# cm021188j.cif data_global _publ_requested_journal 'Chemistry of Materials' loop_ _publ_author_name 'P. C. R. Soares-Santos' 'H.I.S. Nogueira' 'V. Felix' 'M.G.B. Drew' 'R. A. S  Ferreira' 'L. D. Carlos' 'T. Trindade' _publ_contact_author_name Prof. V. Felix _publ_contact_author_email vfelix@dq.ua.pt _publ_contact_author_address ; Prof. V. Felix Department of Chemistry University of Aveiro 3810-193 Aveiro PORTUGAL -------------------------- data section of block --------------------------- #==BEGIN data_compound [Ln(H2O)(picOH)2(m-HpicO)]3H2O 1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H20 Eu N3 O13' _chemical_formula_weight 638.33 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 Monoclinc _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.105(13) _cell_length_b 18.796(25) _cell_length_c 13.531(17) _cell_angle_alpha 90.00 _cell_angle_beta 104.860(10) _cell_angle_gamma 90.00 _cell_volume 2238(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'white' _exptl_crystal_size_max 0.490x0.06x0.08 mm _exptl_crystal_size_mid 0.280x0.04x0.07 mm _exptl_crystal_size_min 0.180x0.02x0.06 mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 2.877 _exptl_absorpt_correction_type 'Empirical, DIFABS (N.Walker and D. Stuart, Acta Cryst. Sect. A,39,158,1983)' _exptl_absorpt_correction_T_min 0.524 _exptl_absorpt_correction_T_max 1.0 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Mar research image plate system' _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 5766 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 26.02 _reflns_number_total 3243 _reflns_number_gt 2629 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'W. Kabsch, J. Appl. Crystallogr. 21,916,1983' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1999) _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+6.0222P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3243 _refine_ls_number_parameters 352 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.077 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu Eu 0.66429(3) 0.791560(13) 0.80736(2) 0.02531(14) Uani 1 d . . . N11 N 0.9498(6) 0.8170(3) 0.8896(4) 0.0383(13) Uani 1 d . . . C12 C 1.0419(7) 0.7605(4) 0.9034(5) 0.0357(15) Uani 1 d . . . C13 C 1.1979(8) 0.7660(4) 0.9439(6) 0.0470(18) Uani 1 d . . . C14 C 1.2599(9) 0.8324(5) 0.9685(6) 0.060(2) Uani 1 d . . . H14 H 1.3643 0.8381 0.9938 0.071 Uiso 1 calc R . . C15 C 1.1651(10) 0.8898(5) 0.9548(6) 0.061(2) Uani 1 d . . . H15 H 1.2048 0.9350 0.9719 0.073 Uiso 1 calc R . . C16 C 1.0102(9) 0.8810(4) 0.9158(6) 0.054(2) Uani 1 d . . . H16 H 0.9469 0.9206 0.9076 0.064 Uiso 1 calc R . . C17 C 0.9652(9) 0.6906(4) 0.8702(6) 0.0439(18) Uani 1 d . . . O131 O 1.2885(6) 0.7083(4) 0.9559(5) 0.0634(17) Uani 1 d D . . H131 H 1.225(10) 0.677(4) 0.939(9) 0.12(5) Uiso 1 d D . . O171 O 0.8260(5) 0.6907(2) 0.8291(4) 0.0395(11) Uani 1 d . . . O172 O 1.0483(6) 0.6356(3) 0.8836(4) 0.0549(14) Uani 1 d . . . N21 N 0.3776(6) 0.8150(3) 0.7366(4) 0.0328(12) Uani 1 d . . . C22 C 0.2875(7) 0.7576(3) 0.7150(5) 0.0315(14) Uani 1 d . . . C23 C 0.1288(8) 0.7636(4) 0.6735(6) 0.0449(18) Uani 1 d . . . C24 C 0.0685(8) 0.8307(4) 0.6553(6) 0.054(2) Uani 1 d . . . H24 H -0.0353 0.8368 0.6274 0.065 Uiso 1 calc R . . C25 C 0.1620(8) 0.8887(4) 0.6786(6) 0.054(2) Uani 1 d . . . H25 H 0.1218 0.9343 0.6677 0.065 Uiso 1 calc R . . C26 C 0.3151(8) 0.8793(4) 0.7181(6) 0.0452(18) Uani 1 d . . . H26 H 0.3774 0.9191 0.7324 0.054 Uiso 1 calc R . . C27 C 0.3637(7) 0.6869(3) 0.7400(5) 0.0301(14) Uani 1 d . . . O231 O 0.0386(6) 0.7069(3) 0.6534(5) 0.0569(15) Uani 1 d D . . H231 H 0.095(10) 0.672(4) 0.668(8) 0.10(4) Uiso 1 d D . . O272 O 0.2835(5) 0.6314(2) 0.7248(4) 0.0466(12) Uani 1 d . . . O271 O 0.5050(4) 0.6873(2) 0.7749(3) 0.0312(10) Uani 1 d . . . N31 N 0.6407(7) 0.8914(2) 0.4481(4) 0.0373(14) Uani 1 d D . . H31 H 0.608(7) 0.861(3) 0.396(3) 0.039(19) Uiso 1 d D . . C32 C 0.6551(7) 0.8646(3) 0.5429(5) 0.0279(14) Uani 1 d . . . C33 C 0.6867(7) 0.9120(3) 0.6260(5) 0.0329(15) Uani 1 d . . . C34 C 0.7057(9) 0.9845(3) 0.6026(6) 0.0458(18) Uani 1 d . . . H34 H 0.7259 1.0177 0.6553 0.055 Uiso 1 calc R . . C35 C 0.6954(10) 1.0068(4) 0.5059(6) 0.055(2) Uani 1 d . . . H35 H 0.7145 1.0541 0.4933 0.066 Uiso 1 calc R . . C36 C 0.6565(10) 0.9590(3) 0.4259(6) 0.053(2) Uani 1 d . . . H36 H 0.6419 0.9739 0.3585 0.064 Uiso 1 calc R . . C37 C 0.6484(7) 0.7859(3) 0.5497(5) 0.0291(15) Uani 1 d . . . O331 O 0.7000(5) 0.8924(2) 0.7189(4) 0.0377(11) Uani 1 d . . . O371 O 0.6494(5) 0.7577(2) 0.6346(3) 0.0334(10) Uani 1 d . . . O372 O 0.6470(5) 0.7505(2) 0.4707(3) 0.0327(10) Uani 1 d . . . O100 O 0.6368(6) 0.8929(2) 0.9077(4) 0.0444(12) Uani 1 d D . . H101 H 0.656(9) 0.890(3) 0.9702(10) 0.053 Uiso 1 d D . . H102 H 0.624(8) 0.9354(10) 0.895(4) 0.053 Uiso 1 d D . . O200 O 0.5422(7) 1.0241(2) 0.8350(5) 0.0598(14) Uani 1 d D . . H201 H 0.581(8) 1.057(2) 0.811(6) 0.072 Uiso 1 d D . . H202 H 0.471(6) 1.042(3) 0.853(6) 0.072 Uiso 1 d D . . O300 O 0.6829(6) 0.8941(2) 1.1131(4) 0.0509(13) Uani 1 d D . . H301 H 0.678(7) 0.8529(15) 1.132(5) 0.061 Uiso 1 d D . . H302 H 0.769(4) 0.907(3) 1.141(6) 0.061 Uiso 1 d D . . O400 O 0.9529(9) 0.5449(4) 0.7239(7) 0.110(3) Uani 1 d D . . H401 H 1.020(9) 0.515(4) 0.730(9) 0.132 Uiso 1 d D . . H402 H 0.987(11) 0.574(5) 0.770(7) 0.132 Uiso 1 d D . . 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 Eu 0.02658(19) 0.02538(17) 0.0237(3) 0.00058(11) 0.00601(17) 0.00106(11) N11 0.038(3) 0.041(3) 0.034(4) 0.004(2) 0.004(3) -0.003(2) C12 0.027(3) 0.053(4) 0.023(5) 0.001(3) -0.002(3) -0.001(3) C13 0.038(4) 0.077(5) 0.025(5) 0.001(4) 0.006(4) 0.003(3) C14 0.033(4) 0.096(7) 0.047(6) -0.007(5) 0.007(4) -0.015(4) C15 0.056(5) 0.071(5) 0.055(6) -0.008(4) 0.011(4) -0.025(4) C16 0.049(4) 0.052(4) 0.056(6) -0.004(4) 0.008(4) -0.011(3) C17 0.046(4) 0.045(4) 0.043(5) 0.009(3) 0.016(4) 0.012(3) O131 0.029(3) 0.094(5) 0.062(5) 0.007(3) 0.003(3) 0.018(3) O171 0.027(2) 0.047(3) 0.042(3) -0.001(2) 0.004(2) 0.0077(17) O172 0.044(3) 0.054(3) 0.063(4) 0.005(3) 0.007(3) 0.017(2) N21 0.028(3) 0.033(3) 0.037(4) 0.003(2) 0.007(3) 0.005(2) C22 0.027(3) 0.041(3) 0.026(4) 0.001(3) 0.005(3) 0.003(2) C23 0.038(4) 0.058(4) 0.041(5) 0.000(3) 0.015(4) -0.006(3) C24 0.030(4) 0.063(5) 0.065(6) 0.011(4) 0.006(4) 0.013(3) C25 0.048(4) 0.052(4) 0.060(6) 0.013(4) 0.009(4) 0.025(3) C26 0.046(4) 0.035(3) 0.051(5) 0.008(3) 0.008(4) 0.013(3) C27 0.037(4) 0.034(3) 0.017(4) -0.001(3) 0.001(3) -0.004(2) O231 0.035(3) 0.070(4) 0.063(5) -0.001(3) 0.009(3) -0.013(3) O272 0.040(3) 0.039(2) 0.062(4) -0.005(2) 0.015(3) -0.011(2) O271 0.027(2) 0.030(2) 0.033(3) 0.0052(18) 0.001(2) -0.0002(15) N31 0.063(4) 0.018(2) 0.030(4) -0.002(2) 0.010(3) -0.002(2) C32 0.031(3) 0.031(3) 0.023(4) 0.000(3) 0.010(3) -0.001(2) C33 0.030(3) 0.034(3) 0.039(5) 0.002(3) 0.015(3) -0.001(2) C34 0.071(5) 0.025(3) 0.040(6) -0.005(3) 0.011(4) -0.009(3) C35 0.094(6) 0.030(3) 0.041(6) -0.001(3) 0.017(5) -0.013(3) C36 0.092(6) 0.036(4) 0.029(5) 0.007(3) 0.010(4) -0.001(4) C37 0.027(3) 0.030(3) 0.031(5) 0.001(3) 0.008(3) 0.001(2) O331 0.057(3) 0.025(2) 0.029(3) -0.0010(18) 0.008(2) -0.0052(17) O371 0.052(3) 0.025(2) 0.025(3) 0.0015(18) 0.014(2) -0.0011(18) O372 0.046(3) 0.028(2) 0.026(3) -0.0021(18) 0.011(2) 0.0002(17) O100 0.076(4) 0.026(2) 0.032(3) 0.0026(19) 0.017(3) 0.009(2) O200 0.065(4) 0.034(3) 0.083(5) 0.008(3) 0.025(3) 0.008(2) O300 0.068(4) 0.036(3) 0.049(4) 0.004(2) 0.014(3) 0.003(2) O400 0.107(6) 0.061(4) 0.133(7) -0.018(4) -0.021(5) 0.014(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 Eu O331 2.309(5) . ? Eu O171 2.373(5) . ? Eu O100 2.389(5) . ? Eu O372 2.390(5) 4_576 ? Eu O371 2.393(5) . ? Eu O271 2.410(5) . ? Eu N21 2.578(6) . ? Eu N11 2.596(6) . ? N11 C16 1.334(9) . ? N11 C12 1.336(9) . ? C12 C13 1.389(10) . ? C12 C17 1.501(10) . ? C13 O131 1.346(10) . ? C13 C14 1.376(12) . ? C14 C15 1.363(12) . ? C14 H14 0.9300 . ? C15 C16 1.383(11) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O171 1.246(9) . ? C17 O172 1.267(8) . ? O131 H131 0.822(11) . ? N21 C26 1.331(8) . ? N21 C22 1.341(8) . ? C22 C23 1.414(9) . ? C22 C27 1.497(9) . ? C23 O231 1.329(9) . ? C23 C24 1.374(11) . ? C24 C25 1.368(11) . ? C24 H24 0.9300 . ? C25 C26 1.370(10) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 O271 1.252(8) . ? C27 O272 1.259(7) . ? O231 H231 0.821(11) . ? N31 C36 1.322(8) . ? N31 C32 1.353(8) . ? N31 H31 0.889(10) . ? C32 C33 1.406(9) . ? C32 C37 1.484(8) . ? C33 O331 1.285(8) . ? C33 C34 1.420(8) . ? C34 C35 1.355(10) . ? C34 H34 0.9300 . ? C35 C36 1.381(10) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 O372 1.257(7) . ? C37 O371 1.263(7) . ? O372 Eu 2.390(5) 4_575 ? O100 H101 0.820(10) . ? O100 H102 0.820(10) . ? O200 H201 0.818(11) . ? O200 H202 0.820(11) . ? O300 H301 0.819(10) . ? O300 H302 0.819(11) . ? O400 H401 0.820(11) . ? O400 H402 0.821(11) . ? 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 O331 Eu O171 123.73(17) . . ? O331 Eu O100 71.90(18) . . ? O171 Eu O100 135.96(18) . . ? O331 Eu O372 143.36(14) . 4_576 ? O171 Eu O372 78.85(15) . 4_576 ? O100 Eu O372 72.36(16) . 4_576 ? O331 Eu O371 72.06(16) . . ? O171 Eu O371 77.68(16) . . ? O100 Eu O371 141.18(14) . . ? O372 Eu O371 144.57(14) 4_576 . ? O331 Eu O271 136.98(16) . . ? O171 Eu O271 72.42(18) . . ? O100 Eu O271 127.28(17) . . ? O372 Eu O271 73.76(15) 4_576 . ? O371 Eu O271 74.05(14) . . ? O331 Eu N21 86.03(17) . . ? O171 Eu N21 136.05(16) . . ? O100 Eu N21 80.27(18) . . ? O372 Eu N21 95.71(16) 4_576 . ? O371 Eu N21 83.36(17) . . ? O271 Eu N21 64.31(16) . . ? O331 Eu N11 79.21(17) . . ? O171 Eu N11 64.69(18) . . ? O100 Eu N11 81.33(19) . . ? O372 Eu N11 87.74(17) 4_576 . ? O371 Eu N11 105.50(17) . . ? O271 Eu N11 135.82(15) . . ? N21 Eu N11 159.26(18) . . ? C16 N11 C12 118.7(6) . . ? C16 N11 Eu 125.4(5) . . ? C12 N11 Eu 115.9(4) . . ? N11 C12 C13 122.5(7) . . ? N11 C12 C17 115.2(6) . . ? C13 C12 C17 122.3(6) . . ? O131 C13 C14 120.0(7) . . ? O131 C13 C12 121.4(7) . . ? C14 C13 C12 118.5(8) . . ? C15 C14 C13 118.6(7) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 C16 120.4(7) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? N11 C16 C15 121.3(7) . . ? N11 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? O171 C17 O172 124.5(7) . . ? O171 C17 C12 118.4(6) . . ? O172 C17 C12 117.1(7) . . ? C13 O131 H131 100(9) . . ? C17 O171 Eu 125.7(4) . . ? C26 N21 C22 118.8(6) . . ? C26 N21 Eu 124.6(4) . . ? C22 N21 Eu 116.6(4) . . ? N21 C22 C23 121.9(6) . . ? N21 C22 C27 116.3(6) . . ? C23 C22 C27 121.8(6) . . ? O231 C23 C24 120.1(7) . . ? O231 C23 C22 122.2(7) . . ? C24 C23 C22 117.7(7) . . ? C25 C24 C23 119.6(7) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 119.9(6) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? N21 C26 C25 122.2(7) . . ? N21 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? O271 C27 O272 124.3(6) . . ? O271 C27 C22 116.9(5) . . ? O272 C27 C22 118.8(6) . . ? C23 O231 H231 105(8) . . ? C27 O271 Eu 125.9(4) . . ? C36 N31 C32 125.7(6) . . ? C36 N31 H31 118(4) . . ? C32 N31 H31 116(4) . . ? N31 C32 C33 118.2(5) . . ? N31 C32 C37 115.8(5) . . ? C33 C32 C37 125.8(6) . . ? O331 C33 C32 123.4(5) . . ? O331 C33 C34 120.4(6) . . ? C32 C33 C34 116.2(6) . . ? C35 C34 C33 122.1(6) . . ? C35 C34 H34 119.0 . . ? C33 C34 H34 119.0 . . ? C34 C35 C36 119.7(6) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? N31 C36 C35 117.9(7) . . ? N31 C36 H36 121.0 . . ? C35 C36 H36 121.0 . . ? O372 C37 O371 123.3(5) . . ? O372 C37 C32 117.8(5) . . ? O371 C37 C32 118.9(5) . . ? C33 O331 Eu 138.7(4) . . ? C37 O371 Eu 139.7(4) . . ? C37 O372 Eu 166.7(4) . 4_575 ? Eu O100 H101 120(4) . . ? Eu O100 H102 134(4) . . ? H101 O100 H102 105.0(18) . . ? H201 O200 H202 105.1(18) . . ? H301 O300 H302 105.2(18) . . ? H401 O400 H402 104.9(18) . . ? _diffrn_measured_fraction_theta_max 0.711 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.711 _refine_diff_density_max 1.188 _refine_diff_density_min -0.914 _refine_diff_density_rms 0.120 #===END