# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ; College of Chemistry and Chemical Engineering, Jiangxi Normal University, Nanchang, Jiangxi 330022, P. R. China ; _publ_contact_author_email qyliuchemistry@gmail.com _publ_contact_author_fax +86-791-8120380 _publ_contact_author_phone +86-791-8120380 #TrackingRef 'LnDHBDC.cif' _publ_contact_author_name 'Qing-Yan Liu' _publ_requested_coeditor_name ? _publ_author_name 'Qing-Yan Liu' # Attachment '- CdMPTRZ.cif' data_{[La2(DHBDC)3(DMF)4](DMF)2}n _database_code_depnum_ccdc_archive 'CCDC 823998' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H54 La2 N6 O24' _chemical_formula_weight 1304.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 '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' _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 10.534(4) _cell_length_b 11.300(4) _cell_length_c 12.661(5) _cell_angle_alpha 101.901(5) _cell_angle_beta 108.730(5) _cell_angle_gamma 99.044(4) _cell_volume 1355.4(9) _cell_formula_units_Z 1 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 4198 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 28.90 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 654 _exptl_absorpt_coefficient_mu 1.639 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.512 _exptl_absorpt_correction_T_max 0.711 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'APEXII CCD' _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 8442 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 29.08 _reflns_number_total 6249 _reflns_number_gt 5540 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+0.4903P] 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 6249 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1039 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 La1 La 0.103198(19) 0.544399(17) 0.682324(17) 0.02578(8) Uani 1 1 d . . . O1 O -0.0160(3) 0.3228(2) 0.5875(3) 0.0426(7) Uani 1 1 d . . . O2 O -0.0813(3) 0.2688(2) 0.3950(3) 0.0454(7) Uani 1 1 d . . . O3 O -0.0624(5) 0.0517(3) 0.2885(3) 0.0788(14) Uani 1 1 d . . . H3 H -0.0739 0.1225 0.2934 0.118 Uiso 1 1 calc R . . O4 O 0.1507(3) 0.4935(3) 0.5011(3) 0.0372(6) Uani 1 1 d . . . O5 O 0.1330(3) 0.4313(3) 0.3203(3) 0.0478(8) Uani 1 1 d . . . O6 O 0.3441(3) 0.3988(4) 0.2676(3) 0.0681(12) Uani 1 1 d . . . H6A H 0.2619 0.3942 0.2552 0.102 Uiso 1 1 calc R . . O7 O 0.1856(3) 0.7485(3) 0.8511(3) 0.0470(7) Uani 1 1 d . . . O8 O 0.3445(3) 0.6941(3) 0.7865(3) 0.0508(8) Uani 1 1 d . . . O9 O 0.2377(18) 0.9804(13) 0.9845(15) 0.164(7) Uani 0.50 1 d P . . H9A H 0.1859 0.9133 0.9427 0.246 Uiso 0.50 1 calc PR . . O9A O 0.6024(5) 0.8234(4) 0.8909(5) 0.0313(12) Uani 0.50 1 d P . . H9A1 H 0.5431 0.7762 0.8311 0.047 Uiso 0.50 1 calc PR . . O10 O 0.2808(4) 0.4222(4) 0.7448(4) 0.0681(11) Uani 1 1 d . . . O11 O 0.0630(4) 0.4634(3) 0.8422(3) 0.0564(9) Uani 1 1 d . . . O12 O 0.3784(10) 0.7637(10) 0.3574(8) 0.189(4) Uani 1 1 d . . . C1 C -0.0319(5) 0.0299(4) 0.3937(4) 0.0448(10) Uani 1 1 d . . . C2 C -0.0229(4) 0.1173(3) 0.4942(4) 0.0361(9) Uani 1 1 d . . . C3 C 0.0085(5) 0.0853(4) 0.5972(4) 0.0463(11) Uani 1 1 d . . . H3A H 0.0142 0.1435 0.6633 0.056 Uiso 1 1 calc R . . C4 C -0.0414(4) 0.2463(3) 0.4929(4) 0.0365(9) Uani 1 1 d . . . C5 C 0.4180(4) 0.4489(4) 0.3823(4) 0.0396(9) Uani 1 1 d . . . C6 C 0.3567(4) 0.4856(4) 0.4629(3) 0.0330(8) Uani 1 1 d . . . C7 C 0.4407(4) 0.5368(4) 0.5789(4) 0.0419(10) Uani 1 1 d . . . H7 H 0.4003 0.5623 0.6323 0.050 Uiso 1 1 calc R . . C8 C 0.2062(4) 0.4689(4) 0.4270(4) 0.0343(8) Uani 1 1 d . . . C9 C 0.3625(4) 0.9820(4) 0.9875(4) 0.0393(9) Uani 1 1 d . . . C10 C 0.4070(4) 0.8894(4) 0.9268(3) 0.0356(8) Uani 1 1 d . . . C11 C 0.5459(4) 0.9078(4) 0.9407(4) 0.0396(9) Uani 1 1 d . . . C12 C 0.3045(4) 0.7711(4) 0.8503(3) 0.0368(9) Uani 1 1 d . . . C13 C 0.3898(9) 0.4233(10) 0.7955(8) 0.110(3) Uani 1 1 d . . . H13 H 0.4534 0.4981 0.8121 0.132 Uiso 1 1 calc R . . C14 C 0.5944(11) 0.3690(12) 0.9082(11) 0.151(4) Uani 1 1 d . . . H14A H 0.6320 0.4561 0.9210 0.226 Uiso 1 1 calc R . . H14B H 0.6411 0.3207 0.8687 0.226 Uiso 1 1 calc R . . H14C H 0.6067 0.3515 0.9814 0.226 Uiso 1 1 calc R . . C15 C 0.3714(14) 0.2161(12) 0.8136(12) 0.200(8) Uani 1 1 d . . . H15A H 0.2768 0.2067 0.7663 0.300 Uiso 1 1 calc R . . H15B H 0.3760 0.1981 0.8854 0.300 Uiso 1 1 calc R . . H15C H 0.4108 0.1596 0.7736 0.300 Uiso 1 1 calc R . . C16 C -0.0251(6) 0.3691(6) 0.8290(5) 0.0636(14) Uani 1 1 d . . . H16A H -0.1059 0.3473 0.7639 0.076 Uiso 1 1 calc R . . C17 C -0.1219(10) 0.1887(8) 0.8760(9) 0.116(3) Uani 1 1 d . . . H17A H -0.2010 0.1872 0.8110 0.174 Uiso 1 1 calc R . . H17B H -0.1470 0.1919 0.9428 0.174 Uiso 1 1 calc R . . H17C H -0.0896 0.1149 0.8585 0.174 Uiso 1 1 calc R . . C18 C 0.1050(11) 0.3244(12) 1.0010(9) 0.154(5) Uani 1 1 d . . . H18A H 0.1687 0.3983 1.0065 0.231 Uiso 1 1 calc R . . H18B H 0.1483 0.2557 0.9981 0.231 Uiso 1 1 calc R . . H18C H 0.0785 0.3374 1.0675 0.231 Uiso 1 1 calc R . . C19 C 0.438(3) 0.8009(17) 0.4435(16) 0.37(2) Uani 1 1 d . . . H19 H 0.4896 0.7390 0.4343 0.449 Uiso 1 1 d R . . C20 C 0.457(3) 0.8829(17) 0.615(2) 0.309(17) Uani 1 1 d . . . H20A H 0.3582 0.8599 0.5753 0.464 Uiso 1 1 calc R . . H20B H 0.4869 0.9717 0.6474 0.464 Uiso 1 1 calc R . . H20C H 0.4806 0.8432 0.6766 0.464 Uiso 1 1 calc R . . C21 C 0.660(2) 0.8685(15) 0.587(3) 0.354(19) Uani 1 1 d . . . H21A H 0.6958 0.8472 0.5264 0.531 Uiso 1 1 calc R . . H21B H 0.6854 0.8191 0.6399 0.531 Uiso 1 1 calc R . . H21C H 0.6980 0.9552 0.6275 0.531 Uiso 1 1 calc R . . N1 N 0.4439(7) 0.3360(7) 0.8359(6) 0.092(2) Uani 1 1 d . . . N2 N -0.0132(6) 0.2977(5) 0.8996(4) 0.0711(14) Uani 1 1 d . . . N3 N 0.5192(11) 0.8458(8) 0.5392(9) 0.123(3) Uani 1 1 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 La1 0.02209(11) 0.01952(11) 0.02872(12) 0.00425(8) 0.00263(8) 0.00290(7) O1 0.0590(19) 0.0179(12) 0.0405(16) 0.0025(11) 0.0114(14) 0.0024(12) O2 0.061(2) 0.0240(13) 0.0395(17) 0.0100(12) 0.0028(14) 0.0082(13) O3 0.158(4) 0.0412(19) 0.0390(19) 0.0164(16) 0.025(2) 0.045(2) O4 0.0268(13) 0.0422(15) 0.0430(16) 0.0083(13) 0.0142(12) 0.0109(11) O5 0.0253(14) 0.074(2) 0.0359(16) 0.0061(15) 0.0053(12) 0.0128(14) O6 0.0321(17) 0.116(3) 0.0351(18) -0.009(2) 0.0053(14) 0.0139(19) O7 0.0418(17) 0.0416(16) 0.0389(17) -0.0048(13) 0.0094(13) -0.0091(13) O8 0.0382(16) 0.0391(16) 0.0503(19) -0.0135(14) 0.0056(14) -0.0027(13) O9 0.176(16) 0.101(10) 0.192(17) -0.015(10) 0.093(13) -0.012(10) O9A 0.015(2) 0.020(2) 0.039(3) -0.020(2) 0.004(2) -0.0016(17) O10 0.045(2) 0.078(3) 0.092(3) 0.044(2) 0.015(2) 0.0367(19) O11 0.070(2) 0.052(2) 0.048(2) 0.0197(16) 0.0232(18) 0.0074(17) O12 0.174(8) 0.206(10) 0.126(7) 0.053(7) -0.013(6) 0.008(7) C1 0.069(3) 0.0264(19) 0.036(2) 0.0127(17) 0.011(2) 0.0147(19) C2 0.043(2) 0.0194(16) 0.039(2) 0.0078(15) 0.0063(17) 0.0073(15) C3 0.071(3) 0.0240(19) 0.033(2) 0.0021(16) 0.008(2) 0.0127(19) C4 0.039(2) 0.0186(16) 0.043(2) 0.0086(16) 0.0065(17) 0.0008(14) C5 0.0291(19) 0.054(3) 0.028(2) 0.0026(18) 0.0062(16) 0.0082(17) C6 0.0244(17) 0.038(2) 0.0323(19) 0.0059(16) 0.0073(15) 0.0080(15) C7 0.032(2) 0.057(3) 0.036(2) 0.0056(19) 0.0135(17) 0.0139(18) C8 0.0270(18) 0.035(2) 0.040(2) 0.0098(17) 0.0115(16) 0.0100(15) C9 0.0274(19) 0.037(2) 0.040(2) 0.0025(18) 0.0051(17) -0.0011(16) C10 0.037(2) 0.0287(18) 0.0300(19) 0.0026(15) 0.0061(16) -0.0018(15) C11 0.040(2) 0.033(2) 0.036(2) -0.0004(17) 0.0100(18) 0.0026(16) C12 0.035(2) 0.0305(19) 0.030(2) 0.0034(16) 0.0012(16) -0.0035(15) C13 0.121(7) 0.157(8) 0.119(7) 0.095(6) 0.067(6) 0.095(7) C14 0.105(8) 0.157(10) 0.165(11) 0.044(9) 0.014(7) 0.040(7) C15 0.174(13) 0.165(12) 0.185(13) 0.109(11) -0.037(10) -0.032(10) C16 0.064(3) 0.078(4) 0.053(3) 0.029(3) 0.019(3) 0.018(3) C17 0.123(7) 0.097(6) 0.128(8) 0.052(6) 0.048(6) -0.010(5) C18 0.137(9) 0.188(11) 0.113(8) 0.097(8) -0.010(7) 0.019(8) C19 0.63(5) 0.136(13) 0.126(13) 0.074(12) -0.10(2) -0.08(2) C20 0.47(4) 0.189(19) 0.44(4) 0.12(2) 0.35(4) 0.10(2) C21 0.19(2) 0.135(13) 0.64(5) 0.16(2) 0.01(3) -0.007(13) N1 0.095(4) 0.117(5) 0.109(5) 0.076(4) 0.045(4) 0.074(4) N2 0.093(4) 0.065(3) 0.062(3) 0.034(3) 0.029(3) 0.012(3) N3 0.137(7) 0.090(5) 0.112(6) 0.042(5) 0.016(6) -0.012(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 La1 O1 2.468(3) . ? La1 O4 2.475(3) . ? La1 O11 2.512(3) . ? La1 O2 2.515(3) 2_566 ? La1 O10 2.519(3) . ? La1 O5 2.537(3) 2_566 ? La1 O8 2.576(3) . ? La1 O7 2.605(3) . ? La1 O4 2.824(3) 2_566 ? O1 C4 1.244(5) . ? O2 C4 1.268(5) . ? O2 La1 2.515(3) 2_566 ? O3 C1 1.350(6) . ? O3 H3 0.8200 . ? O4 C8 1.263(5) . ? O4 La1 2.824(3) 2_566 ? O5 C8 1.262(5) . ? O5 La1 2.537(3) 2_566 ? O6 C5 1.354(5) . ? O6 H6A 0.8200 . ? O7 C12 1.242(5) . ? O8 C12 1.276(5) . ? O9 C9 1.300(17) . ? O9 H9A 0.8200 . ? O9A C11 1.354(6) . ? O9A H9A1 0.8200 . ? O10 C13 1.118(8) . ? O11 C16 1.241(7) . ? O12 C19 1.025(16) . ? C1 C3 1.384(6) 2_556 ? C1 C2 1.407(6) . ? C2 C3 1.376(6) . ? C2 C4 1.504(5) . ? C3 C1 1.384(6) 2_556 ? C3 H3A 0.9300 . ? C5 C7 1.380(6) 2_666 ? C5 C6 1.401(6) . ? C6 C7 1.389(6) . ? C6 C8 1.471(5) . ? C7 C5 1.380(6) 2_666 ? C7 H7 0.9300 . ? C8 La1 3.070(4) 2_566 ? C9 C11 1.379(6) 2_677 ? C9 C10 1.399(6) . ? C10 C11 1.393(6) . ? C10 C12 1.494(5) . ? C11 C9 1.379(6) 2_677 ? C13 N1 1.325(8) . ? C13 H13 0.9300 . ? C14 N1 1.494(11) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N1 1.370(12) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N2 1.312(7) . ? C16 H16A 0.9300 . ? C17 N2 1.450(9) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N2 1.409(10) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N3 1.183(17) . ? C19 H19 0.9601 . ? C20 N3 1.368(18) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N3 1.37(2) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 La1 O4 74.92(10) . . ? O1 La1 O11 75.81(11) . . ? O4 La1 O11 145.52(11) . . ? O1 La1 O2 129.67(10) . 2_566 ? O4 La1 O2 75.14(10) . 2_566 ? O11 La1 O2 138.85(11) . 2_566 ? O1 La1 O10 73.84(13) . . ? O4 La1 O10 81.82(12) . . ? O11 La1 O10 72.84(13) . . ? O2 La1 O10 138.81(12) 2_566 . ? O1 La1 O5 84.24(11) . 2_566 ? O4 La1 O5 121.46(9) . 2_566 ? O11 La1 O5 72.77(12) . 2_566 ? O2 La1 O5 78.16(11) 2_566 2_566 ? O10 La1 O5 142.74(13) . 2_566 ? O1 La1 O8 142.79(11) . . ? O4 La1 O8 90.12(10) . . ? O11 La1 O8 102.54(12) . . ? O2 La1 O8 75.95(11) 2_566 . ? O10 La1 O8 70.36(13) . . ? O5 La1 O8 131.54(11) 2_566 . ? O1 La1 O7 153.68(11) . . ? O4 La1 O7 131.30(10) . . ? O11 La1 O7 78.62(11) . . ? O2 La1 O7 69.07(11) 2_566 . ? O10 La1 O7 104.41(13) . . ? O5 La1 O7 82.35(10) 2_566 . ? O8 La1 O7 50.27(10) . . ? O1 La1 O4 66.24(9) . 2_566 ? O4 La1 O4 73.79(9) . 2_566 ? O11 La1 O4 110.02(11) . 2_566 ? O2 La1 O4 67.04(9) 2_566 2_566 ? O10 La1 O4 137.24(12) . 2_566 ? O5 La1 O4 47.84(9) 2_566 2_566 ? O8 La1 O4 142.23(10) . 2_566 ? O7 La1 O4 118.13(9) . 2_566 ? O1 La1 C12 160.67(11) . . ? O4 La1 C12 110.95(11) . . ? O11 La1 C12 91.70(12) . . ? O2 La1 C12 69.19(11) 2_566 . ? O10 La1 C12 88.52(14) . . ? O5 La1 C12 106.39(12) 2_566 . ? O8 La1 C12 25.53(11) . . ? O7 La1 C12 24.82(11) . . ? O4 La1 C12 132.78(10) 2_566 . ? O1 La1 C8 72.72(11) . 2_566 ? O4 La1 C8 98.07(10) . 2_566 ? O11 La1 C8 90.24(12) . 2_566 ? O2 La1 C8 72.57(11) 2_566 2_566 ? O10 La1 C8 145.32(12) . 2_566 ? O5 La1 C8 23.65(10) 2_566 2_566 ? O8 La1 C8 144.08(11) . 2_566 ? O7 La1 C8 101.43(10) . 2_566 ? O4 La1 C8 24.29(10) 2_566 2_566 ? C12 La1 C8 122.80(11) . 2_566 ? C4 O1 La1 136.9(3) . . ? C4 O2 La1 137.8(3) . 2_566 ? C1 O3 H3 109.5 . . ? C8 O4 La1 164.9(3) . . ? C8 O4 La1 88.8(2) . 2_566 ? La1 O4 La1 106.21(9) . 2_566 ? C8 O5 La1 102.6(2) . 2_566 ? C5 O6 H6A 109.5 . . ? C12 O7 La1 93.5(2) . . ? C12 O8 La1 94.0(2) . . ? C9 O9 H9A 109.5 . . ? C11 O9A H9A1 109.5 . . ? C13 O10 La1 148.0(6) . . ? C16 O11 La1 125.7(4) . . ? O3 C1 C3 118.0(4) . 2_556 ? O3 C1 C2 123.8(4) . . ? C3 C1 C2 118.2(4) 2_556 . ? C3 C2 C1 119.1(4) . . ? C3 C2 C4 119.2(4) . . ? C1 C2 C4 121.6(4) . . ? C2 C3 C1 122.7(4) . 2_556 ? C2 C3 H3A 118.7 . . ? C1 C3 H3A 118.7 2_556 . ? O1 C4 O2 125.1(4) . . ? O1 C4 C2 117.8(4) . . ? O2 C4 C2 117.1(4) . . ? O6 C5 C7 118.4(4) . 2_666 ? O6 C5 C6 122.7(4) . . ? C7 C5 C6 118.9(4) 2_666 . ? C7 C6 C5 118.7(4) . . ? C7 C6 C8 120.0(4) . . ? C5 C6 C8 121.3(4) . . ? C5 C7 C6 122.4(4) 2_666 . ? C5 C7 H7 118.8 2_666 . ? C6 C7 H7 118.8 . . ? O5 C8 O4 120.3(3) . . ? O5 C8 C6 118.8(4) . . ? O4 C8 C6 120.9(4) . . ? O5 C8 La1 53.76(19) . 2_566 ? O4 C8 La1 66.9(2) . 2_566 ? C6 C8 La1 169.6(3) . 2_566 ? O9 C9 C11 111.5(7) . 2_677 ? O9 C9 C10 127.7(7) . . ? C11 C9 C10 120.8(4) 2_677 . ? C11 C10 C9 119.6(4) . . ? C11 C10 C12 121.2(4) . . ? C9 C10 C12 119.1(4) . . ? O9A C11 C9 115.3(4) . 2_677 ? O9A C11 C10 125.2(4) . . ? C9 C11 C10 119.6(4) 2_677 . ? O7 C12 O8 121.8(4) . . ? O7 C12 C10 120.5(4) . . ? O8 C12 C10 117.7(4) . . ? O7 C12 La1 61.7(2) . . ? O8 C12 La1 60.4(2) . . ? C10 C12 La1 175.3(3) . . ? O10 C13 N1 130.9(10) . . ? O10 C13 H13 114.6 . . ? N1 C13 H13 114.6 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O11 C16 N2 125.2(6) . . ? O11 C16 H16A 117.4 . . ? N2 C16 H16A 117.4 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O12 C19 N3 173(4) . . ? N3 C19 H19 88.7 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 H21A 109.5 . . ? N3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C13 N1 C15 124.3(9) . . ? C13 N1 C14 118.2(9) . . ? C15 N1 C14 117.5(8) . . ? C16 N2 C18 121.3(6) . . ? C16 N2 C17 121.0(6) . . ? C18 N2 C17 117.7(7) . . ? C19 N3 C20 112(2) . . ? C19 N3 C21 133(2) . . ? C20 N3 C21 115.2(17) . . ? _diffrn_measured_fraction_theta_max 0.859 _diffrn_reflns_theta_full 29.08 _diffrn_measured_fraction_theta_full 0.859 _refine_diff_density_max 1.234 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.111 #===END OF 1 ## Crystallographic Data for compound 2 data_{[Nd2(DHBDC)3(DMF)4](DMF)2}n _database_code_depnum_ccdc_archive 'CCDC 823999' #TrackingRef 'LnDHBDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H54 N6 Nd2 O24' _chemical_formula_weight 1315.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 '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 10.523(3) _cell_length_b 11.184(3) _cell_length_c 12.700(3) _cell_angle_alpha 102.980(3) _cell_angle_beta 109.329(3) _cell_angle_gamma 97.766(3) _cell_volume 1338.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9174 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.41 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 2.004 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.764 _exptl_absorpt_correction_T_max 0.824 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEXII CCD' _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 12606 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.45 _reflns_number_total 6489 _reflns_number_gt 5919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+1.4378P] 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 6489 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Nd1 Nd 0.102327(14) 0.546329(12) 0.681318(12) 0.02544(6) Uani 1 1 d . . . O1 O -0.0170(3) 0.3278(2) 0.5882(2) 0.0398(5) Uani 1 1 d . . . O2 O -0.0770(3) 0.2713(2) 0.3949(2) 0.0421(5) Uani 1 1 d . . . O3 O -0.0528(5) 0.0520(3) 0.2891(2) 0.0752(11) Uani 1 1 d . . . H3 H -0.0645 0.1237 0.2938 0.113 Uiso 1 1 calc R . . O4 O 0.1532(2) 0.4932(2) 0.5074(2) 0.0379(5) Uani 1 1 d . . . O5 O 0.1297(2) 0.4300(3) 0.3243(2) 0.0453(6) Uani 1 1 d . . . O6 O 0.3382(3) 0.3984(4) 0.2670(2) 0.0673(10) Uani 1 1 d . . . H6A H 0.2563 0.3945 0.2560 0.101 Uiso 1 1 calc R . . O7 O 0.1785(3) 0.7520(2) 0.8492(2) 0.0463(6) Uani 1 1 d . . . O8 O 0.3355(3) 0.6918(2) 0.7837(2) 0.0528(7) Uani 1 1 d . . . O9 O 0.2342(5) 0.9846(5) 0.9916(5) 0.0475(12) Uani 0.50 1 d P . . H9A H 0.1819 0.9169 0.9495 0.071 Uiso 0.50 1 calc PR . . O9A O 0.5984(6) 0.8181(6) 0.8880(6) 0.073(2) Uani 0.50 1 d P . . H9A1 H 0.5400 0.7696 0.8275 0.110 Uiso 0.50 1 calc PR . . O10 O 0.2768(3) 0.4228(3) 0.7411(3) 0.0691(9) Uani 1 1 d . . . O11 O 0.0679(3) 0.4714(3) 0.8404(2) 0.0546(7) Uani 1 1 d . . . O12 O 0.3830(9) 0.7695(9) 0.3582(7) 0.188(4) Uani 1 1 d . . . C1 C -0.0273(4) 0.0300(3) 0.3945(3) 0.0435(8) Uani 1 1 d . . . C2 C -0.0220(3) 0.1189(3) 0.4940(3) 0.0352(6) Uani 1 1 d . . . C3 C 0.0040(4) 0.0870(3) 0.5969(3) 0.0441(8) Uani 1 1 d . . . H3A H 0.0059 0.1459 0.6623 0.053 Uiso 1 1 calc R . . C4 C -0.0401(3) 0.2498(3) 0.4932(3) 0.0330(6) Uani 1 1 d . . . C5 C 0.4155(3) 0.4491(4) 0.3826(3) 0.0403(7) Uani 1 1 d . . . C6 C 0.3572(3) 0.4844(3) 0.4659(3) 0.0335(6) Uani 1 1 d . . . C7 C 0.4428(3) 0.5359(4) 0.5819(3) 0.0399(7) Uani 1 1 d . . . H7 H 0.4042 0.5608 0.6371 0.048 Uiso 1 1 calc R . . C8 C 0.2057(3) 0.4686(3) 0.4320(3) 0.0341(6) Uani 1 1 d . . . C9 C 0.3620(3) 0.9854(3) 0.9909(3) 0.0400(7) Uani 1 1 d . . . C10 C 0.4026(3) 0.8901(3) 0.9264(3) 0.0353(6) Uani 1 1 d . . . C11 C 0.5399(4) 0.9045(3) 0.9356(3) 0.0414(7) Uani 1 1 d . . . C12 C 0.2991(3) 0.7709(3) 0.8481(3) 0.0362(7) Uani 1 1 d . . . C13 C 0.3747(11) 0.4124(11) 0.7895(8) 0.155(5) Uani 1 1 d . . . H13 H 0.4396 0.4871 0.8097 0.186 Uiso 1 1 calc R . . C14 C 0.5822(10) 0.3689(11) 0.9032(10) 0.158(4) Uani 1 1 d . . . H14A H 0.6152 0.4567 0.9136 0.237 Uiso 1 1 calc R . . H14B H 0.6322 0.3202 0.8661 0.237 Uiso 1 1 calc R . . H14C H 0.5960 0.3551 0.9777 0.237 Uiso 1 1 calc R . . C15 C 0.3711(13) 0.2070(11) 0.8085(11) 0.211(8) Uani 1 1 d . . . H15A H 0.2751 0.1931 0.7610 0.316 Uiso 1 1 calc R . . H15B H 0.3794 0.1892 0.8808 0.316 Uiso 1 1 calc R . . H15C H 0.4139 0.1524 0.7684 0.316 Uiso 1 1 calc R . . C16 C -0.0211(5) 0.3793(5) 0.8277(4) 0.0581(10) Uani 1 1 d . . . H16A H -0.1046 0.3603 0.7647 0.070 Uiso 1 1 calc R . . C17 C -0.1155(9) 0.1996(7) 0.8756(7) 0.117(3) Uani 1 1 d . . . H17A H -0.1957 0.1971 0.8103 0.176 Uiso 1 1 calc R . . H17B H -0.1386 0.2077 0.9436 0.176 Uiso 1 1 calc R . . H17C H -0.0842 0.1232 0.8595 0.176 Uiso 1 1 calc R . . C18 C 0.1140(10) 0.3282(10) 0.9950(7) 0.159(5) Uani 1 1 d . . . H18A H 0.1786 0.4016 1.0019 0.239 Uiso 1 1 calc R . . H18B H 0.1548 0.2565 0.9877 0.239 Uiso 1 1 calc R . . H18C H 0.0909 0.3412 1.0632 0.239 Uiso 1 1 calc R . . C19 C 0.453(3) 0.7996(14) 0.4454(14) 0.38(2) Uani 1 1 d . . . H19 H 0.5043 0.7378 0.4362 0.455 Uiso 1 1 d R . . C20 C 0.471(3) 0.8758(16) 0.622(2) 0.38(2) Uani 1 1 d . . . H20A H 0.3717 0.8551 0.5879 0.577 Uiso 1 1 calc R . . H20B H 0.5034 0.9645 0.6609 0.577 Uiso 1 1 calc R . . H20C H 0.5013 0.8296 0.6774 0.577 Uiso 1 1 calc R . . C21 C 0.6548(17) 0.8677(15) 0.582(3) 0.41(2) Uani 1 1 d . . . H21A H 0.6847 0.8448 0.5182 0.612 Uiso 1 1 calc R . . H21B H 0.6853 0.8183 0.6344 0.612 Uiso 1 1 calc R . . H21C H 0.6935 0.9555 0.6229 0.612 Uiso 1 1 calc R . . N1 N 0.4357(5) 0.3304(6) 0.8307(5) 0.0894(16) Uani 1 1 d . . . N2 N -0.0061(5) 0.3068(4) 0.8961(4) 0.0687(11) Uani 1 1 d . . . N3 N 0.5194(8) 0.8467(6) 0.5424(6) 0.1057(19) Uani 1 1 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 Nd1 0.02132(8) 0.02041(8) 0.02858(8) 0.00588(5) 0.00335(5) 0.00281(5) O1 0.0523(14) 0.0216(10) 0.0391(12) 0.0063(9) 0.0121(10) 0.0044(9) O2 0.0573(15) 0.0226(10) 0.0371(12) 0.0103(9) 0.0056(10) 0.0075(9) O3 0.154(4) 0.0421(15) 0.0399(14) 0.0208(12) 0.0346(19) 0.0457(19) O4 0.0292(11) 0.0403(12) 0.0475(13) 0.0114(10) 0.0183(10) 0.0113(9) O5 0.0252(11) 0.0625(16) 0.0418(13) 0.0101(11) 0.0074(9) 0.0107(10) O6 0.0294(13) 0.121(3) 0.0335(13) 0.0010(15) 0.0062(10) 0.0106(15) O7 0.0394(13) 0.0434(13) 0.0391(12) -0.0013(10) 0.0101(10) -0.0111(10) O8 0.0359(12) 0.0415(14) 0.0544(15) -0.0129(11) 0.0057(11) -0.0036(10) O9 0.031(2) 0.045(3) 0.051(3) -0.008(2) 0.016(2) -0.0087(19) O9A 0.051(3) 0.053(3) 0.079(4) -0.023(3) 0.011(3) 0.003(3) O10 0.0517(17) 0.076(2) 0.093(2) 0.0477(19) 0.0190(16) 0.0389(16) O11 0.0660(18) 0.0504(16) 0.0460(15) 0.0193(12) 0.0192(13) 0.0041(13) O12 0.186(8) 0.196(8) 0.133(6) 0.063(6) -0.007(5) 0.030(6) C1 0.068(2) 0.0264(15) 0.0339(16) 0.0116(12) 0.0133(15) 0.0128(14) C2 0.0436(17) 0.0202(13) 0.0357(15) 0.0066(11) 0.0088(13) 0.0060(11) C3 0.069(2) 0.0244(15) 0.0336(16) 0.0060(12) 0.0125(15) 0.0144(14) C4 0.0335(14) 0.0193(12) 0.0383(15) 0.0073(11) 0.0058(12) 0.0017(10) C5 0.0287(15) 0.057(2) 0.0297(15) 0.0054(14) 0.0087(12) 0.0090(13) C6 0.0234(13) 0.0399(16) 0.0349(15) 0.0090(12) 0.0091(11) 0.0075(11) C7 0.0289(15) 0.058(2) 0.0330(15) 0.0083(14) 0.0140(12) 0.0122(13) C8 0.0246(13) 0.0364(15) 0.0403(16) 0.0114(12) 0.0098(12) 0.0086(11) C9 0.0327(15) 0.0377(17) 0.0403(17) 0.0058(13) 0.0094(13) -0.0017(12) C10 0.0338(15) 0.0305(15) 0.0300(14) 0.0044(11) 0.0050(12) -0.0043(11) C11 0.0381(17) 0.0360(16) 0.0399(17) 0.0003(13) 0.0115(14) 0.0012(13) C12 0.0348(15) 0.0312(15) 0.0299(14) 0.0048(12) 0.0028(12) -0.0026(12) C13 0.209(10) 0.256(11) 0.130(6) 0.142(7) 0.113(7) 0.195(10) C14 0.118(8) 0.166(10) 0.163(9) 0.035(8) 0.027(7) 0.033(7) C15 0.181(11) 0.182(11) 0.193(12) 0.126(10) -0.034(9) -0.056(9) C16 0.063(3) 0.066(3) 0.048(2) 0.023(2) 0.0215(19) 0.012(2) C17 0.130(6) 0.102(5) 0.129(6) 0.060(5) 0.056(5) -0.006(5) C18 0.146(8) 0.181(10) 0.112(6) 0.100(7) -0.021(6) -0.006(7) C19 0.60(5) 0.137(11) 0.155(12) 0.087(10) -0.13(2) -0.078(18) C20 0.75(6) 0.167(15) 0.52(4) 0.16(2) 0.53(5) 0.17(2) C21 0.133(12) 0.144(12) 0.84(6) 0.19(2) 0.04(2) -0.009(10) N1 0.084(3) 0.123(4) 0.108(4) 0.081(4) 0.046(3) 0.071(3) N2 0.090(3) 0.065(2) 0.059(2) 0.0353(19) 0.029(2) 0.011(2) N3 0.119(5) 0.088(4) 0.098(4) 0.041(3) 0.025(4) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O4 2.408(2) . ? Nd1 O1 2.416(2) . ? Nd1 O2 2.455(2) 2_566 ? Nd1 O11 2.465(3) . ? Nd1 O10 2.468(3) . ? Nd1 O5 2.470(2) 2_566 ? Nd1 O8 2.494(2) . ? Nd1 O7 2.578(2) . ? Nd1 O4 2.847(2) 2_566 ? O1 C4 1.245(4) . ? O2 C4 1.269(4) . ? O2 Nd1 2.455(2) 2_566 ? O3 C1 1.361(4) . ? O3 H3 0.8200 . ? O4 C8 1.253(4) . ? O4 Nd1 2.847(2) 2_566 ? O5 C8 1.270(4) . ? O5 Nd1 2.470(2) 2_566 ? O6 C5 1.360(4) . ? O6 H6A 0.8200 . ? O7 C12 1.263(4) . ? O8 C12 1.254(4) . ? O9 C9 1.348(6) . ? O9 H9A 0.8200 . ? O9A C11 1.350(7) . ? O9A H9A1 0.8200 . ? O10 C13 1.048(8) . ? O11 C16 1.237(5) . ? O12 C19 1.053(13) . ? C1 C3 1.384(4) 2_556 ? C1 C2 1.401(5) . ? C2 C3 1.381(5) . ? C2 C4 1.503(4) . ? C3 C1 1.384(4) 2_556 ? C3 H3A 0.9300 . ? C5 C7 1.381(4) 2_666 ? C5 C6 1.400(5) . ? C6 C7 1.384(4) . ? C6 C8 1.481(4) . ? C7 C5 1.381(4) 2_666 ? C7 H7 0.9300 . ? C8 Nd1 3.043(3) 2_566 ? C9 C10 1.397(5) . ? C9 C11 1.398(4) 2_677 ? C10 C11 1.394(5) . ? C10 C12 1.499(4) . ? C11 C9 1.398(4) 2_677 ? C13 N1 1.296(7) . ? C13 H13 0.9300 . ? C14 N1 1.454(11) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N1 1.376(11) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N2 1.303(6) . ? C16 H16A 0.9300 . ? C17 N2 1.456(8) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N2 1.402(8) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N3 1.150(15) . ? C19 H19 0.9443 . ? C20 N3 1.276(16) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N3 1.312(16) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 Nd1 O1 76.18(8) . . ? O4 Nd1 O2 75.56(8) . 2_566 ? O1 Nd1 O2 129.11(8) . 2_566 ? O4 Nd1 O11 145.57(9) . . ? O1 Nd1 O11 76.06(9) . . ? O2 Nd1 O11 138.63(9) 2_566 . ? O4 Nd1 O10 80.35(10) . . ? O1 Nd1 O10 74.15(11) . . ? O2 Nd1 O10 139.25(11) 2_566 . ? O11 Nd1 O10 72.79(11) . . ? O4 Nd1 O5 122.21(8) . 2_566 ? O1 Nd1 O5 82.42(9) . 2_566 ? O2 Nd1 O5 78.16(9) 2_566 2_566 ? O11 Nd1 O5 73.36(10) . 2_566 ? O10 Nd1 O5 142.46(11) . 2_566 ? O4 Nd1 O8 89.07(9) . . ? O1 Nd1 O8 143.81(9) . . ? O2 Nd1 O8 76.34(9) 2_566 . ? O11 Nd1 O8 101.69(10) . . ? O10 Nd1 O8 70.85(11) . . ? O5 Nd1 O8 132.31(9) 2_566 . ? O4 Nd1 O7 131.51(8) . . ? O1 Nd1 O7 152.28(9) . . ? O2 Nd1 O7 69.22(9) 2_566 . ? O11 Nd1 O7 77.56(9) . . ? O10 Nd1 O7 105.85(11) . . ? O5 Nd1 O7 82.04(8) 2_566 . ? O8 Nd1 O7 51.35(8) . . ? O4 Nd1 O4 74.30(8) . 2_566 ? O1 Nd1 O4 65.55(8) . 2_566 ? O2 Nd1 O4 66.49(7) 2_566 2_566 ? O11 Nd1 O4 111.42(9) . 2_566 ? O10 Nd1 O4 136.23(10) . 2_566 ? O5 Nd1 O4 48.02(7) 2_566 2_566 ? O8 Nd1 O4 141.91(9) . 2_566 ? O7 Nd1 O4 117.72(8) . 2_566 ? O4 Nd1 C12 110.24(9) . . ? O1 Nd1 C12 160.95(9) . . ? O2 Nd1 C12 69.71(9) 2_566 . ? O11 Nd1 C12 90.71(10) . . ? O10 Nd1 C12 89.00(11) . . ? O5 Nd1 C12 107.18(9) 2_566 . ? O8 Nd1 C12 25.54(9) . . ? O7 Nd1 C12 25.86(9) . . ? O4 Nd1 C12 133.06(8) 2_566 . ? O4 Nd1 C8 98.58(8) . 2_566 ? O1 Nd1 C8 71.11(9) . 2_566 ? O2 Nd1 C8 72.39(9) 2_566 2_566 ? O11 Nd1 C8 91.29(10) . 2_566 ? O10 Nd1 C8 144.38(11) . 2_566 ? O5 Nd1 C8 23.86(8) 2_566 2_566 ? O8 Nd1 C8 144.66(9) . 2_566 ? O7 Nd1 C8 101.26(9) . 2_566 ? O4 Nd1 C8 24.27(8) 2_566 2_566 ? C12 Nd1 C8 123.65(9) . 2_566 ? C4 O1 Nd1 135.5(2) . . ? C4 O2 Nd1 137.87(19) . 2_566 ? C1 O3 H3 109.5 . . ? C8 O4 Nd1 167.6(2) . . ? C8 O4 Nd1 86.68(18) . 2_566 ? Nd1 O4 Nd1 105.70(8) . 2_566 ? C8 O5 Nd1 104.3(2) . 2_566 ? C5 O6 H6A 109.5 . . ? C12 O7 Nd1 91.25(19) . . ? C12 O8 Nd1 95.4(2) . . ? C9 O9 H9A 109.5 . . ? C11 O9A H9A1 109.5 . . ? C13 O10 Nd1 153.7(7) . . ? C16 O11 Nd1 125.3(3) . . ? O3 C1 C3 117.5(3) . 2_556 ? O3 C1 C2 123.9(3) . . ? C3 C1 C2 118.6(3) 2_556 . ? C3 C2 C1 119.4(3) . . ? C3 C2 C4 118.7(3) . . ? C1 C2 C4 121.9(3) . . ? C2 C3 C1 122.0(3) . 2_556 ? C2 C3 H3A 119.0 . . ? C1 C3 H3A 119.0 2_556 . ? O1 C4 O2 125.5(3) . . ? O1 C4 C2 117.9(3) . . ? O2 C4 C2 116.6(3) . . ? O6 C5 C7 117.9(3) . 2_666 ? O6 C5 C6 122.7(3) . . ? C7 C5 C6 119.4(3) 2_666 . ? C7 C6 C5 119.4(3) . . ? C7 C6 C8 119.4(3) . . ? C5 C6 C8 121.2(3) . . ? C5 C7 C6 121.3(3) 2_666 . ? C5 C7 H7 119.4 2_666 . ? C6 C7 H7 119.4 . . ? O4 C8 O5 120.5(3) . . ? O4 C8 C6 121.1(3) . . ? O5 C8 C6 118.5(3) . . ? O4 C8 Nd1 69.05(16) . 2_566 ? O5 C8 Nd1 51.87(15) . 2_566 ? C6 C8 Nd1 168.0(2) . 2_566 ? O9 C9 C10 126.9(3) . . ? O9 C9 C11 113.6(4) . 2_677 ? C10 C9 C11 119.5(3) . 2_677 ? C11 C10 C9 120.2(3) . . ? C11 C10 C12 119.6(3) . . ? C9 C10 C12 120.2(3) . . ? O9A C11 C10 127.7(4) . . ? O9A C11 C9 111.8(4) . 2_677 ? C10 C11 C9 120.3(3) . 2_677 ? O8 C12 O7 121.7(3) . . ? O8 C12 C10 118.7(3) . . ? O7 C12 C10 119.6(3) . . ? O8 C12 Nd1 59.03(16) . . ? O7 C12 Nd1 62.89(16) . . ? C10 C12 Nd1 175.4(2) . . ? O10 C13 N1 141.2(13) . . ? O10 C13 H13 109.4 . . ? N1 C13 H13 109.4 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O11 C16 N2 124.7(4) . . ? O11 C16 H16A 117.7 . . ? N2 C16 H16A 117.7 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O12 C19 N3 170(3) . . ? O12 C19 H19 95.3 . . ? N3 C19 H19 94.8 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 H21A 109.5 . . ? N3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C13 N1 C15 124.1(9) . . ? C13 N1 C14 118.8(9) . . ? C15 N1 C14 117.1(7) . . ? C16 N2 C18 122.6(5) . . ? C16 N2 C17 121.7(5) . . ? C18 N2 C17 115.8(6) . . ? C19 N3 C20 124(2) . . ? C19 N3 C21 122(2) . . ? C20 N3 C21 113.5(18) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.45 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.227 _refine_diff_density_min -1.599 _refine_diff_density_rms 0.097 #===END OF 2 ## Crystallographic Data for compound 3 data_{[Sm2(DHBDC)3(DMF)4](DMF)2}n _database_code_depnum_ccdc_archive 'CCDC 824000' #TrackingRef 'LnDHBDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H54 N6 O24 Sm2' _chemical_formula_weight 1327.63 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5152(5) _cell_length_b 11.1058(5) _cell_length_c 12.7396(6) _cell_angle_alpha 103.891(2) _cell_angle_beta 109.709(2) _cell_angle_gamma 96.684(2) _cell_volume 1327.53(11) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5308 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 28.36 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 2.276 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.504 _exptl_absorpt_correction_T_max 0.642 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEXII CCD' _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 7593 _diffrn_reflns_av_R_equivalents 0.0123 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.36 _reflns_number_total 5800 _reflns_number_gt 5346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+1.1433P] 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 5800 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Sm1 Sm 0.102067(16) 0.547772(14) 0.681555(13) 0.02483(7) Uani 1 1 d . . . O1 O -0.0171(3) 0.3321(2) 0.5878(2) 0.0377(6) Uani 1 1 d . . . O2 O -0.0741(3) 0.2733(2) 0.3945(2) 0.0402(6) Uani 1 1 d . . . O3 O -0.0478(5) 0.0511(3) 0.2900(3) 0.0710(12) Uani 1 1 d . . . H3 H -0.0597 0.1236 0.2950 0.106 Uiso 1 1 calc R . . O4 O 0.1565(3) 0.4926(3) 0.5128(3) 0.0374(6) Uani 1 1 d . . . O5 O 0.1277(3) 0.4285(3) 0.3281(2) 0.0426(7) Uani 1 1 d . . . O6 O 0.3343(3) 0.3974(4) 0.2669(3) 0.0653(11) Uani 1 1 d . . . H6A H 0.2525 0.3939 0.2568 0.098 Uiso 1 1 calc R . . O7 O 0.1759(3) 0.7557(3) 0.8494(2) 0.0426(7) Uani 1 1 d . . . O8 O 0.3305(3) 0.6898(3) 0.7826(3) 0.0528(8) Uani 1 1 d . . . O9 O 0.2362(4) 0.9873(4) 0.9971(4) 0.0739(12) Uani 1 1 d . . . H9A H 0.1846 0.9191 0.9543 0.111 Uiso 1 1 calc R . . O10 O 0.2728(4) 0.4217(4) 0.7408(4) 0.0686(11) Uani 1 1 d . . . O11 O 0.0697(4) 0.4774(3) 0.8396(3) 0.0511(8) Uani 1 1 d . . . O12 O 0.3829(11) 0.7688(10) 0.3593(8) 0.173(4) Uani 1 1 d . . . C1 C -0.0242(5) 0.0293(4) 0.3946(3) 0.0402(9) Uani 1 1 d . . . C2 C -0.0218(4) 0.1203(3) 0.4935(3) 0.0336(8) Uani 1 1 d . . . C3 C 0.0025(5) 0.0883(4) 0.5971(3) 0.0417(9) Uani 1 1 d . . . H3A H 0.0042 0.1486 0.6626 0.050 Uiso 1 1 calc R . . C4 C -0.0397(4) 0.2519(3) 0.4923(3) 0.0327(8) Uani 1 1 d . . . C5 C 0.4134(4) 0.4485(4) 0.3824(3) 0.0384(9) Uani 1 1 d . . . C6 C 0.3568(4) 0.4844(4) 0.4677(3) 0.0326(7) Uani 1 1 d . . . C7 C 0.4454(4) 0.5357(4) 0.5840(3) 0.0381(9) Uani 1 1 d . . . H7 H 0.4084 0.5600 0.6407 0.046 Uiso 1 1 calc R . . C8 C 0.2058(4) 0.4678(3) 0.4356(3) 0.0325(7) Uani 1 1 d . . . C9 C 0.3640(4) 0.9888(4) 0.9952(3) 0.0392(9) Uani 1 1 d . . . C10 C 0.4000(4) 0.8910(3) 0.9266(3) 0.0346(8) Uani 1 1 d . . . C11 C 0.5361(4) 0.9027(4) 0.9321(3) 0.0405(9) Uani 1 1 d . . . H11 H 0.5599 0.8372 0.8867 0.049 Uiso 1 1 calc R . . C12 C 0.2957(4) 0.7722(4) 0.8478(3) 0.0357(8) Uani 1 1 d . . . C13 C 0.3688(14) 0.4088(13) 0.7877(9) 0.154(5) Uani 1 1 d . . . H13 H 0.4329 0.4837 0.8073 0.185 Uiso 1 1 calc R . . C14 C 0.5801(13) 0.3670(13) 0.8980(12) 0.164(5) Uani 1 1 d . . . H14A H 0.6120 0.4551 0.9079 0.246 Uiso 1 1 calc R . . H14B H 0.6281 0.3166 0.8586 0.246 Uiso 1 1 calc R . . H14C H 0.5977 0.3543 0.9731 0.246 Uiso 1 1 calc R . . C15 C 0.3727(13) 0.2019(12) 0.8058(11) 0.174(6) Uani 1 1 d . . . H15A H 0.2762 0.1865 0.7582 0.261 Uiso 1 1 calc R . . H15B H 0.3828 0.1838 0.8778 0.261 Uiso 1 1 calc R . . H15C H 0.4169 0.1482 0.7650 0.261 Uiso 1 1 calc R . . C16 C -0.0194(6) 0.3852(5) 0.8271(4) 0.0549(12) Uani 1 1 d . . . H16A H -0.1043 0.3676 0.7655 0.066 Uiso 1 1 calc R . . C17 C -0.1114(10) 0.2063(8) 0.8749(8) 0.110(3) Uani 1 1 d . . . H17A H -0.1919 0.2040 0.8094 0.165 Uiso 1 1 calc R . . H17B H -0.1336 0.2174 0.9432 0.165 Uiso 1 1 calc R . . H17C H -0.0810 0.1281 0.8591 0.165 Uiso 1 1 calc R . . C18 C 0.1219(11) 0.3321(10) 0.9918(8) 0.144(5) Uani 1 1 d . . . H18A H 0.1856 0.4050 0.9977 0.216 Uiso 1 1 calc R . . H18B H 0.1620 0.2588 0.9824 0.216 Uiso 1 1 calc R . . H18C H 0.1021 0.3464 1.0615 0.216 Uiso 1 1 calc R . . C19 C 0.446(3) 0.8038(16) 0.4493(16) 0.36(2) Uani 1 1 d . . . H19 H 0.4971 0.7419 0.4401 0.428 Uiso 1 1 d R . . C20 C 0.478(4) 0.8788(18) 0.628(3) 0.38(2) Uani 1 1 d . . . H20A H 0.3785 0.8604 0.5975 0.577 Uiso 1 1 calc R . . H20B H 0.5124 0.9682 0.6668 0.577 Uiso 1 1 calc R . . H20C H 0.5113 0.8321 0.6819 0.577 Uiso 1 1 calc R . . C21 C 0.6518(19) 0.8719(16) 0.582(3) 0.42(3) Uani 1 1 d . . . H21A H 0.6800 0.8482 0.5173 0.625 Uiso 1 1 calc R . . H21B H 0.6876 0.8248 0.6356 0.625 Uiso 1 1 calc R . . H21C H 0.6869 0.9612 0.6216 0.625 Uiso 1 1 calc R . . N1 N 0.4344(6) 0.3297(6) 0.8297(5) 0.0808(16) Uani 1 1 d . . . N2 N -0.0019(6) 0.3114(4) 0.8944(4) 0.0644(12) Uani 1 1 d . . . N3 N 0.5184(9) 0.8471(7) 0.5450(8) 0.104(2) Uani 1 1 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 Sm1 0.02009(11) 0.01942(9) 0.02868(10) 0.00665(6) 0.00274(7) 0.00173(6) O1 0.0471(17) 0.0197(11) 0.0377(14) 0.0049(10) 0.0098(12) 0.0023(11) O2 0.0522(18) 0.0230(12) 0.0368(14) 0.0114(11) 0.0057(12) 0.0045(12) O3 0.141(4) 0.0430(18) 0.0407(17) 0.0226(15) 0.035(2) 0.041(2) O4 0.0270(14) 0.0379(14) 0.0506(16) 0.0127(12) 0.0181(12) 0.0098(11) O5 0.0237(14) 0.0554(18) 0.0413(15) 0.0115(13) 0.0053(11) 0.0077(13) O6 0.0274(16) 0.118(3) 0.0321(15) 0.0018(18) 0.0055(12) 0.0087(18) O7 0.0370(16) 0.0386(15) 0.0386(14) 0.0023(12) 0.0097(12) -0.0097(12) O8 0.0309(16) 0.0444(17) 0.0538(18) -0.0125(14) 0.0034(13) -0.0052(13) O9 0.050(2) 0.067(3) 0.083(3) -0.009(2) 0.028(2) -0.0096(19) O10 0.049(2) 0.079(3) 0.089(3) 0.049(2) 0.0150(19) 0.040(2) O11 0.065(2) 0.0476(17) 0.0403(15) 0.0192(14) 0.0172(14) 0.0044(16) O12 0.189(9) 0.183(9) 0.116(6) 0.056(6) 0.010(6) 0.046(7) C1 0.061(3) 0.0257(17) 0.0307(18) 0.0105(14) 0.0117(17) 0.0108(17) C2 0.039(2) 0.0200(15) 0.0349(18) 0.0081(13) 0.0071(15) 0.0040(14) C3 0.062(3) 0.0247(17) 0.0329(18) 0.0066(14) 0.0116(18) 0.0128(18) C4 0.035(2) 0.0198(15) 0.0375(18) 0.0090(14) 0.0078(15) 0.0014(14) C5 0.0260(19) 0.055(2) 0.0293(17) 0.0075(17) 0.0079(14) 0.0076(17) C6 0.0225(18) 0.0377(19) 0.0356(18) 0.0098(15) 0.0096(14) 0.0054(15) C7 0.0248(19) 0.055(2) 0.0319(18) 0.0072(17) 0.0120(14) 0.0093(17) C8 0.0244(18) 0.0312(17) 0.0424(19) 0.0134(15) 0.0108(15) 0.0082(14) C9 0.030(2) 0.039(2) 0.0390(19) 0.0061(16) 0.0076(15) -0.0031(16) C10 0.033(2) 0.0274(17) 0.0303(17) 0.0022(14) 0.0047(14) -0.0069(15) C11 0.038(2) 0.0344(19) 0.0376(19) 0.0005(16) 0.0098(16) -0.0020(17) C12 0.034(2) 0.0291(17) 0.0300(17) 0.0046(14) 0.0012(14) -0.0041(15) C13 0.222(13) 0.243(13) 0.125(7) 0.140(9) 0.118(8) 0.192(12) C14 0.121(10) 0.159(12) 0.164(11) 0.019(9) 0.022(8) 0.013(8) C15 0.155(11) 0.166(12) 0.153(10) 0.096(9) -0.013(8) -0.032(9) C16 0.065(3) 0.059(3) 0.045(2) 0.022(2) 0.022(2) 0.010(2) C17 0.122(7) 0.095(6) 0.129(7) 0.063(5) 0.056(6) -0.003(5) C18 0.148(9) 0.141(9) 0.098(6) 0.077(6) -0.026(6) -0.001(7) C19 0.63(5) 0.121(12) 0.126(12) 0.066(10) -0.08(2) -0.009(19) C20 0.82(7) 0.165(17) 0.45(4) 0.15(2) 0.53(5) 0.18(3) C21 0.131(14) 0.117(12) 0.84(7) 0.17(3) -0.02(3) -0.022(11) N1 0.070(4) 0.104(4) 0.101(4) 0.068(4) 0.035(3) 0.055(3) N2 0.089(4) 0.055(3) 0.056(2) 0.029(2) 0.029(2) 0.011(2) N3 0.116(6) 0.082(4) 0.112(5) 0.045(4) 0.034(5) 0.009(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 Sm1 O4 2.367(3) . ? Sm1 O1 2.378(2) . ? Sm1 O2 2.418(3) 2_566 ? Sm1 O5 2.426(3) 2_566 ? Sm1 O10 2.436(4) . ? Sm1 O11 2.437(3) . ? Sm1 O8 2.444(3) . ? Sm1 O7 2.569(3) . ? Sm1 C12 2.867(3) . ? Sm1 O4 2.893(3) 2_566 ? Sm1 C8 3.037(4) 2_566 ? O1 C4 1.250(4) . ? O2 C4 1.264(4) . ? O2 Sm1 2.418(3) 2_566 ? O3 C1 1.356(5) . ? O3 H3 0.8200 . ? O4 C8 1.249(5) . ? O4 Sm1 2.893(3) 2_566 ? O5 C8 1.270(5) . ? O5 Sm1 2.426(3) 2_566 ? O6 C5 1.358(5) . ? O6 H6A 0.8200 . ? O7 C12 1.260(5) . ? O8 C12 1.256(5) . ? O9 C9 1.350(6) . ? O9 H9A 0.8200 . ? O10 C13 1.032(10) . ? O11 C16 1.244(6) . ? O12 C19 1.057(16) . ? C1 C3 1.374(5) 2_556 ? C1 C2 1.404(5) . ? C2 C3 1.397(5) . ? C2 C4 1.499(5) . ? C3 C1 1.374(5) 2_556 ? C3 H3A 0.9300 . ? C5 C7 1.376(6) 2_666 ? C5 C6 1.406(5) . ? C6 C7 1.388(5) . ? C6 C8 1.477(5) . ? C7 C5 1.376(6) 2_666 ? C7 H7 0.9300 . ? C8 Sm1 3.037(4) 2_566 ? C9 C11 1.388(5) 2_677 ? C9 C10 1.396(6) . ? C10 C11 1.398(6) . ? C10 C12 1.495(5) . ? C11 C9 1.388(5) 2_677 ? C11 H11 0.9300 . ? C13 N1 1.285(9) . ? C13 H13 0.9300 . ? C14 N1 1.434(13) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N1 1.404(12) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N2 1.306(6) . ? C16 H16A 0.9300 . ? C17 N2 1.451(8) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N2 1.411(9) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N3 1.143(17) . ? C19 H19 0.9321 . ? C20 N3 1.26(4) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N3 1.291(18) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 Sm1 O1 76.64(9) . . ? O4 Sm1 O2 75.84(10) . 2_566 ? O1 Sm1 O2 128.05(9) . 2_566 ? O4 Sm1 O5 122.45(10) . 2_566 ? O1 Sm1 O5 81.14(11) . 2_566 ? O2 Sm1 O5 77.83(11) 2_566 2_566 ? O4 Sm1 O10 79.71(12) . . ? O1 Sm1 O10 74.23(13) . . ? O2 Sm1 O10 140.28(13) 2_566 . ? O5 Sm1 O10 141.86(13) 2_566 . ? O4 Sm1 O11 145.58(11) . . ? O1 Sm1 O11 76.70(10) . . ? O2 Sm1 O11 138.44(11) 2_566 . ? O5 Sm1 O11 73.92(11) 2_566 . ? O10 Sm1 O11 72.38(13) . . ? O4 Sm1 O8 88.00(10) . . ? O1 Sm1 O8 144.37(11) . . ? O2 Sm1 O8 76.83(12) 2_566 . ? O5 Sm1 O8 133.25(11) 2_566 . ? O10 Sm1 O8 71.46(14) . . ? O11 Sm1 O8 101.45(12) . . ? O4 Sm1 O7 131.25(9) . . ? O1 Sm1 O7 152.09(9) . . ? O2 Sm1 O7 69.54(9) 2_566 . ? O5 Sm1 O7 82.61(10) 2_566 . ? O10 Sm1 O7 106.46(13) . . ? O11 Sm1 O7 77.07(10) . . ? O8 Sm1 O7 51.82(10) . . ? O4 Sm1 C12 109.54(10) . . ? O1 Sm1 C12 161.73(11) . . ? O2 Sm1 C12 70.07(10) 2_566 . ? O5 Sm1 C12 107.89(12) 2_566 . ? O10 Sm1 C12 89.71(14) . . ? O11 Sm1 C12 90.35(11) . . ? O8 Sm1 C12 25.81(11) . . ? O7 Sm1 C12 26.06(11) . . ? O4 Sm1 O4 74.85(9) . 2_566 ? O1 Sm1 O4 64.88(9) . 2_566 ? O2 Sm1 O4 65.81(9) 2_566 2_566 ? O5 Sm1 O4 47.69(8) 2_566 2_566 ? O10 Sm1 O4 135.58(12) . 2_566 ? O11 Sm1 O4 112.19(10) . 2_566 ? O8 Sm1 O4 141.57(11) . 2_566 ? O7 Sm1 O4 117.73(9) . 2_566 ? C12 Sm1 O4 132.94(10) . 2_566 ? O4 Sm1 C8 99.00(10) . 2_566 ? O1 Sm1 C8 69.89(10) . 2_566 ? O2 Sm1 C8 72.05(10) 2_566 2_566 ? O5 Sm1 C8 23.67(10) 2_566 2_566 ? O10 Sm1 C8 143.30(13) . 2_566 ? O11 Sm1 C8 91.85(11) . 2_566 ? O8 Sm1 C8 145.18(11) . 2_566 ? O7 Sm1 C8 101.67(10) . 2_566 ? C12 Sm1 C8 124.14(11) . 2_566 ? O4 Sm1 C8 24.15(9) 2_566 2_566 ? C4 O1 Sm1 135.5(2) . . ? C4 O2 Sm1 138.4(2) . 2_566 ? C1 O3 H3 109.5 . . ? C8 O4 Sm1 170.4(3) . . ? C8 O4 Sm1 84.4(2) . 2_566 ? Sm1 O4 Sm1 105.15(9) . 2_566 ? C8 O5 Sm1 106.2(2) . 2_566 ? C5 O6 H6A 109.5 . . ? C12 O7 Sm1 90.3(2) . . ? C12 O8 Sm1 96.3(2) . . ? C9 O9 H9A 109.5 . . ? C13 O10 Sm1 154.4(9) . . ? C16 O11 Sm1 125.4(3) . . ? O3 C1 C3 117.9(4) . 2_556 ? O3 C1 C2 123.3(3) . . ? C3 C1 C2 118.9(3) 2_556 . ? C3 C2 C1 118.9(3) . . ? C3 C2 C4 119.1(3) . . ? C1 C2 C4 122.0(3) . . ? C1 C3 C2 122.2(4) 2_556 . ? C1 C3 H3A 118.9 2_556 . ? C2 C3 H3A 118.9 . . ? O1 C4 O2 125.4(3) . . ? O1 C4 C2 117.8(3) . . ? O2 C4 C2 116.9(3) . . ? O6 C5 C7 117.8(3) . 2_666 ? O6 C5 C6 122.8(4) . . ? C7 C5 C6 119.4(3) 2_666 . ? C7 C6 C5 119.0(3) . . ? C7 C6 C8 119.9(3) . . ? C5 C6 C8 121.2(3) . . ? C5 C7 C6 121.6(3) 2_666 . ? C5 C7 H7 119.2 2_666 . ? C6 C7 H7 119.2 . . ? O4 C8 O5 121.0(4) . . ? O4 C8 C6 120.5(3) . . ? O5 C8 C6 118.5(3) . . ? O4 C8 Sm1 71.4(2) . 2_566 ? O5 C8 Sm1 50.09(19) . 2_566 ? C6 C8 Sm1 166.1(3) . 2_566 ? O9 C9 C11 115.6(4) . 2_677 ? O9 C9 C10 124.8(4) . . ? C11 C9 C10 119.5(4) 2_677 . ? C9 C10 C11 119.9(3) . . ? C9 C10 C12 121.2(4) . . ? C11 C10 C12 118.9(4) . . ? C9 C11 C10 120.6(4) 2_677 . ? C9 C11 H11 119.7 2_677 . ? C10 C11 H11 119.7 . . ? O8 C12 O7 121.3(3) . . ? O8 C12 C10 119.1(4) . . ? O7 C12 C10 119.6(4) . . ? O8 C12 Sm1 57.92(19) . . ? O7 C12 Sm1 63.63(19) . . ? C10 C12 Sm1 175.4(3) . . ? O10 C13 N1 144.5(16) . . ? O10 C13 H13 107.8 . . ? N1 C13 H13 107.8 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O11 C16 N2 124.6(5) . . ? O11 C16 H16A 117.7 . . ? N2 C16 H16A 117.7 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O12 C19 N3 176(3) . . ? O12 C19 H19 90.1 . . ? N3 C19 H19 90.3 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 H21A 109.5 . . ? N3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C13 N1 C15 123.3(10) . . ? C13 N1 C14 120.4(11) . . ? C15 N1 C14 116.2(9) . . ? C16 N2 C18 122.1(6) . . ? C16 N2 C17 121.4(6) . . ? C18 N2 C17 116.5(6) . . ? C19 N3 C20 124(3) . . ? C19 N3 C21 125(3) . . ? C20 N3 C21 111(2) . . ? _diffrn_measured_fraction_theta_max 0.873 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.873 _refine_diff_density_max 1.656 _refine_diff_density_min -1.476 _refine_diff_density_rms 0.108 #===END OF 3 ## Crystallographic Data for compound 4 data_{[Gd2(DHBDC)3(DMF)4](DMF)2}n _database_code_depnum_ccdc_archive 'CCDC 824001' #TrackingRef 'LnDHBDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H54 Gd2 N6 O24' _chemical_formula_weight 1341.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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' _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 10.5226(9) _cell_length_b 11.0545(9) _cell_length_c 12.7711(11) _cell_angle_alpha 103.8260(10) _cell_angle_beta 110.0240(10) _cell_angle_gamma 96.6020(10) _cell_volume 1323.41(19) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5340 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 27.79 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 2.570 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.361 _exptl_absorpt_correction_T_max 0.528 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEXII CCD' _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 12457 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 28.25 _reflns_number_total 6361 _reflns_number_gt 5454 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.3859P] 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 6361 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 Gd1 Gd 0.103040(18) 0.547825(17) 0.681682(17) 0.02487(7) Uani 1 1 d . . . O1 O -0.0166(3) 0.3337(3) 0.5876(3) 0.0371(7) Uani 1 1 d . . . O2 O -0.0731(3) 0.2745(3) 0.3943(3) 0.0393(7) Uani 1 1 d . . . O3 O -0.0450(6) 0.0528(4) 0.2917(3) 0.0713(14) Uani 1 1 d . . . H3 H -0.0569 0.1257 0.2968 0.107 Uiso 1 1 calc R . . O4 O 0.1590(3) 0.4937(3) 0.5176(3) 0.0378(7) Uani 1 1 d . . . O5 O 0.1256(3) 0.4300(3) 0.3317(3) 0.0423(8) Uani 1 1 d . . . O6 O 0.3298(4) 0.3985(5) 0.2670(3) 0.0648(12) Uani 1 1 d . . . H6A H 0.2483 0.3954 0.2578 0.097 Uiso 1 1 calc R . . O7 O 0.1755(3) 0.7544(3) 0.8484(3) 0.0422(8) Uani 1 1 d . . . O8 O 0.3293(3) 0.6899(4) 0.7807(3) 0.0540(10) Uani 1 1 d . . . O9 O 0.2351(4) 0.9852(4) 0.9964(4) 0.0740(13) Uani 1 1 d . . . H9A H 0.1840 0.9165 0.9533 0.111 Uiso 1 1 calc R . . O10 O 0.2730(4) 0.4227(5) 0.7426(4) 0.0702(12) Uani 1 1 d . . . O11 O 0.0708(4) 0.4786(4) 0.8374(3) 0.0525(9) Uani 1 1 d . . . O12 O 0.3843(12) 0.7714(10) 0.3604(9) 0.178(4) Uani 1 1 d . . . C1 C -0.0235(5) 0.0299(4) 0.3948(4) 0.0406(10) Uani 1 1 d . . . C2 C -0.0218(4) 0.1212(4) 0.4934(4) 0.0333(9) Uani 1 1 d . . . C3 C 0.0013(6) 0.0884(4) 0.5958(4) 0.0430(11) Uani 1 1 d . . . H3A H 0.0018 0.1487 0.6607 0.052 Uiso 1 1 calc R . . C4 C -0.0386(4) 0.2536(4) 0.4928(4) 0.0334(9) Uani 1 1 d . . . C5 C 0.4110(4) 0.4492(5) 0.3825(4) 0.0371(10) Uani 1 1 d . . . C6 C 0.3573(4) 0.4846(4) 0.4693(4) 0.0328(9) Uani 1 1 d . . . C7 C 0.4475(5) 0.5352(5) 0.5851(4) 0.0394(10) Uani 1 1 d . . . H7 H 0.4118 0.5593 0.6424 0.047 Uiso 1 1 calc R . . C8 C 0.2063(4) 0.4687(4) 0.4389(4) 0.0323(9) Uani 1 1 d . . . C9 C 0.3641(4) 0.9884(5) 0.9951(4) 0.0376(10) Uani 1 1 d . . . C10 C 0.4001(4) 0.8909(4) 0.9264(4) 0.0352(9) Uani 1 1 d . . . C11 C 0.5355(5) 0.9028(5) 0.9319(4) 0.0410(10) Uani 1 1 d . . . H11 H 0.5590 0.8372 0.8862 0.049 Uiso 1 1 calc R . . C12 C 0.2953(5) 0.7716(4) 0.8467(4) 0.0374(10) Uani 1 1 d . . . C13 C 0.3635(15) 0.4033(15) 0.7860(10) 0.178(7) Uani 1 1 d . . . H13 H 0.4290 0.4771 0.8043 0.214 Uiso 1 1 calc R . . C14 C 0.5801(12) 0.3665(13) 0.8965(12) 0.158(5) Uani 1 1 d . . . H14A H 0.6105 0.4551 0.9056 0.237 Uiso 1 1 calc R . . H14B H 0.6282 0.3164 0.8571 0.237 Uiso 1 1 calc R . . H14C H 0.5993 0.3543 0.9719 0.237 Uiso 1 1 calc R . . C15 C 0.3730(14) 0.1994(13) 0.8044(12) 0.177(6) Uani 1 1 d . . . H15A H 0.2763 0.1835 0.7567 0.265 Uiso 1 1 calc R . . H15B H 0.3838 0.1806 0.8762 0.265 Uiso 1 1 calc R . . H15C H 0.4175 0.1461 0.7636 0.265 Uiso 1 1 calc R . . C16 C -0.0178(7) 0.3859(6) 0.8260(5) 0.0558(14) Uani 1 1 d . . . H16A H -0.1028 0.3671 0.7638 0.067 Uiso 1 1 calc R . . C17 C -0.1084(11) 0.2089(9) 0.8763(9) 0.117(3) Uani 1 1 d . . . H17A H -0.1898 0.2055 0.8108 0.175 Uiso 1 1 calc R . . H17B H -0.1296 0.2209 0.9449 0.175 Uiso 1 1 calc R . . H17C H -0.0776 0.1305 0.8613 0.175 Uiso 1 1 calc R . . C18 C 0.1265(12) 0.3314(11) 0.9897(9) 0.158(6) Uani 1 1 d . . . H18A H 0.1903 0.4045 0.9956 0.237 Uiso 1 1 calc R . . H18B H 0.1650 0.2571 0.9774 0.237 Uiso 1 1 calc R . . H18C H 0.1101 0.3446 1.0607 0.237 Uiso 1 1 calc R . . C19 C 0.453(3) 0.8051(17) 0.4514(16) 0.37(3) Uani 1 1 d . . . H19 H 0.5047 0.7432 0.4422 0.445 Uiso 1 1 d R . . C20 C 0.483(4) 0.8772(19) 0.631(2) 0.40(3) Uani 1 1 d . . . H20A H 0.3834 0.8598 0.6035 0.601 Uiso 1 1 calc R . . H20B H 0.5191 0.9664 0.6717 0.601 Uiso 1 1 calc R . . H20C H 0.5180 0.8283 0.6832 0.601 Uiso 1 1 calc R . . C21 C 0.653(2) 0.8712(18) 0.586(3) 0.41(3) Uani 1 1 d . . . H21A H 0.6825 0.8481 0.5223 0.612 Uiso 1 1 calc R . . H21B H 0.6865 0.8227 0.6389 0.612 Uiso 1 1 calc R . . H21C H 0.6883 0.9605 0.6265 0.612 Uiso 1 1 calc R . . N1 N 0.4334(7) 0.3271(7) 0.8287(6) 0.0825(19) Uani 1 1 d . . . N2 N -0.0009(6) 0.3135(5) 0.8940(5) 0.0654(14) Uani 1 1 d . . . N3 N 0.5186(10) 0.8472(7) 0.5462(8) 0.103(2) Uani 1 1 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 Gd1 0.02076(10) 0.01946(10) 0.02765(11) 0.00575(7) 0.00297(7) 0.00140(6) O1 0.0489(18) 0.0183(14) 0.0369(17) 0.0061(13) 0.0107(14) 0.0029(12) O2 0.0513(19) 0.0225(15) 0.0347(17) 0.0094(13) 0.0057(14) 0.0044(13) O3 0.144(4) 0.041(2) 0.041(2) 0.0220(18) 0.037(3) 0.040(3) O4 0.0304(15) 0.0337(17) 0.0512(19) 0.0087(14) 0.0204(14) 0.0073(12) O5 0.0248(15) 0.052(2) 0.0435(18) 0.0125(16) 0.0062(13) 0.0071(14) O6 0.0293(17) 0.115(4) 0.0305(18) 0.002(2) 0.0045(14) 0.006(2) O7 0.0356(17) 0.0381(18) 0.0385(17) 0.0013(14) 0.0095(14) -0.0102(13) O8 0.0319(17) 0.046(2) 0.054(2) -0.0140(17) 0.0029(16) -0.0023(15) O9 0.050(2) 0.069(3) 0.079(3) -0.011(2) 0.026(2) -0.011(2) O10 0.054(2) 0.080(3) 0.091(3) 0.048(3) 0.021(2) 0.041(2) O11 0.069(2) 0.047(2) 0.0393(19) 0.0183(16) 0.0166(18) 0.0030(18) O12 0.198(10) 0.178(9) 0.131(7) 0.060(7) 0.016(7) 0.051(8) C1 0.060(3) 0.029(2) 0.031(2) 0.0110(19) 0.014(2) 0.010(2) C2 0.037(2) 0.0189(19) 0.035(2) 0.0065(17) 0.0052(18) 0.0026(16) C3 0.064(3) 0.027(2) 0.030(2) 0.0058(18) 0.011(2) 0.011(2) C4 0.033(2) 0.022(2) 0.037(2) 0.0053(17) 0.0070(18) -0.0002(16) C5 0.027(2) 0.049(3) 0.028(2) 0.0042(19) 0.0074(17) 0.0060(18) C6 0.0263(19) 0.036(2) 0.034(2) 0.0093(18) 0.0102(17) 0.0075(16) C7 0.032(2) 0.053(3) 0.033(2) 0.007(2) 0.0167(19) 0.007(2) C8 0.027(2) 0.029(2) 0.040(2) 0.0113(18) 0.0104(18) 0.0070(16) C9 0.028(2) 0.040(3) 0.036(2) 0.0068(19) 0.0082(18) -0.0042(17) C10 0.034(2) 0.029(2) 0.029(2) 0.0035(17) 0.0033(17) -0.0051(17) C11 0.037(2) 0.036(3) 0.038(2) 0.001(2) 0.0091(19) -0.0014(19) C12 0.034(2) 0.035(2) 0.029(2) 0.0068(18) 0.0008(17) -0.0056(18) C13 0.249(14) 0.304(17) 0.142(9) 0.171(11) 0.140(10) 0.243(14) C14 0.104(9) 0.148(11) 0.171(12) 0.014(9) 0.019(8) 0.005(8) C15 0.152(11) 0.167(13) 0.158(12) 0.092(10) -0.013(9) -0.036(10) C16 0.064(4) 0.063(4) 0.045(3) 0.022(3) 0.022(3) 0.012(3) C17 0.132(8) 0.098(7) 0.140(9) 0.070(7) 0.059(7) 0.001(6) C18 0.165(11) 0.136(10) 0.110(8) 0.083(8) -0.037(7) -0.023(8) C19 0.64(6) 0.127(14) 0.131(14) 0.086(13) -0.11(2) -0.03(2) C20 0.90(8) 0.20(2) 0.44(4) 0.18(2) 0.56(5) 0.24(3) C21 0.133(16) 0.138(16) 0.79(7) 0.15(3) -0.01(3) -0.015(13) N1 0.073(4) 0.104(5) 0.103(5) 0.067(4) 0.038(4) 0.055(4) N2 0.082(4) 0.061(3) 0.060(3) 0.031(3) 0.029(3) 0.008(3) N3 0.123(7) 0.080(5) 0.107(6) 0.048(5) 0.037(5) 0.010(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 Gd1 O4 2.328(3) . ? Gd1 O1 2.356(3) . ? Gd1 O2 2.397(3) 2_566 ? Gd1 O5 2.399(3) 2_566 ? Gd1 O11 2.405(3) . ? Gd1 O10 2.418(4) . ? Gd1 O8 2.421(3) . ? Gd1 O7 2.548(3) . ? Gd1 O4 2.939(3) 2_566 ? O1 C4 1.245(5) . ? O2 C4 1.270(5) . ? O2 Gd1 2.397(3) 2_566 ? O3 C1 1.349(6) . ? O3 H3 0.8200 . ? O4 C8 1.255(5) . ? O4 Gd1 2.939(3) 2_566 ? O5 C8 1.273(5) . ? O5 Gd1 2.399(3) 2_566 ? O6 C5 1.361(5) . ? O6 H6A 0.8200 . ? O7 C12 1.262(6) . ? O8 C12 1.253(6) . ? O9 C9 1.360(6) . ? O9 H9A 0.8200 . ? O10 C13 1.001(10) . ? O11 C16 1.248(7) . ? O12 C19 1.081(17) . ? C1 C3 1.380(6) 2_556 ? C1 C2 1.406(6) . ? C2 C3 1.389(6) . ? C2 C4 1.496(6) . ? C3 C1 1.380(6) 2_556 ? C3 H3A 0.9300 . ? C5 C7 1.379(6) 2_666 ? C5 C6 1.405(6) . ? C6 C7 1.387(6) . ? C6 C8 1.478(5) . ? C7 C5 1.379(6) 2_666 ? C7 H7 0.9300 . ? C9 C11 1.389(6) 2_677 ? C9 C10 1.395(7) . ? C10 C11 1.392(6) . ? C10 C12 1.499(6) . ? C11 C9 1.389(6) 2_677 ? C11 H11 0.9300 . ? C13 N1 1.278(9) . ? C13 H13 0.9300 . ? C14 N1 1.439(12) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N1 1.394(13) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N2 1.299(7) . ? C16 H16A 0.9300 . ? C17 N2 1.438(9) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N2 1.426(10) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N3 1.115(17) . ? C19 H19 0.9299 . ? C20 N3 1.251(16) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N3 1.295(19) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 Gd1 O1 76.84(11) . . ? O4 Gd1 O2 76.19(11) . 2_566 ? O1 Gd1 O2 127.28(11) . 2_566 ? O4 Gd1 O5 122.28(11) . 2_566 ? O1 Gd1 O5 80.38(12) . 2_566 ? O2 Gd1 O5 77.16(12) 2_566 2_566 ? O4 Gd1 O11 145.64(13) . . ? O1 Gd1 O11 77.06(12) . . ? O2 Gd1 O11 138.04(12) 2_566 . ? O5 Gd1 O11 74.33(13) 2_566 . ? O4 Gd1 O10 79.65(14) . . ? O1 Gd1 O10 74.86(14) . . ? O2 Gd1 O10 140.91(14) 2_566 . ? O5 Gd1 O10 141.90(14) 2_566 . ? O11 Gd1 O10 72.23(15) . . ? O4 Gd1 O8 87.05(12) . . ? O1 Gd1 O8 144.91(12) . . ? O2 Gd1 O8 76.81(13) 2_566 . ? O5 Gd1 O8 133.81(12) 2_566 . ? O11 Gd1 O8 102.03(14) . . ? O10 Gd1 O8 71.66(15) . . ? O4 Gd1 O7 131.28(10) . . ? O1 Gd1 O7 151.87(11) . . ? O2 Gd1 O7 69.86(11) 2_566 . ? O5 Gd1 O7 83.05(11) 2_566 . ? O11 Gd1 O7 76.65(12) . . ? O10 Gd1 O7 106.15(15) . . ? O8 Gd1 O7 52.26(11) . . ? O4 Gd1 C12 109.09(12) . . ? O1 Gd1 C12 162.24(12) . . ? O2 Gd1 C12 70.36(12) 2_566 . ? O5 Gd1 C12 108.48(13) 2_566 . ? O11 Gd1 C12 90.31(13) . . ? O10 Gd1 C12 89.51(16) . . ? O8 Gd1 C12 25.98(13) . . ? O7 Gd1 C12 26.33(12) . . ? O4 Gd1 O4 75.05(10) . 2_566 ? O1 Gd1 O4 64.36(10) . 2_566 ? O2 Gd1 O4 65.31(10) 2_566 2_566 ? O5 Gd1 O4 47.31(10) 2_566 2_566 ? O11 Gd1 O4 112.46(11) . 2_566 ? O10 Gd1 O4 135.68(14) . 2_566 ? O8 Gd1 O4 140.84(12) . 2_566 ? O7 Gd1 O4 117.93(10) . 2_566 ? C12 Gd1 O4 132.98(11) . 2_566 ? C4 O1 Gd1 135.6(3) . . ? C4 O2 Gd1 138.1(3) . 2_566 ? C1 O3 H3 109.5 . . ? C8 O4 Gd1 172.1(3) . . ? C8 O4 Gd1 82.9(2) . 2_566 ? Gd1 O4 Gd1 104.95(10) . 2_566 ? C8 O5 Gd1 108.4(3) . 2_566 ? C5 O6 H6A 109.5 . . ? C12 O7 Gd1 90.0(3) . . ? C12 O8 Gd1 96.2(3) . . ? C9 O9 H9A 109.5 . . ? C13 O10 Gd1 158.8(11) . . ? C16 O11 Gd1 126.1(3) . . ? O3 C1 C3 118.5(4) . 2_556 ? O3 C1 C2 123.0(4) . . ? C3 C1 C2 118.5(4) 2_556 . ? C3 C2 C1 118.7(4) . . ? C3 C2 C4 119.1(4) . . ? C1 C2 C4 122.2(4) . . ? C1 C3 C2 122.8(4) 2_556 . ? C1 C3 H3A 118.6 2_556 . ? C2 C3 H3A 118.6 . . ? O1 C4 O2 125.7(4) . . ? O1 C4 C2 118.1(4) . . ? O2 C4 C2 116.2(4) . . ? O6 C5 C7 117.8(4) . 2_666 ? O6 C5 C6 123.1(4) . . ? C7 C5 C6 119.1(4) 2_666 . ? C7 C6 C5 119.3(4) . . ? C7 C6 C8 119.7(4) . . ? C5 C6 C8 121.0(4) . . ? C5 C7 C6 121.6(4) 2_666 . ? C5 C7 H7 119.2 2_666 . ? C6 C7 H7 119.2 . . ? O4 C8 O5 120.8(4) . . ? O4 C8 C6 120.5(4) . . ? O5 C8 C6 118.7(4) . . ? O9 C9 C11 116.4(4) . 2_677 ? O9 C9 C10 124.4(4) . . ? C11 C9 C10 119.3(4) 2_677 . ? C11 C10 C9 120.1(4) . . ? C11 C10 C12 118.8(4) . . ? C9 C10 C12 121.1(4) . . ? C9 C11 C10 120.7(4) 2_677 . ? C9 C11 H11 119.7 2_677 . ? C10 C11 H11 119.7 . . ? O8 C12 O7 121.3(4) . . ? O8 C12 C10 119.2(4) . . ? O7 C12 C10 119.5(4) . . ? O8 C12 Gd1 57.8(2) . . ? O7 C12 Gd1 63.6(2) . . ? C10 C12 Gd1 175.6(3) . . ? O10 C13 N1 150.6(18) . . ? O10 C13 H13 104.7 . . ? N1 C13 H13 104.7 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O11 C16 N2 125.2(6) . . ? O11 C16 H16A 117.4 . . ? N2 C16 H16A 117.4 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O12 C19 N3 174(3) . . ? O12 C19 H19 92.9 . . ? N3 C19 H19 92.7 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 H21A 109.5 . . ? N3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C13 N1 C15 121.5(12) . . ? C13 N1 C14 121.6(11) . . ? C15 N1 C14 116.8(9) . . ? C16 N2 C18 122.0(6) . . ? C16 N2 C17 122.1(7) . . ? C18 N2 C17 115.8(7) . . ? C19 N3 C20 129(3) . . ? C19 N3 C21 122(3) . . ? C20 N3 C21 108(2) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.297 _refine_diff_density_min -1.395 _refine_diff_density_rms 0.119 #===END OF 4 ## Crystallographic Data for compound 5 data_{[Er2(DHBDC)3(DMF)4](DMF)2}n _database_code_depnum_ccdc_archive 'CCDC 824002' #TrackingRef 'LnDHBDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H54 Er2 N6 O24' _chemical_formula_weight 1361.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5507(9) _cell_length_b 10.9265(10) _cell_length_c 12.8978(11) _cell_angle_alpha 103.1840(10) _cell_angle_beta 111.1470(10) _cell_angle_gamma 96.5660(10) _cell_volume 1318.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3382 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.04 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 3.248 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.381 _exptl_absorpt_correction_T_max 0.501 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'APEXII CCD' _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 8303 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.91 _reflns_number_total 6100 _reflns_number_gt 5363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+1.5643P] 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 6100 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.106461(19) 0.546535(18) 0.682665(17) 0.02297(7) Uani 1 1 d . . . O1 O -0.0149(4) 0.3372(3) 0.5866(3) 0.0323(7) Uani 1 1 d . . . O2 O -0.0717(4) 0.2801(3) 0.3949(3) 0.0345(8) Uani 1 1 d . . . O3 O -0.0411(6) 0.0565(4) 0.2940(3) 0.0644(14) Uani 1 1 d . . . H3 H -0.0532 0.1300 0.2984 0.097 Uiso 1 1 calc R . . O4 O 0.1682(3) 0.4969(3) 0.5301(3) 0.0352(8) Uani 1 1 d . . . O5 O 0.1208(3) 0.4352(3) 0.3428(3) 0.0362(8) Uani 1 1 d . . . O6 O 0.3172(4) 0.4061(5) 0.2697(3) 0.0557(12) Uani 1 1 d . . . H6A H 0.2366 0.4040 0.2628 0.084 Uiso 1 1 calc R . . O7 O 0.1737(4) 0.7503(3) 0.8448(3) 0.0381(8) Uani 1 1 d . . . O8 O 0.3282(4) 0.6880(4) 0.7801(3) 0.0485(10) Uani 1 1 d . . . O9 O 0.2348(4) 0.9809(4) 0.9942(4) 0.0629(13) Uani 1 1 d . . . H9A H 0.1840 0.9116 0.9506 0.094 Uiso 1 1 calc R . . O10 O 0.2709(5) 0.4224(5) 0.7471(4) 0.0685(14) Uani 1 1 d . . . O11 O 0.0714(4) 0.4784(4) 0.8323(3) 0.0459(9) Uani 1 1 d . . . O12 O 0.3821(11) 0.7765(10) 0.3624(8) 0.157(4) Uani 1 1 d . . . C1 C -0.0210(6) 0.0322(5) 0.3969(4) 0.0367(11) Uani 1 1 d . . . C2 C -0.0209(5) 0.1229(4) 0.4936(4) 0.0293(10) Uani 1 1 d . . . C3 C -0.0003(6) 0.0883(5) 0.5947(4) 0.0381(12) Uani 1 1 d . . . H3A H -0.0009 0.1480 0.6587 0.046 Uiso 1 1 calc R . . C4 C -0.0368(5) 0.2567(4) 0.4924(4) 0.0290(10) Uani 1 1 d . . . C5 C 0.4046(5) 0.4530(5) 0.3842(4) 0.0340(11) Uani 1 1 d . . . C6 C 0.3578(5) 0.4861(4) 0.4727(4) 0.0281(9) Uani 1 1 d . . . C7 C 0.4543(5) 0.5330(5) 0.5882(4) 0.0347(11) Uani 1 1 d . . . H7 H 0.4229 0.5552 0.6474 0.042 Uiso 1 1 calc R . . C8 C 0.2068(5) 0.4722(4) 0.4484(4) 0.0290(10) Uani 1 1 d . . . C9 C 0.3640(5) 0.9868(5) 0.9941(4) 0.0359(11) Uani 1 1 d . . . C10 C 0.3993(5) 0.8897(5) 0.9247(4) 0.0347(11) Uani 1 1 d . . . C11 C 0.5358(5) 0.9041(5) 0.9324(5) 0.0405(12) Uani 1 1 d . . . H11 H 0.5598 0.8392 0.8873 0.049 Uiso 1 1 calc R . . C12 C 0.2954(5) 0.7698(5) 0.8457(4) 0.0330(11) Uani 1 1 d . . . C13 C 0.3576(16) 0.3966(16) 0.7848(11) 0.188(8) Uani 1 1 d . . . H13 H 0.4238 0.4698 0.8006 0.226 Uiso 1 1 calc R . . C14 C 0.5825(13) 0.3668(13) 0.8936(12) 0.149(5) Uani 1 1 d . . . H14A H 0.6090 0.4563 0.9008 0.224 Uiso 1 1 calc R . . H14B H 0.6320 0.3183 0.8559 0.224 Uiso 1 1 calc R . . H14C H 0.6047 0.3557 0.9695 0.224 Uiso 1 1 calc R . . C15 C 0.3772(14) 0.1915(13) 0.7974(10) 0.160(6) Uani 1 1 d . . . H15A H 0.2796 0.1742 0.7493 0.240 Uiso 1 1 calc R . . H15B H 0.3897 0.1682 0.8673 0.240 Uiso 1 1 calc R . . H15C H 0.4229 0.1420 0.7562 0.240 Uiso 1 1 calc R . . C16 C -0.0161(7) 0.3886(6) 0.8227(5) 0.0488(14) Uani 1 1 d . . . H16A H -0.1031 0.3720 0.7622 0.059 Uiso 1 1 calc R . . C17 C -0.1059(10) 0.2069(9) 0.8744(9) 0.101(3) Uani 1 1 d . . . H17A H -0.1885 0.2026 0.8085 0.152 Uiso 1 1 calc R . . H17B H -0.1259 0.2201 0.9426 0.152 Uiso 1 1 calc R . . H17C H -0.0749 0.1278 0.8612 0.152 Uiso 1 1 calc R . . C18 C 0.1310(13) 0.3347(12) 0.9868(9) 0.154(6) Uani 1 1 d . . . H18A H 0.1932 0.4086 0.9907 0.230 Uiso 1 1 calc R . . H18B H 0.1713 0.2605 0.9773 0.230 Uiso 1 1 calc R . . H18C H 0.1158 0.3495 1.0572 0.230 Uiso 1 1 calc R . . C19 C 0.446(4) 0.8074(17) 0.4553(17) 0.36(3) Uani 1 1 d . . . H19 H 0.4978 0.7456 0.4461 0.435 Uiso 1 1 d R . . C20 C 0.479(4) 0.8711(18) 0.630(3) 0.42(3) Uani 1 1 d . . . H20A H 0.3793 0.8518 0.5980 0.633 Uiso 1 1 calc R . . H20B H 0.5136 0.9604 0.6735 0.633 Uiso 1 1 calc R . . H20C H 0.5132 0.8189 0.6802 0.633 Uiso 1 1 calc R . . C21 C 0.652(2) 0.8704(18) 0.583(4) 0.44(3) Uani 1 1 d . . . H21A H 0.6745 0.8457 0.5166 0.655 Uiso 1 1 calc R . . H21B H 0.6905 0.8217 0.6356 0.655 Uiso 1 1 calc R . . H21C H 0.6901 0.9606 0.6218 0.655 Uiso 1 1 calc R . . N1 N 0.4340(7) 0.3215(7) 0.8253(6) 0.0743(19) Uani 1 1 d . . . N2 N 0.0021(6) 0.3129(5) 0.8908(5) 0.0605(15) Uani 1 1 d . . . N3 N 0.5197(10) 0.8482(7) 0.5503(9) 0.094(2) Uani 1 1 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 Er1 0.01909(10) 0.01840(10) 0.02592(11) 0.00582(7) 0.00390(7) 0.00161(7) O1 0.0420(19) 0.0200(16) 0.0311(17) 0.0061(13) 0.0121(15) 0.0039(14) O2 0.045(2) 0.0182(16) 0.0308(18) 0.0083(13) 0.0058(15) 0.0021(14) O3 0.133(4) 0.035(2) 0.038(2) 0.0196(18) 0.039(3) 0.038(3) O4 0.0283(17) 0.0359(19) 0.044(2) 0.0086(16) 0.0191(16) 0.0061(14) O5 0.0208(16) 0.042(2) 0.0370(19) 0.0072(16) 0.0043(14) 0.0053(14) O6 0.0257(18) 0.101(4) 0.0266(19) 0.006(2) 0.0052(15) 0.004(2) O7 0.0322(19) 0.0355(19) 0.0340(19) 0.0022(15) 0.0081(15) -0.0072(15) O8 0.0290(18) 0.039(2) 0.052(2) -0.0106(18) 0.0049(17) -0.0023(16) O9 0.044(2) 0.058(3) 0.068(3) -0.007(2) 0.023(2) -0.011(2) O10 0.052(3) 0.084(4) 0.079(3) 0.045(3) 0.016(2) 0.041(3) O11 0.061(3) 0.037(2) 0.0324(19) 0.0152(16) 0.0120(18) -0.0021(18) O12 0.180(9) 0.149(8) 0.109(6) 0.052(6) 0.011(6) 0.034(7) C1 0.054(3) 0.027(2) 0.028(2) 0.009(2) 0.015(2) 0.009(2) C2 0.032(2) 0.021(2) 0.030(2) 0.0073(18) 0.0078(19) 0.0032(18) C3 0.057(3) 0.026(2) 0.028(2) 0.005(2) 0.014(2) 0.012(2) C4 0.025(2) 0.019(2) 0.035(3) 0.0067(18) 0.0059(19) -0.0003(17) C5 0.025(2) 0.044(3) 0.025(2) 0.006(2) 0.0051(18) 0.003(2) C6 0.023(2) 0.028(2) 0.030(2) 0.0061(19) 0.0083(18) 0.0073(18) C7 0.029(2) 0.046(3) 0.031(2) 0.009(2) 0.016(2) 0.009(2) C8 0.025(2) 0.024(2) 0.040(3) 0.0095(19) 0.015(2) 0.0049(18) C9 0.027(2) 0.035(3) 0.035(3) 0.005(2) 0.006(2) -0.004(2) C10 0.033(3) 0.027(2) 0.032(2) 0.005(2) 0.004(2) -0.0052(19) C11 0.038(3) 0.036(3) 0.036(3) 0.002(2) 0.009(2) -0.001(2) C12 0.031(2) 0.026(2) 0.027(2) 0.0077(19) -0.0013(19) -0.0076(19) C13 0.259(16) 0.34(2) 0.171(11) 0.212(14) 0.174(12) 0.267(17) C14 0.126(11) 0.127(11) 0.155(12) 0.003(9) 0.042(10) 0.002(8) C15 0.159(12) 0.133(11) 0.118(10) 0.064(9) -0.016(8) -0.046(9) C16 0.056(4) 0.053(4) 0.043(3) 0.020(3) 0.023(3) 0.010(3) C17 0.109(7) 0.091(7) 0.111(8) 0.056(6) 0.045(6) -0.009(6) C18 0.145(10) 0.153(11) 0.101(8) 0.087(8) -0.033(7) -0.021(9) C19 0.67(6) 0.091(12) 0.122(14) 0.055(12) -0.07(2) 0.02(2) C20 1.00(9) 0.124(15) 0.46(4) 0.13(2) 0.60(6) 0.17(3) C21 0.118(15) 0.119(15) 0.91(8) 0.18(3) 0.01(3) -0.007(12) N1 0.065(4) 0.092(5) 0.102(5) 0.065(4) 0.042(4) 0.051(4) N2 0.078(4) 0.053(3) 0.054(3) 0.028(3) 0.026(3) 0.002(3) N3 0.110(6) 0.066(5) 0.105(6) 0.041(5) 0.037(5) 0.006(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 Er1 O4 2.261(3) . ? Er1 O1 2.302(3) . ? Er1 O5 2.338(3) 2_566 ? Er1 O2 2.342(3) 2_566 ? Er1 O11 2.350(4) . ? Er1 O10 2.356(4) . ? Er1 O8 2.368(4) . ? Er1 O7 2.505(3) . ? Er1 C12 2.805(5) . ? O1 C4 1.252(5) . ? O2 C4 1.272(6) . ? O2 Er1 2.342(3) 2_566 ? O3 C1 1.358(6) . ? O3 H3 0.8200 . ? O4 C8 1.246(6) . ? O5 C8 1.271(6) . ? O5 Er1 2.338(3) 2_566 ? O6 C5 1.364(6) . ? O6 H6A 0.8200 . ? O7 C12 1.272(6) . ? O8 C12 1.254(6) . ? O9 C9 1.358(6) . ? O9 H9A 0.8200 . ? O10 C13 0.976(10) . ? O11 C16 1.219(7) . ? O12 C19 1.089(17) . ? C1 C3 1.383(7) 2_556 ? C1 C2 1.404(7) . ? C2 C3 1.390(7) . ? C2 C4 1.493(6) . ? C3 C1 1.383(7) 2_556 ? C3 H3A 0.9300 . ? C5 C7 1.382(7) 2_666 ? C5 C6 1.391(7) . ? C6 C7 1.399(6) . ? C6 C8 1.491(6) . ? C7 C5 1.382(7) 2_666 ? C7 H7 0.9300 . ? C9 C11 1.383(7) 2_677 ? C9 C10 1.401(7) . ? C10 C11 1.395(7) . ? C10 C12 1.488(6) . ? C11 C9 1.383(7) 2_677 ? C11 H11 0.9300 . ? C13 N1 1.280(19) . ? C13 H13 0.9300 . ? C14 N1 1.451(13) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N1 1.387(13) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N2 1.318(8) . ? C16 H16A 0.9300 . ? C17 N2 1.449(9) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N2 1.420(11) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N3 1.135(18) . ? C19 H19 0.9269 . ? C20 N3 1.24(4) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N3 1.278(19) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Er1 O1 77.38(12) . . ? O4 Er1 O5 121.51(12) . 2_566 ? O1 Er1 O5 78.39(12) . 2_566 ? O4 Er1 O2 76.46(12) . 2_566 ? O1 Er1 O2 124.55(11) . 2_566 ? O5 Er1 O2 75.25(12) 2_566 2_566 ? O4 Er1 O11 146.20(14) . . ? O1 Er1 O11 78.24(12) . . ? O5 Er1 O11 75.34(14) 2_566 . ? O2 Er1 O11 137.19(13) 2_566 . ? O4 Er1 O10 79.51(15) . . ? O1 Er1 O10 75.95(16) . . ? O5 Er1 O10 141.82(16) 2_566 . ? O2 Er1 O10 142.92(16) 2_566 . ? O11 Er1 O10 72.10(16) . . ? O4 Er1 O8 85.09(13) . . ? O1 Er1 O8 146.22(13) . . ? O5 Er1 O8 135.08(13) 2_566 . ? O2 Er1 O8 77.58(13) 2_566 . ? O11 Er1 O8 103.04(14) . . ? O10 Er1 O8 72.57(17) . . ? O4 Er1 O7 130.93(12) . . ? O1 Er1 O7 151.69(12) . . ? O5 Er1 O7 83.98(12) 2_566 . ? O2 Er1 O7 70.64(12) 2_566 . ? O11 Er1 O7 75.95(12) . . ? O10 Er1 O7 106.53(16) . . ? O8 Er1 O7 53.29(12) . . ? O4 Er1 C12 107.86(14) . . ? O1 Er1 C12 164.07(13) . . ? O5 Er1 C12 109.76(14) 2_566 . ? O2 Er1 C12 71.32(13) 2_566 . ? O11 Er1 C12 90.40(14) . . ? O10 Er1 C12 90.02(17) . . ? O8 Er1 C12 26.36(14) . . ? O7 Er1 C12 26.96(13) . . ? C4 O1 Er1 136.1(3) . . ? C4 O2 Er1 139.7(3) . 2_566 ? C1 O3 H3 109.5 . . ? C8 O4 Er1 177.8(3) . . ? C8 O5 Er1 113.8(3) . 2_566 ? C5 O6 H6A 109.5 . . ? C12 O7 Er1 89.8(3) . . ? C12 O8 Er1 96.7(3) . . ? C9 O9 H9A 109.5 . . ? C13 O10 Er1 162.7(12) . . ? C16 O11 Er1 127.7(4) . . ? O3 C1 C3 117.5(4) . 2_556 ? O3 C1 C2 123.3(4) . . ? C3 C1 C2 119.1(4) 2_556 . ? C3 C2 C1 118.9(4) . . ? C3 C2 C4 119.1(4) . . ? C1 C2 C4 122.0(4) . . ? C1 C3 C2 121.9(5) 2_556 . ? C1 C3 H3A 119.0 2_556 . ? C2 C3 H3A 119.0 . . ? O1 C4 O2 124.9(4) . . ? O1 C4 C2 118.0(4) . . ? O2 C4 C2 117.0(4) . . ? O6 C5 C7 117.4(4) . 2_666 ? O6 C5 C6 123.1(4) . . ? C7 C5 C6 119.5(4) 2_666 . ? C5 C6 C7 119.6(4) . . ? C5 C6 C8 122.0(4) . . ? C7 C6 C8 118.5(4) . . ? C5 C7 C6 120.9(4) 2_666 . ? C5 C7 H7 119.5 2_666 . ? C6 C7 H7 119.5 . . ? O4 C8 O5 122.0(4) . . ? O4 C8 C6 120.2(4) . . ? O5 C8 C6 117.8(4) . . ? O9 C9 C11 116.7(5) . 2_677 ? O9 C9 C10 123.8(4) . . ? C11 C9 C10 119.6(5) 2_677 . ? C11 C10 C9 119.3(4) . . ? C11 C10 C12 119.3(5) . . ? C9 C10 C12 121.4(5) . . ? C9 C11 C10 121.1(5) 2_677 . ? C9 C11 H11 119.4 2_677 . ? C10 C11 H11 119.4 . . ? O8 C12 O7 120.1(4) . . ? O8 C12 C10 119.7(5) . . ? O7 C12 C10 120.1(5) . . ? O8 C12 Er1 57.0(2) . . ? O7 C12 Er1 63.3(2) . . ? C10 C12 Er1 175.4(4) . . ? O10 C13 N1 156(2) . . ? O10 C13 H13 101.8 . . ? N1 C13 H13 101.8 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O11 C16 N2 125.5(6) . . ? O11 C16 H16A 117.2 . . ? N2 C16 H16A 117.2 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O12 C19 N3 174(3) . . ? O12 C19 H19 91.0 . . ? N3 C19 H19 90.0 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 H21A 109.5 . . ? N3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C13 N1 C15 120.0(12) . . ? C13 N1 C14 121.6(12) . . ? C15 N1 C14 118.2(9) . . ? C16 N2 C18 120.4(7) . . ? C16 N2 C17 122.9(7) . . ? C18 N2 C17 116.7(7) . . ? C19 N3 C20 123(3) . . ? C19 N3 C21 122(3) . . ? C20 N3 C21 115(2) . . ? _diffrn_measured_fraction_theta_max 0.876 _diffrn_reflns_theta_full 28.91 _diffrn_measured_fraction_theta_full 0.876 _refine_diff_density_max 1.250 _refine_diff_density_min -1.480 _refine_diff_density_rms 0.131 #===END OF 5