0305(14) Uani 1 2 d S . . H8A H 0.7777 1.2500 0.3510 0.037 Uiso 1 2 d SR . . H8B H 0.8000 1.2500 0.2375 0.037 Uiso 1 2 d SR . . O9 O 0.8408(7) 0.7500 0.5457(7) 0.0469(19) Uani 1 2 d S . . H9A H 0.9072 0.7500 0.5127 0.056 Uiso 1 2 d SR . . H9B H 0.8928 0.7500 0.6280 0.056 Uiso 1 2 d SR . . 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 0.0112(2) 0.0114(2) 0.0135(3) 0.000 -0.00007(17) 0.000 O1 0.010(2) 0.037(3) 0.019(3) 0.000 0.002(2) 0.000 O2 0.019(3) 0.052(4) 0.017(3) 0.000 0.002(2) 0.000 O3 0.0271(19) 0.0127(18) 0.033(2) 0.0038(16) 0.0015(16) 0.0051(15) O4 0.017(2) 0.028(3) 0.019(3) 0.000 0.004(2) 0.000 O5 0.024(3) 0.067(5) 0.020(3) 0.000 0.009(3) 0.000 N1 0.016(3) 0.013(3) 0.020(3) 0.000 0.005(3) 0.000 N2 0.015(3) 0.032(4) 0.022(3) 0.000 0.003(3) 0.000 C1 0.016(3) 0.018(3) 0.013(3) 0.000 0.001(3) 0.000 C2 0.015(3) 0.011(3) 0.016(4) 0.000 0.001(3) 0.000 C3 0.015(3) 0.007(3) 0.025(4) 0.000 0.000(3) 0.000 C4 0.008(3) 0.014(3) 0.025(4) 0.000 0.002(3) 0.000 C5 0.019(4) 0.038(5) 0.032(4) 0.000 0.012(3) 0.000 C6 0.014(3) 0.016(3) 0.012(3) 0.000 -0.001(3) 0.000 C7 0.023(4) 0.020(4) 0.017(4) 0.000 0.003(3) 0.000 O6 0.034(2) 0.030(2) 0.027(2) 0.0081(19) -0.0017(19) 0.0063(18) O7 0.049(3) 0.039(2) 0.043(3) 0.013(2) 0.028(2) 0.022(2) O8 0.019(3) 0.047(4) 0.025(3) 0.000 0.007(2) 0.000 O9 0.019(3) 0.083(6) 0.031(4) 0.000 0.002(3) 0.000 _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 2.400(5) . ? Eu1 O3 2.407(4) 2_545 ? Eu1 O3 2.407(4) 3_575 ? Eu1 O4 2.440(6) . ? Eu1 O6 2.468(4) . ? Eu1 O6 2.468(4) 4_575 ? Eu1 O7 2.489(4) 4_575 ? Eu1 O7 2.489(4) . ? Eu1 N1 2.548(6) . ? O1 C1 1.273(8) . ? O2 C1 1.222(9) . ? O3 C4 1.249(5) . ? O3 Eu1 2.407(4) 3_575 ? O4 C7 1.258(10) . ? O5 C7 1.239(11) . ? N1 C6 1.319(10) . ? N1 C2 1.337(10) . ? N2 C5 1.322(12) . ? N2 C3 1.333(11) . ? C1 C2 1.523(10) . ? C2 C3 1.401(9) . ? C3 C4 1.521(10) . ? C4 O3 1.249(5) 4_575 ? C5 C6 1.402(9) . ? C5 H5A 0.9300 . ? C6 C7 1.527(10) . ? O6 H6A 0.8500 . ? O6 H6B 0.8500 . ? O7 H7A 0.8499 . ? O7 H7B 0.8500 . ? O8 H8A 0.8499 . ? O8 H8B 0.8501 . ? O9 H9A 0.8500 . ? O9 H9B 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 Eu1 O3 84.75(11) . 2_545 ? O1 Eu1 O3 84.75(11) . 3_575 ? O3 Eu1 O3 140.90(18) 2_545 3_575 ? O1 Eu1 O4 126.57(17) . . ? O3 Eu1 O4 78.23(11) 2_545 . ? O3 Eu1 O4 78.23(11) 3_575 . ? O1 Eu1 O6 140.87(13) . . ? O3 Eu1 O6 70.41(14) 2_545 . ? O3 Eu1 O6 133.28(14) 3_575 . ? O4 Eu1 O6 78.34(15) . . ? O1 Eu1 O6 140.87(13) . 4_575 ? O3 Eu1 O6 133.28(14) 2_545 4_575 ? O3 Eu1 O6 70.41(14) 3_575 4_575 ? O4 Eu1 O6 78.34(15) . 4_575 ? O6 Eu1 O6 65.6(2) . 4_575 ? O1 Eu1 O7 74.17(15) . 4_575 ? O3 Eu1 O7 139.20(15) 2_545 4_575 ? O3 Eu1 O7 72.25(15) 3_575 4_575 ? O4 Eu1 O7 142.08(12) . 4_575 ? O6 Eu1 O7 105.32(16) . 4_575 ? O6 Eu1 O7 69.75(16) 4_575 4_575 ? O1 Eu1 O7 74.17(15) . . ? O3 Eu1 O7 72.25(15) 2_545 . ? O3 Eu1 O7 139.20(16) 3_575 . ? O4 Eu1 O7 142.08(12) . . ? O6 Eu1 O7 69.75(16) . . ? O6 Eu1 O7 105.32(16) 4_575 . ? O7 Eu1 O7 68.6(2) 4_575 . ? O1 Eu1 N1 63.6(2) . . ? O3 Eu1 N1 70.80(9) 2_545 . ? O3 Eu1 N1 70.80(9) 3_575 . ? O4 Eu1 N1 63.0(2) . . ? O6 Eu1 N1 129.44(15) . . ? O6 Eu1 N1 129.44(15) 4_575 . ? O7 Eu1 N1 125.23(16) 4_575 . ? O7 Eu1 N1 125.23(17) . . ? C1 O1 Eu1 127.3(5) . . ? C4 O3 Eu1 153.6(5) . 3_575 ? C7 O4 Eu1 127.1(5) . . ? C6 N1 C2 119.7(6) . . ? C6 N1 Eu1 120.4(5) . . ? C2 N1 Eu1 119.9(5) . . ? C5 N2 C3 117.8(7) . . ? O2 C1 O1 125.5(7) . . ? O2 C1 C2 119.3(6) . . ? O1 C1 C2 115.2(6) . . ? N1 C2 C3 120.3(7) . . ? N1 C2 C1 114.0(6) . . ? C3 C2 C1 125.7(6) . . ? N2 C3 C2 120.6(7) . . ? N2 C3 C4 116.1(6) . . ? C2 C3 C4 123.3(7) . . ? O3 C4 O3 124.9(7) . 4_575 ? O3 C4 C3 117.5(4) . . ? O3 C4 C3 117.5(4) 4_575 . ? N2 C5 C6 122.5(8) . . ? N2 C5 H5A 118.7 . . ? C6 C5 H5A 118.7 . . ? N1 C6 C5 119.0(7) . . ? N1 C6 C7 115.0(6) . . ? C5 C6 C7 126.0(8) . . ? O5 C7 O4 127.3(8) . . ? O5 C7 C6 118.1(7) . . ? O4 C7 C6 114.6(7) . . ? Eu1 O6 H6A 116.1 . . ? Eu1 O6 H6B 124.5 . . ? H6A O6 H6B 104.5 . . ? Eu1 O7 H7A 121.7 . . ? Eu1 O7 H7B 119.6 . . ? H7A O7 H7B 102.2 . . ? H8A O8 H8B 105.9 . . ? H9A O9 H9B 104.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Eu1 O1 C1 71.14(10) 2_545 . . . ? O3 Eu1 O1 C1 -71.14(10) 3_575 . . . ? O4 Eu1 O1 C1 0.0 . . . . ? O6 Eu1 O1 C1 120.9(2) . . . . ? O6 Eu1 O1 C1 -120.9(2) 4_575 . . . ? O7 Eu1 O1 C1 -144.15(12) 4_575 . . . ? O7 Eu1 O1 C1 144.15(12) . . . . ? N1 Eu1 O1 C1 0.0 . . . . ? O1 Eu1 O4 C7 0.000(2) . . . . ? O3 Eu1 O4 C7 -74.28(9) 2_545 . . . ? O3 Eu1 O4 C7 74.28(9) 3_575 . . . ? O6 Eu1 O4 C7 -146.42(11) . . . . ? O6 Eu1 O4 C7 146.42(11) 4_575 . . . ? O7 Eu1 O4 C7 113.5(2) 4_575 . . . ? O7 Eu1 O4 C7 -113.5(2) . . . . ? N1 Eu1 O4 C7 0.000(2) . . . . ? O1 Eu1 N1 C6 180.0 . . . . ? O3 Eu1 N1 C6 86.27(12) 2_545 . . . ? O3 Eu1 N1 C6 -86.27(12) 3_575 . . . ? O4 Eu1 N1 C6 0.0 . . . . ? O6 Eu1 N1 C6 44.54(17) . . . . ? O6 Eu1 N1 C6 -44.54(17) 4_575 . . . ? O7 Eu1 N1 C6 -136.39(16) 4_575 . . . ? O7 Eu1 N1 C6 136.39(16) . . . . ? O1 Eu1 N1 C2 0.0 . . . . ? O3 Eu1 N1 C2 -93.73(12) 2_545 . . . ? O3 Eu1 N1 C2 93.73(12) 3_575 . . . ? O4 Eu1 N1 C2 180.0 . . . . ? O6 Eu1 N1 C2 -135.46(17) . . . . ? O6 Eu1 N1 C2 135.46(17) 4_575 . . . ? O7 Eu1 N1 C2 43.61(16) 4_575 . . . ? O7 Eu1 N1 C2 -43.61(16) . . . . ? Eu1 O1 C1 O2 180.0 . . . . ? Eu1 O1 C1 C2 0.0 . . . . ? C6 N1 C2 C3 0.0 . . . . ? Eu1 N1 C2 C3 180.0 . . . . ? C6 N1 C2 C1 180.0 . . . . ? Eu1 N1 C2 C1 0.0 . . . . ? O2 C1 C2 N1 180.0 . . . . ? O1 C1 C2 N1 0.0 . . . . ? O2 C1 C2 C3 0.0 . . . . ? O1 C1 C2 C3 180.0 . . . . ? C5 N2 C3 C2 0.0 . . . . ? C5 N2 C3 C4 180.0 . . . . ? N1 C2 C3 N2 0.0 . . . . ? C1 C2 C3 N2 180.0 . . . . ? N1 C2 C3 C4 180.0 . . . . ? C1 C2 C3 C4 0.0 . . . . ? Eu1 O3 C4 O3 136.1(6) 3_575 . . 4_575 ? Eu1 O3 C4 C3 -43.4(12) 3_575 . . . ? N2 C3 C4 O3 89.8(6) . . . . ? C2 C3 C4 O3 -90.2(6) . . . . ? N2 C3 C4 O3 -89.8(6) . . . 4_575 ? C2 C3 C4 O3 90.2(6) . . . 4_575 ? C3 N2 C5 C6 0.0 . . . . ? C2 N1 C6 C5 0.000(1) . . . . ? Eu1 N1 C6 C5 180.0 . . . . ? C2 N1 C6 C7 180.000(1) . . . . ? Eu1 N1 C6 C7 0.000(1) . . . . ? N2 C5 C6 N1 0.0 . . . . ? N2 C5 C6 C7 180.000(2) . . . . ? Eu1 O4 C7 O5 180.000(2) . . . . ? Eu1 O4 C7 C6 0.000(2) . . . . ? N1 C6 C7 O5 180.000(1) . . . . ? C5 C6 C7 O5 0.000(2) . . . . ? N1 C6 C7 O4 0.000(1) . . . . ? C5 C6 C7 O4 180.000(1) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.094 _refine_diff_density_min -2.697 _refine_diff_density_rms 0.258 # Attachment '2-gd.cif' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 291611' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H13 Gd N2 O12' _chemical_formula_weight 474.44 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.6900(16) _cell_length_b 6.8211(14) _cell_length_c 11.236(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.333(8) _cell_angle_gamma 90.00 _cell_volume 681.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2407 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.07 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 458 _exptl_absorpt_coefficient_mu 4.933 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.623 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 3157 _diffrn_reflns_av_R_equivalents 0.0939 _diffrn_reflns_av_sigmaI/netI 0.0901 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 26.02 _reflns_number_total 1437 _reflns_number_gt 1273 _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^)+(0.0989P)^2^+6.0548P] 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 1437 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1653 _refine_ls_wR_factor_gt 0.1555 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.38464(6) 0.7500 0.23036(6) 0.0209(3) Uani 1 2 d S . . O1 O 0.2429(10) 0.7500 -0.0019(10) 0.030(2) Uani 1 2 d S . . O2 O 0.0288(11) 0.7500 -0.1841(11) 0.040(3) Uani 1 2 d S . . O3 O -0.2962(8) 0.9158(11) -0.2188(8) 0.0358(18) Uani 1 1 d . . . O4 O 0.2838(10) 0.7500 0.4015(10) 0.030(2) Uani 1 2 d S . . O5 O 0.0902(12) 0.7500 0.4660(11) 0.045(3) Uani 1 2 d S . . N1 N 0.0975(12) 0.7500 0.1520(11) 0.020(2) Uani 1 2 d S . . N2 N -0.2164(12) 0.7500 0.0645(13) 0.030(3) Uani 1 2 d S . . C1 C 0.0985(15) 0.7500 -0.0639(15) 0.028(3) Uani 1 2 d S . . C2 C 0.0101(14) 0.7500 0.0232(13) 0.022(3) Uani 1 2 d S . . C3 C -0.1504(14) 0.7500 -0.0214(14) 0.023(3) Uani 1 2 d S . . C4 C -0.2560(13) 0.7500 -0.1664(14) 0.024(3) Uani 1 2 d S . . C5 C -0.1270(15) 0.7500 0.1924(16) 0.034(4) Uani 1 2 d S . . H5 H -0.1711 0.7500 0.2523 0.041 Uiso 1 2 calc SR . . C6 C 0.0323(15) 0.7500 0.2378(13) 0.025(3) Uani 1 2 d S . . C7 C 0.1423(16) 0.7500 0.3802(15) 0.027(3) Uani 1 2 d S . . O6 O 0.5763(8) 0.5519(13) 0.4052(8) 0.043(2) Uani 1 1 d . . . H6A H 0.5499 0.4357 0.4138 0.052 Uiso 1 1 d R . . H6B H 0.6250 0.5920 0.4822 0.052 Uiso 1 1 d R . . O7 O 0.5335(9) 0.5444(15) 0.1384(8) 0.049(2) Uani 1 1 d . . . H7A H 0.5705 0.5838 0.0856 0.059 Uiso 1 1 d R . . H7B H 0.5935 0.4565 0.1838 0.059 Uiso 1 1 d R . . O8 O 0.7300(11) 1.2500 0.2686(11) 0.038(3) Uani 1 2 d S . . H8A H 0.7773 1.2500 0.3504 0.046 Uiso 1 2 d SR . . H8B H 0.7982 1.2500 0.2388 0.046 Uiso 1 2 d SR . . O9 O 0.8419(12) 0.7500 0.5442(12) 0.052(4) Uani 1 2 d S . . H9A H 0.9081 0.7500 0.5124 0.063 Uiso 1 2 d SR . . H9B H 0.8912 0.7500 0.6259 0.063 Uiso 1 2 d SR . . 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 0.0102(4) 0.0333(4) 0.0157(4) 0.000 0.0014(3) 0.000 O1 0.010(4) 0.056(7) 0.021(5) 0.000 0.003(4) 0.000 O2 0.018(5) 0.079(9) 0.019(6) 0.000 0.004(4) 0.000 O3 0.030(4) 0.032(4) 0.035(4) 0.003(4) 0.002(3) 0.004(3) O4 0.018(4) 0.052(6) 0.022(5) 0.000 0.010(4) 0.000 O5 0.029(6) 0.084(9) 0.025(6) 0.000 0.014(5) 0.000 N1 0.013(5) 0.032(6) 0.013(6) 0.000 0.005(4) 0.000 N2 0.011(5) 0.053(8) 0.027(7) 0.000 0.006(5) 0.000 C1 0.016(6) 0.041(8) 0.023(8) 0.000 0.003(5) 0.000 C2 0.011(6) 0.030(7) 0.021(7) 0.000 0.004(5) 0.000 C3 0.012(6) 0.029(7) 0.024(8) 0.000 0.002(5) 0.000 C4 0.007(5) 0.041(8) 0.025(8) 0.000 0.006(5) 0.000 C5 0.017(6) 0.062(11) 0.024(8) 0.000 0.007(5) 0.000 C6 0.021(6) 0.041(8) 0.014(7) 0.000 0.007(5) 0.000 C7 0.019(6) 0.041(8) 0.025(8) 0.000 0.010(6) 0.000 O6 0.033(4) 0.053(5) 0.030(4) 0.013(4) -0.002(3) 0.006(4) O7 0.050(5) 0.072(6) 0.035(5) 0.019(5) 0.027(4) 0.031(5) O8 0.019(5) 0.069(8) 0.023(6) 0.000 0.005(4) 0.000 O9 0.019(5) 0.107(11) 0.023(6) 0.000 -0.001(4) 0.000 _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 2.420(10) . ? Gd1 O3 2.421(8) 2_545 ? Gd1 O3 2.421(8) 3_575 ? Gd1 O4 2.478(10) . ? Gd1 O6 2.499(7) 4_575 ? Gd1 O6 2.499(7) . ? Gd1 O7 2.509(8) 4_575 ? Gd1 O7 2.509(8) . ? Gd1 N1 2.565(10) . ? O1 C1 1.293(16) . ? O2 C1 1.248(19) . ? O3 C4 1.263(9) . ? O3 Gd1 2.421(8) 3_575 ? O4 C7 1.295(17) . ? O5 C7 1.253(18) . ? N1 C6 1.346(16) . ? N1 C2 1.357(18) . ? N2 C3 1.353(18) . ? N2 C5 1.35(2) . ? C1 C2 1.535(18) . ? C2 C3 1.432(16) . ? C3 C4 1.543(19) . ? C4 O3 1.263(9) 4_575 ? C5 C6 1.420(18) . ? C5 H5 0.9300 . ? C6 C7 1.53(2) . ? O6 H6A 0.8500 . ? O6 H6B 0.8500 . ? O7 H7A 0.8500 . ? O7 H7B 0.8500 . ? O8 H8A 0.8498 . ? O8 H8B 0.8500 . ? O9 H9A 0.8501 . ? O9 H9B 0.8501 . ? 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 O3 84.5(2) . 2_545 ? O1 Gd1 O3 84.5(2) . 3_575 ? O3 Gd1 O3 140.7(4) 2_545 3_575 ? O1 Gd1 O4 127.4(3) . . ? O3 Gd1 O4 78.6(2) 2_545 . ? O3 Gd1 O4 78.6(2) 3_575 . ? O1 Gd1 O6 140.8(2) . 4_575 ? O3 Gd1 O6 133.5(3) 2_545 4_575 ? O3 Gd1 O6 70.7(3) 3_575 4_575 ? O4 Gd1 O6 77.8(3) . 4_575 ? O1 Gd1 O6 140.8(2) . . ? O3 Gd1 O6 70.7(3) 2_545 . ? O3 Gd1 O6 133.5(3) 3_575 . ? O4 Gd1 O6 77.8(3) . . ? O6 Gd1 O6 65.5(4) 4_575 . ? O1 Gd1 O7 74.3(3) . 4_575 ? O3 Gd1 O7 138.9(3) 2_545 4_575 ? O3 Gd1 O7 72.6(3) 3_575 4_575 ? O4 Gd1 O7 141.9(2) . 4_575 ? O6 Gd1 O7 69.6(3) 4_575 4_575 ? O6 Gd1 O7 104.9(3) . 4_575 ? O1 Gd1 O7 74.3(3) . . ? O3 Gd1 O7 72.6(3) 2_545 . ? O3 Gd1 O7 138.9(3) 3_575 . ? O4 Gd1 O7 141.9(2) . . ? O6 Gd1 O7 104.9(3) 4_575 . ? O6 Gd1 O7 69.6(3) . . ? O7 Gd1 O7 68.0(4) 4_575 . ? O1 Gd1 N1 63.5(3) . . ? O3 Gd1 N1 70.64(18) 2_545 . ? O3 Gd1 N1 70.64(18) 3_575 . ? O4 Gd1 N1 63.8(3) . . ? O6 Gd1 N1 129.6(3) 4_575 . ? O6 Gd1 N1 129.6(3) . . ? O7 Gd1 N1 125.5(3) 4_575 . ? O7 Gd1 N1 125.5(3) . . ? C1 O1 Gd1 127.7(9) . . ? C4 O3 Gd1 154.9(8) . 3_575 ? C7 O4 Gd1 124.8(9) . . ? C6 N1 C2 119.5(11) . . ? C6 N1 Gd1 120.5(8) . . ? C2 N1 Gd1 120.0(8) . . ? C3 N2 C5 118.2(11) . . ? O2 C1 O1 126.2(13) . . ? O2 C1 C2 119.3(11) . . ? O1 C1 C2 114.5(12) . . ? N1 C2 C3 120.3(12) . . ? N1 C2 C1 114.2(10) . . ? C3 C2 C1 125.5(12) . . ? N2 C3 C2 120.4(12) . . ? N2 C3 C4 116.7(11) . . ? C2 C3 C4 122.9(12) . . ? O3 C4 O3 127.1(13) 4_575 . ? O3 C4 C3 116.4(6) 4_575 . ? O3 C4 C3 116.4(6) . . ? N2 C5 C6 122.0(13) . . ? N2 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? N1 C6 C5 119.6(13) . . ? N1 C6 C7 114.7(11) . . ? C5 C6 C7 125.7(12) . . ? O5 C7 O4 125.3(14) . . ? O5 C7 C6 118.5(12) . . ? O4 C7 C6 116.2(12) . . ? Gd1 O6 H6A 115.5 . . ? Gd1 O6 H6B 124.5 . . ? H6A O6 H6B 104.8 . . ? Gd1 O7 H7A 125.6 . . ? Gd1 O7 H7B 121.0 . . ? H7A O7 H7B 105.3 . . ? H8A O8 H8B 104.8 . . ? H9A O9 H9B 105.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Gd1 O1 C1 71.09(19) 2_545 . . . ? O3 Gd1 O1 C1 -71.09(19) 3_575 . . . ? O4 Gd1 O1 C1 0.0 . . . . ? O6 Gd1 O1 C1 -121.1(4) 4_575 . . . ? O6 Gd1 O1 C1 121.1(4) . . . . ? O7 Gd1 O1 C1 -144.5(2) 4_575 . . . ? O7 Gd1 O1 C1 144.5(2) . . . . ? N1 Gd1 O1 C1 0.0 . . . . ? O1 Gd1 O4 C7 0.000(3) . . . . ? O3 Gd1 O4 C7 -73.90(19) 2_545 . . . ? O3 Gd1 O4 C7 73.90(19) 3_575 . . . ? O6 Gd1 O4 C7 146.4(2) 4_575 . . . ? O6 Gd1 O4 C7 -146.4(2) . . . . ? O7 Gd1 O4 C7 115.0(4) 4_575 . . . ? O7 Gd1 O4 C7 -115.0(4) . . . . ? N1 Gd1 O4 C7 0.000(3) . . . . ? O1 Gd1 N1 C6 180.000(2) . . . . ? O3 Gd1 N1 C6 86.5(2) 2_545 . . . ? O3 Gd1 N1 C6 -86.5(2) 3_575 . . . ? O4 Gd1 N1 C6 0.000(2) . . . . ? O6 Gd1 N1 C6 -44.6(3) 4_575 . . . ? O6 Gd1 N1 C6 44.6(3) . . . . ? O7 Gd1 N1 C6 -136.6(3) 4_575 . . . ? O7 Gd1 N1 C6 136.6(3) . . . . ? O1 Gd1 N1 C2 0.0 . . . . ? O3 Gd1 N1 C2 -93.5(2) 2_545 . . . ? O3 Gd1 N1 C2 93.5(2) 3_575 . . . ? O4 Gd1 N1 C2 180.0 . . . . ? O6 Gd1 N1 C2 135.4(3) 4_575 . . . ? O6 Gd1 N1 C2 -135.4(3) . . . . ? O7 Gd1 N1 C2 43.4(3) 4_575 . . . ? O7 Gd1 N1 C2 -43.4(3) . . . . ? Gd1 O1 C1 O2 180.000(2) . . . . ? Gd1 O1 C1 C2 0.000(1) . . . . ? C6 N1 C2 C3 0.000(1) . . . . ? Gd1 N1 C2 C3 180.0 . . . . ? C6 N1 C2 C1 180.000(1) . . . . ? Gd1 N1 C2 C1 0.0 . . . . ? O2 C1 C2 N1 180.000(2) . . . . ? O1 C1 C2 N1 0.0 . . . . ? O2 C1 C2 C3 0.000(2) . . . . ? O1 C1 C2 C3 180.0 . . . . ? C5 N2 C3 C2 0.000(1) . . . . ? C5 N2 C3 C4 180.000(2) . . . . ? N1 C2 C3 N2 0.000(2) . . . . ? C1 C2 C3 N2 180.0 . . . . ? N1 C2 C3 C4 180.000(1) . . . . ? C1 C2 C3 C4 0.0 . . . . ? Gd1 O3 C4 O3 133.9(12) 3_575 . . 4_575 ? Gd1 O3 C4 C3 -44(2) 3_575 . . . ? N2 C3 C4 O3 -89.1(10) . . . 4_575 ? C2 C3 C4 O3 90.9(10) . . . 4_575 ? N2 C3 C4 O3 89.1(10) . . . . ? C2 C3 C4 O3 -90.9(10) . . . . ? C3 N2 C5 C6 0.000(2) . . . . ? C2 N1 C6 C5 0.000(2) . . . . ? Gd1 N1 C6 C5 180.000(1) . . . . ? C2 N1 C6 C7 180.000(3) . . . . ? Gd1 N1 C6 C7 0.000(2) . . . . ? N2 C5 C6 N1 0.000(2) . . . . ? N2 C5 C6 C7 180.000(3) . . . . ? Gd1 O4 C7 O5 180.000(3) . . . . ? Gd1 O4 C7 C6 0.000(4) . . . . ? N1 C6 C7 O5 180.000(3) . . . . ? C5 C6 C7 O5 0.000(3) . . . . ? N1 C6 C7 O4 0.000(3) . . . . ? C5 C6 C7 O4 180.000(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.110 _refine_diff_density_min -2.882 _refine_diff_density_rms 0.316 # Attachment '4-yb.cif' data_compound4 _database_code_depnum_ccdc_archive 'CCDC 692765' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H7 N2 O9 Yb' _chemical_formula_weight 436.19 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 9.5054(10) _cell_length_b 6.5175(7) _cell_length_c 17.0878(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1058.61(19) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3979 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.73 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 8.886 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.223 _exptl_absorpt_correction_T_max 0.414 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 6657 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.78 _reflns_number_total 1359 _reflns_number_gt 1281 _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^)+(0.0504P)^2^+1.4230P] 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 0.0092(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1359 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0704 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Yb1 Yb 0.21920(2) 0.2500 0.379117(11) 0.01140(14) Uani 1 2 d S . . O1 O 0.2522(5) 0.2500 0.5117(2) 0.0194(9) Uani 1 2 d S . . O2 O 0.3868(6) 0.2500 0.61929(19) 0.0256(11) Uani 1 2 d S . . O3 O 0.7108(4) 0.0805(6) 0.63248(18) 0.0255(8) Uani 1 1 d . . . O4 O 0.5976(5) 0.2500 0.2293(2) 0.0374(13) Uani 1 2 d S . . O5 O 0.3805(5) 0.2500 0.2746(2) 0.0214(9) Uani 1 2 d S . . N1 N 0.4646(5) 0.2500 0.4192(2) 0.0117(8) Uani 1 2 d S . . N2 N 0.7431(6) 0.2500 0.4624(3) 0.0203(10) Uani 1 2 d S . . C1 C 0.3697(6) 0.2500 0.5481(3) 0.0156(10) Uani 1 2 d S . . C2 C 0.4981(6) 0.2500 0.4952(3) 0.0117(10) Uani 1 2 d S . . C3 C 0.6407(6) 0.2500 0.5162(3) 0.0147(10) Uani 1 2 d S . . C4 C 0.6923(6) 0.2500 0.6000(3) 0.0128(10) Uani 1 2 d S . . C5 C 0.7038(7) 0.2500 0.3866(3) 0.0193(13) Uani 1 2 d S . . H5 H 0.7726 0.2500 0.3479 0.023 Uiso 1 2 calc SR . . C6 C 0.5641(6) 0.2500 0.3653(3) 0.0147(10) Uani 1 2 d S . . C7 C 0.5104(6) 0.2500 0.2829(3) 0.0168(11) Uani 1 2 d S . . O6 O 0.0256(4) 0.0389(5) 0.41728(17) 0.0336(7) Uani 1 1 d . . . H6A H 0.0473 -0.0710 0.4412 0.040 Uiso 1 1 d R . . H6B H -0.0635 0.0448 0.4132 0.040 Uiso 1 1 d R . . O7 O 0.1115(6) 0.2500 0.6799(3) 0.0453(14) Uani 1 2 d S . . H7A H 0.1820 0.2500 0.6492 0.054 Uiso 1 2 d SR . . H7B H 0.0291 0.2500 0.6604 0.054 Uiso 1 2 d SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.00897(18) 0.01761(18) 0.00760(17) 0.000 -0.00138(7) 0.000 O1 0.0091(17) 0.039(2) 0.0103(17) 0.000 -0.0011(15) 0.000 O2 0.020(2) 0.049(3) 0.0073(17) 0.000 0.0005(14) 0.000 O3 0.036(2) 0.0199(18) 0.0203(14) 0.0037(12) -0.0077(12) 0.0007(13) O4 0.016(2) 0.084(4) 0.0113(18) 0.000 0.0052(19) 0.000 O5 0.013(2) 0.039(2) 0.0129(16) 0.000 0.0007(15) 0.000 N1 0.010(2) 0.0133(17) 0.0122(18) 0.000 -0.0045(17) 0.000 N2 0.013(2) 0.032(3) 0.016(2) 0.000 -0.0027(19) 0.000 C1 0.010(3) 0.021(2) 0.016(2) 0.000 0.0004(19) 0.000 C2 0.014(3) 0.014(2) 0.0073(18) 0.000 -0.0003(18) 0.000 C3 0.017(3) 0.013(2) 0.014(2) 0.000 -0.003(2) 0.000 C4 0.011(2) 0.016(2) 0.011(2) 0.000 -0.002(2) 0.000 C5 0.013(3) 0.033(4) 0.012(3) 0.000 0.0005(19) 0.000 C6 0.013(3) 0.019(2) 0.012(2) 0.000 0.001(2) 0.000 C7 0.013(3) 0.028(3) 0.009(2) 0.000 0.003(2) 0.000 O6 0.0213(16) 0.0453(19) 0.0341(15) 0.0102(15) 0.0010(14) -0.0088(15) O7 0.032(3) 0.073(4) 0.031(2) 0.000 0.003(2) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O4 2.183(4) 6_556 ? Yb1 O3 2.263(4) 4_656 ? Yb1 O1 2.287(4) . ? Yb1 O5 2.354(4) . ? Yb1 O6 2.389(3) . ? Yb1 N1 2.431(5) . ? O1 C1 1.278(7) . ? O2 C1 1.228(6) . ? O3 C4 1.249(5) . ? O4 C7 1.236(7) . ? O5 C7 1.243(7) . ? N1 C6 1.319(7) . ? N1 C2 1.338(6) . ? N2 C3 1.338(8) . ? N2 C5 1.349(7) . ? C1 C2 1.518(7) . ? C2 C3 1.402(8) . ? C3 C4 1.512(7) . ? C4 O3 1.249(5) 8_565 ? C5 C6 1.377(9) . ? C5 H5 0.9300 . ? C6 C7 1.497(7) . ? O6 H6A 0.8500 . ? O6 H6B 0.8500 . ? O7 H7A 0.8501 . ? O7 H7B 0.8501 . ? 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 O4 Yb1 O3 94.67(9) 6_556 4_656 ? O4 Yb1 O3 94.67(9) 6_556 5_656 ? O3 Yb1 O3 144.29(18) 4_656 5_656 ? O4 Yb1 O1 155.91(17) 6_556 . ? O3 Yb1 O1 92.66(9) 4_656 . ? O3 Yb1 O1 92.66(9) 5_656 . ? O4 Yb1 O5 72.64(16) 6_556 . ? O3 Yb1 O5 75.05(9) 4_656 . ? O3 Yb1 O5 75.05(9) 5_656 . ? O1 Yb1 O5 131.46(15) . . ? O4 Yb1 O6 79.84(13) 6_556 . ? O3 Yb1 O6 143.00(13) 4_656 . ? O3 Yb1 O6 72.66(13) 5_656 . ? O1 Yb1 O6 80.52(12) . . ? O5 Yb1 O6 135.16(10) . . ? O4 Yb1 O6 79.84(13) 6_556 8_565 ? O3 Yb1 O6 72.66(13) 4_656 8_565 ? O3 Yb1 O6 143.00(13) 5_656 8_565 ? O1 Yb1 O6 80.52(12) . 8_565 ? O5 Yb1 O6 135.16(10) . 8_565 ? O6 Yb1 O6 70.35(17) . 8_565 ? O4 Yb1 N1 138.33(16) 6_556 . ? O3 Yb1 N1 75.09(9) 4_656 . ? O3 Yb1 N1 75.09(9) 5_656 . ? O1 Yb1 N1 65.77(15) . . ? O5 Yb1 N1 65.69(14) . . ? O6 Yb1 N1 131.49(10) . . ? O6 Yb1 N1 131.49(10) 8_565 . ? C1 O1 Yb1 127.0(4) . . ? C4 O3 Yb1 147.6(3) . 5_656 ? C7 O4 Yb1 169.9(4) . 6_656 ? C7 O5 Yb1 124.1(3) . . ? C6 N1 C2 120.4(5) . . ? C6 N1 Yb1 119.4(3) . . ? C2 N1 Yb1 120.1(4) . . ? C3 N2 C5 117.3(5) . . ? O2 C1 O1 126.7(5) . . ? O2 C1 C2 118.9(5) . . ? O1 C1 C2 114.4(5) . . ? N1 C2 C3 118.6(5) . . ? N1 C2 C1 112.7(5) . . ? C3 C2 C1 128.7(4) . . ? N2 C3 C2 121.8(5) . . ? N2 C3 C4 114.5(5) . . ? C2 C3 C4 123.7(5) . . ? O3 C4 O3 124.4(6) . 8_565 ? O3 C4 C3 117.8(3) . . ? O3 C4 C3 117.8(3) 8_565 . ? N2 C5 C6 121.3(6) . . ? N2 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? N1 C6 C5 120.5(5) . . ? N1 C6 C7 114.3(5) . . ? C5 C6 C7 125.2(5) . . ? O4 C7 O5 125.5(5) . . ? O4 C7 C6 118.0(5) . . ? O5 C7 C6 116.5(5) . . ? Yb1 O6 H6A 115.4 . . ? Yb1 O6 H6B 135.9 . . ? H6A O6 H6B 108.6 . . ? H7A O7 H7B 119.1 . . ? 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 O4 Yb1 O1 C1 180.000(1) 6_556 . . . ? O3 Yb1 O1 C1 -72.34(9) 4_656 . . . ? O3 Yb1 O1 C1 72.34(9) 5_656 . . . ? O5 Yb1 O1 C1 0.000(1) . . . . ? O6 Yb1 O1 C1 144.26(9) . . . . ? O6 Yb1 O1 C1 -144.26(9) 8_565 . . . ? N1 Yb1 O1 C1 0.000(1) . . . . ? O4 Yb1 O5 C7 180.0 6_556 . . . ? O3 Yb1 O5 C7 80.11(9) 4_656 . . . ? O3 Yb1 O5 C7 -80.11(9) 5_656 . . . ? O1 Yb1 O5 C7 0.0 . . . . ? O6 Yb1 O5 C7 -125.22(14) . . . . ? O6 Yb1 O5 C7 125.21(14) 8_565 . . . ? N1 Yb1 O5 C7 0.0 . . . . ? O4 Yb1 N1 C6 0.0 6_556 . . . ? O3 Yb1 N1 C6 -80.06(9) 4_656 . . . ? O3 Yb1 N1 C6 80.06(9) 5_656 . . . ? O1 Yb1 N1 C6 180.0 . . . . ? O5 Yb1 N1 C6 0.0 . . . . ? O6 Yb1 N1 C6 129.74(13) . . . . ? O6 Yb1 N1 C6 -129.74(13) 8_565 . . . ? O4 Yb1 N1 C2 180.0 6_556 . . . ? O3 Yb1 N1 C2 99.94(9) 4_656 . . . ? O3 Yb1 N1 C2 -99.94(9) 5_656 . . . ? O1 Yb1 N1 C2 0.0 . . . . ? O5 Yb1 N1 C2 180.0 . . . . ? O6 Yb1 N1 C2 -50.26(13) . . . . ? O6 Yb1 N1 C2 50.26(13) 8_565 . . . ? Yb1 O1 C1 O2 180.000(1) . . . . ? Yb1 O1 C1 C2 0.000(2) . . . . ? C6 N1 C2 C3 0.000(1) . . . . ? Yb1 N1 C2 C3 180.0 . . . . ? C6 N1 C2 C1 180.000(1) . . . . ? Yb1 N1 C2 C1 0.000(1) . . . . ? O2 C1 C2 N1 180.000(1) . . . . ? O1 C1 C2 N1 0.000(1) . . . . ? O2 C1 C2 C3 0.000(2) . . . . ? O1 C1 C2 C3 180.000(1) . . . . ? C5 N2 C3 C2 0.000(2) . . . . ? C5 N2 C3 C4 180.000(1) . . . . ? N1 C2 C3 N2 0.000(2) . . . . ? C1 C2 C3 N2 180.000(1) . . . . ? N1 C2 C3 C4 180.000(1) . . . . ? C1 C2 C3 C4 0.000(2) . . . . ? Yb1 O3 C4 O3 -145.1(4) 5_656 . . 8_565 ? Yb1 O3 C4 C3 36.4(9) 5_656 . . . ? N2 C3 C4 O3 -90.7(5) . . . . ? C2 C3 C4 O3 89.3(5) . . . . ? N2 C3 C4 O3 90.7(5) . . . 8_565 ? C2 C3 C4 O3 -89.3(5) . . . 8_565 ? C3 N2 C5 C6 0.000(1) . . . . ? C2 N1 C6 C5 0.000(1) . . . . ? Yb1 N1 C6 C5 180.0 . . . . ? C2 N1 C6 C7 180.0 . . . . ? Yb1 N1 C6 C7 0.0 . . . . ? N2 C5 C6 N1 0.000(1) . . . . ? N2 C5 C6 C7 180.000(1) . . . . ? Yb1 O4 C7 O5 0.000(3) 6_656 . . . ? Yb1 O4 C7 C6 180.000(3) 6_656 . . . ? Yb1 O5 C7 O4 180.0 . . . . ? Yb1 O5 C7 C6 0.0 . . . . ? N1 C6 C7 O4 180.0 . . . . ? C5 C6 C7 O4 0.000(1) . . . . ? N1 C6 C7 O5 0.0 . . . . ? C5 C6 C7 O5 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.78 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.279 _refine_diff_density_min -2.186 _refine_diff_density_rms 0.250 # Attachment '3-er.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 692766' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H7 Er N2 O9' _chemical_formula_weight 430.41 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 9.5384(8) _cell_length_b 6.5495(6) _cell_length_c 17.1693(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1072.60(16) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3495 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 27.87 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 7.875 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.272 _exptl_absorpt_correction_T_max 0.452 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 6904 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.90 _reflns_number_total 1392 _reflns_number_gt 1304 _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^)+(0.0222P)^2^+1.1085P] 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 0.0112(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1392 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0214 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0473 _refine_ls_wR_factor_gt 0.0468 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 Er1 Er 0.216620(16) 0.2500 0.379645(9) 0.01202(9) Uani 1 2 d S . . O1 O 0.2537(3) 0.2500 0.51299(18) 0.0206(7) Uani 1 2 d S . . O2 O 0.3900(3) 0.2500 0.61918(16) 0.0267(8) Uani 1 2 d S . . O3 O 0.7131(2) 0.0816(4) 0.63078(14) 0.0255(5) Uani 1 1 d . . . O4 O 0.5950(3) 0.2500 0.22986(19) 0.0366(10) Uani 1 2 d S . . O5 O 0.3782(3) 0.2500 0.27557(18) 0.0228(7) Uani 1 2 d S . . N1 N 0.4635(3) 0.2500 0.41943(19) 0.0130(6) Uani 1 2 d S . . N2 N 0.7414(4) 0.2500 0.4616(2) 0.0200(8) Uani 1 2 d S . . C1 C 0.3709(4) 0.2500 0.5489(2) 0.0156(8) Uani 1 2 d S . . C2 C 0.4979(4) 0.2500 0.4946(2) 0.0127(7) Uani 1 2 d S . . C3 C 0.6403(4) 0.2500 0.5160(2) 0.0142(7) Uani 1 2 d S . . C4 C 0.6916(4) 0.2500 0.5994(3) 0.0144(8) Uani 1 2 d S . . C5 C 0.7027(4) 0.2500 0.3866(3) 0.0209(10) Uani 1 2 d S . . H5 H 0.7711 0.2500 0.3481 0.025 Uiso 1 2 calc SR . . C6 C 0.5622(4) 0.2500 0.3655(2) 0.0157(8) Uani 1 2 d S . . C7 C 0.5082(4) 0.2500 0.2833(2) 0.0191(8) Uani 1 2 d S . . O6 O 0.0215(2) 0.0380(4) 0.41777(15) 0.0339(6) Uani 1 1 d . . . H6A H 0.0432 -0.0712 0.4416 0.041 Uiso 1 1 d R . . H6B H -0.0674 0.0421 0.4142 0.041 Uiso 1 1 d R . . O7 O 0.1146(4) 0.2500 0.6803(2) 0.0483(11) Uani 1 2 d S . . H7A H 0.1832 0.2500 0.6487 0.058 Uiso 1 2 d SR . . H7B H 0.0332 0.2500 0.6601 0.058 Uiso 1 2 d SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.00993(11) 0.01344(13) 0.01267(13) 0.000 -0.00117(6) 0.000 O1 0.0088(11) 0.0346(18) 0.0184(16) 0.000 0.0003(11) 0.000 O2 0.0188(15) 0.047(2) 0.0145(16) 0.000 -0.0001(11) 0.000 O3 0.0356(14) 0.0166(13) 0.0242(12) 0.0028(9) -0.0085(9) 0.0032(9) O4 0.0162(15) 0.079(3) 0.0142(16) 0.000 0.0057(13) 0.000 O5 0.0125(13) 0.0392(19) 0.0167(15) 0.000 0.0005(11) 0.000 N1 0.0126(14) 0.0104(15) 0.0160(16) 0.000 0.0002(13) 0.000 N2 0.0141(15) 0.025(2) 0.0208(19) 0.000 -0.0019(14) 0.000 C1 0.0142(18) 0.0171(19) 0.0156(19) 0.000 0.0026(14) 0.000 C2 0.0115(16) 0.0120(17) 0.0146(18) 0.000 -0.0013(14) 0.000 C3 0.0154(18) 0.0097(17) 0.0173(19) 0.000 -0.0031(15) 0.000 C4 0.0120(16) 0.0139(19) 0.017(2) 0.000 -0.0007(15) 0.000 C5 0.0107(18) 0.031(3) 0.021(2) 0.000 0.0013(15) 0.000 C6 0.0102(16) 0.0171(19) 0.020(2) 0.000 -0.0002(15) 0.000 C7 0.0168(18) 0.024(2) 0.016(2) 0.000 0.0038(16) 0.000 O6 0.0210(11) 0.0393(15) 0.0416(14) 0.0113(12) 0.0020(10) -0.0073(11) O7 0.0279(19) 0.077(3) 0.041(2) 0.000 0.0045(17) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O4 2.209(3) 6_556 ? Er1 O3 2.280(3) 4_656 ? Er1 O1 2.317(3) . ? Er1 O5 2.360(3) . ? Er1 O6 2.412(2) . ? Er1 N1 2.452(3) . ? O1 C1 1.277(5) . ? O2 C1 1.220(5) . ? O3 C4 1.244(3) . ? O4 C7 1.236(5) . ? O5 C7 1.247(5) . ? N1 C6 1.320(5) . ? N1 C2 1.332(5) . ? N2 C5 1.338(6) . ? N2 C3 1.343(6) . ? C1 C2 1.529(5) . ? C2 C3 1.407(5) . ? C3 C4 1.512(6) . ? C4 O3 1.244(3) 8_565 ? C5 C6 1.388(5) . ? C5 H5 0.9300 . ? C6 C7 1.503(6) . ? O6 H6A 0.8500 . ? O6 H6B 0.8501 . ? O7 H7A 0.8499 . ? O7 H7B 0.8501 . ? 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 O4 Er1 O3 95.03(6) 6_556 4_656 ? O4 Er1 O3 95.03(6) 6_556 5_656 ? O3 Er1 O3 144.56(12) 4_656 5_656 ? O4 Er1 O1 157.12(11) 6_556 . ? O3 Er1 O1 91.87(6) 4_656 . ? O3 Er1 O1 91.87(6) 5_656 . ? O4 Er1 O5 72.45(11) 6_556 . ? O3 Er1 O5 75.44(6) 4_656 . ? O3 Er1 O5 75.44(6) 5_656 . ? O1 Er1 O5 130.43(10) . . ? O4 Er1 O6 79.97(9) 6_556 . ? O3 Er1 O6 142.78(9) 4_656 . ? O3 Er1 O6 72.54(9) 5_656 . ? O1 Er1 O6 81.36(9) . . ? O5 Er1 O6 135.18(8) . . ? O4 Er1 O6 79.97(9) 6_556 8_565 ? O3 Er1 O6 72.54(9) 4_656 8_565 ? O3 Er1 O6 142.78(9) 5_656 8_565 ? O1 Er1 O6 81.36(9) . 8_565 ? O5 Er1 O6 135.18(8) . 8_565 ? O6 Er1 O6 70.27(13) . 8_565 ? O4 Er1 N1 137.84(12) 6_556 . ? O3 Er1 N1 74.90(6) 4_656 . ? O3 Er1 N1 74.90(6) 5_656 . ? O1 Er1 N1 65.04(11) . . ? O5 Er1 N1 65.39(10) . . ? O6 Er1 N1 131.71(8) . . ? O6 Er1 N1 131.71(8) 8_565 . ? C1 O1 Er1 127.7(3) . . ? C4 O3 Er1 149.2(3) . 5_656 ? C7 O4 Er1 169.6(3) . 6_656 ? C7 O5 Er1 124.7(3) . . ? C6 N1 C2 120.2(3) . . ? C6 N1 Er1 119.3(3) . . ? C2 N1 Er1 120.4(2) . . ? C5 N2 C3 118.1(4) . . ? O2 C1 O1 127.5(4) . . ? O2 C1 C2 119.0(3) . . ? O1 C1 C2 113.5(3) . . ? N1 C2 C3 119.4(4) . . ? N1 C2 C1 113.3(3) . . ? C3 C2 C1 127.3(4) . . ? N2 C3 C2 120.7(4) . . ? N2 C3 C4 115.3(3) . . ? C2 C3 C4 124.0(4) . . ? O3 C4 O3 124.8(4) 8_565 . ? O3 C4 C3 117.6(2) 8_565 . ? O3 C4 C3 117.6(2) . . ? N2 C5 C6 121.1(4) . . ? N2 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? N1 C6 C5 120.3(4) . . ? N1 C6 C7 114.5(3) . . ? C5 C6 C7 125.2(4) . . ? O4 C7 O5 126.0(4) . . ? O4 C7 C6 117.9(4) . . ? O5 C7 C6 116.2(4) . . ? Er1 O6 H6A 115.3 . . ? Er1 O6 H6B 137.0 . . ? H6A O6 H6B 107.7 . . ? H7A O7 H7B 116.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Er1 O1 C1 180.0 6_556 . . . ? O3 Er1 O1 C1 -72.38(6) 4_656 . . . ? O3 Er1 O1 C1 72.38(6) 5_656 . . . ? O5 Er1 O1 C1 0.0 . . . . ? O6 Er1 O1 C1 144.40(7) . . . . ? O6 Er1 O1 C1 -144.40(7) 8_565 . . . ? N1 Er1 O1 C1 0.0 . . . . ? O4 Er1 O5 C7 180.0 6_556 . . . ? O3 Er1 O5 C7 79.80(6) 4_656 . . . ? O3 Er1 O5 C7 -79.80(6) 5_656 . . . ? O1 Er1 O5 C7 0.0 . . . . ? O6 Er1 O5 C7 -125.27(10) . . . . ? O6 Er1 O5 C7 125.26(10) 8_565 . . . ? N1 Er1 O5 C7 0.0 . . . . ? O4 Er1 N1 C6 0.0 6_556 . . . ? O3 Er1 N1 C6 -80.63(7) 4_656 . . . ? O3 Er1 N1 C6 80.63(7) 5_656 . . . ? O1 Er1 N1 C6 180.0 . . . . ? O5 Er1 N1 C6 0.0 . . . . ? O6 Er1 N1 C6 129.56(10) . . . . ? O6 Er1 N1 C6 -129.56(10) 8_565 . . . ? O4 Er1 N1 C2 180.0 6_556 . . . ? O3 Er1 N1 C2 99.37(7) 4_656 . . . ? O3 Er1 N1 C2 -99.37(7) 5_656 . . . ? O1 Er1 N1 C2 0.0 . . . . ? O5 Er1 N1 C2 180.0 . . . . ? O6 Er1 N1 C2 -50.44(10) . . . . ? O6 Er1 N1 C2 50.44(10) 8_565 . . . ? Er1 O1 C1 O2 180.0 . . . . ? Er1 O1 C1 C2 0.000(1) . . . . ? C6 N1 C2 C3 0.0 . . . . ? Er1 N1 C2 C3 180.0 . . . . ? C6 N1 C2 C1 180.0 . . . . ? Er1 N1 C2 C1 0.0 . . . . ? O2 C1 C2 N1 180.000(1) . . . . ? O1 C1 C2 N1 0.0 . . . . ? O2 C1 C2 C3 0.000(1) . . . . ? O1 C1 C2 C3 180.000(1) . . . . ? C5 N2 C3 C2 0.000(1) . . . . ? C5 N2 C3 C4 180.0 . . . . ? N1 C2 C3 N2 0.000(1) . . . . ? C1 C2 C3 N2 180.0 . . . . ? N1 C2 C3 C4 180.0 . . . . ? C1 C2 C3 C4 0.000(1) . . . . ? Er1 O3 C4 O3 -143.8(3) 5_656 . . 8_565 ? Er1 O3 C4 C3 34.0(7) 5_656 . . . ? N2 C3 C4 O3 89.0(3) . . . 8_565 ? C2 C3 C4 O3 -91.0(3) . . . 8_565 ? N2 C3 C4 O3 -89.0(3) . . . . ? C2 C3 C4 O3 91.0(3) . . . . ? C3 N2 C5 C6 0.0 . . . . ? C2 N1 C6 C5 0.0 . . . . ? Er1 N1 C6 C5 180.0 . . . . ? C2 N1 C6 C7 180.0 . . . . ? Er1 N1 C6 C7 0.0 . . . . ? N2 C5 C6 N1 0.0 . . . . ? N2 C5 C6 C7 180.0 . . . . ? Er1 O4 C7 O5 0.000(2) 6_656 . . . ? Er1 O4 C7 C6 180.000(2) 6_656 . . . ? Er1 O5 C7 O4 180.0 . . . . ? Er1 O5 C7 C6 0.0 . . . . ? N1 C6 C7 O4 180.0 . . . . ? C5 C6 C7 O4 0.0 . . . . ? N1 C6 C7 O5 0.0 . . . . ? C5 C6 C7 O5 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.901 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.162