# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global #TrackingRef '- combined_rev.cif' _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jian-Zhong Wu' _publ_contact_author_email wujzh@scnu.edu.cn _publ_section_title ; Spontaneous resolution of lanthanide coordination polymers with achiral 2-hydroxypyrimidine-4,6-dicarboxylic acid ; loop_ _publ_author_name 'Ming-Juan Gao' 'Ping Yang' 'Bin Cai' 'Jing-Wei Dai' 'Jian-Zhong Wu' 'Ying Yu' # Attachment 'Combined CIFS - .cif' data_1 #TrackingRef '- combined_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 800876' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H5 Eu N2 O7, 1.07(H2 O), 0.34(O), 0.68(H)' _chemical_formula_sum 'C6 H7.83 Eu N2 O8.41' _chemical_formula_weight 394.56 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 trigonal _symmetry_space_group_name_H-M 'R 3 2' _symmetry_space_group_name_Hall 'R 3 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 12.472(2) _cell_length_b 12.472(2) _cell_length_c 19.703(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2654.2(7) _cell_formula_units_Z 9 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4059 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 28.01 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1693.1 _exptl_absorpt_coefficient_mu 5.353 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.349 _exptl_absorpt_correction_T_max 0.807 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 4888 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.95 _reflns_number_total 1168 _reflns_number_gt 1157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2 (Bruker, 2004)' _computing_data_reduction 'APEX2 (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2009)' _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^)+(0.0188P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.011(14) _refine_ls_number_reflns 1168 _refine_ls_number_parameters 89 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0137 _refine_ls_R_factor_gt 0.0135 _refine_ls_wR_factor_ref 0.0330 _refine_ls_wR_factor_gt 0.0329 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 C1 C 0.1120(4) 0.2251(3) 0.22135(13) 0.0237(7) Uani 1 1 d . . . C2 C 0.0825(3) 0.2813(3) 0.28109(18) 0.0222(9) Uani 1 1 d . . . C3 C 0.1672(4) 0.3333 0.3333 0.0299(13) Uani 1 2 d S . . H3 H 0.2417 0.3333 0.3333 0.036 Uiso 1 2 calc SR . . C4 C -0.0517(4) 0.3333 0.3333 0.0185(10) Uani 1 2 d S . . Eu1 Eu 0.3333 0.155012(18) 0.1667 0.01057(7) Uani 1 2 d S . . N1 N -0.0244(2) 0.2802(3) 0.27952(12) 0.0177(6) Uani 1 1 d . . . O1 O 0.2038(3) 0.2115(3) 0.22614(12) 0.0366(7) Uani 1 1 d . . . O2 O 0.0425(2) 0.1979(3) 0.17038(11) 0.0337(7) Uani 1 1 d . . . O3 O -0.1523(3) 0.3333 0.3333 0.0240(8) Uani 1 2 d S . . O1W O 0.2048(2) 0.1739(2) 0.08361(11) 0.0234(5) Uani 1 1 d . . . H1W H 0.1324 0.1599 0.0889 0.035 Uiso 1 1 d R . . H2W H 0.2004 0.1406 0.0465 0.035 Uiso 1 1 d R . . O2W O 0.2582(10) 0.4541(10) 0.0998(7) 0.209(10) Uani 0.537(16) 1 d P . . H3W H 0.2168 0.3771 0.1097 0.313 Uiso 0.537(16) 1 d PR . . H4W H 0.2557 0.4947 0.1320 0.313 Uiso 0.537(16) 1 d PR . . O3W O 0.3333 0.6667 0.0213(8) 0.130(8) Uani 0.510(18) 3 d SP . . H5W H 0.3509 0.6155 0.0404 0.194 Uiso 0.170(6) 1 d PR . . H6W H 0.3939 0.7395 0.0132 0.194 Uiso 0.170(6) 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0201(18) 0.036(2) 0.0209(13) -0.0108(13) -0.0037(16) 0.0182(17) C2 0.0237(17) 0.033(3) 0.0188(18) -0.0075(13) -0.0028(13) 0.0209(16) C3 0.0204(16) 0.055(4) 0.026(2) -0.0197(19) -0.0098(9) 0.028(2) C4 0.019(2) 0.023(2) 0.015(2) -0.0045(17) -0.0022(8) 0.0114(11) Eu1 0.00946(12) 0.01132(9) 0.01032(10) -0.00007(4) -0.00013(7) 0.00473(6) N1 0.0141(13) 0.0265(15) 0.0155(12) -0.0075(11) -0.0048(10) 0.0125(12) O1 0.0317(15) 0.069(2) 0.0278(13) -0.0221(13) -0.0101(12) 0.0396(16) O2 0.0245(13) 0.066(2) 0.0236(13) -0.0228(13) -0.0118(10) 0.0319(14) O3 0.0168(13) 0.037(2) 0.0249(17) -0.0163(15) -0.0081(8) 0.0186(10) O1W 0.0237(13) 0.0358(14) 0.0177(11) -0.0052(10) -0.0053(9) 0.0200(11) O2W 0.107(11) 0.124(10) 0.34(2) 0.100(11) 0.011(11) 0.016(8) O3W 0.108(9) 0.108(9) 0.173(17) 0.000 0.000 0.054(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 C1 O1 1.243(5) . ? C1 O2 1.257(4) . ? C1 C2 1.507(4) . ? C1 Eu1 3.263(4) 2 ? C2 N1 1.327(4) . ? C2 C3 1.382(4) . ? C3 C2 1.382(4) 17 ? C3 H3 0.9300 . ? C4 O3 1.254(7) . ? C4 N1 1.380(4) 17 ? C4 N1 1.380(4) . ? Eu1 O2 2.351(3) 11 ? Eu1 O2 2.351(3) 3 ? Eu1 O1 2.370(2) . ? Eu1 O1 2.370(2) 12 ? Eu1 O1W 2.384(2) . ? Eu1 O1W 2.384(2) 12 ? Eu1 N1 2.673(2) 11 ? Eu1 N1 2.673(2) 3 ? Eu1 C1 3.263(4) 11 ? Eu1 C1 3.263(4) 3 ? N1 Eu1 2.673(2) 2 ? O2 Eu1 2.351(3) 2 ? O1W H1W 0.8355 . ? O1W H2W 0.8288 . ? O2W H3W 0.8546 . ? O2W H4W 0.8222 . ? O3W H5W 0.8583 . ? O3W H6W 0.8571 . ? 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 C1 O2 125.6(3) . . ? O1 C1 C2 117.4(3) . . ? O2 C1 C2 117.0(3) . . ? O1 C1 Eu1 158.2(2) . 2 ? O2 C1 Eu1 35.29(16) . 2 ? C2 C1 Eu1 82.9(2) . 2 ? N1 C2 C3 123.4(3) . . ? N1 C2 C1 117.0(3) . . ? C3 C2 C1 119.6(3) . . ? C2 C3 C2 116.1(5) 17 . ? C2 C3 H3 122.0 17 . ? C2 C3 H3 122.0 . . ? O3 C4 N1 119.2(2) . 17 ? O3 C4 N1 119.2(2) . . ? N1 C4 N1 121.7(4) 17 . ? O2 Eu1 O2 109.69(14) 11 3 ? O2 Eu1 O1 149.89(7) 11 . ? O2 Eu1 O1 82.51(10) 3 . ? O2 Eu1 O1 82.51(10) 11 12 ? O2 Eu1 O1 149.89(7) 3 12 ? O1 Eu1 O1 100.72(16) . 12 ? O2 Eu1 O1W 134.84(8) 11 . ? O2 Eu1 O1W 78.23(8) 3 . ? O1 Eu1 O1W 73.62(8) . . ? O1 Eu1 O1W 74.15(8) 12 . ? O2 Eu1 O1W 78.23(8) 11 12 ? O2 Eu1 O1W 134.84(8) 3 12 ? O1 Eu1 O1W 74.15(8) . 12 ? O1 Eu1 O1W 73.62(8) 12 12 ? O1W Eu1 O1W 128.42(11) . 12 ? O2 Eu1 N1 64.34(7) 11 11 ? O2 Eu1 N1 78.95(9) 3 11 ? O1 Eu1 N1 145.69(8) . 11 ? O1 Eu1 N1 82.31(9) 12 11 ? O1W Eu1 N1 74.48(8) . 11 ? O1W Eu1 N1 137.70(8) 12 11 ? O2 Eu1 N1 78.95(9) 11 3 ? O2 Eu1 N1 64.34(7) 3 3 ? O1 Eu1 N1 82.31(9) . 3 ? O1 Eu1 N1 145.69(8) 12 3 ? O1W Eu1 N1 137.70(8) . 3 ? O1W Eu1 N1 74.48(8) 12 3 ? N1 Eu1 N1 114.29(11) 11 3 ? O2 Eu1 C1 17.99(7) 11 11 ? O2 Eu1 C1 105.10(9) 3 11 ? O1 Eu1 C1 167.47(8) . 11 ? O1 Eu1 C1 77.82(9) 12 11 ? O1W Eu1 C1 117.31(7) . 11 ? O1W Eu1 C1 93.61(8) 12 11 ? N1 Eu1 C1 46.79(7) 11 11 ? N1 Eu1 C1 91.95(8) 3 11 ? O2 Eu1 C1 105.10(9) 11 3 ? O2 Eu1 C1 17.99(7) 3 3 ? O1 Eu1 C1 77.82(9) . 3 ? O1 Eu1 C1 167.47(8) 12 3 ? O1W Eu1 C1 93.61(8) . 3 ? O1W Eu1 C1 117.31(7) 12 3 ? N1 Eu1 C1 91.95(8) 11 3 ? N1 Eu1 C1 46.79(7) 3 3 ? C1 Eu1 C1 106.30(11) 11 3 ? C2 N1 C4 117.7(3) . . ? C2 N1 Eu1 113.24(19) . 2 ? C4 N1 Eu1 129.0(2) . 2 ? C1 O1 Eu1 144.6(2) . . ? C1 O2 Eu1 126.7(2) . 2 ? Eu1 O1W H1W 127.1 . . ? Eu1 O1W H2W 115.8 . . ? H1W O1W H2W 102.2 . . ? H3W O2W H4W 109.2 . . ? H5W O3W H6W 116.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.601 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.072 data_2b #TrackingRef '- combined_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 800877' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H5 Gd N2 O7, 1.18(H2 O), 0.34(O), 0.68(H)' _chemical_formula_sum 'C6 H8.04 Gd N2 O8.52' _chemical_formula_weight 401.73 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 trigonal _symmetry_space_group_name_H-M 'R 3 2' _symmetry_space_group_name_Hall 'R 3 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 12.4390(9) _cell_length_b 12.4390(9) _cell_length_c 19.6700(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2635.8(3) _cell_formula_units_Z 9 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3085 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1711.9 _exptl_absorpt_coefficient_mu 5.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3299 _exptl_absorpt_correction_T_max 0.8041 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 4882 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1165 _reflns_number_gt 1149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2 (Bruker, 2004)' _computing_data_reduction 'APEX2 (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2009)' _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^)+(0.0149P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(15) _refine_ls_number_reflns 1165 _refine_ls_number_parameters 89 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0156 _refine_ls_R_factor_gt 0.0152 _refine_ls_wR_factor_ref 0.0339 _refine_ls_wR_factor_gt 0.0338 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 C1 C 0.1111(4) 0.2241(3) 0.22108(15) 0.0231(8) Uani 1 1 d . . . C2 C 0.0826(3) 0.2813(3) 0.2807(2) 0.0212(11) Uani 1 1 d . . . C3 C 0.1679(5) 0.3333 0.3333 0.0282(14) Uani 1 2 d S . . H3 H 0.2426 0.3333 0.3333 0.034 Uiso 1 2 calc SR . . C4 C -0.0522(5) 0.3333 0.3333 0.0180(12) Uani 1 2 d S . . Gd1 Gd 0.3333 0.15533(2) 0.1667 0.01087(7) Uani 1 2 d S . . N1 N -0.0250(3) 0.2801(3) 0.27935(14) 0.0162(7) Uani 1 1 d . . . O1 O 0.2027(3) 0.2098(3) 0.22605(14) 0.0353(8) Uani 1 1 d . . . O2 O 0.0424(3) 0.1986(3) 0.16980(13) 0.0305(8) Uani 1 1 d . . . O3 O -0.1532(3) 0.3333 0.3333 0.0232(9) Uani 1 2 d S . . O1W O 0.2058(2) 0.1747(2) 0.08410(13) 0.0226(6) Uani 1 1 d . . . H1W H 0.1334 0.1607 0.0894 0.034 Uiso 1 1 d R . . H2W H 0.2014 0.1415 0.0470 0.034 Uiso 1 1 d R . . O2W O 0.2558(13) 0.4573(12) 0.1019(7) 0.264(13) Uani 0.589(17) 1 d P . . H3W H 0.2144 0.3803 0.1118 0.396 Uiso 0.589(17) 1 d PR . . H4W H 0.2533 0.4979 0.1341 0.396 Uiso 0.589(17) 1 d PR . . O3W O 0.3333 0.6667 0.0195(8) 0.126(8) Uani 0.511(18) 3 d SP . . H5W H 0.3509 0.6155 0.0397 0.188 Uiso 0.170(6) 1 d PR . . H6W H 0.3939 0.7395 0.0126 0.188 Uiso 0.170(6) 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.020(2) 0.035(2) 0.0197(16) -0.0136(15) -0.009(2) 0.018(2) C2 0.0201(19) 0.035(3) 0.017(2) -0.0050(15) -0.0019(15) 0.0194(18) C3 0.0195(17) 0.050(4) 0.025(3) -0.019(2) -0.0097(11) 0.025(2) C4 0.017(3) 0.020(3) 0.017(2) -0.004(2) -0.0020(10) 0.0102(13) Gd1 0.00936(13) 0.01190(10) 0.01049(11) 0.00007(5) 0.00015(9) 0.00468(7) N1 0.0124(15) 0.0228(17) 0.0178(15) -0.0065(13) -0.0028(12) 0.0119(13) O1 0.0295(17) 0.070(2) 0.0252(15) -0.0170(15) -0.0091(13) 0.0389(18) O2 0.0231(15) 0.057(2) 0.0211(16) -0.0195(14) -0.0104(12) 0.0276(15) O3 0.0160(15) 0.035(2) 0.025(2) -0.0163(18) -0.0082(9) 0.0173(12) O1W 0.0243(15) 0.0342(16) 0.0157(13) -0.0046(11) -0.0030(11) 0.0194(13) O2W 0.166(16) 0.155(13) 0.35(2) 0.109(12) -0.002(15) -0.011(12) O3W 0.105(9) 0.105(9) 0.167(18) 0.000 0.000 0.053(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 C1 O1 1.243(5) . ? C1 O2 1.256(4) . ? C1 C2 1.503(5) . ? C2 N1 1.331(4) . ? C2 C3 1.389(5) . ? C3 C2 1.389(5) 17 ? C3 H3 0.9300 . ? C4 O3 1.256(8) . ? C4 N1 1.380(4) 17 ? C4 N1 1.380(4) . ? Gd1 O2 2.343(3) 11 ? Gd1 O2 2.343(3) 3 ? Gd1 O1 2.358(3) . ? Gd1 O1 2.358(3) 12 ? Gd1 O1W 2.366(3) 12 ? Gd1 O1W 2.366(3) . ? Gd1 N1 2.664(3) 11 ? Gd1 N1 2.664(3) 3 ? N1 Gd1 2.664(3) 2 ? O2 Gd1 2.343(3) 2 ? O1W H1W 0.8333 . ? O1W H2W 0.8273 . ? O2W H3W 0.8524 . ? O2W H4W 0.8205 . ? O3W H5W 0.8658 . ? O3W H6W 0.8512 . ? 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 C1 O2 125.7(3) . . ? O1 C1 C2 117.2(3) . . ? O2 C1 C2 117.0(4) . . ? N1 C2 C3 123.3(4) . . ? N1 C2 C1 116.9(3) . . ? C3 C2 C1 119.7(4) . . ? C2 C3 C2 115.9(5) 17 . ? C2 C3 H3 122.1 17 . ? C2 C3 H3 122.1 . . ? O3 C4 N1 119.0(2) . 17 ? O3 C4 N1 119.0(2) . . ? N1 C4 N1 122.0(5) 17 . ? O2 Gd1 O2 109.15(16) 11 3 ? O2 Gd1 O1 149.88(8) 11 . ? O2 Gd1 O1 82.37(11) 3 . ? O2 Gd1 O1 82.37(11) 11 12 ? O2 Gd1 O1 149.88(8) 3 12 ? O1 Gd1 O1 101.67(17) . 12 ? O2 Gd1 O1W 78.38(9) 11 12 ? O2 Gd1 O1W 135.11(9) 3 12 ? O1 Gd1 O1W 74.35(9) . 12 ? O1 Gd1 O1W 73.58(9) 12 12 ? O2 Gd1 O1W 135.11(9) 11 . ? O2 Gd1 O1W 78.38(9) 3 . ? O1 Gd1 O1W 73.58(9) . . ? O1 Gd1 O1W 74.35(9) 12 . ? O1W Gd1 O1W 128.13(12) 12 . ? O2 Gd1 N1 64.57(8) 11 11 ? O2 Gd1 N1 78.48(10) 3 11 ? O1 Gd1 N1 145.38(9) . 11 ? O1 Gd1 N1 82.10(10) 12 11 ? O1W Gd1 N1 137.94(9) 12 11 ? O1W Gd1 N1 74.48(9) . 11 ? O2 Gd1 N1 78.48(10) 11 3 ? O2 Gd1 N1 64.57(8) 3 3 ? O1 Gd1 N1 82.10(10) . 3 ? O1 Gd1 N1 145.38(9) 12 3 ? O1W Gd1 N1 74.48(9) 12 3 ? O1W Gd1 N1 137.93(9) . 3 ? N1 Gd1 N1 114.26(13) 11 3 ? C2 N1 C4 117.7(3) . . ? C2 N1 Gd1 113.0(2) . 2 ? C4 N1 Gd1 129.2(3) . 2 ? C1 O1 Gd1 144.6(2) . . ? C1 O2 Gd1 126.4(2) . 2 ? Gd1 O1W H1W 127.0 . . ? Gd1 O1W H2W 115.7 . . ? H1W O1W H2W 102.2 . . ? H3W O2W H4W 109.1 . . ? H5W O3W H6W 116.2 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.361 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.078 data_3 #TrackingRef '- combined_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 800878' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H5 N2 O7 Tb, 1.13(H2 O), 0.4(O), 0.8(H)' _chemical_formula_sum 'C6 H8.06 N2 O8.53 Tb' _chemical_formula_weight 403.65 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 2' _symmetry_space_group_name_Hall 'R 3 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 12.4040(10) _cell_length_b 12.4040(10) _cell_length_c 19.6075(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2612.6(4) _cell_formula_units_Z 9 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4623 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 28.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1722 _exptl_absorpt_coefficient_mu 6.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2987 _exptl_absorpt_correction_T_max 0.7916 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 4781 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1154 _reflns_number_gt 1151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2 (Bruker, 2004)' _computing_data_reduction 'APEX2 (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2009)' _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^)+(0.0120P)^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 SHELXL _refine_ls_extinction_coef 0.00163(5) _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 0.019(12) _refine_ls_number_reflns 1154 _refine_ls_number_parameters 90 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0123 _refine_ls_R_factor_gt 0.0122 _refine_ls_wR_factor_ref 0.0303 _refine_ls_wR_factor_gt 0.0303 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 C1 C 0.1103(3) 0.2235(3) 0.22083(12) 0.0200(6) Uani 1 1 d . . . C2 C 0.0817(3) 0.2812(3) 0.28095(18) 0.0190(9) Uani 1 1 d . . . C3 C 0.1670(4) 0.3333 0.3333 0.0253(12) Uani 1 2 d S . . H3 H 0.2420 0.3333 0.3333 0.030 Uiso 1 2 calc SR . . C4 C -0.0539(4) 0.3333 0.3333 0.0158(9) Uani 1 2 d S . . N1 N -0.0264(2) 0.2800(2) 0.27951(12) 0.0153(5) Uani 1 1 d . . . O1 O 0.2030(2) 0.2105(3) 0.22569(11) 0.0326(6) Uani 1 1 d . . . O2 O 0.0402(2) 0.1961(2) 0.16979(11) 0.0277(6) Uani 1 1 d . . . O3 O -0.1547(3) 0.3333 0.3333 0.0224(7) Uani 1 2 d S . . O1W O 0.20622(19) 0.1759(2) 0.08388(11) 0.0209(5) Uani 1 1 d . . . H1W H 0.1339 0.1619 0.0892 0.031 Uiso 1 1 d R . . H2W H 0.2019 0.1426 0.0468 0.031 Uiso 1 1 d R . . O2W O 0.2591(9) 0.4569(8) 0.1014(6) 0.169(7) Uani 0.567(16) 1 d P . . H3W H 0.2177 0.3799 0.1113 0.253 Uiso 0.567(16) 1 d PR . . H4W H 0.2566 0.4975 0.1336 0.253 Uiso 0.567(16) 1 d PR . . O3W O 0.3333 0.6667 0.0193(7) 0.116(6) Uani 0.597(18) 3 d SP . . H5W H 0.3509 0.6155 0.0402 0.174 Uiso 0.199(6) 1 d PR . . H6W H 0.3939 0.7395 0.0131 0.174 Uiso 0.199(6) 1 d PR . . Tb1 Tb 0.3333 0.156561(19) 0.1667 0.00943(7) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0176(17) 0.0291(16) 0.0176(12) -0.0095(11) -0.0042(15) 0.0149(16) C2 0.0181(15) 0.029(2) 0.0157(17) -0.0031(12) 0.0002(12) 0.0162(14) C3 0.0175(14) 0.040(3) 0.026(2) -0.0154(16) -0.0077(8) 0.0202(16) C4 0.014(2) 0.018(2) 0.017(2) -0.0028(16) -0.0014(8) 0.0088(10) N1 0.0138(12) 0.0213(13) 0.0137(11) -0.0040(10) -0.0020(10) 0.0110(11) O1 0.0262(14) 0.0640(19) 0.0235(12) -0.0186(12) -0.0104(10) 0.0343(14) O2 0.0209(13) 0.0496(16) 0.0211(13) -0.0167(11) -0.0091(9) 0.0241(12) O3 0.0172(12) 0.0327(19) 0.0225(17) -0.0147(14) -0.0074(7) 0.0163(9) O1W 0.0187(12) 0.0325(13) 0.0169(10) -0.0035(9) -0.0029(9) 0.0168(10) O2W 0.106(10) 0.094(7) 0.269(15) 0.060(7) 0.013(8) 0.022(6) O3W 0.086(6) 0.086(6) 0.176(14) 0.000 0.000 0.043(3) Tb1 0.00820(11) 0.00985(9) 0.00969(10) -0.00001(3) -0.00003(6) 0.00410(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 C1 O1 1.242(5) . ? C1 O2 1.256(4) . ? C1 C2 1.510(4) . ? C2 N1 1.334(4) . ? C2 C3 1.382(4) . ? C3 C2 1.382(4) 17 ? C3 H3 0.9300 . ? C4 O3 1.250(6) . ? C4 N1 1.376(3) . ? C4 N1 1.376(3) 17 ? N1 Tb1 2.660(2) 2 ? O1 Tb1 2.341(2) . ? O2 Tb1 2.330(2) 2 ? O1W Tb1 2.357(2) . ? O1W H1W 0.8310 . ? O1W H2W 0.8247 . ? O2W H3W 0.8500 . ? O2W H4W 0.8181 . ? O3W H5W 0.8696 . ? O3W H6W 0.8467 . ? Tb1 O2 2.330(2) 11 ? Tb1 O2 2.330(2) 3 ? Tb1 O1 2.341(2) 12 ? Tb1 O1W 2.357(2) 12 ? Tb1 N1 2.660(2) 11 ? Tb1 N1 2.660(2) 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 C1 O2 125.9(3) . . ? O1 C1 C2 117.0(3) . . ? O2 C1 C2 117.1(3) . . ? N1 C2 C3 123.5(3) . . ? N1 C2 C1 116.8(3) . . ? C3 C2 C1 119.7(3) . . ? C2 C3 C2 115.7(5) 17 . ? C2 C3 H3 122.1 17 . ? C2 C3 H3 122.1 . . ? O3 C4 N1 119.2(2) . . ? O3 C4 N1 119.2(2) . 17 ? N1 C4 N1 121.5(4) . 17 ? C2 N1 C4 117.9(3) . . ? C2 N1 Tb1 112.81(19) . 2 ? C4 N1 Tb1 129.2(2) . 2 ? C1 O1 Tb1 144.63(19) . . ? C1 O2 Tb1 126.6(2) . 2 ? Tb1 O1W H1W 126.9 . . ? Tb1 O1W H2W 115.9 . . ? H1W O1W H2W 102.2 . . ? H3W O2W H4W 109.1 . . ? H5W O3W H6W 115.7 . . ? O2 Tb1 O2 109.79(13) 11 3 ? O2 Tb1 O1 82.02(10) 11 12 ? O2 Tb1 O1 149.86(7) 3 12 ? O2 Tb1 O1 149.85(7) 11 . ? O2 Tb1 O1 82.02(10) 3 . ? O1 Tb1 O1 101.74(15) 12 . ? O2 Tb1 O1W 134.95(7) 11 . ? O2 Tb1 O1W 78.19(8) 3 . ? O1 Tb1 O1W 74.37(8) 12 . ? O1 Tb1 O1W 73.67(7) . . ? O2 Tb1 O1W 78.19(8) 11 12 ? O2 Tb1 O1W 134.94(7) 3 12 ? O1 Tb1 O1W 73.66(8) 12 12 ? O1 Tb1 O1W 74.37(8) . 12 ? O1W Tb1 O1W 128.27(11) . 12 ? O2 Tb1 N1 64.94(7) 11 11 ? O2 Tb1 N1 78.33(8) 3 11 ? O1 Tb1 N1 82.38(9) 12 11 ? O1 Tb1 N1 145.04(7) . 11 ? O1W Tb1 N1 74.19(7) . 11 ? O1W Tb1 N1 138.36(8) 12 11 ? O2 Tb1 N1 78.33(8) 11 3 ? O2 Tb1 N1 64.93(7) 3 3 ? O1 Tb1 N1 145.04(7) 12 3 ? O1 Tb1 N1 82.37(9) . 3 ? O1W Tb1 N1 138.36(8) . 3 ? O1W Tb1 N1 74.19(7) 12 3 ? N1 Tb1 N1 114.06(11) 11 3 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.557 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.075 data_4 #TrackingRef '- combined_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 826767' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H5 Dy N2 O7, 1.12(H2 O), 0.38(O), 0.76(H) ' _chemical_formula_sum 'C6 H8 Dy N2 O8.50' _chemical_formula_weight 406.72 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 2' _symmetry_space_group_name_Hall 'R 3 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 12.359(2) _cell_length_b 12.359(2) _cell_length_c 19.602(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2593.0(7) _cell_formula_units_Z 9 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4232 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.92 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728.1 _exptl_absorpt_coefficient_mu 6.522 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.275 _exptl_absorpt_correction_T_max 0.770 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 4724 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.96 _reflns_number_total 1143 _reflns_number_gt 1139 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2 (Bruker, 2004)' _computing_data_reduction 'APEX2 (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2009)' _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^)+(0.0065P)^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 SHELXL _refine_ls_extinction_coef 0.00133(4) _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 0.000(13) _refine_ls_number_reflns 1143 _refine_ls_number_parameters 90 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0126 _refine_ls_R_factor_gt 0.0125 _refine_ls_wR_factor_ref 0.0291 _refine_ls_wR_factor_gt 0.0291 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 C1 C 0.8901(3) 0.7762(3) 0.77939(14) 0.0196(6) Uani 1 1 d . . . C2 C 0.9186(3) 0.7192(3) 0.7193(2) 0.0184(9) Uani 1 1 d . . . C3 C 0.8331(4) 0.6667 0.6667 0.0240(12) Uani 1 2 d S . . H3 H 0.7578 0.6667 0.6667 0.029 Uiso 1 2 calc SR . . C4 C 1.0546(4) 0.6667 0.6667 0.0141(10) Uani 1 2 d S . . Dy1 Dy 0.6667 0.843485(18) 0.8333 0.00881(7) Uani 1 2 d S . . N1 N 1.0268(2) 0.7199(2) 0.72082(13) 0.0141(5) Uani 1 1 d . . . O1 O 0.7973(2) 0.7905(3) 0.77438(13) 0.0300(6) Uani 1 1 d . . . O2 O 0.9594(2) 0.8026(2) 0.83075(12) 0.0262(6) Uani 1 1 d . . . O3 O 1.1556(3) 0.6667 0.6667 0.0219(8) Uani 1 2 d S . . O1W O 0.79311(19) 0.8237(2) 0.91582(12) 0.0209(5) Uani 1 1 d . . . H1W H 0.8655 0.8377 0.9105 0.031 Uiso 1 1 d R . . H2W H 0.7975 0.8570 0.9529 0.031 Uiso 1 1 d R . . O2W O 0.7401(11) 0.5412(8) 0.8978(7) 0.193(9) Uani 0.562(16) 1 d P . . H3W H 0.7815 0.6181 0.8879 0.290 Uiso 0.562(16) 1 d PR . . H4W H 0.7426 0.5005 0.8656 0.290 Uiso 0.562(16) 1 d PR . . O3W O 0.6667 0.3333 0.9806(8) 0.127(7) Uani 0.570(18) 3 d SP . . H5W H 0.6491 0.3845 0.9606 0.191 Uiso 0.190(6) 1 d PR . . H6W H 0.6061 0.2605 0.9877 0.191 Uiso 0.190(6) 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0173(16) 0.0273(16) 0.0177(15) -0.0090(12) -0.0025(16) 0.0137(15) C2 0.0191(16) 0.028(2) 0.0138(19) -0.0034(12) -0.0004(13) 0.0164(14) C3 0.0175(14) 0.043(3) 0.020(2) -0.0133(17) -0.0066(8) 0.0216(17) C4 0.014(2) 0.016(2) 0.013(2) -0.0038(16) -0.0019(8) 0.0082(10) Dy1 0.00816(10) 0.00966(9) 0.00810(10) -0.00002(3) -0.00004(7) 0.00408(5) N1 0.0131(12) 0.0188(13) 0.0113(13) -0.0029(10) -0.0016(10) 0.0086(11) O1 0.0235(13) 0.0586(18) 0.0215(14) -0.0161(12) -0.0090(10) 0.0308(13) O2 0.0195(12) 0.0476(16) 0.0172(14) -0.0147(11) -0.0099(10) 0.0211(12) O3 0.0190(12) 0.0346(19) 0.0172(19) -0.0130(15) -0.0065(8) 0.0173(9) O1W 0.0201(12) 0.0330(13) 0.0151(12) -0.0057(10) -0.0040(9) 0.0173(10) O2W 0.132(12) 0.097(7) 0.298(19) 0.071(8) 0.002(10) 0.018(7) O3W 0.097(7) 0.097(7) 0.188(17) 0.000 0.000 0.048(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.249(5) . ? C1 O2 1.255(4) . ? C1 C2 1.502(4) . ? C2 N1 1.333(4) . ? C2 C3 1.384(5) . ? C3 C2 1.384(4) 11_566 ? C3 H3 0.9300 . ? C4 O3 1.248(6) . ? C4 N1 1.380(3) 11_566 ? C4 N1 1.380(3) . ? Dy1 O2 2.320(2) 17_566 ? Dy1 O2 2.320(2) 3_675 ? Dy1 O1 2.330(2) 18_656 ? Dy1 O1 2.330(2) . ? Dy1 O1W 2.345(2) . ? Dy1 O1W 2.345(2) 18_656 ? Dy1 N1 2.649(3) 17_566 ? Dy1 N1 2.649(3) 3_675 ? N1 Dy1 2.649(3) 2_765 ? O2 Dy1 2.320(2) 2_765 ? O1W H1W 0.8280 . ? O1W H2W 0.8239 . ? O2W H3W 0.8471 . ? O2W H4W 0.8167 . ? O3W H5W 0.8590 . ? O3W H6W 0.8465 . ? 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 C1 O2 125.6(3) . . ? O1 C1 C2 116.9(3) . . ? O2 C1 C2 117.5(3) . . ? N1 C2 C3 123.2(3) . . ? N1 C2 C1 116.7(3) . . ? C3 C2 C1 120.1(3) . . ? C2 C3 C2 116.1(4) 11_566 . ? C2 C3 H3 122.0 11_566 . ? C2 C3 H3 122.0 . . ? O3 C4 N1 119.2(2) . 11_566 ? O3 C4 N1 119.2(2) . . ? N1 C4 N1 121.6(4) 11_566 . ? O2 Dy1 O2 109.15(13) 17_566 3_675 ? O2 Dy1 O1 82.20(9) 17_566 18_656 ? O2 Dy1 O1 149.70(8) 3_675 18_656 ? O2 Dy1 O1 149.70(8) 17_566 . ? O2 Dy1 O1 82.19(9) 3_675 . ? O1 Dy1 O1 102.25(14) 18_656 . ? O2 Dy1 O1W 135.13(8) 17_566 . ? O2 Dy1 O1W 78.38(8) 3_675 . ? O1 Dy1 O1W 74.32(8) 18_656 . ? O1 Dy1 O1W 73.80(8) . . ? O2 Dy1 O1W 78.38(8) 17_566 18_656 ? O2 Dy1 O1W 135.13(8) 3_675 18_656 ? O1 Dy1 O1W 73.80(8) 18_656 18_656 ? O1 Dy1 O1W 74.32(8) . 18_656 ? O1W Dy1 O1W 128.10(11) . 18_656 ? O2 Dy1 N1 65.14(8) 17_566 17_566 ? O2 Dy1 N1 77.89(8) 3_675 17_566 ? O1 Dy1 N1 82.19(9) 18_656 17_566 ? O1 Dy1 N1 144.91(8) . 17_566 ? O1W Dy1 N1 74.07(8) . 17_566 ? O1W Dy1 N1 138.61(8) 18_656 17_566 ? O2 Dy1 N1 77.88(8) 17_566 3_675 ? O2 Dy1 N1 65.14(8) 3_675 3_675 ? O1 Dy1 N1 144.91(8) 18_656 3_675 ? O1 Dy1 N1 82.19(9) . 3_675 ? O1W Dy1 N1 138.61(8) . 3_675 ? O1W Dy1 N1 74.07(8) 18_656 3_675 ? N1 Dy1 N1 114.14(11) 17_566 3_675 ? C2 N1 C4 117.9(3) . . ? C2 N1 Dy1 112.7(2) . 2_765 ? C4 N1 Dy1 129.4(2) . 2_765 ? C1 O1 Dy1 144.6(2) . . ? C1 O2 Dy1 126.1(2) . 2_765 ? Dy1 O1W H1W 126.7 . . ? Dy1 O1W H2W 115.9 . . ? H1W O1W H2W 102.2 . . ? H3W O2W H4W 109.0 . . ? H5W O3W H6W 116.3 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.439 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.075 data_5 #TrackingRef '- combined_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 826768' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H5 Er N2 O7, 1.36(H2 O), 0.43(O), 0.85(H)' _chemical_formula_sum 'C6 H8.57 Er N2 O8.79' _chemical_formula_weight 416.57 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 trigonal _symmetry_space_group_name_H-M 'R 3 2' _symmetry_space_group_name_Hall 'R 3 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 12.2943(8) _cell_length_b 12.2943(8) _cell_length_c 19.556(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2559.9(4) _cell_formula_units_Z 9 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4175 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.95 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1771.9 _exptl_absorpt_coefficient_mu 7.418 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2486 _exptl_absorpt_correction_T_max 0.7557 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 4682 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.98 _reflns_number_total 1132 _reflns_number_gt 1126 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2 (Bruker, 2004)' _computing_data_reduction 'APEX2 (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2009)' _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^)+(0.0207P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.032(15) _refine_ls_number_reflns 1132 _refine_ls_number_parameters 89 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0167 _refine_ls_R_factor_gt 0.0166 _refine_ls_wR_factor_ref 0.0398 _refine_ls_wR_factor_gt 0.0398 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 C1 C 0.8900(5) 0.7766(4) 0.77955(17) 0.0187(8) Uani 1 1 d . . . C2 C 0.9189(4) 0.7194(4) 0.7191(2) 0.0176(12) Uani 1 1 d . . . C3 C 0.8331(6) 0.6667 0.6667 0.0257(17) Uani 1 2 d S . . H3 H 0.7575 0.6667 0.6667 0.031 Uiso 1 2 calc SR . . C4 C 1.0558(6) 0.6667 0.6667 0.0129(12) Uani 1 2 d S . . Er1 Er 0.6667 0.84335(2) 0.8333 0.00801(8) Uani 1 2 d S . . N1 N 1.0276(3) 0.7204(3) 0.72090(16) 0.0142(7) Uani 1 1 d . . . O1 O 0.7972(3) 0.7911(4) 0.77455(15) 0.0292(8) Uani 1 1 d . . . O2 O 0.9605(3) 0.8029(3) 0.83111(14) 0.0247(8) Uani 1 1 d . . . O3 O 1.1572(4) 0.6667 0.6667 0.0208(10) Uani 1 2 d S . . O1W O 0.7920(3) 0.8223(3) 0.91523(14) 0.0202(7) Uani 1 1 d . . . H1W H 0.8644 0.8363 0.9099 0.030 Uiso 1 1 d R . . H2W H 0.7964 0.8556 0.9523 0.030 Uiso 1 1 d R . . O2W O 0.7361(12) 0.5382(10) 0.8968(7) 0.189(9) Uani 0.68(2) 1 d P . . H3W H 0.7775 0.6152 0.8868 0.284 Uiso 0.68(2) 1 d PR . . H4W H 0.7386 0.4976 0.8646 0.284 Uiso 0.68(2) 1 d PR . . O3W O 0.6667 0.3333 0.9811(9) 0.123(8) Uani 0.64(2) 3 d SP . . H5W H 0.6491 0.3845 0.9604 0.185 Uiso 0.213(8) 1 d PR . . H6W H 0.6061 0.2605 0.9876 0.185 Uiso 0.213(8) 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.016(2) 0.028(2) 0.0163(16) -0.0088(15) -0.006(2) 0.014(2) C2 0.017(2) 0.028(3) 0.012(2) -0.0022(16) 0.0008(16) 0.0147(19) C3 0.019(2) 0.045(5) 0.021(3) -0.015(2) -0.0074(11) 0.022(2) C4 0.012(3) 0.017(3) 0.011(3) -0.002(2) -0.0011(10) 0.0084(14) Er1 0.00763(14) 0.00856(10) 0.00753(12) -0.00005(4) -0.00011(8) 0.00381(7) N1 0.0129(16) 0.0195(18) 0.0119(15) -0.0028(14) -0.0010(13) 0.0093(15) O1 0.0248(18) 0.057(2) 0.0204(16) -0.0144(15) -0.0068(14) 0.0316(19) O2 0.0215(17) 0.044(2) 0.0161(17) -0.0148(14) -0.0100(12) 0.0220(16) O3 0.0173(17) 0.032(3) 0.018(2) -0.0101(19) -0.0051(10) 0.0161(13) O1W 0.0202(16) 0.0329(18) 0.0137(13) -0.0044(13) -0.0030(12) 0.0178(14) O2W 0.133(15) 0.110(10) 0.300(18) 0.075(10) 0.027(12) 0.041(9) O3W 0.103(9) 0.103(9) 0.163(17) 0.000 0.000 0.052(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 C1 O1 1.244(6) . ? C1 O2 1.262(5) . ? C1 C2 1.506(6) . ? C2 N1 1.332(5) . ? C2 C3 1.378(6) . ? C3 C2 1.378(6) 11_566 ? C3 H3 0.9300 . ? C4 O3 1.246(9) . ? C4 N1 1.382(5) 11_566 ? C4 N1 1.382(5) . ? Er1 O2 2.297(3) 17_566 ? Er1 O2 2.297(3) 3_675 ? Er1 O1 2.311(3) 18_656 ? Er1 O1 2.311(3) . ? Er1 O1W 2.325(3) . ? Er1 O1W 2.325(3) 18_656 ? Er1 N1 2.635(3) 3_675 ? Er1 N1 2.635(3) 17_566 ? N1 Er1 2.635(3) 2_765 ? O2 Er1 2.297(3) 2_765 ? O1W H1W 0.8237 . ? O1W H2W 0.8214 . ? O2W H3W 0.8428 . ? O2W H4W 0.8139 . ? O3W H5W 0.8615 . ? O3W H6W 0.8399 . ? 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 C1 O2 126.0(4) . . ? O1 C1 C2 116.9(3) . . ? O2 C1 C2 117.1(4) . . ? N1 C2 C3 123.5(4) . . ? N1 C2 C1 116.4(4) . . ? C3 C2 C1 120.1(4) . . ? C2 C3 C2 116.1(6) 11_566 . ? C2 C3 H3 122.0 11_566 . ? C2 C3 H3 122.0 . . ? O3 C4 N1 119.3(3) . 11_566 ? O3 C4 N1 119.3(3) . . ? N1 C4 N1 121.4(6) 11_566 . ? O2 Er1 O2 109.15(18) 17_566 3_675 ? O2 Er1 O1 82.12(13) 17_566 18_656 ? O2 Er1 O1 149.52(10) 3_675 18_656 ? O2 Er1 O1 149.51(10) 17_566 . ? O2 Er1 O1 82.12(13) 3_675 . ? O1 Er1 O1 102.6(2) 18_656 . ? O2 Er1 O1W 135.33(10) 17_566 . ? O2 Er1 O1W 78.58(11) 3_675 . ? O1 Er1 O1W 74.10(11) 18_656 . ? O1 Er1 O1W 73.79(10) . . ? O2 Er1 O1W 78.57(11) 17_566 18_656 ? O2 Er1 O1W 135.33(10) 3_675 18_656 ? O1 Er1 O1W 73.79(10) 18_656 18_656 ? O1 Er1 O1W 74.10(11) . 18_656 ? O1W Er1 O1W 127.47(15) . 18_656 ? O2 Er1 N1 77.75(11) 17_566 3_675 ? O2 Er1 N1 65.47(10) 3_675 3_675 ? O1 Er1 N1 144.74(11) 18_656 3_675 ? O1 Er1 N1 81.94(12) . 3_675 ? O1W Er1 N1 138.93(11) . 3_675 ? O1W Er1 N1 74.04(10) 18_656 3_675 ? O2 Er1 N1 65.48(10) 17_566 17_566 ? O2 Er1 N1 77.75(11) 3_675 17_566 ? O1 Er1 N1 81.94(12) 18_656 17_566 ? O1 Er1 N1 144.74(11) . 17_566 ? O1W Er1 N1 74.04(10) . 17_566 ? O1W Er1 N1 138.93(11) 18_656 17_566 ? N1 Er1 N1 114.49(15) 3_675 17_566 ? C2 N1 C4 117.8(4) . . ? C2 N1 Er1 112.8(3) . 2_765 ? C4 N1 Er1 129.4(3) . 2_765 ? C1 O1 Er1 144.6(3) . . ? C1 O2 Er1 126.3(3) . 2_765 ? Er1 O1W H1W 126.6 . . ? Er1 O1W H2W 115.8 . . ? H1W O1W H2W 102.3 . . ? H3W O2W H4W 108.9 . . ? H5W O3W H6W 115.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.525 _refine_diff_density_min -2.449 _refine_diff_density_rms 0.131 data_6 #TrackingRef '- combined_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 826770' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H5 N2 O7 Yb, 1.14(H2 O), 0.32(O), 0.65(H)' _chemical_formula_sum 'C6 H7.93 N2 O8.46 Yb' _chemical_formula_weight 416.47 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 trigonal _symmetry_space_group_name_H-M 'R 3 2' _symmetry_space_group_name_Hall 'R 3 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 12.2284(16) _cell_length_b 12.2284(16) _cell_length_c 19.605(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2538.9(8) _cell_formula_units_Z 9 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3639 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760.2 _exptl_absorpt_coefficient_mu 8.326 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2121 _exptl_absorpt_correction_T_max 0.7318 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 4619 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1122 _reflns_number_gt 1115 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2 (Bruker, 2004)' _computing_data_reduction 'APEX2 (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2009)' _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^)+(0.0218P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(17) _refine_ls_number_reflns 1122 _refine_ls_number_parameters 89 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0195 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0454 _refine_ls_wR_factor_gt 0.0454 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 C1 C 0.8899(6) 0.7767(4) 0.7797(2) 0.0168(9) Uani 1 1 d . . . C2 C 0.9195(5) 0.7194(4) 0.7195(3) 0.0151(13) Uani 1 1 d . . . C3 C 0.8323(7) 0.6667 0.6667 0.022(2) Uani 1 2 d S . . H3 H 0.7563 0.6667 0.6667 0.026 Uiso 1 2 calc SR . . C4 C 1.0563(6) 0.6667 0.6667 0.0107(14) Uani 1 2 d S . . N1 N 1.0287(3) 0.7205(4) 0.7212(2) 0.0118(8) Uani 1 1 d . . . O1 O 0.7980(3) 0.7932(4) 0.7748(2) 0.0274(10) Uani 1 1 d . . . O2 O 0.9606(4) 0.8017(4) 0.83140(18) 0.0217(9) Uani 1 1 d . . . O3 O 1.1593(5) 0.6667 0.6667 0.0190(12) Uani 1 2 d S . . O1W O 0.7907(3) 0.8218(3) 0.91434(18) 0.0174(8) Uani 1 1 d . . . H1W H 0.8631 0.8358 0.9090 0.026 Uiso 1 1 d R . . H2W H 0.7951 0.8551 0.9514 0.026 Uiso 1 1 d R . . O2W O 0.7339(17) 0.5371(14) 0.8956(12) 0.204(15) Uani 0.57(3) 1 d P . . H3W H 0.7753 0.6140 0.8857 0.306 Uiso 0.57(3) 1 d PR . . H4W H 0.7364 0.4964 0.8634 0.306 Uiso 0.57(3) 1 d PR . . O3W O 0.6667 0.3333 0.9832(14) 0.113(12) Uani 0.48(3) 3 d SP . . H5W H 0.6491 0.3845 0.9606 0.169 Uiso 0.162(10) 1 d PR . . H6W H 0.6061 0.2605 0.9877 0.169 Uiso 0.162(10) 1 d PR . . Yb1 Yb 0.6667 0.84306(3) 0.8333 0.00761(9) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.015(3) 0.023(2) 0.016(2) -0.0031(18) 0.001(2) 0.011(2) C2 0.014(2) 0.024(4) 0.012(3) -0.0008(18) 0.0007(19) 0.013(2) C3 0.014(2) 0.041(5) 0.020(4) -0.016(3) -0.0080(13) 0.020(3) C4 0.008(3) 0.013(3) 0.013(3) -0.004(2) -0.0019(12) 0.0066(15) N1 0.0096(18) 0.015(2) 0.013(2) -0.0035(16) -0.0014(15) 0.0078(16) O1 0.021(2) 0.054(3) 0.023(2) -0.0168(18) -0.0089(16) 0.030(2) O2 0.018(2) 0.040(2) 0.015(2) -0.0117(16) -0.0088(15) 0.0207(18) O3 0.014(2) 0.027(3) 0.020(3) -0.010(2) -0.0049(11) 0.0134(14) O1W 0.0168(18) 0.030(2) 0.0115(18) -0.0017(15) -0.0020(14) 0.0162(16) O2W 0.13(2) 0.110(14) 0.35(3) 0.065(16) 0.043(18) 0.045(12) O3W 0.088(13) 0.088(13) 0.16(3) 0.000 0.000 0.044(6) Yb1 0.00541(15) 0.00689(11) 0.01005(15) -0.00006(4) -0.00012(9) 0.00271(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.242(7) . ? C1 O2 1.266(6) . ? C1 C2 1.508(7) . ? C1 Yb1 3.197(6) 2_765 ? C2 N1 1.329(6) . ? C2 C3 1.392(7) . ? C3 C2 1.392(7) 11_566 ? C3 H3 0.9300 . ? C4 O3 1.260(10) . ? C4 N1 1.384(5) . ? C4 N1 1.384(5) 11_566 ? N1 Yb1 2.627(4) 2_765 ? O1 Yb1 2.291(3) . ? O2 Yb1 2.279(4) 2_765 ? O1W Yb1 2.299(3) . ? O1W H1W 0.8194 . ? O1W H2W 0.8221 . ? O2W H3W 0.8386 . ? O2W H4W 0.8133 . ? O3W H5W 0.8768 . ? O3W H6W 0.8307 . ? Yb1 O2 2.279(4) 17_566 ? Yb1 O2 2.279(4) 3_675 ? Yb1 O1 2.291(3) 18_656 ? Yb1 O1W 2.299(3) 18_656 ? Yb1 N1 2.627(4) 17_566 ? Yb1 N1 2.627(4) 3_675 ? Yb1 C1 3.197(6) 17_566 ? Yb1 C1 3.197(6) 3_675 ? Yb1 H2W 2.7599 . ? 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 C1 O2 126.0(4) . . ? O1 C1 C2 117.5(4) . . ? O2 C1 C2 116.5(5) . . ? O1 C1 Yb1 157.4(3) . 2_765 ? O2 C1 Yb1 35.0(3) . 2_765 ? C2 C1 Yb1 83.1(3) . 2_765 ? N1 C2 C3 123.9(5) . . ? N1 C2 C1 116.6(5) . . ? C3 C2 C1 119.5(5) . . ? C2 C3 C2 115.4(7) 11_566 . ? C2 C3 H3 122.3 11_566 . ? C2 C3 H3 122.3 . . ? O3 C4 N1 118.8(3) . . ? O3 C4 N1 118.8(3) . 11_566 ? N1 C4 N1 122.4(6) . 11_566 ? C2 N1 C4 117.2(5) . . ? C2 N1 Yb1 112.5(3) . 2_765 ? C4 N1 Yb1 130.3(4) . 2_765 ? C1 O1 Yb1 144.7(3) . . ? C1 O2 Yb1 126.4(3) . 2_765 ? Yb1 O1W H1W 126.4 . . ? Yb1 O1W H2W 116.0 . . ? H1W O1W H2W 102.3 . . ? H3W O2W H4W 108.6 . . ? H5W O3W H6W 114.4 . . ? O2 Yb1 O2 108.4(2) 17_566 3_675 ? O2 Yb1 O1 149.48(12) 17_566 . ? O2 Yb1 O1 81.97(15) 3_675 . ? O2 Yb1 O1 81.98(15) 17_566 18_656 ? O2 Yb1 O1 149.48(12) 3_675 18_656 ? O1 Yb1 O1 103.9(2) . 18_656 ? O2 Yb1 O1W 78.90(13) 17_566 18_656 ? O2 Yb1 O1W 135.31(13) 3_675 18_656 ? O1 Yb1 O1W 74.19(13) . 18_656 ? O1 Yb1 O1W 74.11(13) 18_656 18_656 ? O2 Yb1 O1W 135.31(13) 17_566 . ? O2 Yb1 O1W 78.90(13) 3_675 . ? O1 Yb1 O1W 74.11(13) . . ? O1 Yb1 O1W 74.20(13) 18_656 . ? O1W Yb1 O1W 127.43(18) 18_656 . ? O2 Yb1 N1 65.72(12) 17_566 17_566 ? O2 Yb1 N1 77.35(13) 3_675 17_566 ? O1 Yb1 N1 144.37(12) . 17_566 ? O1 Yb1 N1 81.45(14) 18_656 17_566 ? O1W Yb1 N1 139.33(13) 18_656 17_566 ? O1W Yb1 N1 73.64(12) . 17_566 ? O2 Yb1 N1 77.34(13) 17_566 3_675 ? O2 Yb1 N1 65.72(12) 3_675 3_675 ? O1 Yb1 N1 81.45(14) . 3_675 ? O1 Yb1 N1 144.37(13) 18_656 3_675 ? O1W Yb1 N1 73.64(12) 18_656 3_675 ? O1W Yb1 N1 139.33(13) . 3_675 ? N1 Yb1 N1 114.84(17) 17_566 3_675 ? O2 Yb1 C1 18.57(11) 17_566 17_566 ? O2 Yb1 C1 104.19(13) 3_675 17_566 ? O1 Yb1 C1 167.83(12) . 17_566 ? O1 Yb1 C1 76.28(14) 18_656 17_566 ? O1W Yb1 C1 94.37(12) 18_656 17_566 ? O1W Yb1 C1 117.10(12) . 17_566 ? N1 Yb1 C1 47.78(11) 17_566 17_566 ? N1 Yb1 C1 91.46(12) 3_675 17_566 ? O2 Yb1 C1 104.19(13) 17_566 3_675 ? O2 Yb1 C1 18.57(11) 3_675 3_675 ? O1 Yb1 C1 76.28(14) . 3_675 ? O1 Yb1 C1 167.83(12) 18_656 3_675 ? O1W Yb1 C1 117.10(12) 18_656 3_675 ? O1W Yb1 C1 94.37(12) . 3_675 ? N1 Yb1 C1 91.46(12) 17_566 3_675 ? N1 Yb1 C1 47.78(11) 3_675 3_675 ? C1 Yb1 C1 106.21(16) 17_566 3_675 ? O2 Yb1 H2W 121.4 17_566 . ? O2 Yb1 H2W 75.5 3_675 . ? O1 Yb1 H2W 88.8 . . ? O1 Yb1 H2W 74.7 18_656 . ? O1W Yb1 H2W 139.4 18_656 . ? O1W Yb1 H2W 15.5 . . ? N1 Yb1 H2W 58.2 17_566 . ? N1 Yb1 H2W 140.9 3_675 . ? C1 Yb1 H2W 102.8 17_566 . ? C1 Yb1 H2W 93.2 3_675 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.103 _refine_diff_density_min -1.903 _refine_diff_density_rms 0.148 data_2a #TrackingRef '- combined_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 838099' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H5 Gd N2 O7, 1.1(H2 O), 0.37(O), 0.74(H)' _chemical_formula_sum 'C6 H7.94 Gd N2 O8.47' _chemical_formula_weight 400.39 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 trigonal _symmetry_space_group_name_H-M 'R 3 2' _symmetry_space_group_name_Hall 'R 3 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 12.4387(9) _cell_length_b 12.4387(9) _cell_length_c 19.6706(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2635.7(3) _cell_formula_units_Z 9 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3919 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 27.94 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1707 _exptl_absorpt_coefficient_mu 5.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3300 _exptl_absorpt_correction_T_max 0.8041 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 4851 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1165 _reflns_number_gt 1151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2 (Bruker, 2004)' _computing_data_reduction 'APEX2 (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2009)' _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^)+(0.0368P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 1165 _refine_ls_number_parameters 89 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0616 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 C1 C 0.8888(6) 0.7753(5) 0.7791(2) 0.0240(12) Uani 1 1 d . . . C2 C 0.9174(5) 0.7184(5) 0.7190(3) 0.0232(16) Uani 1 1 d . . . C3 C 0.8325(8) 0.6667 0.6667 0.032(3) Uani 1 2 d S . . H3 H 0.7577 0.6667 0.6667 0.038 Uiso 1 2 calc SR . . C4 C 1.0526(8) 0.6667 0.6667 0.0181(17) Uani 1 2 d S . . Gd1 Gd 0.6667 0.84491(3) 0.8333 0.01116(12) Uani 1 2 d S . . N1 N 1.0250(4) 0.7200(4) 0.7204(2) 0.0186(10) Uani 1 1 d . . . O1 O 0.7960(5) 0.7893(6) 0.7740(2) 0.0379(13) Uani 1 1 d . . . O2 O 0.9566(4) 0.8013(5) 0.8301(2) 0.0340(12) Uani 1 1 d . . . O3 O 1.1531(5) 0.6667 0.6667 0.0255(14) Uani 1 2 d S . . O1W O 0.7946(4) 0.8257(4) 0.9163(2) 0.0233(9) Uani 1 1 d . . . H1W H 0.8670 0.8397 0.9110 0.035 Uiso 1 1 d R . . H2W H 0.7990 0.8590 0.9534 0.035 Uiso 1 1 d R . . O2W O 0.7362(18) 0.5421(19) 0.8973(13) 0.194(17) Uani 0.55(3) 1 d P . . H3W H 0.7776 0.6190 0.8874 0.291 Uiso 0.55(3) 1 d PR . . H4W H 0.7387 0.5014 0.8651 0.291 Uiso 0.55(3) 1 d PR . . O3W O 0.6667 0.3333 0.9797(16) 0.127(14) Uani 0.55(4) 3 d SP . . H5W H 0.6491 0.3845 0.9609 0.190 Uiso 0.184(12) 1 d PR . . H6W H 0.6061 0.2605 0.9881 0.190 Uiso 0.184(12) 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.021(3) 0.036(3) 0.021(2) -0.012(2) -0.009(3) 0.019(3) C2 0.019(3) 0.032(4) 0.025(3) -0.006(2) -0.002(2) 0.017(3) C3 0.023(3) 0.055(7) 0.028(4) -0.022(3) -0.0109(16) 0.028(4) C4 0.020(4) 0.023(4) 0.013(3) -0.007(3) -0.0035(14) 0.0113(19) Gd1 0.0092(2) 0.01054(15) 0.01328(18) -0.00007(6) -0.00014(12) 0.00462(10) N1 0.013(2) 0.025(2) 0.020(2) -0.0058(19) -0.0036(18) 0.011(2) O1 0.030(3) 0.074(4) 0.030(2) -0.023(2) -0.011(2) 0.041(3) O2 0.023(2) 0.064(3) 0.025(2) -0.023(2) -0.0105(18) 0.029(2) O3 0.017(2) 0.039(4) 0.028(3) -0.016(3) -0.0078(13) 0.0194(18) O1W 0.019(2) 0.037(2) 0.0211(19) -0.0070(18) -0.0057(16) 0.0197(19) O2W 0.100(19) 0.14(2) 0.32(4) 0.11(2) 0.047(19) 0.043(14) O3W 0.094(14) 0.094(14) 0.19(3) 0.000 0.000 0.047(7) _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 C1 O2 1.246(7) . ? C1 O1 1.254(8) . ? C1 C2 1.509(8) . ? C2 N1 1.329(7) . ? C2 C3 1.381(8) . ? C3 C2 1.381(8) 11_566 ? C3 H3 0.9300 . ? C4 O3 1.251(13) . ? C4 N1 1.379(7) . ? C4 N1 1.379(7) 11_566 ? Gd1 O2 2.352(5) 17_566 ? Gd1 O2 2.352(5) 3_675 ? Gd1 O1 2.354(4) 18_656 ? Gd1 O1 2.354(4) . ? Gd1 O1W 2.373(4) . ? Gd1 O1W 2.373(4) 18_656 ? Gd1 N1 2.666(4) 17_566 ? Gd1 N1 2.666(4) 3_675 ? N1 Gd1 2.666(4) 2_765 ? O2 Gd1 2.352(5) 2_765 ? O1W H1W 0.8333 . ? O1W H2W 0.8274 . ? O2W H3W 0.8524 . ? O2W H4W 0.8206 . ? O3W H5W 0.8531 . ? O3W H6W 0.8562 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 125.4(5) . . ? O2 C1 C2 117.7(6) . . ? O1 C1 C2 116.9(5) . . ? N1 C2 C3 123.5(6) . . ? N1 C2 C1 116.7(5) . . ? C3 C2 C1 119.8(6) . . ? C2 C3 C2 115.8(8) 11_566 . ? C2 C3 H3 122.1 11_566 . ? C2 C3 H3 122.1 . . ? O3 C4 N1 119.3(4) . . ? O3 C4 N1 119.3(4) . 11_566 ? N1 C4 N1 121.4(8) . 11_566 ? O2 Gd1 O2 109.3(3) 17_566 3_675 ? O2 Gd1 O1 82.7(2) 17_566 18_656 ? O2 Gd1 O1 149.71(14) 3_675 18_656 ? O2 Gd1 O1 149.71(14) 17_566 . ? O2 Gd1 O1 82.7(2) 3_675 . ? O1 Gd1 O1 101.1(3) 18_656 . ? O2 Gd1 O1W 135.01(14) 17_566 . ? O2 Gd1 O1W 78.33(15) 3_675 . ? O1 Gd1 O1W 74.07(15) 18_656 . ? O1 Gd1 O1W 73.75(14) . . ? O2 Gd1 O1W 78.33(15) 17_566 18_656 ? O2 Gd1 O1W 135.00(14) 3_675 18_656 ? O1 Gd1 O1W 73.75(14) 18_656 18_656 ? O1 Gd1 O1W 74.06(16) . 18_656 ? O1W Gd1 O1W 128.3(2) . 18_656 ? O2 Gd1 N1 64.61(14) 17_566 17_566 ? O2 Gd1 N1 78.64(16) 3_675 17_566 ? O1 Gd1 N1 82.10(17) 18_656 17_566 ? O1 Gd1 N1 145.57(14) . 17_566 ? O1W Gd1 N1 74.30(14) . 17_566 ? O1W Gd1 N1 137.91(15) 18_656 17_566 ? O2 Gd1 N1 78.64(16) 17_566 3_675 ? O2 Gd1 N1 64.61(14) 3_675 3_675 ? O1 Gd1 N1 145.57(14) 18_656 3_675 ? O1 Gd1 N1 82.09(17) . 3_675 ? O1W Gd1 N1 137.91(15) . 3_675 ? O1W Gd1 N1 74.30(14) 18_656 3_675 ? N1 Gd1 N1 114.5(2) 17_566 3_675 ? C2 N1 C4 117.9(5) . . ? C2 N1 Gd1 113.1(4) . 2_765 ? C4 N1 Gd1 129.0(4) . 2_765 ? C1 O1 Gd1 144.3(4) . . ? C1 O2 Gd1 126.0(4) . 2_765 ? Gd1 O1W H1W 127.0 . . ? Gd1 O1W H2W 115.8 . . ? H1W O1W H2W 102.2 . . ? H3W O2W H4W 109.1 . . ? H5W O3W H6W 117.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.074 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.154