# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_complex1 _database_code_depnum_ccdc_archive 'CCDC 861207' #TrackingRef 'complex861207.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H17 Eu N2 O9' _chemical_formula_sum 'C14 H17 Eu N2 O9' _chemical_formula_weight 509.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6579(16) _cell_length_b 10.1549(18) _cell_length_c 10.6914(16) _cell_angle_alpha 106.576(2) _cell_angle_beta 107.444(3) _cell_angle_gamma 110.660(4) _cell_volume 841.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293.1500 _cell_measurement_reflns_used 2763 _cell_measurement_theta_min 2.2211 _cell_measurement_theta_max 27.4835 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 3.780 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6223 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293.1500 _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 'Scxmini CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5398 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2908 _reflns_number_gt 2806 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0378P)^2^+0.0372P] 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 2908 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 -0.164999(19) 0.060598(19) 0.885460(16) 0.02072(10) Uani 1 1 d . . . O1 O 0.1571(4) 0.0710(4) 0.3173(3) 0.0490(9) Uani 1 1 d . . . N1 N 0.2578(4) 0.3722(4) 0.9321(4) 0.0294(8) Uani 1 1 d . . . C1 C 0.1354(5) 0.1510(5) 0.4136(4) 0.0317(10) Uani 1 1 d . . . N2 N 0.6791(5) 0.2979(5) 0.4972(5) 0.0550(12) Uani 1 1 d . . . O2 O 0.0547(5) 0.2206(5) 0.3940(4) 0.0563(10) Uani 1 1 d . . . C2 C 0.5436(5) 0.0900(5) 0.7854(4) 0.0247(9) Uani 1 1 d . . . O3 O 0.5682(3) 0.0079(3) 0.6879(3) 0.0292(6) Uani 1 1 d . . . C3 C 0.2220(5) 0.1720(5) 0.5670(4) 0.0277(9) Uani 1 1 d . . . O4 O 0.6307(4) 0.1325(4) 0.9170(3) 0.0368(7) Uani 1 1 d . . . C4 C 0.3310(5) 0.1116(5) 0.5980(4) 0.0287(9) Uani 1 1 d . . . H4 H 0.3472 0.0525 0.5225 0.034 Uiso 1 1 calc R . . O5 O -0.0659(4) 0.4568(4) 0.7703(4) 0.0534(10) Uani 1 1 d . . . C5 C 0.4160(5) 0.1400(5) 0.7429(4) 0.0250(8) Uani 1 1 d . . . O6 O -0.0770(4) 0.2821(4) 0.8538(4) 0.0482(9) Uani 1 1 d . . . C6 C 0.3898(5) 0.2241(4) 0.8519(4) 0.0257(8) Uani 1 1 d . . . H6 H 0.4470 0.2406 0.9490 0.031 Uiso 1 1 calc R . . O7 O 0.1236(3) 0.1127(3) 0.9920(3) 0.0279(6) Uani 1 1 d . . . C7 C 0.2811(5) 0.2855(4) 0.8228(4) 0.0249(8) Uani 1 1 d . . . O8 O 0.3659(3) 0.2040(3) 1.1707(3) 0.0393(8) Uani 1 1 d . . . C8 C 0.1976(5) 0.2567(5) 0.6767(4) 0.0282(9) Uani 1 1 d . . . H8 H 0.1229 0.2966 0.6534 0.034 Uiso 1 1 calc R . . O9 O -0.0480(4) 0.2294(4) 1.1388(3) 0.0414(8) Uani 1 1 d . . . C9 C 0.1895(5) 0.4758(5) 0.9112(4) 0.0296(9) Uani 1 1 d . . . H9A H 0.2312 0.5223 0.8517 0.036 Uiso 1 1 calc R . . H9B H 0.2318 0.5625 1.0076 0.036 Uiso 1 1 calc R . . C10 C 0.0000(5) 0.3982(5) 0.8374(4) 0.0303(9) Uani 1 1 d . . . C11 C 0.3264(5) 0.3804(5) 1.0765(4) 0.0266(9) Uani 1 1 d . . . H11A H 0.2959 0.4448 1.1401 0.032 Uiso 1 1 calc R . . H11B H 0.4485 0.4339 1.1177 0.032 Uiso 1 1 calc R . . C12 C 0.2691(5) 0.2230(5) 1.0792(4) 0.0237(9) Uani 1 1 d . . . C13 C 0.6037(7) 0.3998(7) 0.5198(6) 0.0613(15) Uani 1 1 d . . . H13A H 0.6893 0.5096 0.5657 0.092 Uiso 1 1 calc R . . H13B H 0.5512 0.3819 0.5832 0.092 Uiso 1 1 calc R . . H13C H 0.5202 0.3761 0.4255 0.092 Uiso 1 1 calc R . . C14 C 0.7648(8) 0.3186(8) 0.4064(8) 0.091(2) Uani 1 1 d . . . H14A H 0.6842 0.2844 0.3069 0.136 Uiso 1 1 calc R . . H14B H 0.8222 0.2559 0.4047 0.136 Uiso 1 1 calc R . . H14C H 0.8454 0.4293 0.4469 0.136 Uiso 1 1 calc R . . H9D H -0.0170 0.3297 1.1741 0.070(19) Uiso 1 1 d R . . H9C H -0.0276 0.2109 1.2138 0.074(19) Uiso 1 1 d R . . H1 H 0.6042 0.1987 0.4520 0.15(3) Uiso 1 1 d R . . H13 H 0.7370 0.3137 0.5858 0.063(18) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02087(14) 0.02661(15) 0.01871(14) 0.01190(10) 0.00719(10) 0.01522(11) O1 0.055(2) 0.081(3) 0.0217(16) 0.0170(16) 0.0156(15) 0.049(2) N1 0.0383(19) 0.0366(19) 0.0249(18) 0.0151(15) 0.0167(16) 0.0260(16) C1 0.030(2) 0.050(3) 0.026(2) 0.024(2) 0.0129(18) 0.025(2) N2 0.042(2) 0.048(3) 0.047(3) 0.007(2) 0.005(2) 0.017(2) O2 0.083(3) 0.092(3) 0.0328(19) 0.036(2) 0.0278(19) 0.073(3) C2 0.0208(19) 0.033(2) 0.025(2) 0.0132(18) 0.0120(17) 0.0156(17) O3 0.0287(14) 0.0356(16) 0.0258(14) 0.0091(12) 0.0100(12) 0.0231(13) C3 0.032(2) 0.037(2) 0.023(2) 0.0173(18) 0.0140(18) 0.0199(19) O4 0.0350(16) 0.057(2) 0.0255(16) 0.0157(14) 0.0112(13) 0.0324(15) C4 0.035(2) 0.038(2) 0.022(2) 0.0125(18) 0.0151(18) 0.0245(19) O5 0.052(2) 0.0374(19) 0.051(2) 0.0222(17) -0.0030(17) 0.0213(16) C5 0.0228(19) 0.030(2) 0.026(2) 0.0141(17) 0.0097(16) 0.0151(16) O6 0.0359(17) 0.044(2) 0.078(3) 0.0416(19) 0.0254(18) 0.0199(15) C6 0.0213(18) 0.035(2) 0.023(2) 0.0144(17) 0.0081(16) 0.0147(17) O7 0.0218(14) 0.0281(15) 0.0313(15) 0.0165(13) 0.0075(12) 0.0103(12) C7 0.026(2) 0.027(2) 0.025(2) 0.0137(17) 0.0137(16) 0.0138(16) O8 0.0292(15) 0.0376(17) 0.0374(17) 0.0232(14) -0.0010(13) 0.0101(13) C8 0.028(2) 0.037(2) 0.028(2) 0.0192(19) 0.0119(17) 0.0215(18) O9 0.065(2) 0.0375(19) 0.0213(15) 0.0118(14) 0.0102(15) 0.0324(16) C9 0.033(2) 0.027(2) 0.033(2) 0.0137(18) 0.0147(18) 0.0190(18) C10 0.039(2) 0.028(2) 0.027(2) 0.0128(18) 0.0143(19) 0.0191(19) C11 0.028(2) 0.025(2) 0.023(2) 0.0074(17) 0.0098(17) 0.0113(17) C12 0.0215(19) 0.032(2) 0.0198(19) 0.0124(17) 0.0104(16) 0.0137(17) C13 0.054(3) 0.060(4) 0.053(3) 0.013(3) 0.011(3) 0.031(3) C14 0.054(4) 0.098(6) 0.099(6) 0.023(5) 0.039(4) 0.027(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 Eu1 O1 2.239(3) 2_556 ? Eu1 O6 2.270(3) . ? Eu1 O9 2.388(3) . ? Eu1 O4 2.411(3) 1_455 ? Eu1 O8 2.459(3) 2_557 ? Eu1 O7 2.461(3) . ? Eu1 O7 2.544(3) 2_557 ? Eu1 O3 2.551(3) 1_455 ? Eu1 C2 2.850(4) 1_455 ? Eu1 C12 2.873(4) 2_557 ? Eu1 Eu1 4.1807(5) 2_557 ? O1 C1 1.239(5) . ? O1 Eu1 2.239(3) 2_556 ? N1 C7 1.379(5) . ? N1 C11 1.450(5) . ? N1 C9 1.459(5) . ? C1 O2 1.235(5) . ? C1 C3 1.513(5) . ? N2 C14 1.465(8) . ? N2 C13 1.468(7) . ? N2 H1 0.8778 . ? N2 H13 0.8769 . ? C2 O4 1.249(5) . ? C2 O3 1.277(5) . ? C2 C5 1.490(6) . ? C2 Eu1 2.850(4) 1_655 ? O3 Eu1 2.551(3) 1_655 ? C3 C8 1.380(6) . ? C3 C4 1.399(6) . ? O4 Eu1 2.411(3) 1_655 ? C4 C5 1.404(5) . ? C4 H4 0.9500 . ? O5 C10 1.229(5) . ? C5 C6 1.382(5) . ? O6 C10 1.246(5) . ? C6 C7 1.403(6) . ? C6 H6 0.9500 . ? O7 C12 1.268(5) . ? O7 Eu1 2.544(3) 2_557 ? C7 C8 1.412(5) . ? O8 C12 1.248(5) . ? O8 Eu1 2.459(3) 2_557 ? C8 H8 0.9500 . ? O9 H9D 0.8765 . ? O9 H9C 0.8563 . ? C9 C10 1.534(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.507(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 Eu1 2.873(4) 2_557 ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? 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 O6 90.51(14) 2_556 . ? O1 Eu1 O9 154.54(13) 2_556 . ? O6 Eu1 O9 86.40(12) . . ? O1 Eu1 O4 130.67(11) 2_556 1_455 ? O6 Eu1 O4 81.95(12) . 1_455 ? O9 Eu1 O4 73.90(11) . 1_455 ? O1 Eu1 O8 82.02(12) 2_556 2_557 ? O6 Eu1 O8 155.05(11) . 2_557 ? O9 Eu1 O8 110.24(11) . 2_557 ? O4 Eu1 O8 84.99(11) 1_455 2_557 ? O1 Eu1 O7 80.76(11) 2_556 . ? O6 Eu1 O7 88.81(10) . . ? O9 Eu1 O7 73.91(11) . . ? O4 Eu1 O7 146.96(10) 1_455 . ? O8 Eu1 O7 113.17(9) 2_557 . ? O1 Eu1 O7 95.86(11) 2_556 2_557 ? O6 Eu1 O7 153.20(11) . 2_557 ? O9 Eu1 O7 76.71(10) . 2_557 ? O4 Eu1 O7 112.32(10) 1_455 2_557 ? O8 Eu1 O7 51.71(9) 2_557 2_557 ? O7 Eu1 O7 66.72(10) . 2_557 ? O1 Eu1 O3 78.55(10) 2_556 1_455 ? O6 Eu1 O3 78.98(11) . 1_455 ? O9 Eu1 O3 125.34(10) . 1_455 ? O4 Eu1 O3 52.13(9) 1_455 1_455 ? O8 Eu1 O3 76.22(9) 2_557 1_455 ? O7 Eu1 O3 155.79(9) . 1_455 ? O7 Eu1 O3 127.79(9) 2_557 1_455 ? O1 Eu1 C2 105.06(12) 2_556 1_455 ? O6 Eu1 C2 76.71(12) . 1_455 ? O9 Eu1 C2 98.81(12) . 1_455 ? O4 Eu1 C2 25.78(10) 1_455 1_455 ? O8 Eu1 C2 82.29(11) 2_557 1_455 ? O7 Eu1 C2 164.31(11) . 1_455 ? O7 Eu1 C2 125.94(10) 2_557 1_455 ? O3 Eu1 C2 26.61(10) 1_455 1_455 ? O1 Eu1 C12 87.69(12) 2_556 2_557 ? O6 Eu1 C12 177.85(11) . 2_557 ? O9 Eu1 C12 94.72(11) . 2_557 ? O4 Eu1 C12 100.12(11) 1_455 2_557 ? O8 Eu1 C12 25.58(10) 2_557 2_557 ? O7 Eu1 C12 89.74(10) . 2_557 ? O7 Eu1 C12 26.17(10) 2_557 2_557 ? O3 Eu1 C12 101.80(10) 1_455 2_557 ? C2 Eu1 C12 104.89(11) 1_455 2_557 ? O1 Eu1 Eu1 88.14(8) 2_556 2_557 ? O6 Eu1 Eu1 122.07(8) . 2_557 ? O9 Eu1 Eu1 72.36(8) . 2_557 ? O4 Eu1 Eu1 136.44(7) 1_455 2_557 ? O8 Eu1 Eu1 81.64(7) 2_557 2_557 ? O7 Eu1 Eu1 33.98(6) . 2_557 ? O7 Eu1 Eu1 32.74(6) 2_557 2_557 ? O3 Eu1 Eu1 155.48(6) 1_455 2_557 ? C2 Eu1 Eu1 157.51(8) 1_455 2_557 ? C12 Eu1 Eu1 56.72(8) 2_557 2_557 ? C1 O1 Eu1 168.6(3) . 2_556 ? C7 N1 C11 119.5(3) . . ? C7 N1 C9 120.5(3) . . ? C11 N1 C9 119.2(3) . . ? O2 C1 O1 124.5(4) . . ? O2 C1 C3 117.9(4) . . ? O1 C1 C3 117.5(4) . . ? C14 N2 C13 113.8(5) . . ? C14 N2 H1 105.1 . . ? C13 N2 H1 111.3 . . ? C14 N2 H13 117.6 . . ? C13 N2 H13 103.5 . . ? H1 N2 H13 105.2 . . ? O4 C2 O3 119.7(4) . . ? O4 C2 C5 120.1(4) . . ? O3 C2 C5 120.2(4) . . ? O4 C2 Eu1 57.1(2) . 1_655 ? O3 C2 Eu1 63.5(2) . 1_655 ? C5 C2 Eu1 168.0(3) . 1_655 ? C2 O3 Eu1 89.9(2) . 1_655 ? C8 C3 C4 120.5(4) . . ? C8 C3 C1 119.3(4) . . ? C4 C3 C1 120.1(4) . . ? C2 O4 Eu1 97.1(2) . 1_655 ? C3 C4 C5 118.8(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 120.3(4) . . ? C6 C5 C2 118.1(3) . . ? C4 C5 C2 121.5(4) . . ? C10 O6 Eu1 166.2(3) . . ? C5 C6 C7 121.7(4) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C12 O7 Eu1 141.5(3) . . ? C12 O7 Eu1 91.6(2) . 2_557 ? Eu1 O7 Eu1 113.28(10) . 2_557 ? N1 C7 C6 121.6(3) . . ? N1 C7 C8 121.2(4) . . ? C6 C7 C8 117.2(4) . . ? C12 O8 Eu1 96.1(2) . 2_557 ? C3 C8 C7 121.5(4) . . ? C3 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? Eu1 O9 H9D 124.2 . . ? Eu1 O9 H9C 131.3 . . ? H9D O9 H9C 104.5 . . ? N1 C9 C10 115.3(3) . . ? N1 C9 H9A 108.4 . . ? C10 C9 H9A 108.4 . . ? N1 C9 H9B 108.4 . . ? C10 C9 H9B 108.4 . . ? H9A C9 H9B 107.5 . . ? O5 C10 O6 124.2(4) . . ? O5 C10 C9 118.4(4) . . ? O6 C10 C9 117.3(4) . . ? N1 C11 C12 114.0(3) . . ? N1 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? N1 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? O8 C12 O7 120.4(4) . . ? O8 C12 C11 119.0(3) . . ? O7 C12 C11 120.6(4) . . ? O8 C12 Eu1 58.3(2) . 2_557 ? O7 C12 Eu1 62.3(2) . 2_557 ? C11 C12 Eu1 174.1(3) . 2_557 ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.504 _refine_diff_density_min -1.300 _refine_diff_density_rms 0.126 data_complex2 _database_code_depnum_ccdc_archive 'CCDC 861208' #TrackingRef 'complex861208.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H17 N2 O9 Tb' _chemical_formula_sum 'C14 H17 N2 O9 Tb' _chemical_formula_weight 516.22 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.642(6) _cell_length_b 10.142(7) _cell_length_c 10.654(7) _cell_angle_alpha 106.388(6) _cell_angle_beta 107.720(5) _cell_angle_gamma 110.452(2) _cell_volume 837.1(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293.1500 _cell_measurement_reflns_used 1055 _cell_measurement_theta_min 2.5078 _cell_measurement_theta_max 27.4642 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 4.277 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5277 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293.1500 _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 'Scxmini CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6600 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3812 _reflns_number_gt 3433 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+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 3812 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Tb1 Tb 1.16364(3) 0.43928(2) 0.11371(2) 0.02141(9) Uani 1 1 d . . . O1 O 0.9459(6) 0.2792(6) 0.6077(4) 0.0549(13) Uani 1 1 d . . . N1 N 0.7403(5) 0.1272(5) 0.0666(4) 0.0280(9) Uani 1 1 d . . . C1 C 0.7188(6) 0.2157(5) 0.1790(5) 0.0246(10) Uani 1 1 d . . . O2 O 0.8418(5) 0.4283(5) 0.6841(4) 0.0454(11) Uani 1 1 d . . . N2 N 0.3228(7) 0.2054(6) 0.5019(6) 0.0514(14) Uani 1 1 d . . . C2 C 0.8005(6) 0.2418(6) 0.3231(5) 0.0286(11) Uani 1 1 d . . . H2 H 0.8739 0.2001 0.3463 0.034 Uiso 1 1 calc R . . O3 O 0.4297(4) 0.4915(4) 0.3120(4) 0.0305(8) Uani 1 1 d . . . C3 C 0.7765(6) 0.3277(6) 0.4335(5) 0.0270(10) Uani 1 1 d . . . O4 O 0.3663(5) 0.3674(5) 0.0814(4) 0.0360(9) Uani 1 1 d . . . C4 C 0.6677(6) 0.3881(6) 0.4010(5) 0.0289(11) Uani 1 1 d . . . H4 H 0.6514 0.4474 0.4764 0.035 Uiso 1 1 calc R . . O5 O 1.0751(5) 0.2207(5) 0.1456(5) 0.0489(11) Uani 1 1 d . . . C5 C 0.5839(6) 0.3608(6) 0.2579(5) 0.0266(10) Uani 1 1 d . . . O6 O 1.0680(5) 0.0450(5) 0.2274(5) 0.0516(12) Uani 1 1 d . . . C6 C 0.6083(6) 0.2751(6) 0.1464(5) 0.0262(10) Uani 1 1 d . . . H6 H 0.5498 0.2570 0.0485 0.031 Uiso 1 1 calc R . . O7 O 0.8787(4) 0.3914(4) 0.0114(4) 0.0277(7) Uani 1 1 d . . . C7 C 0.8635(6) 0.3476(6) 0.5865(5) 0.0298(11) Uani 1 1 d . . . O8 O 0.6353(5) 0.2995(5) -0.1705(4) 0.0424(10) Uani 1 1 d . . . C8 C 0.4541(6) 0.4105(6) 0.2143(5) 0.0267(10) Uani 1 1 d . . . O9 O 1.0443(5) 0.2687(4) -0.1378(4) 0.0377(9) Uani 1 1 d . . . C9 C 0.8111(6) 0.0261(6) 0.0889(6) 0.0294(11) Uani 1 1 d . . . H9A H 0.7692 -0.0608 -0.0073 0.035 Uiso 1 1 calc R . . H9B H 0.7712 -0.0199 0.1496 0.035 Uiso 1 1 calc R . . C10 C 0.9991(6) 0.1049(5) 0.1617(5) 0.0270(10) Uani 1 1 d . . . C11 C 0.6746(6) 0.1205(5) -0.0768(5) 0.0253(10) Uani 1 1 d . . . H11A H 0.5522 0.0657 -0.1204 0.030 Uiso 1 1 calc R . . H11B H 0.7078 0.0579 -0.1392 0.030 Uiso 1 1 calc R . . C12 C 0.7315(6) 0.2801(6) -0.0787(5) 0.0240(10) Uani 1 1 d . . . C13 C 0.2383(10) 0.1832(11) 0.5951(11) 0.087(3) Uani 1 1 d . . . H13A H 0.3154 0.1949 0.6873 0.131 Uiso 1 1 calc R . . H13B H 0.1425 0.0784 0.5440 0.131 Uiso 1 1 calc R . . H13C H 0.2010 0.2617 0.6156 0.131 Uiso 1 1 calc R . . C14 C 0.3973(9) 0.1011(8) 0.4823(8) 0.0597(19) Uani 1 1 d . . . H14A H 0.4762 0.1218 0.5782 0.090 Uiso 1 1 calc R . . H14B H 0.4552 0.1203 0.4228 0.090 Uiso 1 1 calc R . . H14C H 0.3101 -0.0080 0.4329 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02233(13) 0.02651(13) 0.01705(13) 0.01027(9) 0.00552(10) 0.01551(10) O1 0.082(3) 0.088(4) 0.030(2) 0.032(2) 0.024(2) 0.071(3) N1 0.036(2) 0.037(2) 0.022(2) 0.0152(18) 0.015(2) 0.026(2) C1 0.023(2) 0.030(2) 0.022(2) 0.0112(19) 0.008(2) 0.016(2) O2 0.057(3) 0.072(3) 0.0205(19) 0.0164(19) 0.016(2) 0.050(3) N2 0.043(3) 0.042(3) 0.052(3) 0.008(3) 0.014(3) 0.019(2) C2 0.031(3) 0.039(3) 0.025(2) 0.016(2) 0.010(2) 0.025(2) O3 0.0306(19) 0.041(2) 0.0219(18) 0.0090(15) 0.0094(16) 0.0243(17) C3 0.030(3) 0.037(3) 0.018(2) 0.014(2) 0.008(2) 0.021(2) O4 0.034(2) 0.052(2) 0.0211(18) 0.0097(16) 0.0061(17) 0.0309(19) C4 0.034(3) 0.040(3) 0.020(2) 0.012(2) 0.013(2) 0.024(2) O5 0.034(2) 0.045(2) 0.069(3) 0.037(2) 0.016(2) 0.016(2) C5 0.023(2) 0.032(3) 0.026(2) 0.014(2) 0.008(2) 0.016(2) O6 0.047(3) 0.042(2) 0.051(3) 0.024(2) -0.003(2) 0.024(2) C6 0.021(2) 0.039(3) 0.021(2) 0.015(2) 0.007(2) 0.017(2) O7 0.0220(17) 0.0318(19) 0.0276(18) 0.0160(15) 0.0052(16) 0.0136(15) C7 0.030(3) 0.043(3) 0.020(2) 0.015(2) 0.010(2) 0.022(2) O8 0.032(2) 0.044(2) 0.037(2) 0.0244(19) -0.0025(19) 0.0135(18) C8 0.022(2) 0.031(3) 0.026(3) 0.012(2) 0.008(2) 0.015(2) O9 0.055(2) 0.036(2) 0.0176(17) 0.0094(15) 0.0060(18) 0.028(2) C9 0.033(3) 0.031(3) 0.030(3) 0.014(2) 0.013(2) 0.021(2) C10 0.032(3) 0.024(2) 0.025(2) 0.0093(19) 0.009(2) 0.017(2) C11 0.026(2) 0.027(2) 0.021(2) 0.0113(19) 0.009(2) 0.011(2) C12 0.024(2) 0.033(3) 0.018(2) 0.0098(19) 0.009(2) 0.017(2) C13 0.051(5) 0.092(7) 0.091(7) 0.016(5) 0.033(5) 0.025(5) C14 0.052(4) 0.058(4) 0.049(4) 0.011(3) 0.006(4) 0.031(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 Tb1 O2 2.221(4) 2_766 ? Tb1 O5 2.245(4) . ? Tb1 O9 2.369(4) . ? Tb1 O4 2.395(4) 1_655 ? Tb1 O7 2.433(4) . ? Tb1 O8 2.436(4) 2_765 ? Tb1 O7 2.519(3) 2_765 ? Tb1 O3 2.539(4) 1_655 ? Tb1 C8 2.828(5) 1_655 ? Tb1 C12 2.842(5) 2_765 ? O1 C7 1.237(6) . ? N1 C1 1.399(6) . ? N1 C11 1.437(6) . ? N1 C9 1.449(6) . ? C1 C2 1.392(7) . ? C1 C6 1.400(6) . ? O2 C7 1.251(6) . ? O2 Tb1 2.221(4) 2_766 ? N2 C14 1.475(8) . ? N2 C13 1.480(9) . ? C2 C3 1.387(7) . ? C2 H2 0.9500 . ? O3 C8 1.271(6) . ? O3 Tb1 2.539(4) 1_455 ? C3 C4 1.394(7) . ? C3 C7 1.505(7) . ? O4 C8 1.255(6) . ? O4 Tb1 2.395(4) 1_455 ? C4 C5 1.382(7) . ? C4 H4 0.9500 . ? O5 C10 1.239(6) . ? C5 C6 1.397(7) . ? C5 C8 1.501(6) . ? O6 C10 1.240(6) . ? C6 H6 0.9500 . ? O7 C12 1.284(6) . ? O7 Tb1 2.519(3) 2_765 ? O8 C12 1.240(6) . ? O8 Tb1 2.436(4) 2_765 ? C8 Tb1 2.828(5) 1_455 ? C9 C10 1.519(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.526(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 Tb1 2.842(5) 2_765 ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? 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 Tb1 O5 90.67(18) 2_766 . ? O2 Tb1 O9 154.49(16) 2_766 . ? O5 Tb1 O9 85.54(16) . . ? O2 Tb1 O4 130.69(13) 2_766 1_655 ? O5 Tb1 O4 82.60(15) . 1_655 ? O9 Tb1 O4 73.85(13) . 1_655 ? O2 Tb1 O7 80.22(14) 2_766 . ? O5 Tb1 O7 88.49(13) . . ? O9 Tb1 O7 74.47(13) . . ? O4 Tb1 O7 147.63(12) 1_655 . ? O2 Tb1 O8 81.53(16) 2_766 2_765 ? O5 Tb1 O8 154.84(15) . 2_765 ? O9 Tb1 O8 111.41(14) . 2_765 ? O4 Tb1 O8 84.51(15) 1_655 2_765 ? O7 Tb1 O8 113.40(12) . 2_765 ? O2 Tb1 O7 96.28(14) 2_766 2_765 ? O5 Tb1 O7 152.59(14) . 2_765 ? O9 Tb1 O7 76.81(13) . 2_765 ? O4 Tb1 O7 111.66(13) 1_655 2_765 ? O7 Tb1 O7 66.79(13) . 2_765 ? O8 Tb1 O7 52.54(12) 2_765 2_765 ? O2 Tb1 O3 78.10(13) 2_766 1_655 ? O5 Tb1 O3 79.34(14) . 1_655 ? O9 Tb1 O3 125.60(12) . 1_655 ? O4 Tb1 O3 52.62(12) 1_655 1_655 ? O7 Tb1 O3 154.92(12) . 1_655 ? O8 Tb1 O3 75.66(12) 2_765 1_655 ? O7 Tb1 O3 128.03(12) 2_765 1_655 ? O2 Tb1 C8 104.74(15) 2_766 1_655 ? O5 Tb1 C8 77.35(15) . 1_655 ? O9 Tb1 C8 99.03(14) . 1_655 ? O4 Tb1 C8 26.16(13) 1_655 1_655 ? O7 Tb1 C8 164.94(13) . 1_655 ? O8 Tb1 C8 81.56(14) 2_765 1_655 ? O7 Tb1 C8 125.69(13) 2_765 1_655 ? O3 Tb1 C8 26.70(12) 1_655 1_655 ? O2 Tb1 C12 87.39(15) 2_766 2_765 ? O5 Tb1 C12 177.73(14) . 2_765 ? O9 Tb1 C12 95.71(14) . 2_765 ? O4 Tb1 C12 99.57(14) 1_655 2_765 ? O7 Tb1 C12 90.02(12) . 2_765 ? O8 Tb1 C12 25.74(13) 2_765 2_765 ? O7 Tb1 C12 26.86(12) 2_765 2_765 ? O3 Tb1 C12 101.39(13) 1_655 2_765 ? C8 Tb1 C12 104.29(14) 1_655 2_765 ? C1 N1 C11 120.5(4) . . ? C1 N1 C9 120.0(4) . . ? C11 N1 C9 119.0(4) . . ? C2 C1 N1 121.5(4) . . ? C2 C1 C6 118.6(4) . . ? N1 C1 C6 119.9(4) . . ? C7 O2 Tb1 168.7(4) . 2_766 ? C14 N2 C13 111.1(6) . . ? C3 C2 C1 121.1(4) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C8 O3 Tb1 89.5(3) . 1_455 ? C2 C3 C4 120.1(4) . . ? C2 C3 C7 118.8(4) . . ? C4 C3 C7 121.0(4) . . ? C8 O4 Tb1 96.6(3) . 1_455 ? C5 C4 C3 119.3(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C10 O5 Tb1 167.0(4) . . ? C4 C5 C6 120.8(4) . . ? C4 C5 C8 121.6(4) . . ? C6 C5 C8 117.5(4) . . ? C5 C6 C1 120.1(4) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C12 O7 Tb1 140.7(3) . . ? C12 O7 Tb1 90.7(3) . 2_765 ? Tb1 O7 Tb1 113.21(13) . 2_765 ? O1 C7 O2 123.9(5) . . ? O1 C7 C3 118.8(4) . . ? O2 C7 C3 117.3(4) . . ? C12 O8 Tb1 95.7(3) . 2_765 ? O4 C8 O3 120.3(4) . . ? O4 C8 C5 119.9(4) . . ? O3 C8 C5 119.8(4) . . ? O4 C8 Tb1 57.3(2) . 1_455 ? O3 C8 Tb1 63.8(2) . 1_455 ? C5 C8 Tb1 168.2(3) . 1_455 ? N1 C9 C10 115.3(4) . . ? N1 C9 H9A 108.5 . . ? C10 C9 H9A 108.5 . . ? N1 C9 H9B 108.5 . . ? C10 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? O5 C10 O6 123.4(5) . . ? O5 C10 C9 118.2(4) . . ? O6 C10 C9 118.3(5) . . ? N1 C11 C12 114.1(4) . . ? N1 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? N1 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? O8 C12 O7 120.8(5) . . ? O8 C12 C11 119.1(4) . . ? O7 C12 C11 120.1(4) . . ? O8 C12 Tb1 58.6(3) . 2_765 ? O7 C12 Tb1 62.4(3) . 2_765 ? C11 C12 Tb1 173.4(3) . 2_765 ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.346 _refine_diff_density_min -1.751 _refine_diff_density_rms 0.158 # start Validation Reply Form _vrf_PLAT041_complex2 ; PROBLEM:Calc. and Reported SumFormula Strings Differ ? RESPONSE:The missing hydrogen atoms of coordination water molecule and free dimethylamine cation are calculated in the formula resulting in the difference. ; _vrf_PLAT042_complex2 ; PROBLEM:Calc. and Reported MoietyFormula Strings Differ RESPONSE:The missing hydrogen atoms of coordination water molecule and free dimethylamine cation are calculated in the formula resulting in the difference. ; _vrf_PLAT068_complex2 ; PROBLEM: Reported F000 Differs from Calcd (or Missing)... ? RESPONSE:The missing hydrogen atoms of coordination water molecule and free dimethylamine cation are calculated in the formula resulting in the difference. ; _vrf_FORMU01_complex2 ; PROBLEM: There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C14 H17 N2 O9 Tb1 Atom count from the _atom_site data: C14 H13 N2 O9 Tb1 RESPONSE:The missing hydrogen atoms of coordination water molecule and free dimethylamine cation are calculated in the formula resulting in the difference. ; _vrf_CELLZ01_complex2 ; PROBLEM:Difference between formula and atom_site contents detected. RESPONSE:The missing hydrogen atoms of coordination water molecule and free dimethylamine cation are calculated in the formula resulting in the difference. ; data_complex3 _database_code_depnum_ccdc_archive 'CCDC 861209' #TrackingRef 'complex861209.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H17 N2 O9 Sm' _chemical_formula_sum 'C14 H17 N2 O9 Sm' _chemical_formula_weight 507.65 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.630(3) _cell_length_b 10.182(3) _cell_length_c 10.687(3) _cell_angle_alpha 106.573(3) _cell_angle_beta 107.20 _cell_angle_gamma 110.615(2) _cell_volume 843.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293.1500 _cell_measurement_reflns_used 2635 _cell_measurement_theta_min 2.2160 _cell_measurement_theta_max 27.4932 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 1.983 _exptl_crystal_density_diffrn 1.999 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 498 _exptl_absorpt_coefficient_mu 3.534 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7738 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293.1500 _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 'Scxmini CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5353 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0674 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2858 _reflns_number_gt 2581 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0389P)^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 2858 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 Sm1 Sm 0.33424(3) 0.06038(3) 0.38556(2) 0.01856(11) Uani 1 1 d . . . O1 O 0.6563(5) 0.0727(6) -0.1824(4) 0.0461(12) Uani 1 1 d . . . N1 N 0.7571(6) 0.3735(5) 0.4325(5) 0.0248(10) Uani 1 1 d . . . C1 C 0.6363(7) 0.1541(7) -0.0847(6) 0.0276(13) Uani 1 1 d . . . O2 O 0.5557(6) 0.2220(6) -0.1048(5) 0.0547(14) Uani 1 1 d . . . N2 N 0.8213(7) 0.7065(6) 0.0013(6) 0.0481(15) Uani 1 1 d . . . C2 C 0.7216(7) 0.1744(6) 0.0678(6) 0.0256(12) Uani 1 1 d . . . O3 O 1.0663(5) 0.0058(4) 0.1874(4) 0.0275(9) Uani 1 1 d . . . C3 C 0.8308(7) 0.1091(6) 0.0992(6) 0.0245(12) Uani 1 1 d . . . H3 H 0.8452 0.0471 0.0240 0.029 Uiso 1 1 calc R . . O4 O 1.1280(5) 0.1305(5) 0.4171(4) 0.0339(10) Uani 1 1 d . . . C4 C 0.9139(7) 0.1398(6) 0.2424(6) 0.0223(12) Uani 1 1 d . . . O5 O 0.6243(4) 0.1113(4) 0.4916(4) 0.0237(8) Uani 1 1 d . . . C5 C 0.8887(6) 0.2228(6) 0.3522(5) 0.0226(12) Uani 1 1 d . . . H5 H 0.9443 0.2374 0.4487 0.027 Uiso 1 1 calc R . . O6 O 0.8662(5) 0.2072(5) 0.6723(4) 0.0364(10) Uani 1 1 d . . . C6 C 0.7800(6) 0.2870(6) 0.3225(5) 0.0215(11) Uani 1 1 d . . . O7 O 0.4228(5) 0.2826(5) 0.3538(5) 0.0456(12) Uani 1 1 d . . . C7 C 0.6984(7) 0.2591(7) 0.1782(6) 0.0244(12) Uani 1 1 d . . . H7 H 0.6245 0.2999 0.1555 0.029 Uiso 1 1 calc R . . O8 O 0.4350(6) 0.4558(5) 0.2691(5) 0.0466(12) Uani 1 1 d . . . C8 C 1.0402(6) 0.0884(6) 0.2838(6) 0.0238(12) Uani 1 1 d . . . O9 O 0.4511(5) 0.2318(4) 0.6414(4) 0.0343(10) Uani 1 1 d . . . C9 C 0.8240(7) 0.3828(6) 0.5767(5) 0.0235(12) Uani 1 1 d . . . H9A H 0.7894 0.4445 0.6383 0.028 Uiso 1 1 calc R . . H9B H 0.9462 0.4391 0.6195 0.028 Uiso 1 1 calc R . . C10 C 0.7695(7) 0.2232(6) 0.5806(5) 0.0236(12) Uani 1 1 d . . . C11 C 0.6876(7) 0.4772(6) 0.4108(6) 0.0264(12) Uani 1 1 d . . . H11A H 0.7300 0.5240 0.3516 0.032 Uiso 1 1 calc R . . H11B H 0.7284 0.5632 0.5068 0.032 Uiso 1 1 calc R . . C12 C 0.4998(7) 0.3992(6) 0.3369(6) 0.0263(13) Uani 1 1 d . . . C13 C 0.8965(9) 0.5993(9) -0.0189(8) 0.0541(19) Uani 1 1 d . . . H13A H 0.9787 0.6233 0.0759 0.081 Uiso 1 1 calc R . . H13B H 0.9502 0.6142 -0.0824 0.081 Uiso 1 1 calc R . . H13C H 0.8096 0.4909 -0.0634 0.081 Uiso 1 1 calc R . . C14 C 0.7344(10) 0.6831(11) 0.0939(10) 0.088(3) Uani 1 1 d . . . H14A H 0.6167 0.6477 0.0380 0.133 Uiso 1 1 calc R . . H14B H 0.7824 0.7817 0.1797 0.133 Uiso 1 1 calc R . . H14C H 0.7469 0.6045 0.1249 0.133 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01909(17) 0.02261(17) 0.01602(15) 0.00940(12) 0.00500(12) 0.01348(13) O1 0.049(3) 0.078(4) 0.019(2) 0.014(2) 0.0129(19) 0.046(3) N1 0.036(3) 0.032(3) 0.020(2) 0.014(2) 0.012(2) 0.029(2) C1 0.027(3) 0.041(4) 0.026(3) 0.019(3) 0.011(2) 0.025(3) O2 0.076(4) 0.088(4) 0.027(2) 0.027(3) 0.024(2) 0.064(3) N2 0.032(3) 0.042(3) 0.044(3) 0.003(3) 0.003(2) 0.014(3) C2 0.029(3) 0.031(3) 0.021(3) 0.013(2) 0.012(2) 0.017(3) O3 0.024(2) 0.037(2) 0.0232(19) 0.0084(18) 0.0080(16) 0.0221(19) C3 0.030(3) 0.027(3) 0.021(3) 0.010(2) 0.012(2) 0.018(3) O4 0.035(2) 0.052(3) 0.0202(19) 0.0123(19) 0.0079(17) 0.033(2) C4 0.024(3) 0.026(3) 0.025(3) 0.015(2) 0.009(2) 0.019(3) O5 0.0170(19) 0.027(2) 0.0265(19) 0.0149(17) 0.0045(16) 0.0107(17) C5 0.018(3) 0.029(3) 0.018(2) 0.011(2) 0.005(2) 0.011(2) O6 0.029(2) 0.035(2) 0.035(2) 0.022(2) -0.0015(18) 0.013(2) C6 0.022(3) 0.028(3) 0.022(3) 0.015(2) 0.010(2) 0.017(2) O7 0.032(2) 0.042(3) 0.069(3) 0.038(3) 0.020(2) 0.015(2) C7 0.028(3) 0.034(3) 0.026(3) 0.018(3) 0.013(2) 0.025(3) O8 0.047(3) 0.032(2) 0.047(3) 0.020(2) -0.002(2) 0.022(2) C8 0.017(3) 0.028(3) 0.023(3) 0.010(2) 0.007(2) 0.011(2) O9 0.053(3) 0.034(2) 0.0167(18) 0.0093(18) 0.0070(18) 0.030(2) C9 0.028(3) 0.025(3) 0.019(3) 0.011(2) 0.009(2) 0.015(3) C10 0.021(3) 0.033(3) 0.019(3) 0.010(2) 0.012(2) 0.012(3) C11 0.028(3) 0.024(3) 0.028(3) 0.010(2) 0.012(2) 0.015(3) C12 0.032(3) 0.025(3) 0.024(3) 0.008(2) 0.010(2) 0.019(3) C13 0.050(5) 0.057(5) 0.042(4) 0.011(4) 0.009(3) 0.031(4) C14 0.043(5) 0.108(8) 0.077(6) 0.007(6) 0.027(5) 0.025(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 Sm1 O1 2.255(4) 2_655 ? Sm1 O7 2.283(4) . ? Sm1 O4 2.413(4) 1_455 ? Sm1 O9 2.421(4) . ? Sm1 O5 2.476(4) . ? Sm1 O6 2.482(4) 2_656 ? Sm1 O5 2.535(3) 2_656 ? Sm1 O3 2.557(4) 1_455 ? Sm1 C8 2.865(6) 1_455 ? Sm1 C10 2.872(6) 2_656 ? O1 C1 1.245(7) . ? O1 Sm1 2.255(4) 2_655 ? N1 C6 1.381(7) . ? N1 C9 1.445(6) . ? N1 C11 1.470(7) . ? C1 O2 1.221(7) . ? C1 C2 1.507(7) . ? N2 C14 1.490(9) . ? N2 C13 1.509(8) . ? C2 C7 1.377(7) . ? C2 C3 1.439(8) . ? O3 C8 1.280(6) . ? O3 Sm1 2.557(4) 1_655 ? C3 C4 1.381(7) . ? C3 H3 0.9500 . ? O4 C8 1.269(6) . ? O4 Sm1 2.413(4) 1_655 ? C4 C5 1.378(7) . ? C4 C8 1.487(7) . ? O5 C10 1.277(6) . ? O5 Sm1 2.535(3) 2_656 ? C5 C6 1.423(7) . ? C5 H5 0.9500 . ? O6 C10 1.231(7) . ? O6 Sm1 2.482(4) 2_656 ? C6 C7 1.397(7) . ? O7 C12 1.255(7) . ? C7 H7 0.9500 . ? O8 C12 1.213(6) . ? C8 Sm1 2.865(6) 1_655 ? C9 C10 1.538(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 Sm1 2.872(6) 2_656 ? C11 C12 1.520(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sm1 O7 91.00(18) 2_655 . ? O1 Sm1 O4 130.89(14) 2_655 1_455 ? O7 Sm1 O4 82.25(15) . 1_455 ? O1 Sm1 O9 154.59(16) 2_655 . ? O7 Sm1 O9 85.96(16) . . ? O4 Sm1 O9 73.71(14) 1_455 . ? O1 Sm1 O5 80.41(14) 2_655 . ? O7 Sm1 O5 88.97(14) . . ? O4 Sm1 O5 147.33(13) 1_455 . ? O9 Sm1 O5 74.32(13) . . ? O1 Sm1 O6 81.01(16) 2_655 2_656 ? O7 Sm1 O6 155.26(15) . 2_656 ? O4 Sm1 O6 85.41(15) 1_455 2_656 ? O9 Sm1 O6 111.00(13) . 2_656 ? O5 Sm1 O6 112.43(12) . 2_656 ? O1 Sm1 O5 95.56(14) 2_655 2_656 ? O7 Sm1 O5 153.07(15) . 2_656 ? O4 Sm1 O5 111.97(13) 1_455 2_656 ? O9 Sm1 O5 76.98(12) . 2_656 ? O5 Sm1 O5 66.57(13) . 2_656 ? O6 Sm1 O5 51.61(12) 2_656 2_656 ? O1 Sm1 O3 78.60(14) 2_655 1_455 ? O7 Sm1 O3 79.42(14) . 1_455 ? O4 Sm1 O3 52.30(12) 1_455 1_455 ? O9 Sm1 O3 125.29(13) . 1_455 ? O5 Sm1 O3 155.75(12) . 1_455 ? O6 Sm1 O3 76.07(12) 2_656 1_455 ? O5 Sm1 O3 127.48(12) 2_656 1_455 ? O1 Sm1 C8 105.04(15) 2_655 1_455 ? O7 Sm1 C8 76.83(16) . 1_455 ? O4 Sm1 C8 26.08(14) 1_455 1_455 ? O9 Sm1 C8 98.82(14) . 1_455 ? O5 Sm1 C8 164.75(14) . 1_455 ? O6 Sm1 C8 82.67(14) 2_656 1_455 ? O5 Sm1 C8 125.92(14) 2_656 1_455 ? O3 Sm1 C8 26.54(13) 1_455 1_455 ? O1 Sm1 C10 86.89(16) 2_655 2_656 ? O7 Sm1 C10 177.58(15) . 2_656 ? O4 Sm1 C10 100.03(15) 1_455 2_656 ? O9 Sm1 C10 95.44(14) . 2_656 ? O5 Sm1 C10 89.51(14) . 2_656 ? O6 Sm1 C10 25.25(14) 2_656 2_656 ? O5 Sm1 C10 26.40(13) 2_656 2_656 ? O3 Sm1 C10 101.31(14) 1_455 2_656 ? C8 Sm1 C10 104.86(15) 1_455 2_656 ? C1 O1 Sm1 169.4(4) . 2_655 ? C6 N1 C9 120.7(4) . . ? C6 N1 C11 120.1(4) . . ? C9 N1 C11 118.6(4) . . ? O2 C1 O1 123.7(5) . . ? O2 C1 C2 118.2(5) . . ? O1 C1 C2 118.0(5) . . ? C14 N2 C13 110.6(6) . . ? C7 C2 C3 119.9(5) . . ? C7 C2 C1 119.9(5) . . ? C3 C2 C1 120.1(5) . . ? C8 O3 Sm1 90.2(3) . 1_655 ? C4 C3 C2 117.7(5) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C8 O4 Sm1 97.2(3) . 1_655 ? C5 C4 C3 122.1(5) . . ? C5 C4 C8 117.6(5) . . ? C3 C4 C8 120.3(5) . . ? C10 O5 Sm1 140.4(4) . . ? C10 O5 Sm1 91.7(3) . 2_656 ? Sm1 O5 Sm1 113.43(13) . 2_656 ? C4 C5 C6 120.6(5) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C10 O6 Sm1 95.4(3) . 2_656 ? N1 C6 C7 121.7(5) . . ? N1 C6 C5 121.0(4) . . ? C7 C6 C5 117.3(5) . . ? C12 O7 Sm1 166.4(4) . . ? C2 C7 C6 122.2(5) . . ? C2 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? O4 C8 O3 118.8(5) . . ? O4 C8 C4 119.9(5) . . ? O3 C8 C4 121.2(5) . . ? O4 C8 Sm1 56.7(3) . 1_655 ? O3 C8 Sm1 63.2(3) . 1_655 ? C4 C8 Sm1 167.3(4) . 1_655 ? N1 C9 C10 114.0(4) . . ? N1 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? N1 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? O6 C10 O5 121.1(5) . . ? O6 C10 C9 119.0(5) . . ? O5 C10 C9 119.9(5) . . ? O6 C10 Sm1 59.4(3) . 2_656 ? O5 C10 Sm1 61.9(3) . 2_656 ? C9 C10 Sm1 174.2(3) . 2_656 ? N1 C11 C12 115.0(5) . . ? N1 C11 H11A 108.5 . . ? C12 C11 H11A 108.5 . . ? N1 C11 H11B 108.5 . . ? C12 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? O8 C12 O7 124.6(6) . . ? O8 C12 C11 118.1(5) . . ? O7 C12 C11 117.3(5) . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.015 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.166 # start Validation Reply Form _vrf_PLAT041_complex3 ; PROBLEM:Calc. and Reported SumFormula Strings Differ ? RESPONSE:The missing hydrogen atoms of coordination water molecule and free dimethylamine cation are calculated in the formula resulting in the difference. ; _vrf_PLAT042_complex3 ; PROBLEM:Calc. and Reported MoietyFormula Strings Differ RESPONSE:The missing hydrogen atoms of coordination water molecule and free dimethylamine cation are calculated in the formula resulting in the difference. ; _vrf_PLAT068_complex3 ; PROBLEM: Reported F000 Differs from Calcd (or Missing)... ? RESPONSE:The missing hydrogen atoms of coordination water molecule and free dimethylamine cation are calculated in the formula resulting in the difference. ; _vrf_FORMU01_complex3 ; PROBLEM: There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C14 H17 N2 O9 Sm1 Atom count from the _atom_site data: C14 H13 N2 O9 Sm1 RESPONSE:The missing hydrogen atoms of coordination water molecule and free dimethylamine cation are calculated in the formula resulting in the difference. ; _vrf_CELLZ01_complex3 ; PROBLEM:Difference between formula and atom_site contents detected. RESPONSE:The missing hydrogen atoms of coordination water molecule and free dimethylamine cation are calculated in the formula resulting in the difference. ; data_complex4 _database_code_depnum_ccdc_archive 'CCDC 861210' #TrackingRef 'complex861210.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H11 Eu N O9.50' _chemical_formula_sum 'C12 H11 Eu N O9.50' _chemical_formula_weight 473.18 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 tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x, -y+1/2, z' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1/2, -y+1, z+1/2' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x, y-1/2, -z' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x+1/2, y, -z+1/2' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 21.6024(8) _cell_length_b 21.6024(8) _cell_length_c 11.3824(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5311.8(5) _cell_formula_units_Z 16 _cell_measurement_temperature 293.1500 _cell_measurement_reflns_used 6766 _cell_measurement_theta_min 2.6669 _cell_measurement_theta_max 27.3852 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3664 _exptl_absorpt_coefficient_mu 4.781 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9503 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293.1500 _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 'Saturn70 CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20423 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 27.38 _reflns_number_total 3011 _reflns_number_gt 2816 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0309P)^2^+19.9186P] 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 3011 _refine_ls_number_parameters 209 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0614 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.003 _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 0.427992(8) 0.563793(7) 0.531093(15) 0.01118(7) Uani 1 1 d . . . O1 O 0.28669(12) 0.63052(13) 0.7895(2) 0.0204(6) Uani 1 1 d . . . O2 O 0.33119(12) 0.57190(13) 0.6483(2) 0.0220(6) Uani 1 1 d . . . N1 N 0.43768(13) 0.56167(13) 0.7714(3) 0.0142(6) Uani 1 1 d . . . O6 O 0.51449(13) 0.39213(12) 0.6455(3) 0.0249(6) Uani 1 1 d . . . O3 O 0.50876(13) 0.62479(13) 0.6119(3) 0.0255(6) Uani 1 1 d . . . O5 O 0.50534(11) 0.49216(11) 0.6159(2) 0.0165(5) Uani 1 1 d . . . C2 C 0.45179(17) 0.44734(17) 0.7835(3) 0.0161(7) Uani 1 1 d . . . C4 C 0.37373(17) 0.49638(17) 0.9040(3) 0.0182(8) Uani 1 1 d . . . H4 H 0.3498 0.5316 0.9251 0.022 Uiso 1 1 calc R . . O4 O 0.58500(14) 0.64116(17) 0.7398(3) 0.0379(8) Uani 1 1 d . . . C3 C 0.42110(16) 0.50205(17) 0.8204(3) 0.0148(7) Uani 1 1 d . . . C9 C 0.53387(18) 0.61854(18) 0.7115(4) 0.0214(8) Uani 1 1 d . . . C10 C 0.39502(16) 0.61260(16) 0.8011(3) 0.0162(7) Uani 1 1 d . . . H10A H 0.4134 0.6524 0.7756 0.019 Uiso 1 1 calc R . . H10B H 0.3895 0.6143 0.8874 0.019 Uiso 1 1 calc R . . O8 O 0.30859(15) 0.38906(15) 1.1126(3) 0.0351(8) Uani 1 1 d . . . C12 C 0.30984(18) 0.43179(19) 1.0434(3) 0.0216(8) Uani 1 1 d . . . C5 C 0.36148(18) 0.43903(19) 0.9566(4) 0.0217(8) Uani 1 1 d . . . C1 C 0.49343(16) 0.44337(16) 0.6766(3) 0.0152(7) Uani 1 1 d . . . C7 C 0.44017(19) 0.39136(18) 0.8409(4) 0.0245(9) Uani 1 1 d . . . H7 H 0.4630 0.3555 0.8193 0.029 Uiso 1 1 calc R . . C6 C 0.3960(2) 0.38719(19) 0.9287(4) 0.0252(9) Uani 1 1 d . . . H6 H 0.3896 0.3493 0.9692 0.030 Uiso 1 1 calc R . . C8 C 0.50181(17) 0.57997(19) 0.8052(3) 0.0197(8) Uani 1 1 d . . . H8A H 0.5265 0.5422 0.8200 0.024 Uiso 1 1 calc R . . H8B H 0.5002 0.6040 0.8792 0.024 Uiso 1 1 calc R . . O7 O 0.26587(15) 0.47305(15) 1.0386(3) 0.0334(7) Uani 1 1 d . . . C11 C 0.33212(16) 0.60450(16) 0.7428(3) 0.0153(7) Uani 1 1 d . . . H9 H 0.2308 0.4600 1.0630 0.13(4) Uiso 1 1 d R . . O9 O 0.50001(16) 0.75000(16) 0.7706(3) 0.052(6) Uani 0.320(16) 2 d SPRU A 1 O9' O 0.50001(16) 0.75000(16) 0.9285(3) 0.141(7) Uani 0.680(16) 2 d SPRU A 2 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 0.01133(10) 0.00988(9) 0.01234(11) 0.00004(6) 0.00105(6) 0.00170(6) O1 0.0125(12) 0.0275(14) 0.0212(15) -0.0032(12) 0.0033(11) 0.0090(11) O2 0.0144(12) 0.0331(15) 0.0184(15) -0.0076(12) -0.0006(11) 0.0023(11) N1 0.0109(14) 0.0119(14) 0.0198(17) 0.0000(12) 0.0020(12) 0.0004(11) O6 0.0298(15) 0.0174(13) 0.0275(16) 0.0027(12) 0.0129(13) 0.0064(11) O3 0.0261(15) 0.0250(14) 0.0253(16) 0.0000(12) 0.0020(12) -0.0131(11) O5 0.0148(12) 0.0175(12) 0.0171(13) 0.0029(10) 0.0023(10) 0.0048(10) C2 0.0153(17) 0.0189(18) 0.0142(19) 0.0031(14) 0.0010(14) -0.0009(14) C4 0.0169(17) 0.0187(17) 0.019(2) 0.0017(15) 0.0037(15) 0.0017(14) O4 0.0232(16) 0.051(2) 0.039(2) -0.0044(16) 0.0013(14) -0.0195(15) C3 0.0151(16) 0.0174(17) 0.0120(18) 0.0014(14) -0.0013(14) -0.0023(13) C9 0.0161(18) 0.0217(19) 0.026(2) -0.0062(16) 0.0051(16) -0.0062(15) C10 0.0146(17) 0.0143(17) 0.020(2) -0.0008(14) 0.0002(14) 0.0003(13) O8 0.0332(17) 0.0377(17) 0.0346(19) 0.0232(15) 0.0146(14) 0.0080(14) C12 0.0233(19) 0.026(2) 0.016(2) 0.0026(16) 0.0023(15) -0.0019(16) C5 0.0230(19) 0.026(2) 0.016(2) 0.0052(16) 0.0047(16) 0.0026(16) C1 0.0134(16) 0.0177(17) 0.0145(18) 0.0044(14) -0.0023(14) 0.0037(13) C7 0.031(2) 0.0192(19) 0.023(2) 0.0048(16) 0.0057(18) 0.0056(16) C6 0.032(2) 0.0192(19) 0.024(2) 0.0085(16) 0.0074(18) 0.0009(16) C8 0.0141(17) 0.026(2) 0.019(2) -0.0051(16) -0.0021(15) -0.0033(14) O7 0.0265(16) 0.0377(18) 0.0360(19) 0.0148(14) 0.0130(14) 0.0087(13) C11 0.0132(16) 0.0144(16) 0.0183(19) 0.0031(14) 0.0016(14) 0.0002(13) O9 0.036(8) 0.047(8) 0.074(10) 0.000 0.000 0.007(6) O9' 0.088(8) 0.148(10) 0.186(11) 0.000 0.000 0.002(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 Eu1 O4 2.339(3) 14_566 ? Eu1 O3 2.372(3) . ? Eu1 O1 2.403(2) 8_454 ? Eu1 O8 2.406(3) 2_554 ? Eu1 O5 2.473(2) . ? Eu1 O2 2.487(3) . ? Eu1 O5 2.517(2) 9_666 ? Eu1 O6 2.547(3) 9_666 ? Eu1 N1 2.744(3) . ? Eu1 C1 2.914(4) 9_666 ? Eu1 Eu1 4.2162(4) 9_666 ? O1 C11 1.250(4) . ? O1 Eu1 2.403(2) 2 ? O2 C11 1.286(5) . ? N1 C3 1.449(4) . ? N1 C10 1.474(4) . ? N1 C8 1.491(4) . ? O6 C1 1.248(4) . ? O6 Eu1 2.547(3) 9_666 ? O3 C9 1.264(5) . ? O5 C1 1.286(4) . ? O5 Eu1 2.517(2) 9_666 ? C2 C7 1.397(5) . ? C2 C3 1.419(5) . ? C2 C1 1.516(5) . ? C4 C5 1.401(5) . ? C4 C3 1.402(5) . ? O4 C9 1.250(5) . ? O4 Eu1 2.339(3) 16_656 ? C9 C8 1.521(6) . ? C10 C11 1.523(5) . ? O8 C12 1.214(5) . ? O8 Eu1 2.406(3) 8_455 ? C12 O7 1.304(5) . ? C12 C5 1.499(5) . ? C5 C6 1.383(6) . ? C1 Eu1 2.914(4) 9_666 ? C7 C6 1.384(6) . ? 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 Eu1 O3 76.72(12) 14_566 . ? O4 Eu1 O1 134.70(11) 14_566 8_454 ? O3 Eu1 O1 143.17(10) . 8_454 ? O4 Eu1 O8 75.99(12) 14_566 2_554 ? O3 Eu1 O8 141.07(10) . 2_554 ? O1 Eu1 O8 74.49(10) 8_454 2_554 ? O4 Eu1 O5 148.68(11) 14_566 . ? O3 Eu1 O5 72.50(9) . . ? O1 Eu1 O5 73.00(9) 8_454 . ? O8 Eu1 O5 133.51(10) 2_554 . ? O4 Eu1 O2 72.69(11) 14_566 . ? O3 Eu1 O2 111.80(9) . . ? O1 Eu1 O2 71.53(9) 8_454 . ? O8 Eu1 O2 85.68(11) 2_554 . ? O5 Eu1 O2 113.75(9) . . ? O4 Eu1 O5 125.18(10) 14_566 9_666 ? O3 Eu1 O5 95.96(9) . 9_666 ? O1 Eu1 O5 80.61(9) 8_454 9_666 ? O8 Eu1 O5 78.01(11) 2_554 9_666 ? O5 Eu1 O5 64.68(10) . 9_666 ? O2 Eu1 O5 150.65(9) . 9_666 ? O4 Eu1 O6 74.72(10) 14_566 9_666 ? O3 Eu1 O6 74.90(10) . 9_666 ? O1 Eu1 O6 125.27(9) 8_454 9_666 ? O8 Eu1 O6 71.48(11) 2_554 9_666 ? O5 Eu1 O6 102.25(9) . 9_666 ? O2 Eu1 O6 143.82(9) . 9_666 ? O5 Eu1 O6 51.39(8) 9_666 9_666 ? O4 Eu1 N1 98.21(10) 14_566 . ? O3 Eu1 N1 64.31(9) . . ? O1 Eu1 N1 88.72(9) 8_454 . ? O8 Eu1 N1 147.12(10) 2_554 . ? O5 Eu1 N1 63.19(8) . . ? O2 Eu1 N1 61.99(9) . . ? O5 Eu1 N1 127.67(8) 9_666 . ? O6 Eu1 N1 139.07(9) 9_666 . ? O4 Eu1 C1 99.52(11) 14_566 9_666 ? O3 Eu1 C1 85.16(10) . 9_666 ? O1 Eu1 C1 103.48(10) 8_454 9_666 ? O8 Eu1 C1 72.64(11) 2_554 9_666 ? O5 Eu1 C1 83.67(9) . 9_666 ? O2 Eu1 C1 158.24(9) . 9_666 ? O5 Eu1 C1 26.11(9) 9_666 9_666 ? O6 Eu1 C1 25.29(9) 9_666 9_666 ? N1 Eu1 C1 139.76(9) . 9_666 ? O4 Eu1 Eu1 147.68(9) 14_566 9_666 ? O3 Eu1 Eu1 83.43(7) . 9_666 ? O1 Eu1 Eu1 74.40(7) 8_454 9_666 ? O8 Eu1 Eu1 106.25(9) 2_554 9_666 ? O5 Eu1 Eu1 32.66(6) . 9_666 ? O2 Eu1 Eu1 139.17(7) . 9_666 ? O5 Eu1 Eu1 32.03(6) 9_666 9_666 ? O6 Eu1 Eu1 75.64(6) 9_666 9_666 ? N1 Eu1 Eu1 95.75(6) . 9_666 ? C1 Eu1 Eu1 53.08(7) 9_666 9_666 ? C11 O1 Eu1 152.2(3) . 2 ? C11 O2 Eu1 118.3(2) . . ? C3 N1 C10 114.9(3) . . ? C3 N1 C8 111.5(3) . . ? C10 N1 C8 108.9(3) . . ? C3 N1 Eu1 112.3(2) . . ? C10 N1 Eu1 99.7(2) . . ? C8 N1 Eu1 108.9(2) . . ? C1 O6 Eu1 94.0(2) . 9_666 ? C9 O3 Eu1 127.2(2) . . ? C1 O5 Eu1 125.9(2) . . ? C1 O5 Eu1 94.5(2) . 9_666 ? Eu1 O5 Eu1 115.32(10) . 9_666 ? C7 C2 C3 119.9(3) . . ? C7 C2 C1 115.7(3) . . ? C3 C2 C1 124.2(3) . . ? C5 C4 C3 120.3(3) . . ? C9 O4 Eu1 158.9(3) . 16_656 ? C4 C3 C2 118.0(3) . . ? C4 C3 N1 121.3(3) . . ? C2 C3 N1 120.7(3) . . ? O4 C9 O3 124.7(4) . . ? O4 C9 C8 115.8(4) . . ? O3 C9 C8 119.5(3) . . ? N1 C10 C11 111.8(3) . . ? C12 O8 Eu1 166.9(3) . 8_455 ? O8 C12 O7 122.1(4) . . ? O8 C12 C5 121.6(4) . . ? O7 C12 C5 116.3(3) . . ? C6 C5 C4 121.1(4) . . ? C6 C5 C12 118.0(4) . . ? C4 C5 C12 121.0(4) . . ? O6 C1 O5 120.1(3) . . ? O6 C1 C2 119.6(3) . . ? O5 C1 C2 120.2(3) . . ? O6 C1 Eu1 60.7(2) . 9_666 ? O5 C1 Eu1 59.43(18) . 9_666 ? C2 C1 Eu1 179.2(3) . 9_666 ? C6 C7 C2 121.2(4) . . ? C5 C6 C7 119.0(4) . . ? N1 C8 C9 112.8(3) . . ? O1 C11 O2 126.2(3) . . ? O1 C11 C10 117.6(3) . . ? O2 C11 C10 116.2(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.38 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.901 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.115 # start Validation Reply Form _vrf_CHEMW03_complex4 ; PROBLEM:The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 16 From the CIF: _chemical_formula_weight 473.18 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 12.00 144.13 H 1.01 8.00 8.06 N 14.01 1.00 14.01 O 16.00 8.50 135.99 Eu 151.96 1.00 151.96 Calculated formula weight 454.15 RESPONSE:Two missing hydrogen atoms of free water molecule and one missing water molecule are calculated in the formula resulting in the difference. ; data_complex5 _database_code_depnum_ccdc_archive 'CCDC 861211' #TrackingRef 'complex861211.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H11 N O9.50 Tb' _chemical_formula_sum 'C12 H11 N O9.50 Tb' _chemical_formula_weight 480.14 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 tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x, -y+1/2, z' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1/2, -y+1, z+1/2' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x, y-1/2, -z' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x+1/2, y, -z+1/2' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 21.4229(6) _cell_length_b 21.4229(6) _cell_length_c 11.3047(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5188.2(3) _cell_formula_units_Z 16 _cell_measurement_temperature 293.1500 _cell_measurement_reflns_used 6745 _cell_measurement_theta_min 2.0370 _cell_measurement_theta_max 27.4816 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 5.512 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8275 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293.1500 _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 'Saturn70 CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20153 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2960 _reflns_number_gt 2710 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0358P)^2^+20.3986P] 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 2960 _refine_ls_number_parameters 211 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0641 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.020 _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 Tb1 Tb 0.428178(8) 0.563644(8) 0.031841(15) 0.01172(7) Uani 1 1 d . . . O1 O 0.50567(12) 0.49201(12) 0.1147(2) 0.0162(6) Uani 1 1 d . . . N1 N 0.43817(14) 0.56186(14) 0.2711(3) 0.0143(7) Uani 1 1 d . . . C1 C 0.49356(18) 0.44297(19) 0.1754(3) 0.0167(8) Uani 1 1 d . . . O4 O 0.26595(17) 0.47241(17) 0.5390(3) 0.0374(9) Uani 1 1 d . . . O2 O 0.51498(15) 0.39162(13) 0.1436(3) 0.0249(7) Uani 1 1 d . . . C2 C 0.45254(18) 0.44675(18) 0.2830(3) 0.0153(8) Uani 1 1 d . . . O3 O 0.30949(16) 0.38914(17) 0.6156(3) 0.0358(8) Uani 1 1 d . . . C3 C 0.42166(18) 0.50177(19) 0.3206(3) 0.0161(8) Uani 1 1 d . . . C4 C 0.3742(2) 0.49625(19) 0.4042(4) 0.0204(8) Uani 1 1 d . . . H4 H 0.3500 0.5317 0.4252 0.024 Uiso 1 1 calc R . . O5 O 0.50936(14) 0.62428(14) 0.1101(3) 0.0255(7) Uani 1 1 d . . . C5 C 0.3621(2) 0.4382(2) 0.4576(4) 0.0227(9) Uani 1 1 d . . . O6 O 0.58554(15) 0.64232(18) 0.2381(3) 0.0385(9) Uani 1 1 d . . . C6 C 0.3967(2) 0.3863(2) 0.4293(4) 0.0272(10) Uani 1 1 d . . . H6 H 0.3904 0.3482 0.4705 0.033 Uiso 1 1 calc R . . O7 O 0.33130(13) 0.57218(14) 0.1472(3) 0.0225(6) Uani 1 1 d . . . C7 C 0.4405(2) 0.3901(2) 0.3411(4) 0.0245(9) Uani 1 1 d . . . H7 H 0.4631 0.3538 0.3189 0.029 Uiso 1 1 calc R . . O8 O 0.28635(13) 0.63083(14) 0.2898(3) 0.0202(6) Uani 1 1 d . . . C8 C 0.3104(2) 0.4315(2) 0.5456(4) 0.0237(9) Uani 1 1 d . . . O9 O 0.5000 0.7500 0.283(2) 0.047(7) Uani 0.264(17) 2 d SPU A 1 C9 C 0.50263(19) 0.5802(2) 0.3044(4) 0.0207(9) Uani 1 1 d . . . H9A H 0.5276 0.5422 0.3191 0.025 Uiso 1 1 calc R . . H9B H 0.5012 0.6045 0.3789 0.025 Uiso 1 1 calc R . . O9' O 0.5000 0.7500 0.4256(15) 0.122(6) Uani 0.736(17) 2 d SPU A 2 C10 C 0.5343(2) 0.6189(2) 0.2098(4) 0.0224(9) Uani 1 1 d . . . C11 C 0.39511(18) 0.61279(18) 0.3014(4) 0.0174(8) Uani 1 1 d . . . H11A H 0.4136 0.6531 0.2765 0.021 Uiso 1 1 calc R . . H11B H 0.3894 0.6141 0.3883 0.021 Uiso 1 1 calc R . . C12 C 0.33215(18) 0.60463(18) 0.2423(3) 0.0149(8) Uani 1 1 d . . . H9 H 0.2345 0.4541 0.5900 0.13(4) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01203(10) 0.01018(10) 0.01297(11) 0.00002(6) 0.00096(6) 0.00169(6) O1 0.0165(13) 0.0158(13) 0.0163(13) 0.0033(11) 0.0030(11) 0.0044(10) N1 0.0089(15) 0.0134(16) 0.0206(17) 0.0002(13) 0.0021(13) 0.0005(12) C1 0.0138(18) 0.020(2) 0.0158(19) 0.0008(16) -0.0008(15) 0.0059(15) O4 0.0319(19) 0.042(2) 0.038(2) 0.0180(16) 0.0146(16) 0.0103(16) O2 0.0304(17) 0.0179(15) 0.0263(16) 0.0008(12) 0.0120(13) 0.0061(12) C2 0.0150(18) 0.0174(19) 0.0136(18) 0.0025(15) 0.0017(15) 0.0001(15) O3 0.0362(19) 0.039(2) 0.0321(19) 0.0217(16) 0.0144(15) 0.0039(15) C3 0.0150(19) 0.020(2) 0.0134(18) 0.0015(15) -0.0021(15) -0.0011(15) C4 0.021(2) 0.021(2) 0.020(2) 0.0029(17) 0.0020(17) 0.0013(16) O5 0.0259(16) 0.0253(16) 0.0253(16) 0.0016(13) -0.0003(13) -0.0125(12) C5 0.022(2) 0.025(2) 0.020(2) 0.0050(17) 0.0054(17) -0.0002(17) O6 0.0207(17) 0.051(2) 0.044(2) -0.0068(18) 0.0009(15) -0.0209(16) C6 0.035(3) 0.021(2) 0.026(2) 0.0065(18) 0.0095(19) 0.0014(18) O7 0.0129(14) 0.0317(17) 0.0228(15) -0.0058(13) -0.0010(12) 0.0059(12) C7 0.028(2) 0.022(2) 0.023(2) 0.0053(18) 0.0045(18) 0.0054(17) O8 0.0151(14) 0.0247(15) 0.0208(15) -0.0041(12) 0.0008(11) 0.0063(11) C8 0.022(2) 0.027(2) 0.022(2) 0.0070(18) 0.0067(17) -0.0019(17) O9 0.028(9) 0.044(10) 0.070(11) 0.000 0.000 0.011(7) C9 0.0144(19) 0.027(2) 0.021(2) -0.0050(17) -0.0026(16) -0.0018(16) O9' 0.076(7) 0.136(9) 0.154(10) 0.000 0.000 0.005(7) C10 0.017(2) 0.023(2) 0.028(2) -0.0057(18) 0.0054(17) -0.0049(16) C11 0.0164(19) 0.0145(19) 0.021(2) -0.0017(15) 0.0009(15) 0.0014(15) C12 0.0158(19) 0.0133(18) 0.0156(18) 0.0026(15) 0.0011(15) -0.0007(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O6 2.303(3) 14_565 ? Tb1 O5 2.344(3) . ? Tb1 O3 2.370(3) 2_554 ? Tb1 O8 2.372(3) 8_454 ? Tb1 O1 2.447(3) . ? Tb1 O7 2.458(3) . ? Tb1 O1 2.485(3) 9_665 ? Tb1 O2 2.517(3) 9_665 ? Tb1 N1 2.713(3) . ? Tb1 C1 2.884(4) 9_665 ? O1 C1 1.281(5) . ? O1 Tb1 2.485(3) 9_665 ? N1 C3 1.448(5) . ? N1 C11 1.469(5) . ? N1 C9 1.485(5) . ? C1 O2 1.245(5) . ? C1 C2 1.503(5) . ? C1 Tb1 2.884(4) 9_665 ? O4 C8 1.298(6) . ? O2 Tb1 2.517(3) 9_665 ? C2 C7 1.404(6) . ? C2 C3 1.417(5) . ? O3 C8 1.204(5) . ? O3 Tb1 2.370(3) 8_455 ? C3 C4 1.393(6) . ? C4 C5 1.406(6) . ? O5 C10 1.253(6) . ? C5 C6 1.375(6) . ? C5 C8 1.495(6) . ? O6 C10 1.248(5) . ? O6 Tb1 2.303(3) 16_655 ? C6 C7 1.372(6) . ? O7 C12 1.281(5) . ? O8 C12 1.251(5) . ? O8 Tb1 2.372(3) 2 ? C9 C10 1.513(6) . ? C11 C12 1.516(5) . ? 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 O6 Tb1 O5 76.40(13) 14_565 . ? O6 Tb1 O3 75.80(13) 14_565 2_554 ? O5 Tb1 O3 140.47(11) . 2_554 ? O6 Tb1 O8 135.06(12) 14_565 8_454 ? O5 Tb1 O8 143.47(11) . 8_454 ? O3 Tb1 O8 74.68(11) 2_554 8_454 ? O6 Tb1 O1 148.41(12) 14_565 . ? O5 Tb1 O1 72.53(10) . . ? O3 Tb1 O1 133.83(11) 2_554 . ? O8 Tb1 O1 73.10(10) 8_454 . ? O6 Tb1 O7 72.58(12) 14_565 . ? O5 Tb1 O7 112.66(10) . . ? O3 Tb1 O7 84.81(11) 2_554 . ? O8 Tb1 O7 71.70(10) 8_454 . ? O1 Tb1 O7 114.62(9) . . ? O6 Tb1 O1 125.09(11) 14_565 9_665 ? O5 Tb1 O1 95.41(10) . 9_665 ? O3 Tb1 O1 78.49(12) 2_554 9_665 ? O8 Tb1 O1 80.55(9) 8_454 9_665 ? O1 Tb1 O1 64.36(10) . 9_665 ? O7 Tb1 O1 150.57(10) . 9_665 ? O6 Tb1 O2 74.17(11) 14_565 9_665 ? O5 Tb1 O2 74.17(11) . 9_665 ? O3 Tb1 O2 71.58(12) 2_554 9_665 ? O8 Tb1 O2 125.50(10) 8_454 9_665 ? O1 Tb1 O2 102.24(9) . 9_665 ? O7 Tb1 O2 142.96(10) . 9_665 ? O1 Tb1 O2 51.79(9) 9_665 9_665 ? O6 Tb1 N1 97.88(11) 14_565 . ? O5 Tb1 N1 64.73(10) . . ? O3 Tb1 N1 146.89(11) 2_554 . ? O8 Tb1 N1 89.05(10) 8_454 . ? O1 Tb1 N1 63.65(9) . . ? O7 Tb1 N1 62.54(9) . . ? O1 Tb1 N1 127.79(9) 9_665 . ? O2 Tb1 N1 138.81(10) 9_665 . ? O6 Tb1 C1 99.23(12) 14_565 9_665 ? O5 Tb1 C1 84.40(11) . 9_665 ? O3 Tb1 C1 73.02(12) 2_554 9_665 ? O8 Tb1 C1 103.59(11) 8_454 9_665 ? O1 Tb1 C1 83.43(10) . 9_665 ? O7 Tb1 C1 157.72(10) . 9_665 ? O1 Tb1 C1 26.29(10) 9_665 9_665 ? O2 Tb1 C1 25.51(10) 9_665 9_665 ? N1 Tb1 C1 139.73(10) . 9_665 ? C1 O1 Tb1 125.6(2) . . ? C1 O1 Tb1 94.5(2) . 9_665 ? Tb1 O1 Tb1 115.64(10) . 9_665 ? C3 N1 C11 114.6(3) . . ? C3 N1 C9 111.4(3) . . ? C11 N1 C9 109.1(3) . . ? C3 N1 Tb1 112.3(2) . . ? C11 N1 Tb1 99.9(2) . . ? C9 N1 Tb1 108.8(2) . . ? O2 C1 O1 119.7(4) . . ? O2 C1 C2 119.8(4) . . ? O1 C1 C2 120.5(3) . . ? O2 C1 Tb1 60.5(2) . 9_665 ? O1 C1 Tb1 59.18(19) . 9_665 ? C2 C1 Tb1 179.6(3) . 9_665 ? C1 O2 Tb1 94.0(2) . 9_665 ? C7 C2 C3 119.5(4) . . ? C7 C2 C1 116.1(4) . . ? C3 C2 C1 124.1(3) . . ? C8 O3 Tb1 168.2(4) . 8_455 ? C4 C3 C2 118.3(4) . . ? C4 C3 N1 121.1(4) . . ? C2 C3 N1 120.6(3) . . ? C3 C4 C5 120.1(4) . . ? C10 O5 Tb1 127.2(3) . . ? C6 C5 C4 121.1(4) . . ? C6 C5 C8 118.4(4) . . ? C4 C5 C8 120.5(4) . . ? C10 O6 Tb1 158.9(3) . 16_655 ? C7 C6 C5 119.4(4) . . ? C12 O7 Tb1 118.3(2) . . ? C6 C7 C2 121.1(4) . . ? C12 O8 Tb1 152.1(3) . 2 ? O3 C8 O4 122.3(4) . . ? O3 C8 C5 121.6(4) . . ? O4 C8 C5 116.1(4) . . ? N1 C9 C10 112.5(3) . . ? O6 C10 O5 124.7(4) . . ? O6 C10 C9 115.7(4) . . ? O5 C10 C9 119.7(4) . . ? N1 C11 C12 111.7(3) . . ? O8 C12 O7 126.3(4) . . ? O8 C12 C11 117.2(3) . . ? O7 C12 C11 116.5(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.210 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.123 # start Validation Reply Form _vrf_CHEMW03_complex5 ; PROBLEM:The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 16 From the CIF: _chemical_formula_weight 480.14 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 12.00 144.13 H 1.01 8.00 8.06 N 14.01 1.00 14.01 O 16.00 8.50 135.99 Tb 158.93 1.00 158.93 Calculated formula weight 461.12 ? RESPONSE:Two missing hydrogen atoms of free water molecule and one missing water molecule are calculated in the formula resulting in the difference. ; data_complex6 _database_code_depnum_ccdc_archive 'CCDC 861212' #TrackingRef 'complex861212.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H11 N O9.50 Sm' _chemical_formula_sum 'C12 H11 N O9.50 Sm' _chemical_formula_weight 471.57 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x, -y+1/2, z' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1/2, -y+1, z+1/2' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x, y-1/2, -z' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x+1/2, y, -z+1/2' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 21.5765(4) _cell_length_b 21.5765(4) _cell_length_c 11.3469(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5282.5(2) _cell_formula_units_Z 16 _cell_measurement_temperature 293.1500 _cell_measurement_reflns_used 8209 _cell_measurement_theta_min 2.0279 _cell_measurement_theta_max 27.4623 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 4.505 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9503 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293.1500 _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 'Saturn70 CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19813 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2999 _reflns_number_gt 2750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0271P)^2^+3.5262P] 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 2999 _refine_ls_number_parameters 211 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0178 _refine_ls_wR_factor_ref 0.0494 _refine_ls_wR_factor_gt 0.0482 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.427757(6) 0.936179(6) 0.030582(10) 0.01118(6) Uani 1 1 d . . . O1 O 0.50522(8) 1.00742(8) 0.11647(15) 0.0159(4) Uani 1 1 d . . . N1 N 0.43745(10) 0.93805(10) 0.2717(2) 0.0132(4) Uani 1 1 d . . . C1 C 0.49328(12) 1.05599(12) 0.1777(2) 0.0163(5) Uani 1 1 d . . . O4 O 0.26566(11) 1.02663(11) 0.53818(19) 0.0336(5) Uani 1 1 d . . . O2 O 0.51452(9) 1.10749(9) 0.14636(18) 0.0249(5) Uani 1 1 d . . . C2 C 0.45175(12) 1.05224(13) 0.2834(2) 0.0164(5) Uani 1 1 d . . . O3 O 0.30853(10) 1.11052(11) 0.61188(19) 0.0365(6) Uani 1 1 d . . . C3 C 0.43926(14) 1.10811(13) 0.3404(3) 0.0242(6) Uani 1 1 d . . . H3 H 0.4617 1.1441 0.3180 0.029 Uiso 1 1 calc R . . C4 C 0.39543(14) 1.11261(14) 0.4281(3) 0.0274(7) Uani 1 1 d . . . H4 H 0.3889 1.1506 0.4686 0.033 Uiso 1 1 calc R . . O5 O 0.33105(8) 0.92806(9) 0.14817(17) 0.0218(4) Uani 1 1 d . . . C5 C 0.36112(13) 1.06061(14) 0.4559(2) 0.0214(6) Uani 1 1 d . . . O6 O 0.28724(9) 0.86938(9) 0.28924(16) 0.0207(4) Uani 1 1 d . . . C6 C 0.37363(13) 1.00338(13) 0.4031(2) 0.0191(6) Uani 1 1 d . . . H6 H 0.3496 0.9681 0.4237 0.023 Uiso 1 1 calc R . . O7 O 0.50873(10) 0.87496(10) 0.11268(18) 0.0267(5) Uani 1 1 d . . . C7 C 0.42078(12) 0.99775(12) 0.3211(2) 0.0143(5) Uani 1 1 d . . . O8 O 0.58463(10) 0.85915(12) 0.2412(2) 0.0390(6) Uani 1 1 d . . . C8 C 0.30951(13) 1.06793(14) 0.5425(2) 0.0228(6) Uani 1 1 d . . . O9 O 0.5000 0.7500 0.4405(13) 0.140(5) Uani 0.615(12) 2 d SPU A 1 C9 C 0.39461(12) 0.88755(12) 0.3009(2) 0.0165(5) Uani 1 1 d . . . H9A H 0.3889 0.8860 0.3874 0.020 Uiso 1 1 calc R . . H9B H 0.4130 0.8477 0.2756 0.020 Uiso 1 1 calc R . . O9' O 0.5000 0.7500 0.2773(10) 0.058(4) Uani 0.385(12) 2 d SPU A 2 C10 C 0.33218(12) 0.89552(12) 0.2424(2) 0.0146(5) Uani 1 1 d . . . C11 C 0.50162(12) 0.92003(14) 0.3055(2) 0.0203(6) Uani 1 1 d . . . H11A H 0.5001 0.8961 0.3799 0.024 Uiso 1 1 calc R . . H11B H 0.5262 0.9580 0.3202 0.024 Uiso 1 1 calc R . . C12 C 0.53396(13) 0.88140(14) 0.2118(3) 0.0223(6) Uani 1 1 d . . . H4A H 0.2378 1.0395 0.5856 0.16(3) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01137(8) 0.00961(8) 0.01256(8) -0.00003(4) 0.00126(5) -0.00185(5) O1 0.0167(9) 0.0164(9) 0.0147(8) -0.0041(7) 0.0038(7) -0.0027(7) N1 0.0095(10) 0.0137(11) 0.0164(11) -0.0004(8) 0.0016(8) 0.0000(8) C1 0.0135(13) 0.0181(14) 0.0174(12) -0.0018(10) -0.0008(10) -0.0036(10) O4 0.0262(12) 0.0408(14) 0.0338(12) -0.0163(10) 0.0125(10) -0.0097(10) O2 0.0311(12) 0.0178(10) 0.0259(11) -0.0040(8) 0.0131(9) -0.0079(9) C2 0.0145(13) 0.0200(14) 0.0148(12) -0.0029(10) 0.0015(10) -0.0007(11) O3 0.0365(13) 0.0387(13) 0.0341(12) -0.0245(10) 0.0170(10) -0.0079(10) C3 0.0292(16) 0.0185(14) 0.0248(14) -0.0034(12) 0.0070(12) -0.0063(12) C4 0.0312(17) 0.0226(15) 0.0284(15) -0.0105(12) 0.0102(13) -0.0020(13) O5 0.0109(9) 0.0312(11) 0.0231(10) 0.0080(8) -0.0001(8) -0.0042(8) C5 0.0217(15) 0.0251(15) 0.0174(13) -0.0062(11) 0.0038(11) -0.0003(12) O6 0.0148(10) 0.0261(11) 0.0213(10) 0.0046(8) 0.0031(8) -0.0079(8) C6 0.0170(13) 0.0215(14) 0.0187(13) -0.0019(11) 0.0029(11) -0.0015(11) O7 0.0294(12) 0.0279(11) 0.0229(11) -0.0001(9) 0.0009(9) 0.0147(9) C7 0.0136(12) 0.0164(13) 0.0130(11) -0.0029(10) -0.0008(10) 0.0006(10) O8 0.0193(12) 0.0527(16) 0.0449(13) 0.0069(12) -0.0003(10) 0.0205(11) C8 0.0218(15) 0.0269(16) 0.0197(14) -0.0050(11) 0.0039(11) 0.0012(12) O9 0.062(6) 0.151(8) 0.206(10) 0.000 0.000 -0.004(6) C9 0.0165(13) 0.0146(13) 0.0184(12) 0.0023(10) 0.0022(10) 0.0005(10) O9' 0.030(5) 0.050(6) 0.093(8) 0.000 0.000 -0.007(4) C10 0.0131(13) 0.0132(13) 0.0175(12) -0.0026(10) 0.0023(10) 0.0003(10) C11 0.0147(13) 0.0259(15) 0.0204(13) 0.0030(11) -0.0019(11) 0.0028(11) C12 0.0174(14) 0.0210(15) 0.0285(15) 0.0057(12) 0.0047(11) 0.0039(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O8 2.344(2) 16_655 ? Sm1 O7 2.380(2) . ? Sm1 O3 2.405(2) 4_464 ? Sm1 O6 2.4081(18) 6_554 ? Sm1 O1 2.4710(17) . ? Sm1 O5 2.4829(18) . ? Sm1 O1 2.5212(17) 9_675 ? Sm1 O2 2.5436(19) 9_675 ? Sm1 N1 2.744(2) . ? Sm1 C1 2.918(3) 9_675 ? O1 C1 1.283(3) . ? O1 Sm1 2.5212(17) 9_675 ? N1 C7 1.451(3) . ? N1 C9 1.467(3) . ? N1 C11 1.489(3) . ? C1 O2 1.253(3) . ? C1 C2 1.500(3) . ? C1 Sm1 2.918(3) 9_675 ? O4 C8 1.301(4) . ? O2 Sm1 2.5436(19) 9_675 ? C2 C3 1.394(4) . ? C2 C7 1.419(4) . ? O3 C8 1.210(3) . ? O3 Sm1 2.405(2) 6 ? C3 C4 1.376(4) . ? C4 C5 1.381(4) . ? O5 C10 1.279(3) . ? C5 C6 1.399(4) . ? C5 C8 1.494(4) . ? O6 C10 1.241(3) . ? O6 Sm1 2.4081(18) 4_465 ? C6 C7 1.384(4) . ? O7 C12 1.257(3) . ? O8 C12 1.240(4) . ? O8 Sm1 2.344(2) 14_565 ? C9 C10 1.511(4) . ? C11 C12 1.521(4) . ? 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 O8 Sm1 O7 76.81(9) 16_655 . ? O8 Sm1 O3 75.86(8) 16_655 4_464 ? O7 Sm1 O3 141.34(7) . 4_464 ? O8 Sm1 O6 135.01(8) 16_655 6_554 ? O7 Sm1 O6 142.80(7) . 6_554 ? O3 Sm1 O6 74.61(7) 4_464 6_554 ? O8 Sm1 O1 148.50(8) 16_655 . ? O7 Sm1 O1 72.20(7) . . ? O3 Sm1 O1 133.83(7) 4_464 . ? O6 Sm1 O1 72.92(6) 6_554 . ? O8 Sm1 O5 72.85(8) 16_655 . ? O7 Sm1 O5 111.56(7) . . ? O3 Sm1 O5 85.65(7) 4_464 . ? O6 Sm1 O5 71.76(7) 6_554 . ? O1 Sm1 O5 113.60(6) . . ? O8 Sm1 O1 125.19(7) 16_655 9_675 ? O7 Sm1 O1 96.08(7) . 9_675 ? O3 Sm1 O1 78.25(8) 4_464 9_675 ? O6 Sm1 O1 80.34(6) 6_554 9_675 ? O1 Sm1 O1 64.71(7) . 9_675 ? O5 Sm1 O1 150.66(6) . 9_675 ? O8 Sm1 O2 74.75(7) 16_655 9_675 ? O7 Sm1 O2 75.17(7) . 9_675 ? O3 Sm1 O2 71.62(8) 4_464 9_675 ? O6 Sm1 O2 125.06(6) 6_554 9_675 ? O1 Sm1 O2 102.16(6) . 9_675 ? O5 Sm1 O2 144.05(6) . 9_675 ? O1 Sm1 O2 51.36(6) 9_675 9_675 ? O8 Sm1 N1 98.31(7) 16_655 . ? O7 Sm1 N1 64.02(7) . . ? O3 Sm1 N1 147.03(7) 4_464 . ? O6 Sm1 N1 88.75(6) 6_554 . ? O1 Sm1 N1 63.01(6) . . ? O5 Sm1 N1 61.92(6) . . ? O1 Sm1 N1 127.52(6) 9_675 . ? O2 Sm1 N1 139.03(7) 9_675 . ? O8 Sm1 C1 99.63(8) 16_655 9_675 ? O7 Sm1 C1 85.44(7) . 9_675 ? O3 Sm1 C1 72.84(8) 4_464 9_675 ? O6 Sm1 C1 103.13(7) 6_554 9_675 ? O1 Sm1 C1 83.59(7) . 9_675 ? O5 Sm1 C1 158.42(7) . 9_675 ? O1 Sm1 C1 26.00(6) 9_675 9_675 ? O2 Sm1 C1 25.36(7) 9_675 9_675 ? N1 Sm1 C1 139.64(7) . 9_675 ? C1 O1 Sm1 125.85(16) . . ? C1 O1 Sm1 94.53(15) . 9_675 ? Sm1 O1 Sm1 115.29(7) . 9_675 ? C7 N1 C9 114.6(2) . . ? C7 N1 C11 111.3(2) . . ? C9 N1 C11 109.5(2) . . ? C7 N1 Sm1 112.34(15) . . ? C9 N1 Sm1 99.57(15) . . ? C11 N1 Sm1 108.93(15) . . ? O2 C1 O1 119.8(2) . . ? O2 C1 C2 119.5(2) . . ? O1 C1 C2 120.6(2) . . ? O2 C1 Sm1 60.37(14) . 9_675 ? O1 C1 Sm1 59.46(13) . 9_675 ? C2 C1 Sm1 179.01(19) . 9_675 ? C1 O2 Sm1 94.26(16) . 9_675 ? C3 C2 C7 119.0(2) . . ? C3 C2 C1 116.1(2) . . ? C7 C2 C1 124.6(2) . . ? C8 O3 Sm1 167.2(2) . 6 ? C4 C3 C2 121.9(3) . . ? C3 C4 C5 118.5(3) . . ? C10 O5 Sm1 118.16(16) . . ? C4 C5 C6 121.1(3) . . ? C4 C5 C8 117.7(2) . . ? C6 C5 C8 121.3(3) . . ? C10 O6 Sm1 151.86(18) . 4_465 ? C7 C6 C5 120.5(3) . . ? C12 O7 Sm1 127.35(18) . . ? C6 C7 C2 118.5(2) . . ? C6 C7 N1 121.4(2) . . ? C2 C7 N1 120.2(2) . . ? C12 O8 Sm1 158.1(2) . 14_565 ? O3 C8 O4 122.2(3) . . ? O3 C8 C5 121.4(3) . . ? O4 C8 C5 116.4(2) . . ? N1 C9 C10 112.2(2) . . ? O6 C10 O5 126.3(2) . . ? O6 C10 C9 117.2(2) . . ? O5 C10 C9 116.5(2) . . ? N1 C11 C12 112.9(2) . . ? O8 C12 O7 125.4(3) . . ? O8 C12 C11 115.4(3) . . ? O7 C12 C11 119.2(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.901 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.095 # start Validation Reply Form _vrf_CHEMW03_complex6 ; PROBLEM:The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 16 From the CIF: _chemical_formula_weight 471.57 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 12.00 144.13 H 1.01 8.00 8.06 N 14.01 1.00 14.01 O 16.00 8.50 135.99 Sm 150.36 1.00 150.36 Calculated formula weight 452.55 RESPONSE:Two missing hydrogen atoms of free water molecule and one missing water molecule are calculated in the formula resulting in the difference. ;