# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 _publ_requested_journal CrystEngComm loop_ _publ_author_name 'I. Goldberg' _publ_contact_author_name 'I. Goldberg' _publ_contact_author_address ; Rama Aviv Campus Ramat Aviv Tel Aviv Israel 69978 ; _publ_contact_author_email GOLDBERG@POST.TAU.AC.IL data_1 _database_code_depnum_ccdc_archive 'CCDC 775250' #TrackingRef '- ti7-19.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 N2, 2(C10 H5 O5)' _chemical_formula_sum 'C30 H20 N2 O10' _chemical_formula_weight 568.48 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.9487(3) _cell_length_b 7.0921(2) _cell_length_c 15.4021(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.2276(12) _cell_angle_gamma 90.00 _cell_volume 1195.06(7) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2655 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 27.87 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 0.121 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8847 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.87 _reflns_number_total 2825 _reflns_number_gt 1869 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 2825 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.005 _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 O1 O 0.67209(11) 0.06026(17) 0.00749(8) 0.0221(3) Uani 1 1 d . . . C2 C 0.78813(16) 0.1148(2) -0.01202(11) 0.0205(4) Uani 1 1 d . . . C3 C 0.84566(16) 0.2062(2) 0.05651(11) 0.0203(4) Uani 1 1 d . . . C4 C 0.75809(16) 0.2123(2) 0.12479(12) 0.0203(4) Uani 1 1 d . . . C5 C 0.75568(16) 0.2868(2) 0.20917(12) 0.0216(4) Uani 1 1 d . . . H5 H 0.8244 0.3515 0.2342 0.026 Uiso 1 1 calc R . . C6 C 0.65056(16) 0.2634(3) 0.25474(12) 0.0233(4) Uani 1 1 d . . . H6 H 0.6476 0.3121 0.3121 0.028 Uiso 1 1 calc R . . C7 C 0.54806(17) 0.1696(3) 0.21852(12) 0.0230(4) Uani 1 1 d . . . H7 H 0.4774 0.1564 0.2519 0.028 Uiso 1 1 calc R . . C8 C 0.54721(16) 0.0957(2) 0.13545(12) 0.0205(4) Uani 1 1 d . . . H8 H 0.4782 0.0320 0.1103 0.025 Uiso 1 1 calc R . . C9 C 0.65408(16) 0.1208(2) 0.09133(12) 0.0202(4) Uani 1 1 d . . . C10 C 0.82467(16) 0.0670(2) -0.10130(12) 0.0215(4) Uani 1 1 d . . . O11 O 0.74731(11) -0.01346(19) -0.15130(8) 0.0268(3) Uani 1 1 d . . . O12 O 0.93149(12) 0.11244(19) -0.12184(8) 0.0270(3) Uani 1 1 d . . . C13 C 0.97202(16) 0.2825(2) 0.06649(12) 0.0213(4) Uani 1 1 d . . . O14 O 1.04377(11) 0.27438(18) -0.00001(8) 0.0255(3) Uani 1 1 d . . . H14 H 0.999(2) 0.209(3) -0.0555(15) 0.038 Uiso 1 1 d . . . O15 O 1.00759(11) 0.34959(19) 0.13618(8) 0.0259(3) Uani 1 1 d . . . N16 N 0.84349(14) -0.0398(2) -0.30653(10) 0.0226(4) Uani 1 1 d . . . H16 H 0.8013(18) -0.039(3) -0.2470(14) 0.034 Uiso 1 1 d . . . C17 C 0.95752(17) -0.1092(3) -0.31019(12) 0.0263(4) Uani 1 1 d . . . H17 H 0.9953 -0.1666 -0.2603 0.032 Uiso 1 1 calc R . . C18 C 1.01936(18) -0.0971(3) -0.38579(12) 0.0250(4) Uani 1 1 d . . . H18 H 1.0994 -0.1482 -0.3881 0.030 Uiso 1 1 calc R . . C19 C 0.96613(16) -0.0106(2) -0.45930(12) 0.0202(4) Uani 1 1 d . . . C20 C 0.84648(17) 0.0562(3) -0.45276(12) 0.0244(4) Uani 1 1 d . . . H20 H 0.8059 0.1128 -0.5018 0.029 Uiso 1 1 calc R . . C21 C 0.78715(17) 0.0406(3) -0.37573(12) 0.0243(4) Uani 1 1 d . . . H21 H 0.7062 0.0870 -0.3718 0.029 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0192(7) 0.0276(7) 0.0196(7) -0.0026(5) 0.0037(5) -0.0026(5) C2 0.0172(9) 0.0219(9) 0.0227(10) 0.0016(7) 0.0027(7) 0.0012(7) C3 0.0200(9) 0.0188(9) 0.0222(9) 0.0009(7) 0.0014(7) 0.0001(7) C4 0.0200(9) 0.0185(9) 0.0226(9) 0.0024(7) 0.0021(7) 0.0021(7) C5 0.0206(9) 0.0217(9) 0.0225(10) 0.0001(7) -0.0005(7) 0.0015(7) C6 0.0247(10) 0.0237(9) 0.0213(9) -0.0008(7) 0.0001(8) 0.0016(8) C7 0.0215(9) 0.0228(9) 0.0251(10) 0.0032(8) 0.0062(7) 0.0016(8) C8 0.0169(9) 0.0198(9) 0.0248(10) 0.0016(7) 0.0019(7) 0.0002(7) C9 0.0218(9) 0.0201(9) 0.0186(9) 0.0002(7) 0.0014(7) 0.0026(8) C10 0.0209(10) 0.0211(9) 0.0225(10) 0.0030(8) 0.0020(8) 0.0017(8) O11 0.0243(7) 0.0344(8) 0.0217(7) -0.0035(6) 0.0008(5) -0.0018(6) O12 0.0233(7) 0.0339(8) 0.0240(7) -0.0019(6) 0.0047(5) -0.0033(6) C13 0.0197(9) 0.0203(9) 0.0240(10) 0.0024(7) 0.0011(8) 0.0006(7) O14 0.0214(7) 0.0320(8) 0.0232(7) -0.0008(6) 0.0038(6) -0.0032(6) O15 0.0214(7) 0.0312(8) 0.0251(7) -0.0017(6) -0.0008(5) -0.0028(6) N16 0.0214(8) 0.0248(9) 0.0217(8) -0.0013(6) 0.0020(6) -0.0008(6) C17 0.0251(10) 0.0308(10) 0.0230(10) 0.0012(8) 0.0015(8) 0.0012(8) C18 0.0232(9) 0.0266(10) 0.0253(10) 0.0018(8) 0.0033(8) 0.0035(8) C19 0.0217(9) 0.0170(9) 0.0219(10) -0.0019(7) 0.0018(7) -0.0018(7) C20 0.0230(10) 0.0267(10) 0.0235(10) -0.0009(8) 0.0003(8) 0.0021(8) C21 0.0195(9) 0.0274(10) 0.0259(10) -0.0004(8) 0.0005(8) 0.0017(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.372(2) . ? O1 C9 1.382(2) . ? C2 C3 1.371(2) . ? C2 C10 1.486(3) . ? C3 C4 1.451(3) . ? C3 C13 1.488(3) . ? C4 C9 1.392(3) . ? C4 C5 1.404(3) . ? C5 C6 1.381(3) . ? C5 H5 0.9500 . ? C6 C7 1.402(3) . ? C6 H6 0.9500 . ? C7 C8 1.382(3) . ? C7 H7 0.9500 . ? C8 C9 1.387(2) . ? C8 H8 0.9500 . ? C10 O11 1.259(2) . ? C10 O12 1.265(2) . ? C13 O15 1.224(2) . ? C13 O14 1.316(2) . ? O14 H14 1.07(2) . ? N16 C21 1.338(2) . ? N16 C17 1.345(2) . ? N16 H16 1.04(2) . ? C17 C18 1.372(3) . ? C17 H17 0.9500 . ? C18 C19 1.395(3) . ? C18 H18 0.9500 . ? C19 C20 1.400(3) . ? C19 C19 1.489(4) 3_754 ? C20 C21 1.379(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? 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 C2 O1 C9 106.49(13) . . ? C3 C2 O1 111.49(15) . . ? C3 C2 C10 133.48(16) . . ? O1 C2 C10 115.03(15) . . ? C2 C3 C4 105.98(15) . . ? C2 C3 C13 130.47(17) . . ? C4 C3 C13 123.52(16) . . ? C9 C4 C5 118.27(17) . . ? C9 C4 C3 105.78(16) . . ? C5 C4 C3 135.95(17) . . ? C6 C5 C4 118.10(17) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? C5 C6 C7 121.67(18) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C8 C7 C6 121.65(17) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C7 C8 C9 115.41(17) . . ? C7 C8 H8 122.3 . . ? C9 C8 H8 122.3 . . ? O1 C9 C8 124.84(16) . . ? O1 C9 C4 110.27(15) . . ? C8 C9 C4 124.89(17) . . ? O11 C10 O12 124.67(17) . . ? O11 C10 C2 118.06(15) . . ? O12 C10 C2 117.27(16) . . ? O15 C13 O14 121.36(16) . . ? O15 C13 C3 119.66(16) . . ? O14 C13 C3 118.98(16) . . ? C13 O14 H14 111.9(12) . . ? C21 N16 C17 121.49(17) . . ? C21 N16 H16 119.4(11) . . ? C17 N16 H16 118.9(11) . . ? N16 C17 C18 120.15(18) . . ? N16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C19 120.77(18) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C18 C19 C20 116.93(17) . . ? C18 C19 C19 121.5(2) . 3_754 ? C20 C19 C19 121.6(2) . 3_754 ? C21 C20 C19 120.52(18) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? N16 C21 C20 120.11(17) . . ? N16 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H14 O12 1.07(2) 1.42(2) 2.4844(18) 173(2) . N16 H16 O11 1.04(2) 1.62(2) 2.656(2) 172(2) . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.257 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.061 #======================END================================= data_2 _database_code_depnum_ccdc_archive 'CCDC 775251' #TrackingRef '- ti7-19.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 N2, 2(C10 H5 O5)' _chemical_formula_sum 'C32 H22 N2 O10' _chemical_formula_weight 594.52 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 4.76900(10) _cell_length_b 19.0764(5) _cell_length_c 14.6179(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.2751(9) _cell_angle_gamma 90.00 _cell_volume 1321.90(6) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3024 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 27.84 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.113 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f & \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12223 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 27.84 _reflns_number_total 3051 _reflns_number_gt 1880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 3051 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0996 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1379 _refine_ls_wR_factor_gt 0.1166 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.3805(3) 0.41214(7) 0.05443(10) 0.0223(3) Uani 1 1 d . . . C2 C 0.2363(4) 0.36166(10) 0.09781(14) 0.0203(4) Uani 1 1 d . . . C3 C 0.2953(4) 0.29588(10) 0.06839(14) 0.0209(4) Uani 1 1 d . . . C4 C 0.4907(4) 0.30486(10) 0.00029(14) 0.0210(4) Uani 1 1 d . . . C5 C 0.6280(4) 0.26042(11) -0.05640(15) 0.0254(5) Uani 1 1 d . . . H5 H 0.6025 0.2111 -0.0545 0.030 Uiso 1 1 calc R . . C6 C 0.8017(4) 0.29018(11) -0.11527(15) 0.0285(5) Uani 1 1 d . . . H6 H 0.8964 0.2608 -0.1544 0.034 Uiso 1 1 calc R . . C7 C 0.8413(4) 0.36307(11) -0.11842(15) 0.0276(5) Uani 1 1 d . . . H7 H 0.9619 0.3818 -0.1599 0.033 Uiso 1 1 calc R . . C8 C 0.7099(4) 0.40823(11) -0.06303(15) 0.0245(5) Uani 1 1 d . . . H8 H 0.7376 0.4575 -0.0643 0.029 Uiso 1 1 calc R . . C9 C 0.5350(4) 0.37681(10) -0.00552(14) 0.0217(4) Uani 1 1 d . . . C10 C 0.0429(4) 0.38956(10) 0.16294(14) 0.0221(5) Uani 1 1 d . . . O11 O 0.0137(3) 0.45429(7) 0.16837(10) 0.0240(4) Uani 1 1 d . . . O12 O -0.0793(3) 0.34476(7) 0.20877(10) 0.0285(4) Uani 1 1 d . . . C13 C 0.1859(4) 0.22675(10) 0.09415(15) 0.0245(5) Uani 1 1 d . . . O14 O 0.0188(3) 0.22305(8) 0.16005(11) 0.0320(4) Uani 1 1 d . . . H14 H -0.024(5) 0.2705(14) 0.1819(18) 0.048 Uiso 1 1 d . . . O15 O 0.2538(3) 0.17385(7) 0.05508(11) 0.0319(4) Uani 1 1 d . . . N16 N -0.3702(3) 0.48001(8) 0.28012(12) 0.0217(4) Uani 1 1 d . . . H16 H -0.220(4) 0.4692(11) 0.2321(16) 0.032 Uiso 1 1 d . . . C17 C -0.4571(4) 0.54580(10) 0.29248(15) 0.0240(5) Uani 1 1 d . . . H17 H -0.3848 0.5829 0.2586 0.029 Uiso 1 1 calc R . . C18 C -0.6495(4) 0.56041(11) 0.35346(14) 0.0235(5) Uani 1 1 d . . . H18 H -0.7122 0.6071 0.3609 0.028 Uiso 1 1 calc R . . C19 C -0.7524(4) 0.50573(10) 0.40463(14) 0.0205(4) Uani 1 1 d . . . C20 C -0.6580(4) 0.43777(10) 0.38977(14) 0.0223(5) Uani 1 1 d . . . H20 H -0.7250 0.3995 0.4228 0.027 Uiso 1 1 calc R . . C21 C -0.4671(4) 0.42664(10) 0.32700(14) 0.0232(5) Uani 1 1 d . . . H21 H -0.4034 0.3804 0.3169 0.028 Uiso 1 1 calc R . . C22 C -0.9490(4) 0.52311(10) 0.47133(14) 0.0207(4) Uani 1 1 d . . . H22 H -1.0088 0.5705 0.4743 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0214(7) 0.0210(7) 0.0263(8) -0.0012(6) 0.0102(6) 0.0001(5) C2 0.0170(9) 0.0216(10) 0.0230(11) 0.0023(8) 0.0049(8) -0.0029(7) C3 0.0178(9) 0.0216(10) 0.0234(12) 0.0004(8) 0.0034(8) -0.0009(7) C4 0.0168(9) 0.0228(10) 0.0236(11) -0.0017(8) 0.0031(7) 0.0004(7) C5 0.0238(10) 0.0262(11) 0.0267(12) -0.0040(9) 0.0048(8) 0.0001(8) C6 0.0254(11) 0.0344(12) 0.0267(13) -0.0045(10) 0.0076(9) 0.0034(8) C7 0.0214(10) 0.0393(13) 0.0235(12) 0.0037(10) 0.0079(8) 0.0019(8) C8 0.0203(10) 0.0262(11) 0.0280(12) 0.0049(9) 0.0072(8) -0.0011(7) C9 0.0194(9) 0.0249(10) 0.0215(11) -0.0020(9) 0.0058(8) 0.0015(7) C10 0.0185(9) 0.0246(11) 0.0237(12) -0.0020(9) 0.0035(8) -0.0014(7) O11 0.0244(7) 0.0222(8) 0.0270(9) -0.0035(6) 0.0096(6) 0.0003(5) O12 0.0294(7) 0.0283(8) 0.0304(9) -0.0014(7) 0.0149(6) -0.0029(6) C13 0.0226(10) 0.0227(11) 0.0285(12) 0.0003(9) 0.0044(8) -0.0009(8) O14 0.0371(9) 0.0259(8) 0.0362(10) 0.0010(7) 0.0180(7) -0.0036(6) O15 0.0333(8) 0.0222(8) 0.0416(10) -0.0044(7) 0.0109(7) -0.0008(6) N16 0.0184(8) 0.0246(9) 0.0227(10) -0.0020(7) 0.0054(7) 0.0000(6) C17 0.0200(10) 0.0272(11) 0.0254(12) 0.0019(9) 0.0050(8) -0.0005(7) C18 0.0200(10) 0.0264(11) 0.0247(12) -0.0019(9) 0.0055(8) 0.0013(7) C19 0.0149(9) 0.0237(10) 0.0229(11) -0.0006(8) 0.0010(7) -0.0012(7) C20 0.0193(9) 0.0248(11) 0.0236(12) 0.0012(9) 0.0051(8) -0.0002(7) C21 0.0206(10) 0.0242(10) 0.0254(12) -0.0013(9) 0.0046(8) 0.0008(7) C22 0.0171(9) 0.0222(10) 0.0234(12) -0.0024(8) 0.0042(7) 0.0025(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.378(2) . ? O1 C9 1.381(2) . ? C2 C3 1.366(3) . ? C2 C10 1.494(3) . ? C3 C4 1.447(3) . ? C3 C13 1.482(3) . ? C4 C9 1.393(3) . ? C4 C5 1.397(3) . ? C5 C6 1.380(3) . ? C5 H5 0.9500 . ? C6 C7 1.405(3) . ? C6 H6 0.9500 . ? C7 C8 1.379(3) . ? C7 H7 0.9500 . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C10 O11 1.246(2) . ? C10 O12 1.266(2) . ? C13 O15 1.221(2) . ? C13 O14 1.318(3) . ? O14 H14 0.99(3) . ? N16 C21 1.338(3) . ? N16 C17 1.340(2) . ? N16 H16 1.08(2) . ? C17 C18 1.376(3) . ? C17 H17 0.9500 . ? C18 C19 1.403(3) . ? C18 H18 0.9500 . ? C19 C20 1.397(3) . ? C19 C22 1.463(3) . ? C20 C21 1.378(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C22 1.344(4) 3_366 ? C22 H22 0.9500 . ? 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 C2 O1 C9 106.19(14) . . ? C3 C2 O1 111.54(16) . . ? C3 C2 C10 133.67(17) . . ? O1 C2 C10 114.72(15) . . ? C2 C3 C4 106.15(16) . . ? C2 C3 C13 130.35(18) . . ? C4 C3 C13 123.47(17) . . ? C9 C4 C5 118.54(18) . . ? C9 C4 C3 105.79(17) . . ? C5 C4 C3 135.66(18) . . ? C6 C5 C4 118.18(19) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? C5 C6 C7 121.30(19) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C6 121.86(19) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C7 C8 C9 115.41(18) . . ? C7 C8 H8 122.3 . . ? C9 C8 H8 122.3 . . ? O1 C9 C8 124.97(17) . . ? O1 C9 C4 110.33(17) . . ? C8 C9 C4 124.70(19) . . ? O11 C10 O12 125.02(19) . . ? O11 C10 C2 118.33(17) . . ? O12 C10 C2 116.65(17) . . ? O15 C13 O14 120.68(18) . . ? O15 C13 C3 119.88(18) . . ? O14 C13 C3 119.43(17) . . ? C13 O14 H14 110.5(15) . . ? C21 N16 C17 120.96(17) . . ? C21 N16 H16 118.7(11) . . ? C17 N16 H16 120.4(11) . . ? N16 C17 C18 121.01(19) . . ? N16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C19 119.44(19) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 118.01(18) . . ? C20 C19 C22 123.71(18) . . ? C18 C19 C22 118.28(17) . . ? C21 C20 C19 119.62(18) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? N16 C21 C20 120.95(18) . . ? N16 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C22 C22 C19 124.7(2) 3_366 . ? C22 C22 H22 117.7 3_366 . ? C19 C22 H22 117.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H14 O12 0.99(3) 1.50(3) 2.488(2) 176(3) . N16 H16 O11 1.08(2) 1.55(2) 2.629(2) 176(2) . _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.84 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.244 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.061 #======================END================================= data_3 _database_code_depnum_ccdc_archive 'CCDC 775252' #TrackingRef '- ti7-19.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 N2, 2(C10 H5 O5)' _chemical_formula_sum 'C32 H22 N2 O10' _chemical_formula_weight 594.52 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' _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 5.68760(10) _cell_length_b 9.1917(2) _cell_length_c 12.9214(4) _cell_angle_alpha 82.4657(12) _cell_angle_beta 82.5927(11) _cell_angle_gamma 80.3885(12) _cell_volume 656.31(3) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2339 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.82 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 308 _exptl_absorpt_coefficient_mu 0.114 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7125 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.82 _reflns_number_total 3049 _reflns_number_gt 2326 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+0.0487P] 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 SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 3049 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1581 _refine_ls_wR_factor_gt 0.1406 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.21690(19) 0.55684(11) 0.37709(8) 0.0218(3) Uani 1 1 d . . . C2 C 0.3336(3) 0.63784(16) 0.29585(11) 0.0204(4) Uani 1 1 d . . . C3 C 0.5636(3) 0.57038(17) 0.27014(12) 0.0213(4) Uani 1 1 d . . . C4 C 0.5965(3) 0.43595(16) 0.34227(11) 0.0206(4) Uani 1 1 d . . . C5 C 0.7854(3) 0.32036(17) 0.36077(13) 0.0254(4) Uani 1 1 d . . . H5 H 0.9379 0.3201 0.3209 0.030 Uiso 1 1 calc R . . C6 C 0.7438(3) 0.20660(18) 0.43873(13) 0.0286(4) Uani 1 1 d . . . H6 H 0.8694 0.1267 0.4519 0.034 Uiso 1 1 calc R . . C7 C 0.5206(3) 0.20657(18) 0.49868(13) 0.0279(4) Uani 1 1 d . . . H7 H 0.4982 0.1260 0.5512 0.034 Uiso 1 1 calc R . . C8 C 0.3312(3) 0.32075(17) 0.48368(12) 0.0242(4) Uani 1 1 d . . . H8 H 0.1798 0.3223 0.5247 0.029 Uiso 1 1 calc R . . C9 C 0.3791(3) 0.43281(16) 0.40434(12) 0.0211(4) Uani 1 1 d . . . C10 C 0.1878(3) 0.78047(17) 0.25625(12) 0.0224(4) Uani 1 1 d . . . O11 O 0.2851(2) 0.85621(12) 0.17777(9) 0.0286(3) Uani 1 1 d . . . O12 O -0.0162(2) 0.81689(12) 0.30183(9) 0.0272(3) Uani 1 1 d . . . C13 C 0.7497(3) 0.61509(17) 0.18604(12) 0.0235(4) Uani 1 1 d . . . O14 O 0.7020(2) 0.74154(13) 0.12560(9) 0.0272(3) Uani 1 1 d . . . H14 H 0.526(4) 0.786(2) 0.1456(15) 0.041 Uiso 1 1 d . . . O15 O 0.9423(2) 0.53417(13) 0.17232(9) 0.0303(3) Uani 1 1 d . . . N16 N 0.7697(3) 0.05333(15) 0.19031(11) 0.0252(3) Uani 1 1 d . . . H16 H 0.849(4) -0.036(2) 0.2294(15) 0.038 Uiso 1 1 d . . . C17 C 0.8965(3) 0.12016(18) 0.10793(13) 0.0256(4) Uani 1 1 d . . . H17 H 1.0566 0.0773 0.0869 0.031 Uiso 1 1 calc R . . C18 C 0.7964(3) 0.25046(17) 0.05353(12) 0.0251(4) Uani 1 1 d . . . H18 H 0.8866 0.2967 -0.0049 0.030 Uiso 1 1 calc R . . C19 C 0.5618(3) 0.31370(16) 0.08501(12) 0.0221(4) Uani 1 1 d . . . C20 C 0.4345(3) 0.23963(17) 0.16950(13) 0.0245(4) Uani 1 1 d . . . H20 H 0.2729 0.2785 0.1913 0.029 Uiso 1 1 calc R . . C21 C 0.5429(3) 0.10995(18) 0.22150(13) 0.0267(4) Uani 1 1 d . . . H21 H 0.4564 0.0606 0.2797 0.032 Uiso 1 1 calc R . . C22 C 0.4433(3) 0.45429(16) 0.03523(12) 0.0227(4) Uani 1 1 d . . . H22 H 0.2763 0.4820 0.0541 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0196(6) 0.0201(6) 0.0231(6) 0.0009(4) 0.0002(4) -0.0004(4) C2 0.0223(8) 0.0192(7) 0.0194(7) -0.0012(6) -0.0006(6) -0.0042(6) C3 0.0221(8) 0.0214(7) 0.0216(7) -0.0029(6) -0.0037(6) -0.0054(6) C4 0.0211(8) 0.0186(7) 0.0229(8) -0.0051(6) -0.0039(6) -0.0022(6) C5 0.0203(8) 0.0253(8) 0.0293(8) -0.0037(6) -0.0025(6) 0.0007(6) C6 0.0284(9) 0.0247(8) 0.0306(9) -0.0002(7) -0.0066(7) 0.0024(7) C7 0.0320(10) 0.0234(8) 0.0277(8) 0.0006(6) -0.0058(7) -0.0032(7) C8 0.0265(9) 0.0230(8) 0.0230(8) -0.0001(6) -0.0033(6) -0.0054(6) C9 0.0213(8) 0.0179(7) 0.0238(8) -0.0041(6) -0.0034(6) -0.0004(6) C10 0.0227(8) 0.0201(7) 0.0244(8) -0.0019(6) -0.0036(6) -0.0031(6) O11 0.0262(7) 0.0246(6) 0.0316(6) 0.0060(5) -0.0010(5) -0.0028(5) O12 0.0247(7) 0.0245(6) 0.0282(6) 0.0013(5) -0.0001(5) 0.0032(5) C13 0.0243(9) 0.0237(8) 0.0234(8) -0.0048(6) -0.0010(6) -0.0059(6) O14 0.0252(7) 0.0276(6) 0.0272(6) 0.0017(5) 0.0015(5) -0.0062(5) O15 0.0231(7) 0.0327(7) 0.0327(7) -0.0043(5) 0.0040(5) -0.0025(5) N16 0.0275(8) 0.0189(6) 0.0288(7) -0.0009(5) -0.0070(6) -0.0012(5) C17 0.0248(9) 0.0223(8) 0.0287(8) -0.0037(6) -0.0042(7) 0.0012(6) C18 0.0253(9) 0.0233(8) 0.0250(8) -0.0004(6) -0.0014(6) -0.0014(6) C19 0.0257(9) 0.0201(7) 0.0214(8) -0.0044(6) -0.0043(6) -0.0030(6) C20 0.0223(8) 0.0239(8) 0.0266(8) -0.0028(6) -0.0019(6) -0.0024(6) C21 0.0276(9) 0.0243(8) 0.0278(8) 0.0017(6) -0.0040(7) -0.0059(7) C22 0.0202(8) 0.0222(8) 0.0241(8) -0.0017(6) -0.0019(6) 0.0000(6) _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 O1 C2 1.3700(18) . ? O1 C9 1.3790(18) . ? C2 C3 1.370(2) . ? C2 C10 1.496(2) . ? C3 C4 1.448(2) . ? C3 C13 1.484(2) . ? C4 C9 1.387(2) . ? C4 C5 1.400(2) . ? C5 C6 1.382(2) . ? C5 H5 0.9500 . ? C6 C7 1.399(3) . ? C6 H6 0.9500 . ? C7 C8 1.387(2) . ? C7 H7 0.9500 . ? C8 C9 1.389(2) . ? C8 H8 0.9500 . ? C10 O12 1.246(2) . ? C10 O11 1.2720(19) . ? C13 O15 1.223(2) . ? C13 O14 1.3213(19) . ? O14 H14 1.03(2) . ? N16 C21 1.339(2) . ? N16 C17 1.345(2) . ? N16 H16 0.98(2) . ? C17 C18 1.381(2) . ? C17 H17 0.9500 . ? C18 C19 1.396(2) . ? C18 H18 0.9500 . ? C19 C20 1.395(2) . ? C19 C22 1.463(2) . ? C20 C21 1.380(2) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C22 1.334(3) 2_665 ? C22 H22 0.9500 . ? 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 C2 O1 C9 106.03(12) . . ? O1 C2 C3 111.78(13) . . ? O1 C2 C10 114.30(13) . . ? C3 C2 C10 133.90(14) . . ? C2 C3 C4 105.78(13) . . ? C2 C3 C13 130.23(15) . . ? C4 C3 C13 123.97(15) . . ? C9 C4 C5 118.69(15) . . ? C9 C4 C3 105.70(14) . . ? C5 C4 C3 135.62(16) . . ? C6 C5 C4 118.10(16) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? C5 C6 C7 121.43(16) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C6 121.90(15) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C7 C8 C9 115.10(15) . . ? C7 C8 H8 122.4 . . ? C9 C8 H8 122.4 . . ? O1 C9 C8 124.54(15) . . ? O1 C9 C4 110.70(13) . . ? C8 C9 C4 124.76(15) . . ? O12 C10 O11 124.94(14) . . ? O12 C10 C2 118.58(14) . . ? O11 C10 C2 116.47(14) . . ? O15 C13 O14 120.99(15) . . ? O15 C13 C3 120.05(15) . . ? O14 C13 C3 118.95(15) . . ? C13 O14 H14 108.1(11) . . ? C21 N16 C17 121.27(14) . . ? C21 N16 H16 120.2(13) . . ? C17 N16 H16 118.5(13) . . ? N16 C17 C18 120.69(16) . . ? N16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 119.50(15) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 118.11(15) . . ? C20 C19 C22 118.27(15) . . ? C18 C19 C22 123.62(15) . . ? C21 C20 C19 120.14(16) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? N16 C21 C20 120.27(15) . . ? N16 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C22 C22 C19 123.67(19) 2_665 . ? C22 C22 H22 118.2 2_665 . ? C19 C22 H22 118.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H14 O11 1.03(2) 1.45(2) 2.4751(17) 175.7(19) . N16 H16 O12 0.98(2) 1.67(2) 2.6514(18) 176.7(17) 1_645 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.82 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.468 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.066 #======================END=================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 775253' #TrackingRef '- ti7-19.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H12 N6 Nd2 O30, 2(C12 H12 N2), 2(C H4 O), 2(H2 O)' _chemical_formula_sum 'C46 H48 N10 Nd2 O34' _chemical_formula_weight 1573.42 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 10.4000(3) _cell_length_b 11.6437(3) _cell_length_c 13.3175(4) _cell_angle_alpha 81.3223(17) _cell_angle_beta 79.558(2) _cell_angle_gamma 64.6966(14) _cell_volume 1428.91(7) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5241 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.85 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 786 _exptl_absorpt_coefficient_mu 1.908 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5158 _exptl_absorpt_correction_T_max 0.7629 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15828 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.85 _reflns_number_total 6714 _reflns_number_gt 5783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+0.0122P] 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 SHELXL _refine_ls_extinction_coef 0.0045(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6714 _refine_ls_number_parameters 438 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1121 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 Nd Nd 0.38084(2) 0.193307(16) 0.363263(12) 0.02195(10) Uani 1 1 d . . . O1 O 0.3174(3) 0.4552(2) 0.69907(18) 0.0254(5) Uani 1 1 d . . . C2 C 0.3424(4) 0.3720(3) 0.6274(3) 0.0240(7) Uani 1 1 d . . . C3 C 0.3853(4) 0.2490(3) 0.6699(2) 0.0205(7) Uani 1 1 d . . . C4 C 0.3860(4) 0.2549(3) 0.7777(3) 0.0209(7) Uani 1 1 d . . . C5 C 0.4204(4) 0.1647(4) 0.8633(3) 0.0248(7) Uani 1 1 d . . . H5 H 0.4528 0.0762 0.8570 0.030 Uiso 1 1 calc R . . C6 C 0.4047(4) 0.2110(4) 0.9571(3) 0.0270(8) Uani 1 1 d . . . H6 H 0.4248 0.1527 1.0163 0.032 Uiso 1 1 calc R . . C7 C 0.3603(4) 0.3407(4) 0.9669(3) 0.0288(8) Uani 1 1 d . . . H7 H 0.3527 0.3679 1.0323 0.035 Uiso 1 1 calc R . . C8 C 0.3271(4) 0.4304(4) 0.8842(3) 0.0277(8) Uani 1 1 d . . . H8 H 0.2961 0.5188 0.8906 0.033 Uiso 1 1 calc R . . C9 C 0.3418(4) 0.3834(3) 0.7909(3) 0.0242(7) Uani 1 1 d . . . C10 C 0.4248(4) 0.1284(3) 0.6229(3) 0.0205(7) Uani 1 1 d . . . O11 O 0.3707(3) 0.1305(2) 0.54415(18) 0.0256(5) Uani 1 1 d . . . O12 O 0.5079(3) 0.0296(2) 0.66719(19) 0.0249(5) Uani 1 1 d . . . C13 C 0.3238(4) 0.4380(3) 0.5208(3) 0.0254(7) Uani 1 1 d . . . O14 O 0.3250(3) 0.3787(2) 0.44990(18) 0.0276(6) Uani 1 1 d . . . O15 O 0.3052(4) 0.5517(3) 0.5125(2) 0.0423(8) Uani 1 1 d . . . N16 N 0.5693(3) 0.2630(3) 0.1847(2) 0.0252(7) Uani 1 1 d . . . O17 O 0.5152(3) 0.3303(2) 0.26001(19) 0.0273(6) Uani 1 1 d . . . O18 O 0.5349(3) 0.1697(2) 0.1857(2) 0.0283(6) Uani 1 1 d . . . O19 O 0.6504(4) 0.2855(3) 0.1133(2) 0.0384(7) Uani 1 1 d . . . N20 N 0.1760(3) 0.3126(3) 0.2065(2) 0.0253(7) Uani 1 1 d . . . O21 O 0.2237(3) 0.3778(2) 0.24535(18) 0.0255(5) Uani 1 1 d . . . O22 O 0.2320(3) 0.1934(2) 0.22645(19) 0.0267(5) Uani 1 1 d . . . O23 O 0.0802(3) 0.3637(3) 0.1520(2) 0.0352(7) Uani 1 1 d . . . N24 N 0.1152(3) 0.1650(3) 0.4764(2) 0.0254(7) Uani 1 1 d . . . O25 O 0.2145(3) 0.0706(2) 0.43372(19) 0.0265(6) Uani 1 1 d . . . O26 O 0.1109(3) 0.2749(2) 0.44175(19) 0.0279(6) Uani 1 1 d . . . O27 O 0.0293(3) 0.1521(3) 0.5480(2) 0.0368(7) Uani 1 1 d . . . O28 O 0.6239(3) 0.1209(3) 0.4040(2) 0.0360(7) Uani 1 1 d D . . H28A H 0.666(5) 0.053(3) 0.440(3) 0.054 Uiso 1 1 d D . . H28B H 0.666(5) 0.167(4) 0.409(4) 0.054 Uiso 1 1 d D . . N29 N 0.0457(4) 1.2732(4) -0.2276(3) 0.0329(8) Uani 1 1 d . . . H29 H 0.023(5) 1.325(5) -0.290(4) 0.049 Uiso 1 1 d . . . C30 C 0.1072(4) 1.1464(4) -0.2286(3) 0.0323(9) Uani 1 1 d . . . H30 H 0.1258 1.1087 -0.2912 0.039 Uiso 1 1 calc R . . C31 C 0.1437(4) 1.0704(4) -0.1403(3) 0.0304(8) Uani 1 1 d . . . H31 H 0.1897 0.9804 -0.1419 0.036 Uiso 1 1 calc R . . C32 C 0.1131(4) 1.1254(4) -0.0481(3) 0.0260(8) Uani 1 1 d . . . C33 C 0.0477(5) 1.2584(4) -0.0500(3) 0.0314(9) Uani 1 1 d . . . H33 H 0.0254 1.2988 0.0116 0.038 Uiso 1 1 calc R . . C34 C 0.0159(5) 1.3299(4) -0.1406(3) 0.0345(9) Uani 1 1 d . . . H34 H -0.0275 1.4203 -0.1421 0.041 Uiso 1 1 calc R . . C35 C 0.1490(4) 1.0516(4) 0.0511(3) 0.0282(8) Uani 1 1 d . . . H35 H 0.1219 1.0965 0.1107 0.034 Uiso 1 1 calc R . . C36 C 0.2176(4) 0.9251(4) 0.0608(3) 0.0290(8) Uani 1 1 d . . . H36 H 0.2494 0.8822 -0.0002 0.035 Uiso 1 1 calc R . . C37 C 0.2481(4) 0.8463(4) 0.1581(3) 0.0252(7) Uani 1 1 d . . . C38 C 0.2962(4) 0.7153(4) 0.1574(3) 0.0277(8) Uani 1 1 d . . . H38 H 0.3142 0.6787 0.0945 0.033 Uiso 1 1 calc R . . C39 C 0.3180(4) 0.6386(4) 0.2470(3) 0.0275(8) Uani 1 1 d . . . H39 H 0.3513 0.5489 0.2462 0.033 Uiso 1 1 calc R . . N40 N 0.2920(4) 0.6908(3) 0.3363(2) 0.0276(7) Uani 1 1 d . . . H40 H 0.304(5) 0.630(4) 0.403(3) 0.033 Uiso 1 1 d . . . C41 C 0.2492(4) 0.8160(4) 0.3404(3) 0.0249(7) Uani 1 1 d . . . H41 H 0.2338 0.8493 0.4045 0.030 Uiso 1 1 calc R . . C42 C 0.2270(4) 0.8978(4) 0.2517(3) 0.0262(8) Uani 1 1 d . . . H42 H 0.1982 0.9866 0.2542 0.031 Uiso 1 1 calc R . . O43 O 0.7903(4) 0.2372(3) 0.3909(2) 0.0381(7) Uani 1 1 d D . . H43 H 0.769(6) 0.3143(14) 0.397(4) 0.057 Uiso 1 1 d D . . C44 C 0.8852(5) 0.2169(6) 0.2988(4) 0.0498(12) Uani 1 1 d . . . H44A H 0.8319 0.2647 0.2415 0.075 Uiso 1 1 calc R . . H44B H 0.9300 0.1258 0.2883 0.075 Uiso 1 1 calc R . . H44C H 0.9596 0.2461 0.3024 0.075 Uiso 1 1 calc R . . O45 O 0.0213(4) 0.5711(3) 0.3948(2) 0.0376(7) Uani 1 1 d D . . H45A H 0.1074(19) 0.520(4) 0.396(4) 0.056 Uiso 1 1 d D . . H45B H -0.008(6) 0.605(5) 0.451(2) 0.056 Uiso 1 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 Nd 0.03070(14) 0.01696(13) 0.01684(12) -0.00199(7) -0.00557(8) -0.00736(9) O1 0.0398(15) 0.0189(12) 0.0164(11) -0.0023(9) -0.0071(11) -0.0096(11) C2 0.0297(18) 0.0206(17) 0.0197(16) -0.0059(13) -0.0047(14) -0.0066(15) C3 0.0224(16) 0.0201(17) 0.0175(15) -0.0029(13) -0.0044(13) -0.0063(14) C4 0.0212(16) 0.0220(17) 0.0203(16) -0.0027(13) -0.0016(13) -0.0099(14) C5 0.0279(18) 0.0234(17) 0.0228(18) 0.0001(14) -0.0045(14) -0.0104(15) C6 0.0314(19) 0.032(2) 0.0198(17) 0.0002(14) -0.0045(15) -0.0150(17) C7 0.034(2) 0.039(2) 0.0146(16) -0.0050(15) -0.0023(15) -0.0155(18) C8 0.034(2) 0.0245(19) 0.0233(17) -0.0075(14) -0.0026(15) -0.0097(16) C9 0.0308(19) 0.0232(18) 0.0183(16) 0.0002(13) -0.0060(14) -0.0102(15) C10 0.0243(17) 0.0201(17) 0.0178(15) -0.0009(13) -0.0010(13) -0.0107(14) O11 0.0407(15) 0.0167(12) 0.0178(12) 0.0007(9) -0.0099(11) -0.0086(11) O12 0.0303(13) 0.0171(12) 0.0250(13) -0.0005(10) -0.0090(11) -0.0059(11) C13 0.0327(19) 0.0185(17) 0.0219(17) -0.0008(13) -0.0043(15) -0.0077(15) O14 0.0452(16) 0.0196(13) 0.0176(12) -0.0022(10) -0.0079(11) -0.0114(12) O15 0.088(2) 0.0196(14) 0.0223(13) 0.0018(11) -0.0149(15) -0.0226(15) N16 0.0357(17) 0.0222(15) 0.0188(14) 0.0002(12) -0.0065(13) -0.0123(14) O17 0.0355(15) 0.0198(13) 0.0243(13) -0.0056(10) -0.0036(11) -0.0081(11) O18 0.0364(15) 0.0239(13) 0.0270(13) -0.0041(10) -0.0055(11) -0.0137(12) O19 0.0547(18) 0.0416(17) 0.0281(14) -0.0077(13) 0.0059(13) -0.0314(15) N20 0.0320(17) 0.0249(16) 0.0173(14) -0.0019(12) -0.0040(13) -0.0099(14) O21 0.0353(14) 0.0223(13) 0.0205(12) 0.0006(10) -0.0085(11) -0.0122(11) O22 0.0342(14) 0.0208(13) 0.0242(12) -0.0032(10) -0.0063(11) -0.0090(11) O23 0.0373(15) 0.0343(16) 0.0336(15) 0.0034(12) -0.0192(13) -0.0106(13) N24 0.0291(16) 0.0292(17) 0.0178(14) -0.0004(12) -0.0058(12) -0.0112(14) O25 0.0313(14) 0.0216(13) 0.0241(13) -0.0033(10) -0.0036(11) -0.0082(11) O26 0.0334(14) 0.0242(14) 0.0218(12) -0.0003(10) -0.0035(11) -0.0085(12) O27 0.0361(16) 0.0439(18) 0.0294(14) -0.0015(12) 0.0011(12) -0.0183(14) O28 0.0416(17) 0.0262(15) 0.0456(17) 0.0114(13) -0.0214(14) -0.0176(13) N29 0.0335(18) 0.040(2) 0.0276(17) 0.0087(15) -0.0122(14) -0.0174(16) C30 0.032(2) 0.041(2) 0.0245(18) -0.0026(16) -0.0054(16) -0.0150(18) C31 0.031(2) 0.029(2) 0.030(2) -0.0027(16) -0.0053(16) -0.0104(17) C32 0.0293(19) 0.031(2) 0.0211(17) 0.0036(14) -0.0065(15) -0.0159(16) C33 0.039(2) 0.030(2) 0.0270(19) -0.0020(16) -0.0113(17) -0.0143(18) C34 0.038(2) 0.030(2) 0.038(2) 0.0076(17) -0.0149(18) -0.0164(18) C35 0.033(2) 0.030(2) 0.0218(17) -0.0023(15) -0.0064(15) -0.0123(17) C36 0.033(2) 0.034(2) 0.0206(17) -0.0001(15) -0.0076(15) -0.0136(17) C37 0.0261(18) 0.0281(19) 0.0197(16) 0.0005(14) -0.0033(14) -0.0101(16) C38 0.0310(19) 0.029(2) 0.0225(17) -0.0055(15) -0.0043(15) -0.0107(16) C39 0.0290(19) 0.0214(18) 0.0321(19) -0.0030(15) -0.0066(16) -0.0090(15) N40 0.0341(17) 0.0263(17) 0.0235(15) 0.0013(13) -0.0051(13) -0.0140(14) C41 0.0265(18) 0.0266(19) 0.0209(17) -0.0032(14) -0.0028(14) -0.0100(16) C42 0.0268(18) 0.0212(18) 0.0285(19) -0.0005(14) -0.0036(15) -0.0085(15) O43 0.0488(18) 0.0306(16) 0.0415(16) -0.0069(13) -0.0085(14) -0.0205(15) C44 0.036(2) 0.060(3) 0.050(3) -0.012(2) 0.002(2) -0.017(2) O45 0.0485(18) 0.0257(15) 0.0228(14) -0.0012(11) -0.0029(13) -0.0013(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd O14 2.401(2) . ? Nd O11 2.407(2) . ? Nd O12 2.413(2) 2_656 ? Nd O28 2.436(3) . ? Nd O21 2.581(2) . ? Nd O18 2.585(3) . ? Nd O22 2.595(2) . ? Nd O26 2.614(3) . ? Nd O17 2.634(3) . ? Nd O25 2.652(3) . ? Nd N20 3.006(3) . ? O1 C2 1.374(4) . ? O1 C9 1.372(4) . ? C2 C3 1.369(5) . ? C2 C13 1.512(5) . ? C3 C4 1.449(5) . ? C3 C10 1.487(5) . ? C4 C9 1.393(5) . ? C4 C5 1.413(5) . ? C5 C6 1.390(5) . ? C5 H5 0.9500 . ? C6 C7 1.398(6) . ? C6 H6 0.9500 . ? C7 C8 1.381(5) . ? C7 H7 0.9500 . ? C8 C9 1.390(5) . ? C8 H8 0.9500 . ? C10 O12 1.244(4) . ? C10 O11 1.270(4) . ? O12 Nd 2.413(2) 2_656 ? C13 O15 1.244(5) . ? C13 O14 1.247(4) . ? N16 O19 1.227(4) . ? N16 O17 1.262(4) . ? N16 O18 1.279(4) . ? N20 O23 1.224(4) . ? N20 O22 1.261(4) . ? N20 O21 1.274(4) . ? N24 O27 1.222(4) . ? N24 O25 1.266(4) . ? N24 O26 1.277(4) . ? O28 H28A 0.84(4) . ? O28 H28B 0.84(5) . ? N29 C30 1.336(6) . ? N29 C34 1.342(6) . ? N29 H29 0.95(5) . ? C30 C31 1.367(6) . ? C30 H30 0.9500 . ? C31 C32 1.393(5) . ? C31 H31 0.9500 . ? C32 C33 1.398(6) . ? C32 C35 1.478(5) . ? C33 C34 1.366(5) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.331(6) . ? C35 H35 0.9500 . ? C36 C37 1.471(5) . ? C36 H36 0.9500 . ? C37 C38 1.389(5) . ? C37 C42 1.405(5) . ? C38 C39 1.370(5) . ? C38 H38 0.9500 . ? C39 N40 1.349(5) . ? C39 H39 0.9500 . ? N40 C41 1.336(5) . ? N40 H40 1.03(4) . ? C41 C42 1.388(5) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? O43 C44 1.409(6) . ? O43 H43 0.84(2) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? O45 H45A 0.84(4) . ? O45 H45B 0.84(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O14 Nd O11 72.60(8) . . ? O14 Nd O12 156.95(9) . 2_656 ? O11 Nd O12 88.33(8) . 2_656 ? O14 Nd O28 86.28(10) . . ? O11 Nd O28 73.83(10) . . ? O12 Nd O28 75.82(9) 2_656 . ? O14 Nd O21 76.77(8) . . ? O11 Nd O21 136.39(8) . . ? O12 Nd O21 126.22(8) 2_656 . ? O28 Nd O21 134.29(9) . . ? O14 Nd O18 118.27(9) . . ? O11 Nd O18 147.51(9) . . ? O12 Nd O18 71.86(8) 2_656 . ? O28 Nd O18 76.43(10) . . ? O21 Nd O18 75.14(8) . . ? O14 Nd O22 122.56(8) . . ? O11 Nd O22 132.05(9) . . ? O12 Nd O22 79.82(8) 2_656 . ? O28 Nd O22 143.76(10) . . ? O21 Nd O22 49.37(8) . . ? O18 Nd O22 70.67(8) . . ? O14 Nd O26 72.66(9) . . ? O11 Nd O26 72.06(8) . . ? O12 Nd O26 114.30(9) 2_656 . ? O28 Nd O26 143.91(9) . . ? O21 Nd O26 69.62(8) . . ? O18 Nd O26 139.35(8) . . ? O22 Nd O26 71.21(8) . . ? O14 Nd O17 69.59(9) . . ? O11 Nd O17 126.47(8) . . ? O12 Nd O17 114.92(8) 2_656 . ? O28 Nd O17 67.31(9) . . ? O21 Nd O17 67.00(8) . . ? O18 Nd O17 48.95(8) . . ? O22 Nd O17 100.32(8) . . ? O26 Nd O17 127.32(8) . . ? O14 Nd O25 114.50(9) . . ? O11 Nd O25 65.01(8) . . ? O12 Nd O25 66.20(8) 2_656 . ? O28 Nd O25 123.40(9) . . ? O21 Nd O25 102.21(8) . . ? O18 Nd O25 124.57(8) . . ? O22 Nd O25 67.71(8) . . ? O26 Nd O25 48.47(8) . . ? O17 Nd O25 167.87(8) . . ? O14 Nd N20 99.14(8) . . ? O11 Nd N20 137.97(9) . . ? O12 Nd N20 103.75(8) 2_656 . ? O28 Nd N20 147.99(9) . . ? O21 Nd N20 24.90(8) . . ? O18 Nd N20 73.24(8) . . ? O22 Nd N20 24.65(8) . . ? O26 Nd N20 66.24(8) . . ? O17 Nd N20 84.94(8) . . ? O25 Nd N20 83.12(8) . . ? C2 O1 C9 106.5(3) . . ? C3 C2 O1 111.6(3) . . ? C3 C2 C13 136.0(3) . . ? O1 C2 C13 112.3(3) . . ? C2 C3 C4 105.8(3) . . ? C2 C3 C10 130.7(3) . . ? C4 C3 C10 123.5(3) . . ? C9 C4 C5 119.0(3) . . ? C9 C4 C3 105.8(3) . . ? C5 C4 C3 135.2(3) . . ? C6 C5 C4 117.2(3) . . ? C6 C5 H5 121.4 . . ? C4 C5 H5 121.4 . . ? C5 C6 C7 121.9(3) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C6 121.8(3) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C9 C8 C7 115.8(3) . . ? C9 C8 H8 122.1 . . ? C7 C8 H8 122.1 . . ? O1 C9 C8 125.4(3) . . ? O1 C9 C4 110.4(3) . . ? C8 C9 C4 124.2(3) . . ? O12 C10 O11 124.2(3) . . ? O12 C10 C3 116.0(3) . . ? O11 C10 C3 119.8(3) . . ? C10 O11 Nd 142.1(2) . . ? C10 O12 Nd 134.9(2) . 2_656 ? O15 C13 O14 125.1(3) . . ? O15 C13 C2 115.0(3) . . ? O14 C13 C2 119.8(3) . . ? C13 O14 Nd 155.8(2) . . ? O19 N16 O17 122.3(3) . . ? O19 N16 O18 121.0(3) . . ? O17 N16 O18 116.7(3) . . ? N16 O17 Nd 96.2(2) . . ? N16 O18 Nd 98.1(2) . . ? O23 N20 O22 121.6(3) . . ? O23 N20 O21 121.3(3) . . ? O22 N20 O21 117.1(3) . . ? O23 N20 Nd 172.6(2) . . ? O22 N20 Nd 59.12(16) . . ? O21 N20 Nd 58.54(16) . . ? N20 O21 Nd 96.56(19) . . ? N20 O22 Nd 96.24(19) . . ? O27 N24 O25 122.0(3) . . ? O27 N24 O26 121.5(3) . . ? O25 N24 O26 116.4(3) . . ? N24 O25 Nd 94.2(2) . . ? N24 O26 Nd 95.7(2) . . ? Nd O28 H28A 124(4) . . ? Nd O28 H28B 127(4) . . ? H28A O28 H28B 104(5) . . ? C30 N29 C34 121.5(3) . . ? C30 N29 H29 119(3) . . ? C34 N29 H29 119(3) . . ? N29 C30 C31 120.5(4) . . ? N29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C32 119.8(4) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C31 C32 C33 118.0(3) . . ? C31 C32 C35 123.8(4) . . ? C33 C32 C35 118.1(3) . . ? C34 C33 C32 119.8(4) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? N29 C34 C33 120.3(4) . . ? N29 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C36 C35 C32 123.1(4) . . ? C36 C35 H35 118.4 . . ? C32 C35 H35 118.4 . . ? C35 C36 C37 125.4(4) . . ? C35 C36 H36 117.3 . . ? C37 C36 H36 117.3 . . ? C38 C37 C42 118.8(3) . . ? C38 C37 C36 118.1(3) . . ? C42 C37 C36 123.1(3) . . ? C39 C38 C37 120.3(3) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? N40 C39 C38 119.7(4) . . ? N40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C41 N40 C39 122.0(3) . . ? C41 N40 H40 121(2) . . ? C39 N40 H40 117(2) . . ? N40 C41 C42 120.6(3) . . ? N40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C37 118.5(3) . . ? C41 C42 H42 120.7 . . ? C37 C42 H42 120.7 . . ? C44 O43 H43 102(4) . . ? O43 C44 H44A 109.5 . . ? O43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? H45A O45 H45B 108(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O28 H28B O43 0.84(4) 1.77(5) 2.586(4) 164(6) . O28 H28A O25 0.84(5) 2.23(2) 3.021(4) 158(5) 2_656 N29 H29 O45 0.95(5) 1.70(5) 2.644(4) 174(5) 2_575 N40 H40 O15 1.03(4) 1.60(4) 2.632(4) 172(4) . O43 H43 O15 0.84(2) 1.92(3) 2.662(4) 147(5) 2_666 O45 H45A O14 0.84(4) 2.32(4) 3.135(4) 164(5) . O45 H45B O26 0.84(5) 1.98(4) 2.799(4) 164(5) 2_566 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.028 _refine_diff_density_min -1.684 _refine_diff_density_rms 0.135 #=======================END======================== data_5 _database_code_depnum_ccdc_archive 'CCDC 775254' #TrackingRef '- ti7-19.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H16 Ce2 N4 O26, C24 H23 N4, N O3, 2(H2 O)' _chemical_formula_sum 'C44 H43 Ce2 N9 O31' _chemical_formula_weight 1474.11 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' Ce Ce -0.2486 2.6331 '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 10.7265(2) _cell_length_b 11.2537(2) _cell_length_c 13.3313(2) _cell_angle_alpha 109.3038(12) _cell_angle_beta 97.3572(9) _cell_angle_gamma 113.6834(8) _cell_volume 1326.02(4) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4895 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.80 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 734 _exptl_absorpt_coefficient_mu 1.804 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7143 _exptl_absorpt_correction_T_max 0.7736 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14839 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.80 _reflns_number_total 6184 _reflns_number_gt 5223 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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. One of the nitrate ions and the bipyridyl fragment are partially disordered. A number of ISOR and SIMU constraints were used in the crystallographic refinement to avoid unreasonable ADP values. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+3.8736P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6184 _refine_ls_number_parameters 407 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1307 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.002 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 Ce Ce 0.63528(3) 0.94906(3) 0.15723(2) 0.01874(12) Uani 1 1 d . . . O1 O 0.2162(3) 0.3991(3) -0.1331(3) 0.0175(7) Uani 1 1 d . . . C2 C 0.3067(5) 0.5427(5) -0.0708(4) 0.0158(9) Uani 1 1 d . . . C3 C 0.2897(5) 0.6224(5) -0.1252(4) 0.0144(9) Uani 1 1 d . . . C4 C 0.1809(5) 0.5202(5) -0.2308(4) 0.0166(9) Uani 1 1 d . . . C5 C 0.1171(5) 0.5284(5) -0.3257(4) 0.0203(10) Uani 1 1 d . . . H5 H 0.1394 0.6179 -0.3281 0.024 Uiso 1 1 calc R . . C6 C 0.0208(5) 0.4007(5) -0.4153(4) 0.0214(10) Uani 1 1 d . . . H6 H -0.0235 0.4035 -0.4803 0.026 Uiso 1 1 calc R . . C7 C -0.0136(5) 0.2683(5) -0.4135(4) 0.0214(10) Uani 1 1 d . . . H7 H -0.0796 0.1837 -0.4774 0.026 Uiso 1 1 calc R . . C8 C 0.0462(5) 0.2569(5) -0.3208(4) 0.0213(10) Uani 1 1 d . . . H8 H 0.0238 0.1673 -0.3187 0.026 Uiso 1 1 calc R . . C9 C 0.1412(5) 0.3859(5) -0.2316(4) 0.0164(9) Uani 1 1 d . . . C10 C 0.3948(5) 0.5738(5) 0.0403(4) 0.0156(9) Uani 1 1 d . . . O11 O 0.4800(4) 0.7010(4) 0.1075(3) 0.0195(7) Uani 1 1 d . . . O12 O 0.3771(4) 0.4678(3) 0.0603(3) 0.0188(7) Uani 1 1 d . . . C13 C 0.3698(5) 0.7790(5) -0.0942(4) 0.0161(9) Uani 1 1 d . . . O14 O 0.4999(4) 0.8482(3) -0.0359(3) 0.0190(7) Uani 1 1 d . . . O15 O 0.3027(4) 0.8309(4) -0.1334(3) 0.0226(7) Uani 1 1 d . . . N16 N 0.6316(5) 1.0538(5) 0.3964(4) 0.0259(9) Uani 1 1 d . . . O17 O 0.5665(4) 0.9224(4) 0.3322(3) 0.0258(8) Uani 1 1 d . . . O18 O 0.6857(4) 1.1408(4) 0.3540(3) 0.0251(8) Uani 1 1 d . . . O19 O 0.6445(4) 1.0976(4) 0.4971(3) 0.0334(9) Uani 1 1 d . . . N20 N 0.9375(5) 1.0519(5) 0.2941(4) 0.0334(11) Uani 1 1 d U . . O21 O 0.9129(4) 1.1104(4) 0.2342(3) 0.0331(9) Uani 1 1 d . . . O22 O 0.8341(4) 0.9610(4) 0.3077(3) 0.0313(9) Uani 1 1 d . . . O23 O 1.0615(6) 1.0842(6) 0.3397(5) 0.0660(15) Uani 1 1 d U . . O24 O 0.4058(4) 0.9599(4) 0.1604(3) 0.0301(8) Uani 1 1 d . . . H24A H 0.3752 1.0045 0.1183 0.045 Uiso 1 1 d . . . H24B H 0.4000 0.9991 0.2256 0.045 Uiso 1 1 d . . . O25 O 0.7610(4) 0.8245(4) 0.0570(3) 0.0240(7) Uani 1 1 d . . . H25A H 0.7037 0.7203 0.0271 0.036 Uiso 1 1 d R . . H25B H 0.8533 0.8509 0.0814 0.036 Uiso 1 1 d R . . O26 O 0.3329(5) 1.0383(5) 0.3565(4) 0.0451(11) Uani 1 1 d . . . H26A H 0.2409 1.0512 0.3516 0.068 Uiso 1 1 d . . . H26B H 0.3530 1.0188 0.4235 0.068 Uiso 1 1 d . . . N27 N 0.1170(15) 0.0040(14) 0.1069(11) 0.053(3) Uani 0.50 1 d PU . . O28 O 0.0519(10) -0.0925(10) 0.1337(8) 0.046(2) Uani 0.50 1 d PU . . O29 O 0.0506(10) 0.0164(12) 0.0306(8) 0.051(2) Uani 0.50 1 d PU . . O30 O 0.2201(9) 0.0831(9) 0.1448(7) 0.0339(17) Uani 0.50 1 d PU . . N31 N 0.4846(4) 0.4883(5) 0.7410(3) 0.0208(9) Uani 1 1 d . A . H31 H 0.5260 0.4945 0.8092 0.031 Uiso 1 1 d R . . C32 C 0.5180(6) 0.6142(6) 0.7362(5) 0.0259(11) Uani 1 1 d . . . H32 H 0.5838 0.7011 0.7985 0.031 Uiso 1 1 calc R . . C33 C 0.4567(7) 0.6167(8) 0.6410(6) 0.0368(15) Uani 1 1 d . A . H33 H 0.4799 0.7058 0.6376 0.044 Uiso 1 1 calc R . . C34 C 0.3611(7) 0.4906(9) 0.5494(5) 0.0436(18) Uani 1 1 d . . . C35 C 0.3312(6) 0.3637(8) 0.5581(5) 0.0413(16) Uani 1 1 d . A . H35 H 0.2671 0.2753 0.4966 0.050 Uiso 1 1 calc R . . C36 C 0.3932(6) 0.3645(6) 0.6546(5) 0.0294(12) Uani 1 1 d . . . H36 H 0.3711 0.2768 0.6602 0.035 Uiso 1 1 calc R A . C37A C 0.3200(11) 0.5424(12) 0.4639(9) 0.030(3) Uiso 0.457(14) 1 d P A 1 H37A H 0.3511 0.6410 0.4823 0.036 Uiso 0.457(14) 1 calc PR A 1 C38A C 0.2386(12) 0.4420(13) 0.3631(9) 0.034(3) Uiso 0.457(14) 1 d P A 1 H38A H 0.2045 0.3429 0.3436 0.041 Uiso 0.457(14) 1 calc PR A 1 C37B C 0.2753(10) 0.4467(10) 0.4325(8) 0.032(2) Uiso 0.543(15) 1 d P A 2 H37B H 0.2129 0.3491 0.3838 0.038 Uiso 0.543(15) 1 calc PR A 2 C38B C 0.2911(10) 0.5520(10) 0.4005(8) 0.032(2) Uiso 0.543(15) 1 d P A 2 H38B H 0.3512 0.6503 0.4486 0.038 Uiso 0.543(15) 1 calc PR A 2 C39 C 0.2044(8) 0.5005(12) 0.2805(6) 0.057(2) Uani 1 1 d . . . C40 C 0.2356(7) 0.6251(9) 0.2681(5) 0.050(2) Uani 1 1 d . A . H40 H 0.3044 0.7143 0.3269 0.060 Uiso 1 1 calc R . . C41 C 0.1685(6) 0.6213(7) 0.1720(5) 0.0317(12) Uani 1 1 d . . . H41 H 0.1914 0.7087 0.1655 0.038 Uiso 1 1 calc R A . N42 N 0.0721(5) 0.4992(5) 0.0874(3) 0.0250(9) Uani 1 1 d . A . H42 H 0.0283 0.4995 0.0271 0.030 Uiso 0.50 1 calc PR . . C43 C 0.0426(6) 0.3767(7) 0.0952(6) 0.0364(13) Uani 1 1 d . . . H43 H -0.0243 0.2891 0.0340 0.044 Uiso 1 1 calc R A . C44 C 0.1069(8) 0.3741(10) 0.1898(8) 0.058(2) Uani 1 1 d . A . H44 H 0.0844 0.2850 0.1932 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.02118(17) 0.01453(16) 0.01641(16) 0.00628(11) -0.00049(11) 0.00677(12) O1 0.0190(16) 0.0114(15) 0.0142(15) 0.0041(13) -0.0022(13) 0.0033(13) C2 0.017(2) 0.013(2) 0.014(2) 0.0061(18) 0.0050(17) 0.0047(18) C3 0.017(2) 0.015(2) 0.014(2) 0.0084(18) 0.0054(17) 0.0080(18) C4 0.016(2) 0.017(2) 0.018(2) 0.0083(19) 0.0039(18) 0.0078(18) C5 0.024(2) 0.021(2) 0.016(2) 0.010(2) 0.0021(19) 0.010(2) C6 0.020(2) 0.027(3) 0.016(2) 0.011(2) 0.0018(18) 0.010(2) C7 0.018(2) 0.016(2) 0.019(2) 0.0019(19) -0.0034(18) 0.0039(19) C8 0.024(3) 0.018(2) 0.019(2) 0.007(2) 0.0037(19) 0.008(2) C9 0.016(2) 0.017(2) 0.014(2) 0.0071(18) 0.0021(17) 0.0067(18) C10 0.016(2) 0.015(2) 0.015(2) 0.0081(18) 0.0052(17) 0.0053(18) O11 0.0229(17) 0.0170(17) 0.0133(15) 0.0052(14) 0.0006(13) 0.0069(14) O12 0.0252(18) 0.0148(16) 0.0164(15) 0.0085(13) 0.0032(13) 0.0087(14) C13 0.022(2) 0.017(2) 0.0106(19) 0.0083(18) 0.0053(17) 0.0076(19) O14 0.0207(17) 0.0151(16) 0.0158(15) 0.0072(14) 0.0005(13) 0.0045(14) O15 0.0234(18) 0.0187(17) 0.0236(17) 0.0131(15) 0.0001(14) 0.0068(14) N16 0.021(2) 0.027(2) 0.022(2) 0.0077(19) 0.0008(17) 0.0076(19) O17 0.028(2) 0.0181(18) 0.0203(17) 0.0060(15) 0.0014(15) 0.0048(15) O18 0.032(2) 0.0177(17) 0.0226(17) 0.0080(15) 0.0052(15) 0.0105(16) O19 0.034(2) 0.036(2) 0.0167(17) 0.0064(17) 0.0060(16) 0.0080(18) N20 0.0312(18) 0.0276(18) 0.0382(19) 0.0129(15) -0.0032(14) 0.0158(15) O21 0.029(2) 0.0212(19) 0.041(2) 0.0132(18) -0.0022(17) 0.0075(16) O22 0.039(2) 0.029(2) 0.0266(19) 0.0120(17) 0.0016(17) 0.0187(18) O23 0.057(2) 0.056(2) 0.080(2) 0.0327(18) -0.0063(16) 0.0276(17) O24 0.028(2) 0.034(2) 0.031(2) 0.0138(18) 0.0063(16) 0.0172(18) O25 0.0230(18) 0.0191(17) 0.0264(18) 0.0061(15) 0.0065(15) 0.0098(15) O26 0.048(3) 0.059(3) 0.047(3) 0.027(3) 0.020(2) 0.037(3) N27 0.054(3) 0.050(3) 0.058(3) 0.026(2) 0.011(2) 0.026(2) O28 0.046(3) 0.040(3) 0.053(3) 0.020(2) 0.009(2) 0.022(2) O29 0.049(3) 0.055(3) 0.044(3) 0.024(2) 0.018(2) 0.017(2) O30 0.026(3) 0.033(3) 0.049(3) 0.026(2) 0.0028(19) 0.015(2) N31 0.021(2) 0.032(2) 0.0161(19) 0.0147(18) 0.0074(16) 0.0145(19) C32 0.024(3) 0.025(3) 0.030(3) 0.010(2) 0.010(2) 0.012(2) C33 0.040(3) 0.061(4) 0.051(4) 0.045(4) 0.031(3) 0.039(3) C34 0.033(3) 0.101(6) 0.029(3) 0.043(4) 0.019(3) 0.046(4) C35 0.023(3) 0.067(5) 0.017(3) 0.005(3) 0.003(2) 0.017(3) C36 0.027(3) 0.029(3) 0.028(3) 0.011(2) 0.008(2) 0.010(2) C39 0.044(4) 0.141(8) 0.038(4) 0.061(5) 0.027(3) 0.067(5) C40 0.035(4) 0.085(6) 0.020(3) 0.004(3) 0.002(2) 0.036(4) C41 0.029(3) 0.037(3) 0.029(3) 0.010(3) 0.006(2) 0.019(3) N42 0.025(2) 0.040(3) 0.019(2) 0.019(2) 0.0075(17) 0.017(2) C43 0.027(3) 0.038(3) 0.045(3) 0.021(3) 0.010(3) 0.014(3) C44 0.050(4) 0.097(6) 0.092(6) 0.085(6) 0.046(5) 0.052(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce O11 2.401(3) . ? Ce O14 2.410(3) . ? Ce O15 2.435(3) 2_675 ? Ce O25 2.512(4) . ? Ce O24 2.518(4) . ? Ce O18 2.605(4) . ? Ce O17 2.607(4) . ? Ce O21 2.619(4) . ? Ce O22 2.661(4) . ? Ce N16 3.023(4) . ? O1 C2 1.375(5) . ? O1 C9 1.378(5) . ? C2 C3 1.374(6) . ? C2 C10 1.498(6) . ? C3 C4 1.449(6) . ? C3 C13 1.493(6) . ? C4 C9 1.393(6) . ? C4 C5 1.407(6) . ? C5 C6 1.384(7) . ? C5 H5 0.9500 . ? C6 C7 1.393(7) . ? C6 H6 0.9500 . ? C7 C8 1.386(7) . ? C7 H7 0.9500 . ? C8 C9 1.385(7) . ? C8 H8 0.9500 . ? C10 O12 1.254(5) . ? C10 O11 1.256(6) . ? C13 O15 1.254(6) . ? C13 O14 1.268(6) . ? O15 Ce 2.435(3) 2_675 ? N16 O19 1.235(6) . ? N16 O17 1.260(6) . ? N16 O18 1.267(6) . ? N20 O23 1.237(7) . ? N20 O21 1.254(6) . ? N20 O22 1.254(6) . ? O24 H24A 0.9732 . ? O24 H24B 0.8581 . ? O25 H25A 0.9800 . ? O25 H25B 0.8903 . ? O26 H26A 1.0512 . ? O26 H26B 1.0050 . ? N27 O30 1.019(14) . ? N27 O28 1.226(15) . ? N27 O29 1.246(15) . ? O29 O29 1.110(19) 2 ? N31 C36 1.334(7) . ? N31 C32 1.342(7) . ? N31 H31 0.9260 . ? C32 C33 1.366(8) . ? C32 H32 0.9500 . ? C33 C34 1.386(10) . ? C33 H33 0.9500 . ? C34 C35 1.380(11) . ? C34 C37B 1.509(10) . ? C34 C37A 1.535(12) . ? C35 C36 1.365(8) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37A C38A 1.322(16) . ? C37A H37A 0.9500 . ? C38A C39 1.533(13) . ? C38A H38A 0.9500 . ? C37B C38B 1.344(13) . ? C37B H37B 0.9500 . ? C38B C39 1.528(11) . ? C38B H38B 0.9500 . ? C39 C40 1.376(12) . ? C39 C44 1.387(13) . ? C40 C41 1.366(8) . ? C40 H40 0.9500 . ? C41 N42 1.328(8) . ? C41 H41 0.9500 . ? N42 C43 1.328(8) . ? N42 H42 0.8800 . ? C43 C44 1.374(9) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? 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 O11 Ce O14 73.85(11) . . ? O11 Ce O15 152.17(11) . 2_675 ? O14 Ce O15 80.81(11) . 2_675 ? O11 Ce O25 76.41(12) . . ? O14 Ce O25 76.89(12) . . ? O15 Ce O25 109.10(12) 2_675 . ? O11 Ce O24 81.25(12) . . ? O14 Ce O24 74.81(12) . . ? O15 Ce O24 81.17(12) 2_675 . ? O25 Ce O24 147.82(12) . . ? O11 Ce O18 119.84(11) . . ? O14 Ce O18 142.73(11) . . ? O15 Ce O18 75.10(11) 2_675 . ? O25 Ce O18 137.91(12) . . ? O24 Ce O18 73.74(12) . . ? O11 Ce O17 71.24(11) . . ? O14 Ce O17 133.09(11) . . ? O15 Ce O17 121.65(12) 2_675 . ? O25 Ce O17 122.55(12) . . ? O24 Ce O17 69.80(12) . . ? O18 Ce O17 48.95(11) . . ? O11 Ce O21 133.62(12) . . ? O14 Ce O21 123.76(12) . . ? O15 Ce O21 70.89(12) 2_675 . ? O25 Ce O21 68.59(13) . . ? O24 Ce O21 141.70(13) . . ? O18 Ce O21 74.11(13) . . ? O17 Ce O21 103.03(12) . . ? O11 Ce O22 92.56(12) . . ? O14 Ce O22 147.62(12) . . ? O15 Ce O22 115.17(12) 2_675 . ? O25 Ce O22 71.32(12) . . ? O24 Ce O22 133.11(13) . . ? O18 Ce O22 69.51(12) . . ? O17 Ce O22 64.29(12) . . ? O21 Ce O22 48.25(12) . . ? O11 Ce N16 95.67(12) . . ? O14 Ce N16 145.97(12) . . ? O15 Ce N16 99.03(12) 2_675 . ? O25 Ce N16 133.07(12) . . ? O24 Ce N16 71.59(12) . . ? O18 Ce N16 24.60(12) . . ? O17 Ce N16 24.46(12) . . ? O21 Ce N16 87.18(13) . . ? O22 Ce N16 62.80(12) . . ? C2 O1 C9 106.6(3) . . ? C3 C2 O1 111.4(4) . . ? C3 C2 C10 136.0(4) . . ? O1 C2 C10 112.6(4) . . ? C2 C3 C4 105.7(4) . . ? C2 C3 C13 130.6(4) . . ? C4 C3 C13 123.5(4) . . ? C9 C4 C5 118.5(4) . . ? C9 C4 C3 106.0(4) . . ? C5 C4 C3 135.4(4) . . ? C6 C5 C4 117.3(4) . . ? C6 C5 H5 121.4 . . ? C4 C5 H5 121.4 . . ? C5 C6 C7 122.3(4) . . ? C5 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C8 C7 C6 121.7(4) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C9 C8 C7 115.1(4) . . ? C9 C8 H8 122.5 . . ? C7 C8 H8 122.5 . . ? O1 C9 C8 124.7(4) . . ? O1 C9 C4 110.2(4) . . ? C8 C9 C4 125.0(4) . . ? O12 C10 O11 123.9(4) . . ? O12 C10 C2 116.4(4) . . ? O11 C10 C2 119.7(4) . . ? C10 O11 Ce 154.4(3) . . ? O15 C13 O14 124.9(4) . . ? O15 C13 C3 116.1(4) . . ? O14 C13 C3 118.9(4) . . ? C13 O14 Ce 137.8(3) . . ? C13 O15 Ce 136.0(3) . 2_675 ? O19 N16 O17 121.9(4) . . ? O19 N16 O18 120.6(5) . . ? O17 N16 O18 117.4(4) . . ? O19 N16 Ce 173.1(4) . . ? O17 N16 Ce 59.0(2) . . ? O18 N16 Ce 58.9(2) . . ? N16 O17 Ce 96.6(3) . . ? N16 O18 Ce 96.5(3) . . ? O23 N20 O21 120.6(5) . . ? O23 N20 O22 120.6(5) . . ? O21 N20 O22 118.8(5) . . ? N20 O21 Ce 97.2(3) . . ? N20 O22 Ce 95.1(3) . . ? Ce O24 H24A 119.3 . . ? Ce O24 H24B 115.1 . . ? H24A O24 H24B 104.2 . . ? Ce O25 H25A 111.4 . . ? Ce O25 H25B 124.8 . . ? H25A O25 H25B 110.5 . . ? H26A O26 H26B 108.5 . . ? O30 N27 O28 127.3(14) . . ? O30 N27 O29 114.0(13) . . ? O28 N27 O29 118.5(13) . . ? O29 O29 N27 150.6(16) 2 . ? C36 N31 C32 121.5(4) . . ? C36 N31 H31 123.4 . . ? C32 N31 H31 115.0 . . ? N31 C32 C33 119.5(5) . . ? N31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C32 C33 C34 120.7(6) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C35 C34 C33 117.6(5) . . ? C35 C34 C37B 105.0(7) . . ? C33 C34 C37B 137.4(7) . . ? C35 C34 C37A 139.2(7) . . ? C33 C34 C37A 103.3(7) . . ? C36 C35 C34 120.4(6) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? N31 C36 C35 120.2(6) . . ? N31 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38A C37A C34 116.1(10) . . ? C38A C37A H37A 121.9 . . ? C34 C37A H37A 121.9 . . ? C37A C38A C39 113.7(10) . . ? C37A C38A H38A 123.1 . . ? C39 C38A H38A 123.1 . . ? C38B C37B C34 117.0(9) . . ? C38B C37B H37B 121.5 . . ? C34 C37B H37B 121.5 . . ? C37B C38B C39 114.5(9) . . ? C37B C38B H38B 122.8 . . ? C39 C38B H38B 122.8 . . ? C40 C39 C44 116.6(5) . . ? C40 C39 C38B 103.8(8) . . ? C44 C39 C38B 139.6(8) . . ? C40 C39 C38A 143.0(9) . . ? C44 C39 C38A 100.4(8) . . ? C41 C40 C39 120.4(7) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? N42 C41 C40 122.0(6) . . ? N42 C41 H41 119.0 . . ? C40 C41 H41 119.0 . . ? C43 N42 C41 119.1(5) . . ? C43 N42 H42 120.4 . . ? C41 N42 H42 120.4 . . ? N42 C43 C44 121.4(7) . . ? N42 C43 H43 119.3 . . ? C44 C43 H43 119.3 . . ? C43 C44 C39 120.4(7) . . ? C43 C44 H44 119.8 . . ? C39 C44 H44 119.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O24 H24A O30 0.97 2.19 2.871(9) 126 1_565 O24 H24B O26 0.86 1.96 2.789(6) 163 . O25 H25A O12 0.98 1.80 2.748(5) 163 2_665 O25 H25B O28 0.89 1.91 2.805(10) 180 1_665 O26 H26A O23 1.05 2.10 3.148(7) 177 1_455 O26 H26B O19 1.01 1.94 2.891(6) 156 2_676 N31 H31 O12 0.93 1.73 2.645(5) 171 2_666 N42 H42 N42 0.88 1.76 2.637(8) 174 2_565 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.80 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.241 _refine_diff_density_min -1.370 _refine_diff_density_rms 0.171 #=======================END========================== data_6 _database_code_depnum_ccdc_archive 'CCDC 775255' #TrackingRef '- ti7-19.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H24 Dy2 O24, C12 H12 N2, C12 H10 N2' _chemical_formula_sum 'C64 H46 Dy2 N4 O24' _chemical_formula_weight 1580.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2635(2) _cell_length_b 11.0169(3) _cell_length_c 15.9085(5) _cell_angle_alpha 72.2962(11) _cell_angle_beta 76.7147(10) _cell_angle_gamma 88.2306(13) _cell_volume 1503.93(7) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5255 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 27.86 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 782 _exptl_absorpt_coefficient_mu 2.555 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6290 _exptl_absorpt_correction_T_max 0.7005 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16194 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 27.86 _reflns_number_total 7063 _reflns_number_gt 5973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+0.5333P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0035(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7063 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1087 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Dy Dy 0.20796(2) 0.991452(17) -0.018714(13) 0.01796(10) Uani 1 1 d . . . O1 O 0.1896(4) 1.2656(3) 0.2114(2) 0.0256(7) Uani 1 1 d . . . C2 C 0.1666(5) 1.2154(4) 0.1460(3) 0.0198(9) Uani 1 1 d . . . C3 C 0.0184(5) 1.1955(4) 0.1538(3) 0.0204(9) Uani 1 1 d . . . C4 C -0.0596(5) 1.2377(4) 0.2292(3) 0.0239(9) Uani 1 1 d . . . C5 C -0.2075(5) 1.2447(5) 0.2729(4) 0.0306(11) Uani 1 1 d . . . H5 H -0.2863 1.2225 0.2505 0.037 Uiso 1 1 calc R . . C6 C -0.2367(6) 1.2842(5) 0.3490(4) 0.0371(12) Uani 1 1 d . . . H6 H -0.3368 1.2879 0.3798 0.044 Uiso 1 1 calc R . . C7 C -0.1211(6) 1.3195(5) 0.3821(4) 0.0380(12) Uani 1 1 d . . . H7 H -0.1451 1.3457 0.4351 0.046 Uiso 1 1 calc R . . C8 C 0.0265(6) 1.3170(5) 0.3394(4) 0.0328(11) Uani 1 1 d . . . H8 H 0.1051 1.3413 0.3610 0.039 Uiso 1 1 calc R . . C9 C 0.0520(5) 1.2768(4) 0.2630(3) 0.0257(10) Uani 1 1 d . . . C10 C 0.3078(5) 1.1938(4) 0.0849(3) 0.0204(9) Uani 1 1 d . . . O11 O 0.3055(3) 1.1055(3) 0.0501(2) 0.0215(6) Uani 1 1 d . . . O12 O 0.4176(3) 1.2622(3) 0.0739(2) 0.0289(7) Uani 1 1 d . . . C13 C -0.0592(5) 1.1484(4) 0.0973(3) 0.0197(9) Uani 1 1 d . . . O14 O 0.0126(3) 1.1149(3) 0.0292(2) 0.0184(6) Uani 1 1 d . . . O15 O -0.1991(3) 1.1408(3) 0.1174(2) 0.0252(7) Uani 1 1 d . . . O16 O 0.0021(3) 0.5843(3) 0.3830(2) 0.0241(7) Uani 1 1 d . . . C17 C 0.0507(5) 0.6519(4) 0.2925(3) 0.0226(9) Uani 1 1 d . . . C18 C -0.0491(4) 0.7380(4) 0.2636(3) 0.0183(8) Uani 1 1 d . . . C19 C -0.1737(5) 0.7240(4) 0.3401(3) 0.0228(9) Uani 1 1 d . . . C20 C -0.3110(5) 0.7800(5) 0.3545(3) 0.0325(11) Uani 1 1 d . . . H20 H -0.3386 0.8462 0.3074 0.039 Uiso 1 1 calc R . . C21 C -0.4057(6) 0.7360(6) 0.4398(4) 0.0418(14) Uani 1 1 d . . . H21 H -0.5001 0.7717 0.4510 0.050 Uiso 1 1 calc R . . C22 C -0.3639(6) 0.6391(5) 0.5099(4) 0.0421(14) Uani 1 1 d . . . H22 H -0.4307 0.6118 0.5678 0.051 Uiso 1 1 calc R . . C23 C -0.2291(5) 0.5829(5) 0.4970(3) 0.0310(11) Uani 1 1 d . . . H23 H -0.2013 0.5168 0.5440 0.037 Uiso 1 1 calc R . . C24 C -0.1369(5) 0.6283(4) 0.4117(3) 0.0243(9) Uani 1 1 d . . . C25 C 0.1968(5) 0.6149(4) 0.2435(3) 0.0224(9) Uani 1 1 d . . . O26 O 0.2943(3) 0.5830(3) 0.2884(2) 0.0289(7) Uani 1 1 d . . . O27 O 0.2075(3) 0.6187(3) 0.1629(2) 0.0238(7) Uani 1 1 d . . . C28 C -0.0324(5) 0.8335(4) 0.1725(3) 0.0202(9) Uani 1 1 d . . . O29 O 0.0968(3) 0.8729(3) 0.12842(19) 0.0189(6) Uani 1 1 d . . . O30 O -0.1505(3) 0.8701(3) 0.1484(2) 0.0198(6) Uani 1 1 d . . . O31 O 0.3623(3) 0.8232(3) 0.0361(2) 0.0214(6) Uani 1 1 d . . . H31A H 0.4413 0.8047 0.0049 0.032 Uiso 1 1 d R . . H31B H 0.3108 0.7550 0.0784 0.032 Uiso 1 1 d R . . O32 O 0.4380(3) 1.0676(3) -0.1148(2) 0.0215(6) Uani 1 1 d . . . H32A H 0.4838 1.0517 -0.1679 0.032 Uiso 1 1 d . . . H32B H 0.5106 1.1084 -0.0979 0.032 Uiso 1 1 d . . . N33 N 0.5436(4) 0.5488(3) 0.1808(3) 0.0240(8) Uani 1 1 d . . . H33 H 0.4496 0.5640 0.2271 0.036 Uiso 1 1 d . . . C34 C 0.6723(5) 0.6074(5) 0.1742(4) 0.0310(11) Uani 1 1 d . . . H34 H 0.6750 0.6626 0.2095 0.037 Uiso 1 1 calc R . . C35 C 0.8001(5) 0.5884(5) 0.1170(4) 0.0303(11) Uani 1 1 d . . . H35 H 0.8906 0.6300 0.1135 0.036 Uiso 1 1 calc R . . C36 C 0.7986(5) 0.5085(4) 0.0638(3) 0.0220(9) Uani 1 1 d . . . C37 C 0.6623(5) 0.4511(4) 0.0724(4) 0.0290(11) Uani 1 1 d . . . H37 H 0.6557 0.3967 0.0370 0.035 Uiso 1 1 calc R . . C38 C 0.5373(5) 0.4716(4) 0.1309(4) 0.0297(11) Uani 1 1 d . . . H38 H 0.4455 0.4306 0.1362 0.036 Uiso 1 1 calc R . . C39 C 0.9302(5) 0.4844(4) 0.0015(3) 0.0246(10) Uani 1 1 d . . . H39 H 0.9154 0.4429 -0.0404 0.030 Uiso 1 1 calc R . . N40 N 0.5977(5) 0.0224(4) 0.7350(3) 0.0301(9) Uani 1 1 d . . . C41 C 0.5691(6) -0.0353(6) 0.6789(4) 0.0416(13) Uani 1 1 d . . . H41 H 0.4713 -0.0696 0.6899 0.050 Uiso 1 1 calc R . . C42 C 0.6727(6) -0.0489(6) 0.6051(4) 0.0429(14) Uani 1 1 d . . . H42 H 0.6448 -0.0905 0.5666 0.052 Uiso 1 1 calc R . . C43 C 0.8178(6) -0.0019(5) 0.5870(3) 0.0319(11) Uani 1 1 d . . . C44 C 0.8482(6) 0.0594(5) 0.6467(4) 0.0348(12) Uani 1 1 d . . . H44 H 0.9452 0.0940 0.6379 0.042 Uiso 1 1 calc R . . C45 C 0.7366(6) 0.0692(5) 0.7185(4) 0.0322(11) Uani 1 1 d . . . H45 H 0.7596 0.1112 0.7581 0.039 Uiso 1 1 calc R . . C46 C 0.9283(6) -0.0174(5) 0.5105(4) 0.0355(12) Uani 1 1 d . . . H46 H 0.8954 -0.0558 0.4719 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy 0.01519(13) 0.01953(13) 0.01847(13) -0.00548(8) -0.00317(8) 0.00224(8) O1 0.0256(16) 0.0284(16) 0.0263(18) -0.0143(13) -0.0048(13) 0.0004(13) C2 0.020(2) 0.019(2) 0.020(2) -0.0073(16) -0.0019(17) -0.0005(16) C3 0.021(2) 0.0171(19) 0.019(2) -0.0046(16) 0.0023(17) 0.0002(16) C4 0.028(2) 0.020(2) 0.022(2) -0.0078(17) -0.0001(18) 0.0009(18) C5 0.025(2) 0.031(2) 0.036(3) -0.014(2) 0.000(2) -0.004(2) C6 0.032(3) 0.039(3) 0.037(3) -0.020(2) 0.008(2) 0.000(2) C7 0.047(3) 0.038(3) 0.027(3) -0.015(2) 0.003(2) -0.001(2) C8 0.039(3) 0.031(2) 0.030(3) -0.014(2) -0.004(2) -0.002(2) C9 0.026(2) 0.024(2) 0.024(2) -0.0087(18) 0.0003(19) 0.0005(18) C10 0.020(2) 0.019(2) 0.023(2) -0.0073(17) -0.0058(17) 0.0029(17) O11 0.0168(14) 0.0226(15) 0.0287(17) -0.0138(13) -0.0051(13) 0.0039(12) O12 0.0177(15) 0.0302(17) 0.041(2) -0.0189(15) 0.0012(14) -0.0014(13) C13 0.017(2) 0.0178(19) 0.020(2) -0.0028(16) -0.0013(17) 0.0027(16) O14 0.0164(14) 0.0188(14) 0.0226(16) -0.0087(12) -0.0068(12) 0.0026(11) O15 0.0171(15) 0.0320(17) 0.0307(18) -0.0182(14) -0.0030(13) 0.0048(13) O16 0.0217(15) 0.0264(16) 0.0195(16) -0.0020(12) -0.0027(13) 0.0075(12) C17 0.019(2) 0.026(2) 0.020(2) -0.0037(17) -0.0045(17) 0.0007(17) C18 0.0158(19) 0.020(2) 0.017(2) -0.0040(16) -0.0012(16) -0.0016(16) C19 0.021(2) 0.023(2) 0.022(2) -0.0048(17) -0.0031(18) 0.0030(17) C20 0.024(2) 0.040(3) 0.025(3) -0.001(2) -0.002(2) 0.013(2) C21 0.032(3) 0.055(3) 0.028(3) -0.005(2) 0.000(2) 0.017(2) C22 0.032(3) 0.056(3) 0.023(3) 0.001(2) 0.004(2) 0.015(2) C23 0.030(3) 0.040(3) 0.016(2) -0.0001(19) -0.0020(19) 0.005(2) C24 0.019(2) 0.029(2) 0.024(2) -0.0062(18) -0.0050(18) 0.0058(18) C25 0.022(2) 0.0164(19) 0.024(2) -0.0001(16) -0.0037(18) -0.0009(17) O26 0.0199(16) 0.0393(18) 0.0251(18) -0.0078(14) -0.0042(13) 0.0109(14) O27 0.0260(16) 0.0238(15) 0.0188(17) -0.0066(12) 0.0003(13) 0.0029(13) C28 0.020(2) 0.021(2) 0.021(2) -0.0101(17) -0.0048(17) 0.0066(17) O29 0.0147(14) 0.0215(14) 0.0156(15) -0.0005(11) -0.0004(11) -0.0002(11) O30 0.0162(14) 0.0229(15) 0.0199(16) -0.0052(12) -0.0057(12) 0.0030(12) O31 0.0137(14) 0.0227(15) 0.0238(17) -0.0052(12) 0.0006(12) 0.0042(12) O32 0.0140(14) 0.0299(16) 0.0212(16) -0.0105(13) -0.0016(12) 0.0006(12) N33 0.0192(18) 0.0250(19) 0.026(2) -0.0082(15) -0.0015(15) 0.0033(15) C34 0.024(2) 0.033(3) 0.040(3) -0.021(2) -0.001(2) -0.002(2) C35 0.020(2) 0.031(2) 0.043(3) -0.021(2) 0.002(2) -0.0081(19) C36 0.017(2) 0.019(2) 0.029(3) -0.0066(17) -0.0040(18) 0.0022(16) C37 0.022(2) 0.030(2) 0.042(3) -0.022(2) -0.006(2) 0.0001(19) C38 0.018(2) 0.029(2) 0.043(3) -0.017(2) -0.002(2) 0.0007(19) C39 0.023(2) 0.022(2) 0.029(3) -0.0105(18) -0.0023(19) 0.0025(18) N40 0.027(2) 0.037(2) 0.024(2) -0.0106(17) -0.0011(17) 0.0010(17) C41 0.027(3) 0.054(3) 0.047(3) -0.026(3) 0.001(2) -0.006(2) C42 0.034(3) 0.051(3) 0.051(4) -0.031(3) -0.005(3) -0.005(3) C43 0.032(3) 0.035(3) 0.027(3) -0.013(2) 0.000(2) 0.000(2) C44 0.027(2) 0.044(3) 0.036(3) -0.020(2) 0.001(2) -0.004(2) C45 0.033(3) 0.035(3) 0.030(3) -0.017(2) -0.002(2) 0.000(2) C46 0.031(3) 0.044(3) 0.034(3) -0.021(2) 0.001(2) 0.001(2) _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 Dy O11 2.227(3) . ? Dy O29 2.315(3) . ? Dy O30 2.325(3) 2_575 ? Dy O32 2.327(3) . ? Dy O14 2.356(3) . ? Dy O31 2.381(3) . ? Dy O14 2.449(3) 2_575 ? Dy O15 2.460(3) 2_575 ? Dy C13 2.816(4) 2_575 ? Dy Dy 3.7688(4) 2_575 ? O1 C9 1.372(6) . ? O1 C2 1.376(5) . ? C2 C3 1.368(6) . ? C2 C10 1.501(6) . ? C3 C4 1.448(6) . ? C3 C13 1.482(6) . ? C4 C5 1.398(7) . ? C4 C9 1.404(7) . ? C5 C6 1.375(8) . ? C5 H5 0.9500 . ? C6 C7 1.409(8) . ? C6 H6 0.9500 . ? C7 C8 1.383(8) . ? C7 H7 0.9500 . ? C8 C9 1.384(7) . ? C8 H8 0.9500 . ? C10 O12 1.233(5) . ? C10 O11 1.258(5) . ? C13 O15 1.260(5) . ? C13 O14 1.284(5) . ? C13 Dy 2.816(4) 2_575 ? O14 Dy 2.449(3) 2_575 ? O15 Dy 2.460(3) 2_575 ? O16 C17 1.378(5) . ? O16 C24 1.388(5) . ? C17 C18 1.356(6) . ? C17 C25 1.511(6) . ? C18 C19 1.445(6) . ? C18 C28 1.487(6) . ? C19 C20 1.398(7) . ? C19 C24 1.397(6) . ? C20 C21 1.387(7) . ? C20 H20 0.9500 . ? C21 C22 1.408(7) . ? C21 H21 0.9500 . ? C22 C23 1.378(7) . ? C22 H22 0.9500 . ? C23 C24 1.379(6) . ? C23 H23 0.9500 . ? C25 O27 1.250(6) . ? C25 O26 1.254(6) . ? C28 O29 1.254(5) . ? C28 O30 1.256(5) . ? O30 Dy 2.325(3) 2_575 ? O31 H31A 0.8416 . ? O31 H31B 0.9006 . ? O32 H32A 0.9194 . ? O32 H32B 0.9490 . ? N33 C38 1.338(6) . ? N33 C34 1.341(6) . ? N33 H33 1.0489 . ? C34 C35 1.370(7) . ? C34 H34 0.9500 . ? C35 C36 1.397(7) . ? C35 H35 0.9500 . ? C36 C37 1.389(6) . ? C36 C39 1.457(6) . ? C37 C38 1.369(7) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C39 1.335(9) 2_765 ? C39 H39 0.9500 . ? N40 C41 1.318(7) . ? N40 C45 1.339(6) . ? C41 C42 1.379(8) . ? C41 H41 0.9500 . ? C42 C43 1.390(7) . ? C42 H42 0.9500 . ? C43 C44 1.401(7) . ? C43 C46 1.449(7) . ? C44 C45 1.382(7) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C46 1.331(10) 2_756 ? C46 H46 0.9500 . ? 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 O11 Dy O29 83.29(11) . . ? O11 Dy O30 108.51(11) . 2_575 ? O29 Dy O30 141.13(10) . 2_575 ? O11 Dy O32 75.16(11) . . ? O29 Dy O32 142.39(10) . . ? O30 Dy O32 75.82(10) 2_575 . ? O11 Dy O14 75.38(10) . . ? O29 Dy O14 74.97(10) . . ? O30 Dy O14 72.76(10) 2_575 . ? O32 Dy O14 126.57(10) . . ? O11 Dy O31 88.07(11) . . ? O29 Dy O31 69.97(10) . . ? O30 Dy O31 144.53(11) 2_575 . ? O32 Dy O31 78.73(10) . . ? O14 Dy O31 142.69(10) . . ? O11 Dy O14 147.85(11) . 2_575 ? O29 Dy O14 74.29(10) . 2_575 ? O30 Dy O14 77.69(10) 2_575 2_575 ? O32 Dy O14 135.63(10) . 2_575 ? O14 Dy O14 76.71(11) . 2_575 ? O31 Dy O14 105.01(10) . 2_575 ? O11 Dy O15 158.62(11) . 2_575 ? O29 Dy O15 107.61(11) . 2_575 ? O30 Dy O15 74.85(11) 2_575 2_575 ? O32 Dy O15 85.60(10) . 2_575 ? O14 Dy O15 124.71(10) . 2_575 ? O31 Dy O15 78.96(11) . 2_575 ? O14 Dy O15 53.23(10) 2_575 2_575 ? O11 Dy C13 174.83(11) . 2_575 ? O29 Dy C13 93.84(11) . 2_575 ? O30 Dy C13 71.15(11) 2_575 2_575 ? O32 Dy C13 109.50(11) . 2_575 ? O14 Dy C13 99.74(11) . 2_575 ? O31 Dy C13 95.01(11) . 2_575 ? O14 Dy C13 27.09(11) 2_575 2_575 ? O15 Dy C13 26.55(11) 2_575 2_575 ? O11 Dy Dy 113.10(8) . 2_575 ? O29 Dy Dy 70.24(7) . 2_575 ? O30 Dy Dy 71.10(7) 2_575 2_575 ? O32 Dy Dy 146.83(8) . 2_575 ? O14 Dy Dy 39.23(7) . 2_575 ? O31 Dy Dy 131.73(7) . 2_575 ? O14 Dy Dy 37.48(7) 2_575 2_575 ? O15 Dy Dy 88.11(7) 2_575 2_575 ? C13 Dy Dy 61.79(9) 2_575 2_575 ? C9 O1 C2 106.7(3) . . ? C3 C2 O1 111.2(4) . . ? C3 C2 C10 135.4(4) . . ? O1 C2 C10 113.4(4) . . ? C2 C3 C4 106.5(4) . . ? C2 C3 C13 130.6(4) . . ? C4 C3 C13 122.8(4) . . ? C5 C4 C9 118.1(4) . . ? C5 C4 C3 136.7(5) . . ? C9 C4 C3 105.2(4) . . ? C6 C5 C4 118.7(5) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C5 C6 C7 121.3(5) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C6 121.7(5) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C7 C8 C9 115.6(5) . . ? C7 C8 H8 122.2 . . ? C9 C8 H8 122.2 . . ? O1 C9 C8 125.0(4) . . ? O1 C9 C4 110.4(4) . . ? C8 C9 C4 124.6(5) . . ? O12 C10 O11 125.1(4) . . ? O12 C10 C2 117.5(4) . . ? O11 C10 C2 117.4(4) . . ? C10 O11 Dy 154.5(3) . . ? O15 C13 O14 119.6(4) . . ? O15 C13 C3 118.7(4) . . ? O14 C13 C3 121.6(4) . . ? O15 C13 Dy 60.8(2) . 2_575 ? O14 C13 Dy 60.3(2) . 2_575 ? C3 C13 Dy 167.8(3) . 2_575 ? C13 O14 Dy 144.1(3) . . ? C13 O14 Dy 92.6(2) . 2_575 ? Dy O14 Dy 103.29(10) . 2_575 ? C13 O15 Dy 92.7(3) . 2_575 ? C17 O16 C24 106.2(3) . . ? C18 C17 O16 111.5(4) . . ? C18 C17 C25 132.0(4) . . ? O16 C17 C25 116.4(4) . . ? C17 C18 C19 106.8(4) . . ? C17 C18 C28 127.3(4) . . ? C19 C18 C28 125.8(4) . . ? C20 C19 C24 119.1(4) . . ? C20 C19 C18 135.4(4) . . ? C24 C19 C18 105.5(4) . . ? C21 C20 C19 117.9(4) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? C20 C21 C22 121.0(5) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C23 C22 C21 121.9(5) . . ? C23 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C22 C23 C24 116.0(4) . . ? C22 C23 H23 122.0 . . ? C24 C23 H23 122.0 . . ? C23 C24 O16 125.9(4) . . ? C23 C24 C19 124.1(4) . . ? O16 C24 C19 110.0(4) . . ? O27 C25 O26 127.0(4) . . ? O27 C25 C17 116.8(4) . . ? O26 C25 C17 116.2(4) . . ? O29 C28 O30 126.1(4) . . ? O29 C28 C18 117.5(4) . . ? O30 C28 C18 116.3(4) . . ? C28 O29 Dy 136.5(3) . . ? C28 O30 Dy 135.0(3) . 2_575 ? Dy O31 H31A 125.0 . . ? Dy O31 H31B 113.0 . . ? H31A O31 H31B 113.7 . . ? Dy O32 H32A 129.1 . . ? Dy O32 H32B 123.0 . . ? H32A O32 H32B 106.8 . . ? C38 N33 C34 120.5(4) . . ? C38 N33 H33 121.6 . . ? C34 N33 H33 117.8 . . ? N33 C34 C35 120.7(5) . . ? N33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C34 C35 C36 120.6(4) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C37 C36 C35 116.4(4) . . ? C37 C36 C39 120.1(4) . . ? C35 C36 C39 123.5(4) . . ? C38 C37 C36 121.2(4) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? N33 C38 C37 120.5(4) . . ? N33 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C39 C39 C36 125.4(6) 2_765 . ? C39 C39 H39 117.3 2_765 . ? C36 C39 H39 117.3 . . ? C41 N40 C45 117.0(4) . . ? N40 C41 C42 123.9(5) . . ? N40 C41 H41 118.1 . . ? C42 C41 H41 118.1 . . ? C41 C42 C43 120.1(5) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C42 C43 C44 116.0(5) . . ? C42 C43 C46 120.7(5) . . ? C44 C43 C46 123.4(5) . . ? C45 C44 C43 119.7(5) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? N40 C45 C44 123.4(5) . . ? N40 C45 H45 118.3 . . ? C44 C45 H45 118.3 . . ? C46 C46 C43 125.9(7) 2_756 . ? C46 C46 H46 117.0 2_756 . ? C43 C46 H46 117.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O31 H31A O12 0.84 1.89 2.710(4) 165 2_675 O31 H31B O27 0.90 1.80 2.703(4) 180 . O32 H32A N40 0.92 1.77 2.684(5) 171 1_564 O32 H32B O31 0.95 1.99 2.924(4) 168 2_675 N33 H33 O26 1.05 1.59 2.632(5) 172 . _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 3.395 _refine_diff_density_min -1.972 _refine_diff_density_rms 0.167 #===========================END======================= data_7 _database_code_depnum_ccdc_archive 'CCDC 775256' #TrackingRef '- ti7-19.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H26 O24 Tb2, 2(C12 H10 N2)' _chemical_formula_sum 'C64 H46 N4 O24 Tb2' _chemical_formula_weight 1572.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2559(3) _cell_length_b 10.9405(4) _cell_length_c 16.0001(7) _cell_angle_alpha 72.5854(15) _cell_angle_beta 76.3961(13) _cell_angle_gamma 86.9620(17) _cell_volume 1502.34(10) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5633 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.99 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 2.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5300 _exptl_absorpt_correction_T_max 0.7936 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16180 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 26.99 _reflns_number_total 6424 _reflns_number_gt 5128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo $ Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0048(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6424 _refine_ls_number_parameters 431 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 Tb Tb 0.70852(3) 0.99426(2) -0.018468(17) 0.03052(13) Uani 1 1 d . . . O1 O 0.3186(5) 0.7201(5) -0.2054(3) 0.0546(13) Uani 1 1 d . . . C2 C 0.3384(8) 0.7715(9) -0.1409(6) 0.069(2) Uani 1 1 d . . . C3 C 0.4901(9) 0.7901(9) -0.1481(6) 0.074(3) Uani 1 1 d . . . C4 C 0.5677(8) 0.7541(6) -0.2257(4) 0.0459(16) Uani 1 1 d . . . C5 C 0.7135(7) 0.7524(6) -0.2725(5) 0.0434(15) Uani 1 1 d . . . H5 H 0.7927 0.7734 -0.2506 0.052 Uiso 1 1 calc R . . C6 C 0.7421(9) 0.7197(7) -0.3518(5) 0.0579(19) Uani 1 1 d . . . H6 H 0.8415 0.7223 -0.3860 0.069 Uiso 1 1 calc R . . C7 C 0.6253(8) 0.6824(8) -0.3824(5) 0.0580(19) Uani 1 1 d . . . H7 H 0.6479 0.6585 -0.4364 0.070 Uiso 1 1 calc R . . C8 C 0.4802(8) 0.6798(6) -0.3362(4) 0.0463(15) Uani 1 1 d . . . H8 H 0.4008 0.6558 -0.3567 0.056 Uiso 1 1 calc R . . C9 C 0.4569(7) 0.7142(6) -0.2580(4) 0.0421(14) Uani 1 1 d . . . C10 C 0.1991(7) 0.7934(7) -0.0805(4) 0.0454(16) Uani 1 1 d . . . O11 O 0.2018(5) 0.8890(4) -0.0516(3) 0.0406(10) Uani 1 1 d . . . O12 O 0.0884(5) 0.7284(4) -0.0687(3) 0.0449(11) Uani 1 1 d . . . C13 C 0.5677(6) 0.8464(5) -0.0959(4) 0.0331(12) Uani 1 1 d . . . O14 O 0.4940(4) 0.8809(3) -0.0287(3) 0.0314(8) Uani 1 1 d . . . O15 O 0.7051(4) 0.8620(4) -0.1202(3) 0.0394(10) Uani 1 1 d . . . O16 O 0.5066(4) 0.5864(4) 0.3821(3) 0.0376(9) Uani 1 1 d . . . C17 C 0.5559(6) 0.6541(5) 0.2916(4) 0.0338(12) Uani 1 1 d . . . C18 C 0.4550(6) 0.7400(5) 0.2626(4) 0.0321(12) Uani 1 1 d . . . C19 C 0.3293(6) 0.7277(5) 0.3379(4) 0.0347(12) Uani 1 1 d . . . C20 C 0.1896(7) 0.7834(6) 0.3522(4) 0.0422(14) Uani 1 1 d . . . H20 H 0.1612 0.8495 0.3054 0.051 Uiso 1 1 calc R . . C21 C 0.0942(8) 0.7405(8) 0.4356(5) 0.0583(19) Uani 1 1 d . . . H21 H -0.0019 0.7762 0.4456 0.070 Uiso 1 1 calc R . . C22 C 0.1360(8) 0.6454(7) 0.5057(5) 0.059(2) Uani 1 1 d . . . H22 H 0.0683 0.6190 0.5627 0.071 Uiso 1 1 calc R . . C23 C 0.2734(8) 0.5887(7) 0.4941(4) 0.0476(16) Uani 1 1 d . . . H23 H 0.3018 0.5233 0.5413 0.057 Uiso 1 1 calc R . . C24 C 0.3671(7) 0.6331(6) 0.4096(4) 0.0377(13) Uani 1 1 d . . . C25 C 0.7041(7) 0.6143(5) 0.2446(4) 0.0354(13) Uani 1 1 d . . . O26 O 0.7185(5) 0.6216(4) 0.1637(3) 0.0374(9) Uani 1 1 d . . . O27 O 0.7974(5) 0.5788(5) 0.2914(3) 0.0521(12) Uani 1 1 d . . . H27 H 0.8834 0.5965 0.2585 0.078 Uiso 1 1 calc R . . C28 C 0.4704(6) 0.8352(5) 0.1723(4) 0.0280(11) Uani 1 1 d . . . O29 O 0.3504(4) 0.8672(3) 0.1476(3) 0.0327(8) Uani 1 1 d . . . O30 O 0.5980(4) 0.8775(3) 0.1289(2) 0.0310(8) Uani 1 1 d . . . O31 O 0.8657(4) 0.8228(3) 0.0359(3) 0.0312(8) Uani 1 1 d . . . H31A H 0.9399 0.7935 -0.0002 0.047 Uiso 1 1 d R . . H31B H 0.8196 0.7607 0.0845 0.047 Uiso 1 1 d R . . O32 O 0.9399(4) 1.0681(4) -0.1134(3) 0.0376(9) Uani 1 1 d . . . H32A H 0.9811 1.0473 -0.1641 0.056 Uiso 1 1 d R . . H32B H 1.0077 1.0942 -0.0899 0.056 Uiso 1 1 d R . . N33 N 0.1012(6) 0.0166(5) 0.7386(4) 0.0423(12) Uani 1 1 d . . . C34 C 0.2381(8) 0.0635(7) 0.7212(5) 0.0503(17) Uani 1 1 d . . . H34 H 0.2614 0.1043 0.7613 0.060 Uiso 1 1 calc R . . C35 C 0.3471(8) 0.0563(7) 0.6490(5) 0.0524(17) Uani 1 1 d . . . H35 H 0.4422 0.0940 0.6388 0.063 Uiso 1 1 calc R . . C36 C 0.3194(7) -0.0064(6) 0.5896(4) 0.0432(14) Uani 1 1 d . . . C37 C 0.1766(8) -0.0557(8) 0.6090(6) 0.062(2) Uani 1 1 d . . . H37 H 0.1498 -0.0993 0.5715 0.075 Uiso 1 1 calc R . . C38 C 0.0732(8) -0.0415(7) 0.6831(5) 0.059(2) Uani 1 1 d . . . H38 H -0.0241 -0.0758 0.6946 0.070 Uiso 1 1 calc R . . C39 C 0.4297(7) -0.0203(7) 0.5121(5) 0.0476(16) Uani 1 1 d . . . H39 H 0.3984 -0.0623 0.4752 0.057 Uiso 1 1 calc R . . N40 N 0.0487(6) 0.5433(5) 0.1845(4) 0.0438(12) Uani 1 1 d . . . C41 C 0.1755(7) 0.5996(6) 0.1794(4) 0.0415(14) Uani 1 1 d . . . H41 H 0.1781 0.6512 0.2173 0.050 Uiso 1 1 calc R . . C42 C 0.3006(9) 0.5837(7) 0.1206(5) 0.063(2) Uani 1 1 d . . . H42 H 0.3907 0.6249 0.1168 0.076 Uiso 1 1 calc R . . C43 C 0.2982(8) 0.5070(8) 0.0652(6) 0.071(3) Uani 1 1 d . . . C44 C 0.1654(7) 0.4500(6) 0.0721(4) 0.0428(15) Uani 1 1 d . . . H44 H 0.1594 0.3976 0.0352 0.051 Uiso 1 1 calc R . . C45 C 0.0424(7) 0.4695(6) 0.1324(5) 0.0463(16) Uani 1 1 d . . . H45 H -0.0494 0.4298 0.1376 0.056 Uiso 1 1 calc R . . C46 C 0.424(2) 0.494(3) -0.0025(9) 0.080(2) Uani 1 1 d . . . H46 H 0.4068 0.4776 -0.0543 0.120 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb 0.03222(18) 0.03320(19) 0.02693(18) -0.00697(11) -0.01004(11) -0.00292(11) O1 0.043(3) 0.079(3) 0.055(3) -0.045(3) -0.002(2) -0.015(2) C2 0.040(4) 0.113(7) 0.071(5) -0.060(5) 0.000(4) -0.022(4) C3 0.054(5) 0.111(7) 0.067(5) -0.063(5) 0.024(4) -0.047(5) C4 0.051(4) 0.045(4) 0.040(4) -0.020(3) 0.006(3) -0.010(3) C5 0.041(3) 0.045(4) 0.047(4) -0.021(3) -0.003(3) -0.006(3) C6 0.052(4) 0.072(5) 0.050(4) -0.028(4) 0.003(3) -0.003(3) C7 0.059(5) 0.080(5) 0.041(4) -0.027(4) -0.009(3) -0.003(4) C8 0.057(4) 0.046(4) 0.039(4) -0.017(3) -0.009(3) -0.003(3) C9 0.050(4) 0.040(3) 0.039(3) -0.017(3) -0.007(3) -0.004(3) C10 0.045(4) 0.060(4) 0.038(3) -0.026(3) -0.004(3) -0.021(3) O11 0.050(3) 0.038(2) 0.038(2) -0.0087(18) -0.021(2) -0.0064(19) O12 0.035(2) 0.050(3) 0.053(3) -0.027(2) 0.000(2) -0.0122(19) C13 0.038(3) 0.033(3) 0.027(3) -0.007(2) -0.004(2) -0.005(2) O14 0.034(2) 0.032(2) 0.029(2) -0.0119(16) -0.0049(17) -0.0040(15) O15 0.034(2) 0.050(2) 0.043(2) -0.0236(19) -0.0136(19) 0.0038(18) O16 0.040(2) 0.044(2) 0.024(2) -0.0035(16) -0.0056(18) 0.0064(17) C17 0.037(3) 0.038(3) 0.025(3) -0.006(2) -0.012(2) 0.001(2) C18 0.037(3) 0.036(3) 0.026(3) -0.010(2) -0.010(2) -0.005(2) C19 0.036(3) 0.038(3) 0.031(3) -0.007(2) -0.014(3) 0.002(2) C20 0.039(3) 0.053(4) 0.029(3) -0.003(3) -0.011(3) 0.010(3) C21 0.043(4) 0.080(5) 0.042(4) -0.011(4) -0.003(3) 0.016(3) C22 0.054(4) 0.081(5) 0.027(3) -0.002(3) 0.000(3) 0.019(4) C23 0.054(4) 0.057(4) 0.024(3) -0.001(3) -0.009(3) 0.009(3) C24 0.035(3) 0.046(3) 0.030(3) -0.007(2) -0.010(3) 0.004(2) C25 0.038(3) 0.033(3) 0.034(3) -0.007(2) -0.010(3) -0.002(2) O26 0.045(2) 0.033(2) 0.031(2) -0.0063(16) -0.0057(19) 0.0002(17) O27 0.039(2) 0.081(3) 0.039(3) -0.023(2) -0.012(2) 0.017(2) C28 0.034(3) 0.026(3) 0.028(3) -0.010(2) -0.011(2) 0.001(2) O29 0.033(2) 0.036(2) 0.030(2) -0.0072(16) -0.0094(17) -0.0019(16) O30 0.034(2) 0.0320(19) 0.0242(19) -0.0022(15) -0.0081(16) -0.0028(15) O31 0.0290(19) 0.0309(19) 0.032(2) -0.0063(16) -0.0074(16) 0.0002(15) O32 0.035(2) 0.048(2) 0.031(2) -0.0114(18) -0.0091(18) -0.0055(17) N33 0.041(3) 0.046(3) 0.041(3) -0.014(2) -0.009(2) -0.006(2) C34 0.050(4) 0.062(4) 0.043(4) -0.022(3) -0.008(3) -0.011(3) C35 0.045(4) 0.065(4) 0.049(4) -0.027(3) 0.003(3) -0.016(3) C36 0.044(4) 0.052(4) 0.035(3) -0.015(3) -0.008(3) -0.006(3) C37 0.046(4) 0.089(6) 0.067(5) -0.051(4) -0.004(4) -0.016(4) C38 0.045(4) 0.073(5) 0.066(5) -0.036(4) -0.004(4) -0.017(3) C39 0.049(4) 0.057(4) 0.042(4) -0.026(3) -0.005(3) -0.005(3) N40 0.036(3) 0.055(3) 0.048(3) -0.027(3) -0.011(2) 0.005(2) C41 0.052(4) 0.037(3) 0.038(3) -0.015(3) -0.011(3) -0.003(3) C42 0.059(5) 0.072(5) 0.063(5) -0.042(4) 0.017(4) -0.040(4) C43 0.050(4) 0.093(6) 0.079(6) -0.063(5) 0.026(4) -0.040(4) C44 0.045(4) 0.044(3) 0.043(4) -0.020(3) -0.006(3) -0.008(3) C45 0.032(3) 0.057(4) 0.063(4) -0.031(3) -0.020(3) 0.007(3) C46 0.067(5) 0.081(5) 0.072(5) -0.032(4) 0.018(4) 0.005(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 Tb O11 2.232(4) 2_675 ? Tb O29 2.330(4) 2_675 ? Tb O30 2.332(4) . ? Tb O32 2.338(4) . ? Tb O14 2.372(4) 2_675 ? Tb O31 2.392(4) . ? Tb O14 2.458(4) . ? Tb O15 2.486(4) . ? Tb C13 2.834(6) . ? Tb Tb 3.7663(5) 2_675 ? O1 C2 1.364(8) . ? O1 C9 1.367(8) . ? C2 C3 1.402(10) . ? C2 C10 1.475(10) . ? C3 C4 1.433(9) . ? C3 C13 1.493(9) . ? C4 C5 1.383(9) . ? C4 C9 1.393(9) . ? C5 C6 1.383(10) . ? C5 H5 0.9500 . ? C6 C7 1.410(10) . ? C6 H6 0.9500 . ? C7 C8 1.369(10) . ? C7 H7 0.9500 . ? C8 C9 1.379(9) . ? C8 H8 0.9500 . ? C10 O12 1.224(7) . ? C10 O11 1.267(7) . ? O11 Tb 2.232(4) 2_675 ? C13 O15 1.244(7) . ? C13 O14 1.280(7) . ? O14 Tb 2.372(4) 2_675 ? O16 C24 1.386(7) . ? O16 C17 1.391(7) . ? C17 C18 1.349(8) . ? C17 C25 1.512(8) . ? C18 C19 1.444(8) . ? C18 C28 1.486(7) . ? C19 C20 1.399(9) . ? C19 C24 1.397(8) . ? C20 C21 1.376(9) . ? C20 H20 0.9500 . ? C21 C22 1.398(10) . ? C21 H21 0.9500 . ? C22 C23 1.382(10) . ? C22 H22 0.9500 . ? C23 C24 1.383(8) . ? C23 H23 0.9500 . ? C25 O27 1.245(7) . ? C25 O26 1.248(7) . ? O27 H27 0.8400 . ? C28 O30 1.253(6) . ? C28 O29 1.263(6) . ? O29 Tb 2.330(4) 2_675 ? O31 H31A 0.8997 . ? O31 H31B 0.8990 . ? O32 H32A 0.9006 . ? O32 H32B 0.9003 . ? N33 C38 1.313(9) . ? N33 C34 1.328(8) . ? C34 C35 1.363(10) . ? C34 H34 0.9500 . ? C35 C36 1.401(9) . ? C35 H35 0.9500 . ? C36 C37 1.384(9) . ? C36 C39 1.450(9) . ? C37 C38 1.380(10) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C39 1.328(13) 2_656 ? C39 H39 0.9500 . ? N40 C41 1.329(8) . ? N40 C45 1.333(8) . ? C41 C42 1.349(10) . ? C41 H41 0.9500 . ? C42 C43 1.394(9) . ? C42 H42 0.9500 . ? C43 C44 1.374(9) . ? C43 C46 1.425(14) . ? C44 C45 1.361(9) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C46 1.44(4) 2_665 ? C46 H46 0.9500 . ? 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 O11 Tb O29 108.26(14) 2_675 2_675 ? O11 Tb O30 82.30(14) 2_675 . ? O29 Tb O30 141.27(13) 2_675 . ? O11 Tb O32 76.18(15) 2_675 . ? O29 Tb O32 76.12(13) 2_675 . ? O30 Tb O32 141.88(13) . . ? O11 Tb O14 75.04(15) 2_675 2_675 ? O29 Tb O14 72.57(13) 2_675 2_675 ? O30 Tb O14 74.72(13) . 2_675 ? O32 Tb O14 127.44(13) . 2_675 ? O11 Tb O31 89.38(14) 2_675 . ? O29 Tb O31 144.30(14) 2_675 . ? O30 Tb O31 70.06(13) . . ? O32 Tb O31 78.54(13) . . ? O14 Tb O31 143.05(13) 2_675 . ? O11 Tb O14 147.68(15) 2_675 . ? O29 Tb O14 78.97(12) 2_675 . ? O30 Tb O14 74.21(12) . . ? O32 Tb O14 135.27(13) . . ? O14 Tb O14 77.53(13) 2_675 . ? O31 Tb O14 102.74(12) . . ? O11 Tb O15 159.47(16) 2_675 . ? O29 Tb O15 73.90(14) 2_675 . ? O30 Tb O15 109.12(14) . . ? O32 Tb O15 84.82(14) . . ? O14 Tb O15 123.82(13) 2_675 . ? O31 Tb O15 79.16(13) . . ? O14 Tb O15 52.60(13) . . ? O11 Tb C13 174.47(16) 2_675 . ? O29 Tb C13 72.45(14) 2_675 . ? O30 Tb C13 93.78(14) . . ? O32 Tb C13 109.20(15) . . ? O14 Tb C13 100.20(15) 2_675 . ? O31 Tb C13 92.96(15) . . ? O14 Tb C13 26.79(14) . . ? O15 Tb C13 26.01(15) . . ? O11 Tb Tb 112.89(12) 2_675 2_675 ? O29 Tb Tb 71.73(9) 2_675 2_675 ? O30 Tb Tb 69.90(9) . 2_675 ? O32 Tb Tb 147.83(10) . 2_675 ? O14 Tb Tb 39.59(8) 2_675 2_675 ? O31 Tb Tb 130.33(8) . 2_675 ? O14 Tb Tb 37.94(9) . 2_675 ? O15 Tb Tb 87.37(9) . 2_675 ? C13 Tb Tb 61.90(12) . 2_675 ? C2 O1 C9 106.2(5) . . ? O1 C2 C3 110.7(6) . . ? O1 C2 C10 114.2(6) . . ? C3 C2 C10 135.0(6) . . ? C2 C3 C4 106.1(6) . . ? C2 C3 C13 131.2(7) . . ? C4 C3 C13 122.5(6) . . ? C5 C4 C9 117.9(6) . . ? C5 C4 C3 137.1(7) . . ? C9 C4 C3 105.0(6) . . ? C6 C5 C4 119.0(7) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C7 120.6(7) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 121.7(7) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C7 C8 C9 115.6(6) . . ? C7 C8 H8 122.2 . . ? C9 C8 H8 122.2 . . ? O1 C9 C8 123.0(6) . . ? O1 C9 C4 111.8(5) . . ? C8 C9 C4 125.0(6) . . ? O12 C10 O11 125.0(6) . . ? O12 C10 C2 119.4(6) . . ? O11 C10 C2 115.2(5) . . ? C10 O11 Tb 154.2(4) . 2_675 ? O15 C13 O14 120.5(5) . . ? O15 C13 C3 118.9(5) . . ? O14 C13 C3 120.6(5) . . ? O15 C13 Tb 61.2(3) . . ? O14 C13 Tb 60.0(3) . . ? C3 C13 Tb 170.1(5) . . ? C13 O14 Tb 143.8(4) . 2_675 ? C13 O14 Tb 93.2(3) . . ? Tb O14 Tb 102.47(13) 2_675 . ? C13 O15 Tb 92.8(3) . . ? C24 O16 C17 105.8(4) . . ? C18 C17 O16 111.5(5) . . ? C18 C17 C25 132.8(5) . . ? O16 C17 C25 115.6(5) . . ? C17 C18 C19 107.0(5) . . ? C17 C18 C28 127.6(5) . . ? C19 C18 C28 125.3(5) . . ? C20 C19 C24 118.4(5) . . ? C20 C19 C18 136.0(5) . . ? C24 C19 C18 105.6(5) . . ? C21 C20 C19 118.7(6) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? C20 C21 C22 121.2(7) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C23 C22 C21 121.7(6) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C24 C23 C22 116.0(6) . . ? C24 C23 H23 122.0 . . ? C22 C23 H23 122.0 . . ? C23 C24 O16 125.7(5) . . ? C23 C24 C19 124.0(6) . . ? O16 C24 C19 110.2(5) . . ? O27 C25 O26 127.9(6) . . ? O27 C25 C17 115.9(5) . . ? O26 C25 C17 116.2(5) . . ? C25 O27 H27 109.5 . . ? O30 C28 O29 126.2(5) . . ? O30 C28 C18 118.3(5) . . ? O29 C28 C18 115.6(5) . . ? C28 O29 Tb 134.2(3) . 2_675 ? C28 O30 Tb 136.8(3) . . ? Tb O31 H31A 123.6 . . ? Tb O31 H31B 114.4 . . ? H31A O31 H31B 113.0 . . ? Tb O32 H32A 125.3 . . ? Tb O32 H32B 118.0 . . ? H32A O32 H32B 112.8 . . ? C38 N33 C34 116.9(6) . . ? N33 C34 C35 123.5(6) . . ? N33 C34 H34 118.3 . . ? C35 C34 H34 118.3 . . ? C34 C35 C36 120.3(6) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.9 . . ? C37 C36 C35 115.5(6) . . ? C37 C36 C39 120.7(6) . . ? C35 C36 C39 123.8(6) . . ? C38 C37 C36 119.8(6) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? N33 C38 C37 124.0(6) . . ? N33 C38 H38 118.0 . . ? C37 C38 H38 118.0 . . ? C39 C39 C36 126.1(8) 2_656 . ? C39 C39 H39 116.9 2_656 . ? C36 C39 H39 116.9 . . ? C41 N40 C45 121.0(6) . . ? N40 C41 C42 120.3(6) . . ? N40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C43 120.3(6) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.8 . . ? C44 C43 C42 118.0(7) . . ? C44 C43 C46 119.2(7) . . ? C42 C43 C46 122.6(7) . . ? C45 C44 C43 119.3(6) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? N40 C45 C44 121.1(6) . . ? N40 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C46 C46 C43 124(2) 2_665 . ? C46 C46 H46 118.0 2_665 . ? C43 C46 H46 117.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O27 H27 N40 0.84 1.88 2.630(7) 147 1_655 O31 H31A O12 0.90 1.80 2.702(6) 178 1_655 O31 H31B O26 0.90 1.80 2.682(5) 167 . O32 H32A N33 0.90 1.80 2.684(7) 167 1_664 O32 H32B O31 0.90 2.00 2.892(5) 170 2_775 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.891 _refine_diff_density_min -2.113 _refine_diff_density_rms 0.158 #========================END=========================== data_8 _database_code_depnum_ccdc_archive 'CCDC 775257' #TrackingRef '- ti7-19.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H20 N2 O28 Sm2, 2(C12 H12 N2), 6(H2 O)' _chemical_formula_sum 'C64 H56 N6 O34 Sm2' _chemical_formula_weight 1753.86 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 11.0888(2) _cell_length_b 12.6273(4) _cell_length_c 12.7130(3) _cell_angle_alpha 95.0127(19) _cell_angle_beta 99.521(2) _cell_angle_gamma 110.2074(9) _cell_volume 1627.31(7) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5932 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 27.86 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 878 _exptl_absorpt_coefficient_mu 1.892 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5182 _exptl_absorpt_correction_T_max 0.8333 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18203 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.86 _reflns_number_total 7583 _reflns_number_gt 6352 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0912P)^2^+2.6694P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0042(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7583 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm Sm 0.93153(2) 0.10710(2) 0.407829(18) 0.02235(13) Uani 1 1 d . . . O1 O 0.7256(3) 0.4105(3) 0.3907(3) 0.0260(7) Uani 1 1 d . . . C2 C 0.8228(5) 0.3655(4) 0.3906(4) 0.0227(10) Uani 1 1 d . . . C3 C 0.8527(5) 0.3550(4) 0.2920(4) 0.0241(10) Uani 1 1 d . . . C4 C 0.7652(5) 0.3942(4) 0.2215(4) 0.0210(9) Uani 1 1 d . . . C5 C 0.7423(6) 0.4013(5) 0.1112(4) 0.0308(12) Uani 1 1 d . . . H5 H 0.7920 0.3796 0.0652 0.037 Uiso 1 1 calc R . . C6 C 0.6453(6) 0.4409(5) 0.0715(5) 0.0366(13) Uani 1 1 d . . . H6 H 0.6276 0.4465 -0.0031 0.044 Uiso 1 1 calc R . . C7 C 0.5713(6) 0.4736(5) 0.1406(5) 0.0371(13) Uani 1 1 d . . . H7 H 0.5058 0.5014 0.1109 0.045 Uiso 1 1 calc R . . C8 C 0.5911(5) 0.4663(5) 0.2481(5) 0.0327(12) Uani 1 1 d . . . H8 H 0.5410 0.4873 0.2941 0.039 Uiso 1 1 calc R . . C9 C 0.6907(5) 0.4257(5) 0.2858(4) 0.0265(10) Uani 1 1 d . . . C10 C 0.8829(5) 0.3519(4) 0.4992(4) 0.0237(10) Uani 1 1 d . . . O11 O 0.9439(4) 0.2835(3) 0.5045(3) 0.0271(8) Uani 1 1 d . . . O12 O 0.8692(4) 0.4088(3) 0.5795(3) 0.0312(8) Uani 1 1 d . . . C13 C 0.9619(6) 0.3245(4) 0.2601(4) 0.0267(11) Uani 1 1 d . . . O14 O 0.9819(5) 0.2370(4) 0.2910(4) 0.0420(10) Uani 1 1 d U . . O15 O 1.0263(4) 0.3862(3) 0.2024(3) 0.0307(8) Uani 1 1 d . . . O16 O 0.6595(3) 0.1357(3) 0.7173(3) 0.0220(7) Uani 1 1 d . . . C17 C 0.7262(5) 0.1012(4) 0.6480(4) 0.0195(9) Uani 1 1 d . . . C18 C 0.8195(4) 0.0648(4) 0.7031(3) 0.0182(9) Uani 1 1 d . . . C19 C 0.8092(5) 0.0773(4) 0.8156(4) 0.0191(9) Uani 1 1 d . . . C20 C 0.8739(5) 0.0571(4) 0.9114(4) 0.0216(10) Uani 1 1 d . . . H20 H 0.9409 0.0263 0.9114 0.026 Uiso 1 1 calc R . . C21 C 0.8370(5) 0.0835(4) 1.0063(4) 0.0242(10) Uani 1 1 d . . . H21 H 0.8792 0.0703 1.0725 0.029 Uiso 1 1 calc R . . C22 C 0.7384(5) 0.1294(5) 1.0063(4) 0.0266(11) Uani 1 1 d . . . H22 H 0.7154 0.1463 1.0728 0.032 Uiso 1 1 calc R . . C23 C 0.6736(5) 0.1509(5) 0.9129(4) 0.0265(11) Uani 1 1 d . . . H23 H 0.6077 0.1829 0.9130 0.032 Uiso 1 1 calc R . . C24 C 0.7116(5) 0.1224(4) 0.8191(4) 0.0213(9) Uani 1 1 d . . . C25 C 0.9139(5) 0.0211(4) 0.6651(4) 0.0194(9) Uani 1 1 d . . . O26 O 0.9471(3) 0.0369(3) 0.5748(3) 0.0214(7) Uani 1 1 d . . . O27 O 0.9622(4) -0.0339(3) 0.7252(3) 0.0288(8) Uani 1 1 d . . . C28 C 0.6774(5) 0.1072(4) 0.5323(4) 0.0214(9) Uani 1 1 d . . . O29 O 0.7272(3) 0.0739(3) 0.4604(3) 0.0272(8) Uani 1 1 d . . . O30 O 0.5878(4) 0.1454(3) 0.5147(3) 0.0290(8) Uani 1 1 d . . . N31 N 0.7121(5) -0.0793(5) 0.2552(4) 0.0369(11) Uani 1 1 d U . . O32 O 0.7436(4) 0.0197(4) 0.2377(3) 0.0396(9) Uani 1 1 d U . . O33 O 0.7789(4) -0.0990(4) 0.3343(3) 0.0359(9) Uani 1 1 d . . . O34 O 0.6173(5) -0.1592(5) 0.1943(4) 0.0532(12) Uani 1 1 d U . . O35 O 1.1647(4) 0.2158(3) 0.4870(4) 0.0366(9) Uani 1 1 d . . . H35A H 1.2135 0.2060 0.5461 0.055 Uiso 1 1 d . . . H35B H 1.1930 0.2849 0.4653 0.055 Uiso 1 1 d . . . N36 N 0.4818(4) 0.1649(4) 0.3197(3) 0.0250(9) Uani 1 1 d . . . H36 H 0.5362 0.1536 0.3864 0.037 Uiso 1 1 d R . . C37 C 0.3880(5) 0.2053(5) 0.3285(4) 0.0260(10) Uani 1 1 d . . . H37 H 0.3697 0.2197 0.3976 0.031 Uiso 1 1 calc R . . C38 C 0.3163(5) 0.2267(5) 0.2393(4) 0.0274(11) Uani 1 1 d . . . H38 H 0.2480 0.2543 0.2464 0.033 Uiso 1 1 calc R . . C39 C 0.3452(5) 0.2075(4) 0.1379(4) 0.0225(10) Uani 1 1 d . . . C40 C 0.4427(5) 0.1626(4) 0.1319(4) 0.0250(10) Uani 1 1 d . . . H40 H 0.4628 0.1463 0.0639 0.030 Uiso 1 1 calc R . . C41 C 0.5099(5) 0.1419(4) 0.2234(4) 0.0259(10) Uani 1 1 d . . . H41 H 0.5763 0.1112 0.2188 0.031 Uiso 1 1 calc R . . C42 C 0.2783(5) 0.2326(4) 0.0393(4) 0.0247(10) Uani 1 1 d . . . H42 H 0.3049 0.2179 -0.0260 0.030 Uiso 1 1 calc R . . C43 C 0.1823(5) 0.2747(4) 0.0347(4) 0.0232(10) Uani 1 1 d . . . H43 H 0.1543 0.2868 0.0999 0.028 Uiso 1 1 calc R . . C44 C 0.1169(5) 0.3037(4) -0.0620(4) 0.0223(10) Uani 1 1 d . . . C45 C 0.0203(5) 0.3494(4) -0.0532(4) 0.0224(10) Uani 1 1 d . . . H45 H -0.0009 0.3626 0.0149 0.027 Uiso 1 1 calc R . . C46 C -0.0441(5) 0.3754(4) -0.1433(4) 0.0236(10) Uani 1 1 d . . . H46 H -0.1102 0.4060 -0.1372 0.028 Uiso 1 1 calc R . . N47 N -0.0147(4) 0.3580(4) -0.2392(3) 0.0239(9) Uani 1 1 d . . . H47 H -0.0496 0.3857 -0.2926 0.036 Uiso 1 1 d R . . C48 C 0.0782(5) 0.3148(4) -0.2515(4) 0.0255(10) Uani 1 1 d . . . H48 H 0.0973 0.3036 -0.3208 0.031 Uiso 1 1 calc R . . C49 C 0.1453(5) 0.2870(4) -0.1649(4) 0.0239(10) Uani 1 1 d . . . H49 H 0.2109 0.2565 -0.1739 0.029 Uiso 1 1 calc R . . O50 O 0.2915(5) 0.5353(5) 0.1940(4) 0.0601(14) Uani 1 1 d . . . H50A H 0.2671 0.4688 0.2201 0.090 Uiso 1 1 d R . . H50B H 0.3589 0.5912 0.2392 0.090 Uiso 1 1 d R . . O51 O 0.2465(5) 0.4193(4) 0.4197(4) 0.0507(12) Uani 1 1 d . . . H51A H 0.1863 0.4106 0.3605 0.076 Uiso 1 1 d R . . H51B H 0.2548 0.4712 0.4777 0.076 Uiso 1 1 d R . . O52 O 0.5013(6) 0.2924(5) 0.6382(4) 0.0596(13) Uani 1 1 d U . . H52A H 0.5559 0.3011 0.5915 0.089 Uiso 1 1 d R . . H52B H 0.4179 0.2296 0.6066 0.089 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm 0.02962(18) 0.03121(18) 0.01667(16) 0.00939(10) 0.00928(10) 0.02064(12) O1 0.0256(18) 0.034(2) 0.0226(17) 0.0048(14) 0.0045(14) 0.0160(16) C2 0.025(2) 0.023(2) 0.023(2) 0.0037(18) 0.0057(18) 0.012(2) C3 0.030(3) 0.024(2) 0.018(2) 0.0069(18) -0.0024(18) 0.012(2) C4 0.023(2) 0.016(2) 0.027(2) 0.0059(17) 0.0033(18) 0.0115(19) C5 0.042(3) 0.030(3) 0.021(2) 0.009(2) 0.005(2) 0.014(2) C6 0.033(3) 0.046(3) 0.028(3) 0.013(2) 0.001(2) 0.012(3) C7 0.030(3) 0.043(3) 0.039(3) 0.013(3) -0.001(2) 0.016(3) C8 0.026(3) 0.034(3) 0.038(3) 0.008(2) 0.001(2) 0.013(2) C9 0.025(3) 0.030(3) 0.024(2) 0.007(2) 0.0032(19) 0.011(2) C10 0.029(3) 0.024(2) 0.022(2) 0.0059(18) 0.0067(19) 0.013(2) O11 0.038(2) 0.0270(19) 0.0238(17) 0.0046(14) 0.0054(14) 0.0221(16) O12 0.040(2) 0.043(2) 0.0215(18) 0.0042(15) 0.0071(15) 0.0285(19) C13 0.045(3) 0.027(3) 0.015(2) 0.0060(18) 0.009(2) 0.020(2) O14 0.0531(18) 0.0439(17) 0.0411(17) 0.0168(14) 0.0194(14) 0.0261(14) O15 0.041(2) 0.034(2) 0.0248(18) 0.0098(15) 0.0134(16) 0.0187(18) O16 0.0252(17) 0.0335(19) 0.0158(15) 0.0058(13) 0.0068(13) 0.0195(15) C17 0.021(2) 0.026(2) 0.016(2) 0.0057(17) 0.0076(17) 0.0114(19) C18 0.021(2) 0.022(2) 0.014(2) 0.0044(16) 0.0055(16) 0.0090(18) C19 0.019(2) 0.020(2) 0.021(2) 0.0027(17) 0.0050(17) 0.0094(18) C20 0.024(2) 0.025(2) 0.020(2) 0.0047(18) 0.0067(18) 0.013(2) C21 0.027(3) 0.030(3) 0.017(2) 0.0027(18) 0.0045(18) 0.013(2) C22 0.032(3) 0.035(3) 0.017(2) 0.0042(19) 0.0082(19) 0.016(2) C23 0.028(3) 0.033(3) 0.023(2) 0.004(2) 0.008(2) 0.017(2) C24 0.022(2) 0.027(3) 0.018(2) 0.0032(18) 0.0045(17) 0.013(2) C25 0.022(2) 0.023(2) 0.017(2) 0.0037(17) 0.0025(17) 0.0132(19) O26 0.0279(18) 0.0297(19) 0.0159(16) 0.0099(13) 0.0095(13) 0.0184(15) O27 0.041(2) 0.044(2) 0.0171(16) 0.0132(15) 0.0124(15) 0.0315(19) C28 0.026(2) 0.025(2) 0.017(2) 0.0081(17) 0.0062(18) 0.012(2) O29 0.0283(19) 0.045(2) 0.0151(16) 0.0037(14) 0.0059(13) 0.0208(17) O30 0.033(2) 0.048(2) 0.0153(16) 0.0054(15) 0.0029(14) 0.0267(18) N31 0.0358(18) 0.0432(19) 0.0338(18) -0.0012(14) 0.0077(14) 0.0186(15) O32 0.0379(16) 0.0560(18) 0.0317(16) 0.0091(13) 0.0081(13) 0.0246(14) O33 0.028(2) 0.043(2) 0.035(2) -0.0065(17) -0.0045(16) 0.0201(18) O34 0.0469(18) 0.062(2) 0.0484(18) -0.0026(15) 0.0077(15) 0.0211(15) O35 0.030(2) 0.033(2) 0.052(3) 0.0174(18) 0.0102(18) 0.0150(17) N36 0.025(2) 0.029(2) 0.022(2) 0.0075(16) 0.0046(16) 0.0104(18) C37 0.028(3) 0.033(3) 0.022(2) 0.0069(19) 0.0080(19) 0.015(2) C38 0.031(3) 0.035(3) 0.021(2) 0.009(2) 0.007(2) 0.017(2) C39 0.022(2) 0.025(2) 0.021(2) 0.0043(18) 0.0040(18) 0.008(2) C40 0.026(3) 0.030(3) 0.022(2) 0.0065(19) 0.0084(19) 0.011(2) C41 0.024(2) 0.028(3) 0.027(3) 0.005(2) 0.0054(19) 0.011(2) C42 0.030(3) 0.032(3) 0.016(2) 0.0065(19) 0.0060(18) 0.015(2) C43 0.028(3) 0.025(2) 0.016(2) 0.0020(17) 0.0009(18) 0.012(2) C44 0.020(2) 0.023(2) 0.022(2) 0.0048(18) 0.0026(18) 0.0077(19) C45 0.026(2) 0.028(3) 0.017(2) 0.0055(18) 0.0076(18) 0.013(2) C46 0.024(2) 0.025(2) 0.024(2) 0.0058(18) 0.0050(19) 0.012(2) N47 0.027(2) 0.025(2) 0.021(2) 0.0088(16) 0.0012(16) 0.0110(18) C48 0.032(3) 0.028(3) 0.018(2) 0.0014(18) 0.0056(19) 0.012(2) C49 0.027(3) 0.029(3) 0.019(2) 0.0016(18) 0.0035(18) 0.015(2) O50 0.051(3) 0.072(4) 0.060(3) 0.012(3) 0.015(2) 0.023(3) O51 0.070(3) 0.038(3) 0.046(3) 0.002(2) 0.017(2) 0.022(2) O52 0.064(2) 0.061(2) 0.060(2) 0.0091(16) 0.0157(16) 0.0302(16) _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 Sm O14 2.297(4) . ? Sm O26 2.374(3) . ? Sm O29 2.377(4) . ? Sm O11 2.397(3) . ? Sm O35 2.455(4) . ? Sm O27 2.498(3) 2_756 ? Sm O33 2.553(4) . ? Sm O32 2.596(4) . ? Sm O26 2.614(3) 2_756 ? Sm C25 2.932(5) 2_756 ? Sm N31 2.985(5) . ? O1 C9 1.375(6) . ? O1 C2 1.381(6) . ? C2 C3 1.356(7) . ? C2 C10 1.482(7) . ? C3 C4 1.453(6) . ? C3 C13 1.495(8) . ? C4 C9 1.380(7) . ? C4 C5 1.400(7) . ? C5 C6 1.377(8) . ? C5 H5 0.9500 . ? C6 C7 1.423(9) . ? C6 H6 0.9500 . ? C7 C8 1.363(8) . ? C7 H7 0.9500 . ? C8 C9 1.404(7) . ? C8 H8 0.9500 . ? C10 O12 1.258(6) . ? C10 O11 1.268(6) . ? C13 O15 1.243(6) . ? C13 O14 1.281(7) . ? O16 C17 1.373(5) . ? O16 C24 1.376(6) . ? C17 C18 1.385(6) . ? C17 C28 1.499(6) . ? C18 C19 1.453(6) . ? C18 C25 1.468(6) . ? C19 C24 1.391(6) . ? C19 C20 1.398(6) . ? C20 C21 1.387(7) . ? C20 H20 0.9500 . ? C21 C22 1.403(7) . ? C21 H21 0.9500 . ? C22 C23 1.381(7) . ? C22 H22 0.9500 . ? C23 C24 1.388(7) . ? C23 H23 0.9500 . ? C25 O27 1.252(6) . ? C25 O26 1.274(6) . ? C25 Sm 2.932(5) 2_756 ? O26 Sm 2.614(3) 2_756 ? O27 Sm 2.498(3) 2_756 ? C28 O30 1.243(6) . ? C28 O29 1.256(6) . ? N31 O32 1.228(7) . ? N31 O33 1.244(6) . ? N31 O34 1.258(7) . ? O35 H35A 0.8947 . ? O35 H35B 0.9043 . ? N36 C37 1.323(7) . ? N36 C41 1.344(7) . ? N36 H36 1.0077 . ? C37 C38 1.377(7) . ? C37 H37 0.9500 . ? C38 C39 1.399(7) . ? C38 H38 0.9500 . ? C39 C40 1.393(7) . ? C39 C42 1.465(6) . ? C40 C41 1.370(7) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.341(7) . ? C42 H42 0.9500 . ? C43 C44 1.462(6) . ? C43 H43 0.9500 . ? C44 C45 1.395(7) . ? C44 C49 1.411(7) . ? C45 C46 1.373(7) . ? C45 H45 0.9500 . ? C46 N47 1.332(7) . ? C46 H46 0.9500 . ? N47 C48 1.345(7) . ? N47 H47 0.8844 . ? C48 C49 1.366(7) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? O50 H50A 0.9001 . ? O50 H50B 0.8997 . ? O51 H51A 0.8904 . ? O51 H51B 0.9132 . ? O52 H52A 0.9035 . ? O52 H52B 0.9799 . ? 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 O14 Sm O26 156.75(15) . . ? O14 Sm O29 115.47(15) . . ? O26 Sm O29 73.14(11) . . ? O14 Sm O11 74.93(14) . . ? O26 Sm O11 88.31(12) . . ? O29 Sm O11 72.63(13) . . ? O14 Sm O35 79.31(15) . . ? O26 Sm O35 80.49(13) . . ? O29 Sm O35 136.93(13) . . ? O11 Sm O35 73.16(13) . . ? O14 Sm O27 72.44(14) . 2_756 ? O26 Sm O27 114.69(11) . 2_756 ? O29 Sm O27 142.92(13) . 2_756 ? O11 Sm O27 140.36(13) . 2_756 ? O35 Sm O27 79.17(14) . 2_756 ? O14 Sm O33 119.63(15) . . ? O26 Sm O33 83.37(13) . . ? O29 Sm O33 71.03(13) . . ? O11 Sm O33 143.60(13) . . ? O35 Sm O33 139.11(13) . . ? O27 Sm O33 73.99(13) 2_756 . ? O14 Sm O32 75.56(16) . . ? O26 Sm O32 127.07(13) . . ? O29 Sm O32 71.30(12) . . ? O11 Sm O32 116.06(13) . . ? O35 Sm O32 149.25(14) . . ? O27 Sm O32 76.57(13) 2_756 . ? O33 Sm O32 48.53(14) . . ? O14 Sm O26 119.21(13) . 2_756 ? O26 Sm O26 64.12(12) . 2_756 ? O29 Sm O26 122.32(12) . 2_756 ? O11 Sm O26 138.20(11) . 2_756 ? O35 Sm O26 71.78(12) . 2_756 ? O27 Sm O26 50.58(10) 2_756 2_756 ? O33 Sm O26 67.37(11) . 2_756 ? O32 Sm O26 105.71(12) . 2_756 ? O14 Sm C25 94.69(14) . 2_756 ? O26 Sm C25 89.71(12) . 2_756 ? O29 Sm C25 139.77(14) . 2_756 ? O11 Sm C25 144.54(13) . 2_756 ? O35 Sm C25 71.59(13) . 2_756 ? O27 Sm C25 25.05(12) 2_756 2_756 ? O33 Sm C25 71.02(13) . 2_756 ? O32 Sm C25 92.97(13) . 2_756 ? O26 Sm C25 25.74(11) 2_756 2_756 ? O14 Sm N31 97.98(16) . . ? O26 Sm N31 105.24(14) . . ? O29 Sm N31 68.36(13) . . ? O11 Sm N31 132.24(13) . . ? O35 Sm N31 153.27(14) . . ? O27 Sm N31 74.73(13) 2_756 . ? O33 Sm N31 24.41(14) . . ? O32 Sm N31 24.15(14) . . ? O26 Sm N31 87.06(13) 2_756 . ? C25 Sm N31 82.23(13) 2_756 . ? C9 O1 C2 105.3(4) . . ? C3 C2 O1 112.4(4) . . ? C3 C2 C10 133.2(5) . . ? O1 C2 C10 114.0(4) . . ? C2 C3 C4 105.4(5) . . ? C2 C3 C13 129.5(4) . . ? C4 C3 C13 124.7(4) . . ? C9 C4 C5 119.7(5) . . ? C9 C4 C3 105.8(4) . . ? C5 C4 C3 134.5(5) . . ? C6 C5 C4 117.7(5) . . ? C6 C5 H5 121.2 . . ? C4 C5 H5 121.2 . . ? C5 C6 C7 121.0(5) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C6 122.3(5) . . ? C8 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? C7 C8 C9 115.3(6) . . ? C7 C8 H8 122.4 . . ? C9 C8 H8 122.4 . . ? O1 C9 C4 111.1(4) . . ? O1 C9 C8 124.8(5) . . ? C4 C9 C8 124.1(5) . . ? O12 C10 O11 124.7(4) . . ? O12 C10 C2 117.5(4) . . ? O11 C10 C2 117.8(4) . . ? C10 O11 Sm 138.8(3) . . ? O15 C13 O14 124.3(5) . . ? O15 C13 C3 116.5(4) . . ? O14 C13 C3 119.2(5) . . ? C13 O14 Sm 143.6(4) . . ? C17 O16 C24 106.8(3) . . ? O16 C17 C18 110.9(4) . . ? O16 C17 C28 113.3(4) . . ? C18 C17 C28 135.8(4) . . ? C17 C18 C19 105.9(4) . . ? C17 C18 C25 131.2(4) . . ? C19 C18 C25 122.9(4) . . ? C24 C19 C20 119.4(4) . . ? C24 C19 C18 105.6(4) . . ? C20 C19 C18 135.0(4) . . ? C21 C20 C19 117.7(4) . . ? C21 C20 H20 121.1 . . ? C19 C20 H20 121.1 . . ? C20 C21 C22 121.1(4) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C23 C22 C21 122.3(4) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C22 C23 C24 115.3(5) . . ? C22 C23 H23 122.3 . . ? C24 C23 H23 122.3 . . ? O16 C24 C23 125.0(4) . . ? O16 C24 C19 110.7(4) . . ? C23 C24 C19 124.2(4) . . ? O27 C25 O26 119.9(4) . . ? O27 C25 C18 117.5(4) . . ? O26 C25 C18 122.6(4) . . ? O27 C25 Sm 57.7(2) . 2_756 ? O26 C25 Sm 63.0(2) . 2_756 ? C18 C25 Sm 169.6(3) . 2_756 ? C25 O26 Sm 152.1(3) . . ? C25 O26 Sm 91.2(3) . 2_756 ? Sm O26 Sm 115.88(12) . 2_756 ? C25 O27 Sm 97.3(3) . 2_756 ? O30 C28 O29 124.4(4) . . ? O30 C28 C17 116.1(4) . . ? O29 C28 C17 119.4(4) . . ? C28 O29 Sm 141.9(3) . . ? O32 N31 O33 117.8(5) . . ? O32 N31 O34 121.6(5) . . ? O33 N31 O34 120.6(6) . . ? O32 N31 Sm 59.9(3) . . ? O33 N31 Sm 58.0(3) . . ? O34 N31 Sm 177.5(4) . . ? N31 O32 Sm 96.0(3) . . ? N31 O33 Sm 97.6(3) . . ? Sm O35 H35A 127.9 . . ? Sm O35 H35B 111.8 . . ? H35A O35 H35B 117.2 . . ? C37 N36 C41 121.4(4) . . ? C37 N36 H36 119.9 . . ? C41 N36 H36 118.6 . . ? N36 C37 C38 121.2(5) . . ? N36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C37 C38 C39 119.3(5) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C40 C39 C38 117.7(5) . . ? C40 C39 C42 119.1(4) . . ? C38 C39 C42 123.2(5) . . ? C41 C40 C39 120.4(5) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? N36 C41 C40 120.0(5) . . ? N36 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C43 C42 C39 124.6(5) . . ? C43 C42 H42 117.7 . . ? C39 C42 H42 117.7 . . ? C42 C43 C44 125.7(5) . . ? C42 C43 H43 117.2 . . ? C44 C43 H43 117.2 . . ? C45 C44 C49 117.7(4) . . ? C45 C44 C43 118.9(4) . . ? C49 C44 C43 123.4(5) . . ? C46 C45 C44 119.9(4) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? N47 C46 C45 120.5(5) . . ? N47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C46 N47 C48 121.7(4) . . ? C46 N47 H47 117.2 . . ? C48 N47 H47 120.4 . . ? N47 C48 C49 120.4(5) . . ? N47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C48 C49 C44 119.7(5) . . ? C48 C49 H49 120.2 . . ? C44 C49 H49 120.2 . . ? H50A O50 H50B 112.9 . . ? H51A O51 H51B 118.8 . . ? H52A O52 H52B 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O35 H35A O33 0.89 2.13 2.911(6) 145 2_756 O35 H35B O51 0.90 1.78 2.681(6) 179 1_655 N36 H36 O30 1.01 1.66 2.633(5) 161 . N47 H47 O12 0.88 1.82 2.689(5) 166 1_454 O50 H50A O51 0.90 2.69 3.366(7) 132 . O50 H50B O52 0.90 2.05 2.945(8) 171 2_666 O51 H51A O15 0.89 2.37 3.261(6) 180 1_455 O51 H51B O1 0.91 2.07 2.985(6) 180 2_666 O52 H52A O30 0.90 2.28 2.838(6) 120 . O52 H52B O33 0.98 2.51 3.318(7) 139 2_656 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 2.740 _refine_diff_density_min -1.791 _refine_diff_density_rms 0.169 #========================END============================== data_9 _database_code_depnum_ccdc_archive 'CCDC 775258' #TrackingRef '- ti7-19.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H24 Ag4 O22, 2(H2 O)' _chemical_formula_sum 'C40 H28 Ag4 O24' _chemical_formula_weight 1324.10 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 8.4379(3) _cell_length_b 9.2408(4) _cell_length_c 14.2462(6) _cell_angle_alpha 72.944(2) _cell_angle_beta 85.254(3) _cell_angle_gamma 66.2703(14) _cell_volume 971.39(7) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3986 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 2.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6232 _exptl_absorpt_correction_T_max 0.8183 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15013 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4211 _reflns_number_gt 3228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0014(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4211 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.11594(4) 0.63391(4) 0.336296(19) 0.02179(10) Uani 1 1 d . . . Ag2 Ag 0.11172(4) 0.68986(4) 0.12495(2) 0.02616(11) Uani 1 1 d . . . O3 O 0.3420(3) 1.0561(3) 0.28356(17) 0.0184(5) Uani 1 1 d . . . C4 C 0.3128(4) 1.0336(4) 0.1959(2) 0.0160(7) Uani 1 1 d . . . C5 C 0.3379(4) 1.1463(4) 0.1166(3) 0.0183(8) Uani 1 1 d . . . C6 C 0.3854(4) 1.2517(4) 0.1570(3) 0.0176(7) Uani 1 1 d . . . C7 C 0.4225(5) 1.3921(4) 0.1169(3) 0.0197(8) Uani 1 1 d . . . H7 H 0.4229 1.4371 0.0478 0.024 Uiso 1 1 calc R . . C8 C 0.4586(5) 1.4633(5) 0.1811(3) 0.0227(8) Uani 1 1 d . . . H8 H 0.4833 1.5589 0.1556 0.027 Uiso 1 1 calc R . . C9 C 0.4592(5) 1.3960(5) 0.2838(3) 0.0198(8) Uani 1 1 d . . . H9 H 0.4852 1.4472 0.3258 0.024 Uiso 1 1 calc R . . C10 C 0.4231(5) 1.2575(5) 0.3251(3) 0.0201(8) Uani 1 1 d . . . H10 H 0.4243 1.2110 0.3941 0.024 Uiso 1 1 calc R . . C11 C 0.3850(4) 1.1917(4) 0.2582(3) 0.0177(8) Uani 1 1 d . . . C12 C 0.2545(4) 0.8969(4) 0.2085(3) 0.0160(7) Uani 1 1 d . . . O13 O 0.2602(3) 0.8046(3) 0.29411(18) 0.0211(6) Uani 1 1 d . . . O14 O 0.1987(3) 0.8882(3) 0.13157(17) 0.0195(5) Uani 1 1 d . . . C15 C 0.3244(5) 1.1700(5) 0.0087(3) 0.0217(8) Uani 1 1 d . . . O16 O 0.3771(4) 1.2642(3) -0.04957(19) 0.0272(6) Uani 1 1 d . . . O17 O 0.2503(4) 1.0887(3) -0.02200(18) 0.0252(6) Uani 1 1 d . . . H17 H 0.2262 1.0248 0.0267 0.038 Uiso 1 1 calc R . . O18 O -0.0985(3) 0.2005(3) 0.36460(17) 0.0170(5) Uani 1 1 d . . . C19 C -0.0840(4) 0.2863(4) 0.2704(2) 0.0142(7) Uani 1 1 d . . . C20 C -0.1183(4) 0.2216(4) 0.2033(3) 0.0159(7) Uani 1 1 d . . . C21 C -0.1574(4) 0.0832(4) 0.2596(2) 0.0147(7) Uani 1 1 d . . . C22 C -0.2021(4) -0.0341(4) 0.2371(3) 0.0176(8) Uani 1 1 d . . . H22 H -0.2156 -0.0313 0.1709 0.021 Uiso 1 1 calc R . . C23 C -0.2258(5) -0.1547(4) 0.3155(3) 0.0199(8) Uani 1 1 d . . . H23 H -0.2556 -0.2357 0.3022 0.024 Uiso 1 1 calc R . . C24 C -0.2070(5) -0.1596(4) 0.4134(3) 0.0207(8) Uani 1 1 d . . . H24 H -0.2224 -0.2448 0.4648 0.025 Uiso 1 1 calc R . . C25 C -0.1662(5) -0.0423(5) 0.4368(3) 0.0204(8) Uani 1 1 d . . . H25 H -0.1555 -0.0433 0.5028 0.024 Uiso 1 1 calc R . . C26 C -0.1423(4) 0.0753(4) 0.3583(3) 0.0167(7) Uani 1 1 d . . . C27 C -0.0289(4) 0.4239(4) 0.2632(2) 0.0143(7) Uani 1 1 d . . . O28 O -0.0033(3) 0.4484(3) 0.34148(17) 0.0187(5) Uani 1 1 d . . . O29 O -0.0094(3) 0.5038(3) 0.17741(17) 0.0182(5) Uani 1 1 d . . . C30 C -0.1185(4) 0.2704(4) 0.0942(2) 0.0125(7) Uani 1 1 d . . . O31 O -0.0748(3) 0.3947(3) 0.04853(17) 0.0212(6) Uani 1 1 d . . . H31 H -0.0549 0.4344 0.0900 0.032 Uiso 1 1 calc R . . O32 O -0.1583(3) 0.1986(3) 0.04764(17) 0.0217(6) Uani 1 1 d . . . O33 O 0.2361(3) 0.5444(3) 0.50426(18) 0.0212(6) Uani 1 1 d . . . H33A H 0.3008 0.6043 0.4939 0.032 Uiso 1 1 d . . . H33B H 0.1661 0.5676 0.5538 0.032 Uiso 1 1 d . . . O34 O 0.4325(3) 0.7252(3) 0.47231(18) 0.0244(6) Uani 1 1 d . . . H34A H 0.4079 0.8162 0.4125 0.037 Uiso 1 1 d . . . H34B H 0.5367 0.6405 0.4797 0.037 Uiso 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 Ag1 0.02897(18) 0.02658(18) 0.01756(16) -0.00615(12) -0.00029(12) -0.01860(14) Ag2 0.0453(2) 0.03100(19) 0.01532(16) -0.00604(13) 0.00154(13) -0.02867(16) O3 0.0211(13) 0.0202(14) 0.0168(12) -0.0051(10) -0.0001(10) -0.0108(11) C4 0.0133(17) 0.0181(19) 0.0164(17) -0.0069(15) 0.0024(14) -0.0049(15) C5 0.0125(18) 0.0157(19) 0.0250(19) -0.0059(15) 0.0022(14) -0.0040(15) C6 0.0141(18) 0.0154(18) 0.0228(19) -0.0071(15) -0.0007(14) -0.0039(15) C7 0.0195(19) 0.0169(19) 0.0203(19) -0.0034(15) -0.0011(15) -0.0057(16) C8 0.0158(19) 0.019(2) 0.034(2) -0.0076(17) -0.0019(16) -0.0072(16) C9 0.0173(19) 0.0207(19) 0.024(2) -0.0091(16) -0.0008(15) -0.0081(16) C10 0.0177(19) 0.020(2) 0.0215(19) -0.0083(16) -0.0018(15) -0.0048(16) C11 0.0139(18) 0.0163(18) 0.0230(19) -0.0051(15) 0.0011(14) -0.0066(15) C12 0.0106(17) 0.0147(18) 0.0216(19) -0.0072(15) 0.0006(14) -0.0024(14) O13 0.0270(15) 0.0225(14) 0.0179(13) -0.0035(11) -0.0012(11) -0.0151(12) O14 0.0259(14) 0.0205(14) 0.0178(13) -0.0065(11) -0.0006(10) -0.0140(12) C15 0.023(2) 0.0180(19) 0.021(2) -0.0052(16) 0.0015(16) -0.0053(16) O16 0.0350(16) 0.0310(16) 0.0201(14) -0.0039(12) 0.0027(12) -0.0203(14) O17 0.0412(17) 0.0245(15) 0.0178(13) -0.0064(11) 0.0025(12) -0.0209(13) O18 0.0210(13) 0.0181(13) 0.0153(12) -0.0039(10) 0.0002(10) -0.0117(11) C19 0.0145(18) 0.0140(17) 0.0138(17) -0.0023(14) 0.0009(13) -0.0067(14) C20 0.0131(17) 0.0169(18) 0.0184(18) -0.0063(15) 0.0004(14) -0.0058(15) C21 0.0134(17) 0.0152(18) 0.0154(17) -0.0042(14) -0.0007(14) -0.0055(14) C22 0.0149(18) 0.0205(19) 0.0197(19) -0.0080(15) 0.0003(14) -0.0075(15) C23 0.0174(19) 0.0134(18) 0.031(2) -0.0086(16) 0.0023(16) -0.0069(15) C24 0.0208(19) 0.0144(19) 0.025(2) 0.0000(15) 0.0008(15) -0.0090(16) C25 0.021(2) 0.024(2) 0.0145(18) -0.0003(15) -0.0024(14) -0.0100(17) C26 0.0153(18) 0.0174(19) 0.0204(18) -0.0065(15) 0.0015(14) -0.0088(15) C27 0.0092(17) 0.0133(18) 0.0191(18) -0.0050(14) -0.0003(13) -0.0029(14) O28 0.0240(14) 0.0210(14) 0.0172(13) -0.0072(11) 0.0014(10) -0.0138(11) O29 0.0246(14) 0.0172(13) 0.0172(13) -0.0028(10) 0.0021(10) -0.0144(11) C30 0.0097(16) 0.0125(17) 0.0129(16) -0.0004(14) 0.0001(13) -0.0043(14) O31 0.0309(15) 0.0254(15) 0.0135(12) -0.0041(11) -0.0011(11) -0.0179(12) O32 0.0300(15) 0.0278(15) 0.0152(13) -0.0082(11) 0.0003(11) -0.0177(13) O33 0.0230(14) 0.0252(14) 0.0183(13) -0.0078(11) 0.0035(10) -0.0117(12) O34 0.0253(14) 0.0267(15) 0.0210(14) -0.0041(12) -0.0018(11) -0.0116(12) _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 Ag1 O13 2.280(2) . ? Ag1 O28 2.293(2) . ? Ag1 O33 2.450(2) . ? Ag1 Ag2 2.9023(4) . ? Ag2 O29 2.257(2) . ? Ag2 O14 2.259(2) . ? Ag2 O32 2.438(2) 2_565 ? O3 C4 1.381(4) . ? O3 C11 1.383(4) . ? C4 C5 1.362(5) . ? C4 C12 1.490(5) . ? C5 C6 1.457(5) . ? C5 C15 1.495(5) . ? C6 C11 1.385(5) . ? C6 C7 1.403(5) . ? C7 C8 1.386(5) . ? C7 H7 0.9500 . ? C8 C9 1.411(5) . ? C8 H8 0.9500 . ? C9 C10 1.386(5) . ? C9 H9 0.9500 . ? C10 C11 1.388(5) . ? C10 H10 0.9500 . ? C12 O13 1.258(4) . ? C12 O14 1.264(4) . ? C15 O16 1.214(5) . ? C15 O17 1.328(4) . ? O17 H17 0.8400 . ? O18 C19 1.368(4) . ? O18 C26 1.376(4) . ? C19 C20 1.369(5) . ? C19 C27 1.495(5) . ? C20 C21 1.444(5) . ? C20 C30 1.485(5) . ? C21 C26 1.400(5) . ? C21 C22 1.404(5) . ? C22 C23 1.393(5) . ? C22 H22 0.9500 . ? C23 C24 1.402(5) . ? C23 H23 0.9500 . ? C24 C25 1.391(5) . ? C24 H24 0.9500 . ? C25 C26 1.378(5) . ? C25 H25 0.9500 . ? C27 O28 1.252(4) . ? C27 O29 1.266(4) . ? C30 O32 1.212(4) . ? C30 O31 1.319(4) . ? O31 H31 0.8400 . ? O32 Ag2 2.438(2) 2_565 ? O33 H33A 0.8991 . ? O33 H33B 0.8999 . ? O34 H34A 0.9721 . ? O34 H34B 0.8998 . ? 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 O13 Ag1 O28 165.31(9) . . ? O13 Ag1 O33 88.22(9) . . ? O28 Ag1 O33 102.37(8) . . ? O13 Ag1 Ag2 81.07(6) . . ? O28 Ag1 Ag2 85.54(6) . . ? O33 Ag1 Ag2 158.40(6) . . ? O29 Ag2 O14 157.24(9) . . ? O29 Ag2 O32 123.17(8) . 2_565 ? O14 Ag2 O32 78.46(8) . 2_565 ? O29 Ag2 Ag1 77.60(6) . . ? O14 Ag2 Ag1 81.02(6) . . ? O32 Ag2 Ag1 159.23(6) 2_565 . ? C4 O3 C11 105.9(3) . . ? C5 C4 O3 112.1(3) . . ? C5 C4 C12 134.2(3) . . ? O3 C4 C12 113.6(3) . . ? C4 C5 C6 105.4(3) . . ? C4 C5 C15 131.6(3) . . ? C6 C5 C15 123.0(3) . . ? C11 C6 C7 118.8(3) . . ? C11 C6 C5 106.2(3) . . ? C7 C6 C5 135.0(3) . . ? C8 C7 C6 118.1(3) . . ? C8 C7 H7 121.0 . . ? C6 C7 H7 121.0 . . ? C7 C8 C9 121.0(4) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 122.0(3) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C11 115.1(3) . . ? C9 C10 H10 122.5 . . ? C11 C10 H10 122.5 . . ? O3 C11 C6 110.4(3) . . ? O3 C11 C10 124.6(3) . . ? C6 C11 C10 125.0(3) . . ? O13 C12 O14 126.1(3) . . ? O13 C12 C4 117.7(3) . . ? O14 C12 C4 116.2(3) . . ? C12 O13 Ag1 123.2(2) . . ? C12 O14 Ag2 124.8(2) . . ? O16 C15 O17 120.8(3) . . ? O16 C15 C5 120.5(3) . . ? O17 C15 C5 118.7(3) . . ? C15 O17 H17 109.5 . . ? C19 O18 C26 106.7(3) . . ? O18 C19 C20 111.5(3) . . ? O18 C19 C27 114.1(3) . . ? C20 C19 C27 134.3(3) . . ? C19 C20 C21 106.0(3) . . ? C19 C20 C30 131.5(3) . . ? C21 C20 C30 122.5(3) . . ? C26 C21 C22 119.0(3) . . ? C26 C21 C20 105.8(3) . . ? C22 C21 C20 135.2(3) . . ? C23 C22 C21 117.4(3) . . ? C23 C22 H22 121.3 . . ? C21 C22 H22 121.3 . . ? C22 C23 C24 121.8(3) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C25 C24 C23 121.4(3) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C26 C25 C24 115.9(3) . . ? C26 C25 H25 122.0 . . ? C24 C25 H25 122.0 . . ? O18 C26 C25 125.6(3) . . ? O18 C26 C21 109.9(3) . . ? C25 C26 C21 124.5(3) . . ? O28 C27 O29 125.8(3) . . ? O28 C27 C19 118.0(3) . . ? O29 C27 C19 116.2(3) . . ? C27 O28 Ag1 119.5(2) . . ? C27 O29 Ag2 131.1(2) . . ? O32 C30 O31 120.3(3) . . ? O32 C30 C20 121.1(3) . . ? O31 C30 C20 118.6(3) . . ? C30 O31 H31 109.5 . . ? C30 O32 Ag2 107.6(2) . 2_565 ? Ag1 O33 H33A 98.0 . . ? Ag1 O33 H33B 120.5 . . ? H33A O33 H33B 107.8 . . ? H34A O34 H34B 117.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O17 H17 O14 0.84 1.72 2.554(4) 174 . O31 H31 O29 0.84 1.69 2.529(3) 177 . O33 H33A O34 0.90 1.82 2.720(4) 180 . O33 H33B O28 0.90 1.96 2.821(3) 160 2_566 O34 H34A O3 0.97 2.32 3.287(4) 172 . O34 H34B O33 0.90 1.96 2.863(4) 180 2_666 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.225 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.125 #==========================END======================== data_10 _database_code_depnum_ccdc_archive 'CCDC 775259' #TrackingRef '- ti7-19.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H12 La O12, 1/2(C12 H12 N2), H2 O, O' _chemical_formula_sum 'C26 H20 La N O14' _chemical_formula_weight 709.34 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 7.94910(10) _cell_length_b 12.8013(3) _cell_length_c 13.5316(4) _cell_angle_alpha 97.5992(8) _cell_angle_beta 105.3403(8) _cell_angle_gamma 103.7083(15) _cell_volume 1261.84(5) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4442 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 27.83 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.867 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.773 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4710 _exptl_absorpt_correction_T_max 0.7768 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13832 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.83 _reflns_number_total 5929 _reflns_number_gt 5036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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. One of the water solvent species is disordered between two sites. ; _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^)+(0.0797P)^2^+3.1953P] 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 5929 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1359 _refine_ls_wR_factor_gt 0.1275 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 La La 0.26784(3) 0.05330(2) -0.04456(2) 0.01687(11) Uani 1 1 d . . . O1 O 0.5967(5) 0.1055(3) 0.3853(3) 0.0320(9) Uani 1 1 d . . . C2 C 0.4837(7) 0.0657(4) 0.2823(4) 0.0205(10) Uani 1 1 d . . . C3 C 0.3078(6) 0.0531(4) 0.2781(4) 0.0193(10) Uani 1 1 d . . . C4 C 0.2992(7) 0.0832(4) 0.3804(4) 0.0233(11) Uani 1 1 d . . . C5 C 0.1760(11) 0.0952(8) 0.4340(6) 0.059(2) Uani 1 1 d . . . H5 H 0.0501 0.0779 0.3968 0.071 Uiso 1 1 calc R . . C6 C 0.2375(13) 0.1330(8) 0.5433(7) 0.068(3) Uani 1 1 d . . . H6 H 0.1522 0.1399 0.5797 0.081 Uiso 1 1 calc R . . C7 C 0.4222(12) 0.1604(8) 0.5990(7) 0.064(2) Uani 1 1 d . . . H7 H 0.4594 0.1845 0.6730 0.077 Uiso 1 1 calc R . . C8 C 0.5427(13) 0.1543(6) 0.5539(5) 0.053(2) Uani 1 1 d . . . H8 H 0.6683 0.1746 0.5926 0.064 Uiso 1 1 calc R . . C9 C 0.4822(9) 0.1163(5) 0.4451(4) 0.0328(13) Uani 1 1 d . . . C10 C 0.5722(6) 0.0408(4) 0.2024(4) 0.0185(10) Uani 1 1 d . . . O11 O 0.4713(4) -0.0033(3) 0.1079(3) 0.0195(7) Uani 1 1 d . . . O12 O 0.7410(5) 0.0600(3) 0.2287(3) 0.0241(8) Uani 1 1 d . . . C13 C 0.1365(6) 0.0109(4) 0.1881(4) 0.0203(10) Uani 1 1 d . . . O14 O 0.0004(5) -0.0458(4) 0.2063(3) 0.0303(9) Uani 1 1 d . . . O15 O 0.1269(5) 0.0356(3) 0.1000(3) 0.0238(8) Uani 1 1 d . . . O16 O 0.9915(5) 0.5227(3) 0.1389(3) 0.0215(7) Uani 1 1 d . . . C17 C 0.8506(6) 0.4323(4) 0.0754(4) 0.0192(10) Uani 1 1 d . . . C18 C 0.8575(6) 0.3388(4) 0.1107(4) 0.0174(9) Uani 1 1 d . . . C19 C 1.0146(6) 0.3702(4) 0.2049(4) 0.0191(10) Uani 1 1 d . . . C20 C 1.0916(7) 0.3154(5) 0.2799(4) 0.0225(10) Uani 1 1 d . . . H20 H 1.0423 0.2388 0.2741 0.027 Uiso 1 1 calc R . . C21 C 1.2414(7) 0.3765(5) 0.3627(4) 0.0242(11) Uani 1 1 d . . . H21 H 1.2974 0.3409 0.4139 0.029 Uiso 1 1 calc R . . C22 C 1.3132(7) 0.4906(5) 0.3728(4) 0.0263(11) Uani 1 1 d . . . H22 H 1.4153 0.5304 0.4313 0.032 Uiso 1 1 calc R . . C23 C 1.2389(7) 0.5457(5) 0.3001(4) 0.0262(11) Uani 1 1 d . . . H23 H 1.2877 0.6223 0.3060 0.031 Uiso 1 1 calc R . . C24 C 1.0884(6) 0.4829(4) 0.2175(4) 0.0207(10) Uani 1 1 d . . . C25 C 0.7382(6) 0.2237(4) 0.0683(4) 0.0188(10) Uani 1 1 d . . . O26 O 0.8221(4) 0.1521(3) 0.0579(3) 0.0214(7) Uani 1 1 d . . . O27 O 0.5686(4) 0.2048(3) 0.0491(3) 0.0195(7) Uani 1 1 d . . . C28 C 0.7255(6) 0.4567(4) -0.0174(4) 0.0194(10) Uani 1 1 d . . . O29 O 0.6298(5) 0.3770(3) -0.0895(3) 0.0237(8) Uani 1 1 d . . . O30 O 0.7263(5) 0.5552(3) -0.0157(3) 0.0262(8) Uani 1 1 d . . . N31 N -0.4782(6) -0.5564(4) 0.1940(3) 0.0245(9) Uani 1 1 d . . . H31 H -0.5639 -0.5431 0.1407 0.037 Uiso 1 1 d . . . C32 C -0.3525(8) -0.4611(5) 0.2416(5) 0.0346(13) Uani 1 1 d . . . H32 H -0.3563 -0.3980 0.2122 0.042 Uiso 1 1 calc R . . C33 C -0.2167(7) -0.4523(5) 0.3332(5) 0.0296(12) Uani 1 1 d . . . H33 H -0.1297 -0.3834 0.3670 0.036 Uiso 1 1 calc R . . C34 C -0.2079(7) -0.5452(4) 0.3757(4) 0.0217(10) Uani 1 1 d . . . C35 C -0.3420(7) -0.6442(5) 0.3223(4) 0.0234(11) Uani 1 1 d . . . H35 H -0.3406 -0.7093 0.3487 0.028 Uiso 1 1 calc R . . C36 C -0.4758(7) -0.6476(5) 0.2319(4) 0.0249(11) Uani 1 1 d . . . H36 H -0.5662 -0.7148 0.1964 0.030 Uiso 1 1 calc R . . C37 C -0.0667(7) -0.5442(5) 0.4711(4) 0.0249(11) Uani 1 1 d . . . H37 H -0.0705 -0.6119 0.4934 0.030 Uiso 1 1 calc R . . O38 O 0.1591(5) 0.2186(3) 0.0162(3) 0.0261(8) Uani 1 1 d . . . H38A H 0.0603 0.2133 0.0368 0.039 Uiso 1 1 d . . . H38B H 0.1953 0.2902 0.0155 0.039 Uiso 1 1 d . . . O39 O 0.3476(5) 0.1920(3) -0.1528(3) 0.0275(8) Uani 1 1 d . . . H39A H 0.4439 0.2549 -0.1315 0.041 Uiso 1 1 d . . . H39B H 0.2617 0.2037 -0.2010 0.041 Uiso 1 1 d . . . O40 O 0.7700(8) 0.2177(6) -0.1646(6) 0.0737(18) Uani 1 1 d . . . H40A H 0.7978 0.1535 -0.1338 0.111 Uiso 1 1 d . . . H40B H 0.7892 0.2672 -0.1071 0.111 Uiso 1 1 d . . . O41A O 0.0303(15) 0.2388(16) 0.730(2) 0.088(8) Uani 0.72(4) 1 d P . . O41B O 0.076(3) 0.2808(18) 0.798(2) 0.041(7) Uani 0.28(4) 1 d P . . 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 La 0.01298(15) 0.01732(17) 0.01934(16) 0.00450(11) 0.00311(10) 0.00422(11) O1 0.035(2) 0.029(2) 0.026(2) 0.0040(17) 0.0015(16) 0.0071(17) C2 0.020(2) 0.017(2) 0.022(2) 0.0053(19) 0.0021(18) 0.0042(19) C3 0.019(2) 0.016(2) 0.020(2) 0.0018(19) 0.0030(18) 0.0027(18) C4 0.034(3) 0.023(3) 0.023(3) 0.010(2) 0.018(2) 0.012(2) C5 0.050(4) 0.074(6) 0.046(4) 0.000(4) 0.021(3) 0.004(4) C6 0.073(6) 0.069(6) 0.053(5) -0.007(4) 0.036(4) -0.004(5) C7 0.063(5) 0.066(6) 0.045(4) 0.003(4) 0.013(4) -0.007(4) C8 0.107(7) 0.032(4) 0.027(3) 0.008(3) 0.026(4) 0.024(4) C9 0.054(4) 0.023(3) 0.021(3) 0.004(2) 0.007(2) 0.014(3) C10 0.015(2) 0.017(2) 0.022(2) 0.0077(19) 0.0025(18) 0.0032(18) O11 0.0175(16) 0.0238(19) 0.0163(16) 0.0052(14) 0.0026(13) 0.0064(14) O12 0.0157(16) 0.028(2) 0.0253(19) 0.0017(15) 0.0033(14) 0.0063(15) C13 0.019(2) 0.019(3) 0.021(2) -0.0008(19) 0.0023(18) 0.0084(19) O14 0.0183(17) 0.039(2) 0.030(2) 0.0133(18) 0.0045(15) 0.0022(16) O15 0.0223(17) 0.032(2) 0.0202(17) 0.0097(15) 0.0059(14) 0.0112(15) O16 0.0176(16) 0.0175(18) 0.0257(18) 0.0035(14) 0.0029(14) 0.0027(14) C17 0.013(2) 0.019(3) 0.024(2) 0.0029(19) 0.0035(18) 0.0034(18) C18 0.012(2) 0.021(3) 0.020(2) 0.0041(19) 0.0044(17) 0.0065(18) C19 0.014(2) 0.021(3) 0.023(2) 0.003(2) 0.0071(18) 0.0049(18) C20 0.018(2) 0.027(3) 0.025(3) 0.007(2) 0.0068(19) 0.008(2) C21 0.019(2) 0.036(3) 0.018(2) 0.005(2) 0.0045(19) 0.009(2) C22 0.018(2) 0.032(3) 0.022(3) 0.000(2) 0.0022(19) 0.002(2) C23 0.022(2) 0.025(3) 0.025(3) -0.001(2) 0.004(2) 0.002(2) C24 0.016(2) 0.026(3) 0.019(2) 0.004(2) 0.0050(18) 0.0057(19) C25 0.016(2) 0.022(3) 0.018(2) 0.0043(19) 0.0025(17) 0.0061(19) O26 0.0167(16) 0.0193(19) 0.0282(19) 0.0049(15) 0.0050(14) 0.0069(14) O27 0.0128(15) 0.0195(18) 0.0249(18) 0.0048(14) 0.0051(13) 0.0025(13) C28 0.014(2) 0.021(3) 0.025(2) 0.008(2) 0.0073(18) 0.0049(19) O29 0.0216(17) 0.0199(19) 0.0256(19) 0.0079(15) 0.0018(14) 0.0030(14) O30 0.0224(18) 0.0191(19) 0.034(2) 0.0071(16) 0.0041(15) 0.0054(15) N31 0.021(2) 0.032(3) 0.023(2) 0.0102(19) 0.0050(17) 0.0130(19) C32 0.034(3) 0.031(3) 0.037(3) 0.017(3) 0.003(2) 0.009(3) C33 0.021(2) 0.026(3) 0.037(3) 0.011(2) 0.001(2) 0.003(2) C34 0.020(2) 0.025(3) 0.024(3) 0.009(2) 0.0095(19) 0.009(2) C35 0.024(2) 0.027(3) 0.027(3) 0.012(2) 0.010(2) 0.014(2) C36 0.028(3) 0.025(3) 0.024(3) 0.007(2) 0.007(2) 0.013(2) C37 0.022(2) 0.026(3) 0.031(3) 0.014(2) 0.009(2) 0.010(2) O38 0.0202(17) 0.0190(19) 0.042(2) 0.0051(16) 0.0145(16) 0.0064(14) O39 0.0209(17) 0.028(2) 0.0239(19) 0.0099(16) -0.0030(14) -0.0022(15) O40 0.055(3) 0.066(4) 0.098(5) 0.004(4) 0.020(3) 0.023(3) O41A 0.048(5) 0.103(12) 0.120(18) 0.082(13) 0.009(7) 0.021(6) O41B 0.033(10) 0.050(12) 0.030(14) 0.012(10) -0.002(9) 0.004(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La O15 2.508(4) . ? La O39 2.520(4) . ? La O26 2.524(4) 2_655 ? La O11 2.566(3) . ? La O27 2.575(3) . ? La O38 2.584(4) . ? La O14 2.593(4) 2 ? La O11 2.621(3) 2_655 ? La O12 2.686(4) 2_655 ? La O15 2.922(3) 2 ? La C10 3.018(5) 2_655 ? La C13 3.131(5) 2 ? O1 C9 1.386(8) . ? O1 C2 1.393(6) . ? C2 C3 1.354(7) . ? C2 C10 1.478(7) . ? C3 C4 1.411(7) . ? C3 C13 1.493(6) . ? C4 C5 1.388(9) . ? C4 C9 1.413(8) . ? C5 C6 1.407(11) . ? C5 H5 0.9500 . ? C6 C7 1.395(12) . ? C6 H6 0.9500 . ? C7 C8 1.276(12) . ? C7 H7 0.9500 . ? C8 C9 1.401(9) . ? C8 H8 0.9500 . ? C10 O12 1.247(6) . ? C10 O11 1.284(6) . ? C10 La 3.018(5) 2_655 ? O11 La 2.621(3) 2_655 ? O12 La 2.686(4) 2_655 ? C13 O14 1.255(6) . ? C13 O15 1.260(6) . ? C13 La 3.131(5) 2 ? O14 La 2.593(4) 2 ? O15 La 2.922(3) 2 ? O16 C24 1.371(6) . ? O16 C17 1.395(6) . ? C17 C18 1.353(7) . ? C17 C28 1.501(7) . ? C18 C19 1.460(6) . ? C18 C25 1.492(7) . ? C19 C24 1.391(7) . ? C19 C20 1.400(7) . ? C20 C21 1.381(7) . ? C20 H20 0.9500 . ? C21 C22 1.410(8) . ? C21 H21 0.9500 . ? C22 C23 1.374(8) . ? C22 H22 0.9500 . ? C23 C24 1.387(7) . ? C23 H23 0.9500 . ? C25 O27 1.260(6) . ? C25 O26 1.269(6) . ? O26 La 2.524(4) 2_655 ? C28 O29 1.244(6) . ? C28 O30 1.257(6) . ? N31 C32 1.333(8) . ? N31 C36 1.338(7) . ? N31 H31 0.9167 . ? C32 C33 1.383(8) . ? C32 H32 0.9500 . ? C33 C34 1.395(8) . ? C33 H33 0.9500 . ? C34 C35 1.406(8) . ? C34 C37 1.466(7) . ? C35 C36 1.380(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C37 1.333(11) 2_546 ? C37 H37 0.9500 . ? O38 H38A 0.8921 . ? O38 H38B 0.8954 . ? O39 H39A 0.9199 . ? O39 H39B 0.8673 . ? O40 H40A 1.0127 . ? O40 H40B 0.8899 . ? O41A O41B 0.928(19) . ? 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 O15 La O39 138.60(13) . . ? O15 La O26 78.17(12) . 2_655 ? O39 La O26 140.04(12) . 2_655 ? O15 La O11 68.99(11) . . ? O39 La O11 130.52(11) . . ? O26 La O11 67.96(11) 2_655 . ? O15 La O27 101.80(11) . . ? O39 La O27 66.40(11) . . ? O26 La O27 132.33(11) 2_655 . ? O11 La O27 67.88(11) . . ? O15 La O38 64.62(12) . . ? O39 La O38 74.00(13) . . ? O26 La O38 137.67(11) 2_655 . ? O11 La O38 112.84(12) . . ? O27 La O38 77.14(11) . . ? O15 La O14 104.22(11) . 2 ? O39 La O14 66.24(12) . 2 ? O26 La O14 93.96(12) 2_655 2 ? O11 La O14 161.44(13) . 2 ? O27 La O14 130.61(12) . 2 ? O38 La O14 77.27(13) . 2 ? O15 La O11 140.90(11) . 2_655 ? O39 La O11 75.22(12) . 2_655 ? O26 La O11 79.88(11) 2_655 2_655 ? O11 La O11 72.89(12) . 2_655 ? O27 La O11 70.84(11) . 2_655 ? O38 La O11 142.27(11) . 2_655 ? O14 La O11 109.24(12) 2 2_655 ? O15 La O12 141.27(12) . 2_655 ? O39 La O12 73.05(12) . 2_655 ? O26 La O12 67.01(12) 2_655 2_655 ? O11 La O12 110.35(11) . 2_655 ? O27 La O12 113.89(11) . 2_655 ? O38 La O12 136.25(12) . 2_655 ? O14 La O12 63.49(12) 2 2_655 ? O11 La O12 49.26(10) 2_655 2_655 ? O15 La O15 61.42(13) . 2 ? O39 La O15 110.29(11) . 2 ? O26 La O15 69.02(10) 2_655 2 ? O11 La O15 118.96(10) . 2 ? O27 La O15 152.30(11) . 2 ? O38 La O15 75.65(11) . 2 ? O14 La O15 46.48(11) 2 2 ? O11 La O15 136.38(11) 2_655 2 ? O12 La O15 89.69(10) 2_655 2 ? O15 La C10 151.04(13) . 2_655 ? O39 La C10 70.31(13) . 2_655 ? O26 La C10 73.86(12) 2_655 2_655 ? O11 La C10 93.34(12) . 2_655 ? O27 La C10 91.69(12) . 2_655 ? O38 La C10 144.14(13) . 2_655 ? O14 La C10 85.21(13) 2 2_655 ? O11 La C10 25.07(11) 2_655 2_655 ? O12 La C10 24.38(11) 2_655 2_655 ? O15 La C10 113.59(11) 2 2_655 ? O15 La C13 83.86(12) . 2 ? O39 La C13 88.54(12) . 2 ? O26 La C13 79.43(12) 2_655 2 ? O11 La C13 140.78(13) . 2 ? O27 La C13 148.23(12) . 2 ? O38 La C13 77.33(12) . 2 ? O14 La C13 22.96(13) 2 2 ? O11 La C13 123.10(12) 2_655 2 ? O12 La C13 73.86(11) 2_655 2 ? O15 La C13 23.70(12) 2 2 ? C10 La C13 98.06(12) 2_655 2 ? C9 O1 C2 105.8(4) . . ? C3 C2 O1 110.2(4) . . ? C3 C2 C10 133.0(5) . . ? O1 C2 C10 116.7(4) . . ? C2 C3 C4 109.0(4) . . ? C2 C3 C13 131.1(5) . . ? C4 C3 C13 119.9(4) . . ? C5 C4 C3 141.3(6) . . ? C5 C4 C9 113.7(6) . . ? C3 C4 C9 104.9(4) . . ? C4 C5 C6 120.0(8) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 120.8(8) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C8 C7 C6 122.2(8) . . ? C8 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? C7 C8 C9 117.3(9) . . ? C7 C8 H8 121.4 . . ? C9 C8 H8 121.4 . . ? O1 C9 C8 123.9(6) . . ? O1 C9 C4 110.1(5) . . ? C8 C9 C4 126.0(7) . . ? O12 C10 O11 121.9(5) . . ? O12 C10 C2 119.6(4) . . ? O11 C10 C2 118.5(4) . . ? O12 C10 La 62.7(3) . 2_655 ? O11 C10 La 59.9(2) . 2_655 ? C2 C10 La 169.4(3) . 2_655 ? C10 O11 La 137.5(3) . . ? C10 O11 La 95.1(3) . 2_655 ? La O11 La 107.11(12) . 2_655 ? C10 O12 La 92.9(3) . 2_655 ? O14 C13 O15 121.8(5) . . ? O14 C13 C3 116.4(5) . . ? O15 C13 C3 121.7(5) . . ? O14 C13 La 53.7(2) . 2 ? O15 C13 La 68.8(3) . 2 ? C3 C13 La 164.4(3) . 2 ? C13 O14 La 103.3(3) . 2 ? C13 O15 La 147.6(3) . . ? C13 O15 La 87.5(3) . 2 ? La O15 La 118.58(13) . 2 ? C24 O16 C17 105.6(4) . . ? C18 C17 O16 111.8(4) . . ? C18 C17 C28 133.1(5) . . ? O16 C17 C28 115.0(4) . . ? C17 C18 C19 106.0(4) . . ? C17 C18 C25 130.8(4) . . ? C19 C18 C25 123.2(4) . . ? C24 C19 C20 119.3(4) . . ? C24 C19 C18 105.5(4) . . ? C20 C19 C18 135.2(5) . . ? C21 C20 C19 117.8(5) . . ? C21 C20 H20 121.1 . . ? C19 C20 H20 121.1 . . ? C20 C21 C22 121.4(5) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C23 C22 C21 121.6(5) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 116.2(5) . . ? C22 C23 H23 121.9 . . ? C24 C23 H23 121.9 . . ? O16 C24 C23 125.2(5) . . ? O16 C24 C19 111.1(4) . . ? C23 C24 C19 123.8(5) . . ? O27 C25 O26 125.8(5) . . ? O27 C25 C18 119.3(4) . . ? O26 C25 C18 114.8(4) . . ? C25 O26 La 132.3(3) . 2_655 ? C25 O27 La 141.6(3) . . ? O29 C28 O30 125.7(5) . . ? O29 C28 C17 116.7(4) . . ? O30 C28 C17 117.5(4) . . ? C32 N31 C36 121.3(5) . . ? C32 N31 H31 107.7 . . ? C36 N31 H31 130.6 . . ? N31 C32 C33 121.2(5) . . ? N31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C32 C33 C34 119.7(5) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C33 C34 C35 117.2(5) . . ? C33 C34 C37 123.5(5) . . ? C35 C34 C37 119.3(5) . . ? C36 C35 C34 120.5(5) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? N31 C36 C35 120.1(5) . . ? N31 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C37 C37 C34 125.0(6) 2_546 . ? C37 C37 H37 117.5 2_546 . ? C34 C37 H37 117.5 . . ? La O38 H38A 124.6 . . ? La O38 H38B 132.6 . . ? H38A O38 H38B 102.4 . . ? La O39 H39A 126.7 . . ? La O39 H39B 119.6 . . ? H39A O39 H39B 107.5 . . ? H40A O40 H40B 101.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N31 H31 O30 0.92 1.80 2.686(5) 162 2 O38 H38A O26 0.89 1.98 2.841(5) 161 1_455 O38 H38B O30 0.90 1.93 2.824(5) 179 2_665 O39 H39A O29 0.92 1.78 2.702(5) 180 . O39 H39B O41A 0.87 2.01 2.844(11) 160 1_554 O40 H40A O26 1.01 2.55 3.181(8) 120 . O40 H40B O29 0.89 2.13 2.751(7) 126 . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.83 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.663 _refine_diff_density_min -2.032 _refine_diff_density_rms 0.181 #=============================END======================== data_11 _database_code_depnum_ccdc_archive 'CCDC 775260' #TrackingRef '- ti7-19.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H10 Gd O11, 0.5(C12 H12 N2), 3(H2 O)' _chemical_formula_sum 'C26 H22 Gd N O14' _chemical_formula_weight 729.70 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 monoclinic _symmetry_space_group_name_H-M 'P 21/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 12.9328(4) _cell_length_b 23.7681(7) _cell_length_c 8.4679(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.3430(12) _cell_angle_gamma 90.00 _cell_volume 2602.88(13) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5327 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 26.37 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 2.626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6217 _exptl_absorpt_correction_T_max 0.7792 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '0.5 deg. \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20163 _diffrn_reflns_av_R_equivalents 0.0950 _diffrn_reflns_av_sigmaI/netI 0.1008 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5277 _reflns_number_gt 3480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+3.1301P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5277 _refine_ls_number_parameters 375 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1110 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 Gd Gd 0.90571(4) 0.017567(19) 0.80381(5) 0.03204(18) Uani 1 1 d . . . O1 O 0.8202(5) 0.1982(3) 0.5112(7) 0.0406(15) Uani 1 1 d . . . C2 C 0.8257(7) 0.1409(4) 0.5338(9) 0.034(2) Uani 1 1 d . . . C3 C 0.8983(7) 0.1156(4) 0.4413(9) 0.033(2) Uani 1 1 d . . . C4 C 0.9458(7) 0.1621(4) 0.3500(9) 0.034(2) Uani 1 1 d . . . C5 C 1.0258(7) 0.1664(4) 0.2446(11) 0.046(2) Uani 1 1 d . . . H5 H 1.0613 0.1341 0.2073 0.055 Uiso 1 1 calc R . . C6 C 1.0526(8) 0.2204(4) 0.1948(11) 0.048(3) Uani 1 1 d . . . H6 H 1.1070 0.2249 0.1210 0.057 Uiso 1 1 calc R . . C7 C 1.0021(8) 0.2675(4) 0.2500(11) 0.045(2) Uani 1 1 d . . . H7 H 1.0244 0.3036 0.2159 0.053 Uiso 1 1 calc R . . C8 C 0.9217(8) 0.2641(4) 0.3513(11) 0.046(3) Uani 1 1 d . . . H8 H 0.8858 0.2965 0.3866 0.055 Uiso 1 1 calc R . . C9 C 0.8945(7) 0.2098(4) 0.4013(10) 0.038(2) Uani 1 1 d . . . C10 C 0.7487(7) 0.1216(4) 0.6534(9) 0.037(2) Uani 1 1 d . . . O11 O 0.7696(4) 0.0758(3) 0.7262(6) 0.0364(15) Uani 1 1 d . . . O12 O 0.6737(5) 0.1514(3) 0.6822(8) 0.0496(17) Uani 1 1 d . . . C13 C 0.9215(6) 0.0551(4) 0.4188(9) 0.031(2) Uani 1 1 d . . . O14 O 0.9634(5) 0.0428(2) 0.2873(6) 0.0362(15) Uani 1 1 d . . . O15 O 0.8994(4) 0.0200(2) 0.5248(6) 0.0323(13) Uani 1 1 d . . . O16 O 0.6496(5) -0.1436(2) 1.0533(6) 0.0369(15) Uani 1 1 d . . . C17 C 0.7322(7) -0.1108(3) 1.0078(8) 0.029(2) Uani 1 1 d . . . C18 C 0.8058(7) -0.1083(3) 1.1240(9) 0.0299(19) Uani 1 1 d . . . C19 C 0.7688(7) -0.1414(3) 1.2544(9) 0.034(2) Uani 1 1 d . . . C20 C 0.7996(8) -0.1553(4) 1.4094(10) 0.045(2) Uani 1 1 d . . . H20 H 0.8627 -0.1415 1.4524 0.054 Uiso 1 1 calc R . . C21 C 0.7363(8) -0.1892(4) 1.4966(12) 0.053(3) Uani 1 1 d . . . H21 H 0.7566 -0.1994 1.6007 0.063 Uiso 1 1 calc R . . C22 C 0.6418(9) -0.2095(4) 1.4360(12) 0.054(3) Uani 1 1 d . . . H22 H 0.6021 -0.2339 1.5007 0.065 Uiso 1 1 calc R . . C23 C 0.6040(9) -0.1963(4) 1.2910(11) 0.053(3) Uani 1 1 d . . . H23 H 0.5389 -0.2088 1.2520 0.064 Uiso 1 1 calc R . . C24 C 0.6728(8) -0.1618(4) 1.2042(9) 0.039(2) Uani 1 1 d . . . C25 C 0.7163(7) -0.0866(4) 0.8422(10) 0.033(2) Uani 1 1 d . . . O26 O 0.7824(4) -0.0514(3) 0.7929(6) 0.0356(14) Uani 1 1 d . . . O27 O 0.6412(5) -0.1044(3) 0.7722(7) 0.0455(17) Uani 1 1 d . . . C28 C 0.9079(6) -0.0793(4) 1.1327(9) 0.0302(19) Uani 1 1 d . . . O29 O 0.9678(5) -0.0910(2) 1.2405(7) 0.0381(15) Uani 1 1 d . . . O30 O 0.9346(4) -0.0427(2) 1.0280(6) 0.0329(14) Uani 1 1 d . . . O31 O 0.8473(5) 0.0696(3) 1.0253(6) 0.0442(16) Uani 1 1 d . . . H31A H 0.8851 0.0611 1.1126 0.066 Uiso 1 1 d . . . H31B H 0.7957 0.0952 1.0207 0.066 Uiso 1 1 d . . . N32 N 0.6087(6) -0.0588(3) 0.4952(8) 0.0368(18) Uani 1 1 d . . . H32 H 0.6256 -0.0820 0.5933 0.055 Uiso 1 1 d . . . C33 C 0.5173(7) -0.0718(4) 0.4242(9) 0.037(2) Uani 1 1 d . . . H33 H 0.4705 -0.0963 0.4764 0.044 Uiso 1 1 calc R . . C34 C 0.4915(7) -0.0508(4) 0.2809(9) 0.035(2) Uani 1 1 d . . . H34 H 0.4275 -0.0606 0.2328 0.042 Uiso 1 1 calc R . . C35 C 0.5590(7) -0.0148(4) 0.2048(9) 0.0329(19) Uani 1 1 d . . . C36 C 0.6523(7) -0.0016(4) 0.2815(11) 0.039(2) Uani 1 1 d . . . H36 H 0.6989 0.0238 0.2326 0.047 Uiso 1 1 calc R . . C37 C 0.6775(8) -0.0241(4) 0.4233(10) 0.043(2) Uani 1 1 d . . . H37 H 0.7422 -0.0158 0.4718 0.051 Uiso 1 1 calc R . . C38 C 0.5384(7) 0.0081(4) 0.0447(10) 0.041(2) Uani 1 1 d . . . H38 H 0.5837 0.0362 0.0052 0.049 Uiso 1 1 calc R . . O39 O 0.6969(6) 0.1448(4) 1.0108(9) 0.083(3) Uani 1 1 d . . . H39A H 0.6891 0.1474 0.9037 0.125 Uiso 1 1 d . . . H39B H 0.6501 0.1467 1.0883 0.125 Uiso 1 1 d . . . O40 O 0.5978(6) 0.2333(4) 0.4616(11) 0.089(3) Uani 1 1 d . . . H40A H 0.6225 0.2074 0.5299 0.133 Uiso 1 1 d . . . H40B H 0.6613 0.2434 0.4233 0.133 Uiso 1 1 d . . . O41 O 0.5599(8) 0.1489(5) 1.2416(12) 0.107(3) Uiso 1 1 d . . . H41A H 0.4952 0.1347 1.2367 0.161 Uiso 1 1 d . . . H41B H 0.5725 0.1763 1.3128 0.161 Uiso 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 Gd 0.0371(3) 0.0328(3) 0.0262(2) 0.0045(2) 0.00332(16) -0.0039(3) O1 0.045(4) 0.047(4) 0.030(3) 0.003(3) -0.001(3) 0.001(3) C2 0.053(6) 0.029(5) 0.020(4) 0.005(4) -0.015(4) 0.004(4) C3 0.041(5) 0.036(5) 0.021(4) 0.002(4) 0.001(4) -0.007(4) C4 0.028(5) 0.053(6) 0.022(4) 0.008(4) -0.006(4) -0.009(4) C5 0.039(6) 0.044(6) 0.055(6) 0.003(5) 0.011(5) -0.001(5) C6 0.053(6) 0.046(6) 0.044(5) 0.013(5) 0.006(5) -0.010(5) C7 0.053(6) 0.042(6) 0.038(5) 0.007(4) -0.003(5) -0.005(5) C8 0.052(7) 0.043(6) 0.043(5) 0.003(4) -0.007(5) -0.001(5) C9 0.042(6) 0.037(6) 0.037(5) 0.002(4) -0.006(4) -0.001(5) C10 0.047(6) 0.041(6) 0.023(4) 0.006(4) -0.001(4) -0.006(5) O11 0.036(4) 0.049(4) 0.024(3) 0.006(3) 0.001(3) -0.002(3) O12 0.048(4) 0.048(4) 0.053(4) 0.009(3) 0.009(3) 0.015(4) C13 0.032(5) 0.037(5) 0.026(4) 0.004(4) -0.009(4) -0.004(4) O14 0.050(4) 0.040(4) 0.019(3) 0.003(3) 0.003(3) 0.010(3) O15 0.038(3) 0.034(3) 0.025(3) 0.007(3) 0.005(2) -0.005(3) O16 0.044(4) 0.036(4) 0.031(3) -0.001(3) 0.006(3) -0.007(3) C17 0.046(6) 0.028(5) 0.013(4) -0.002(3) 0.008(4) 0.001(4) C18 0.044(5) 0.026(5) 0.020(4) -0.005(3) 0.007(4) -0.002(4) C19 0.062(6) 0.024(5) 0.017(4) 0.005(3) 0.005(4) 0.012(4) C20 0.048(6) 0.050(6) 0.036(5) -0.008(5) 0.010(4) -0.002(5) C21 0.061(7) 0.046(6) 0.051(6) 0.021(5) 0.002(5) 0.010(6) C22 0.058(7) 0.054(7) 0.051(6) 0.009(5) -0.002(5) -0.006(6) C23 0.069(8) 0.047(7) 0.044(6) -0.011(5) 0.015(5) 0.000(6) C24 0.055(6) 0.039(6) 0.022(4) -0.002(4) 0.012(4) -0.009(5) C25 0.043(6) 0.026(5) 0.031(5) 0.002(4) 0.004(4) 0.002(4) O26 0.038(4) 0.038(4) 0.031(3) 0.009(3) -0.002(3) -0.011(3) O27 0.048(4) 0.059(5) 0.029(3) 0.008(3) -0.010(3) -0.024(4) C28 0.028(5) 0.033(5) 0.030(5) -0.002(4) -0.002(4) 0.003(4) O29 0.042(4) 0.037(4) 0.035(3) 0.006(3) -0.007(3) -0.008(3) O30 0.037(4) 0.034(3) 0.028(3) 0.007(3) 0.000(3) -0.003(3) O31 0.049(4) 0.055(4) 0.029(3) 0.004(3) -0.004(3) 0.013(3) N32 0.040(5) 0.035(4) 0.036(4) -0.001(3) -0.002(3) 0.005(4) C33 0.045(6) 0.038(5) 0.027(4) 0.009(4) 0.012(4) -0.004(4) C34 0.034(5) 0.037(5) 0.033(5) 0.003(4) -0.006(4) -0.003(4) C35 0.037(5) 0.028(5) 0.034(4) -0.001(4) 0.004(4) 0.004(4) C36 0.036(5) 0.035(5) 0.047(5) 0.005(4) 0.005(4) -0.010(4) C37 0.053(6) 0.039(6) 0.035(5) 0.014(4) 0.004(4) 0.004(5) C38 0.045(6) 0.045(6) 0.034(5) 0.007(4) 0.008(4) 0.002(5) O39 0.064(5) 0.131(8) 0.055(5) -0.021(5) -0.004(4) 0.041(5) O40 0.063(6) 0.080(7) 0.123(8) 0.013(6) -0.017(5) -0.001(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 Gd O26 2.288(6) . ? Gd O11 2.331(6) . ? Gd O14 2.353(6) 3_756 ? Gd O15 2.364(5) . ? Gd O31 2.374(6) . ? Gd O30 2.406(5) . ? Gd O29 2.423(6) 3_757 ? Gd O30 2.572(5) 3_757 ? Gd C28 2.870(8) 3_757 ? O1 C9 1.369(11) . ? O1 C2 1.378(10) . ? C2 C3 1.366(12) . ? C2 C10 1.496(12) . ? C3 C13 1.481(12) . ? C3 C4 1.485(12) . ? C4 C5 1.374(12) . ? C4 C9 1.384(13) . ? C5 C6 1.396(13) . ? C5 H5 0.9500 . ? C6 C7 1.379(14) . ? C6 H6 0.9500 . ? C7 C8 1.353(13) . ? C7 H7 0.9500 . ? C8 C9 1.403(13) . ? C8 H8 0.9500 . ? C10 O12 1.226(11) . ? C10 O11 1.279(10) . ? C13 O15 1.259(9) . ? C13 O14 1.275(10) . ? O14 Gd 2.353(6) 3_756 ? O16 C17 1.379(10) . ? O16 C24 1.381(10) . ? C17 C18 1.367(11) . ? C17 C25 1.528(11) . ? C18 C19 1.441(11) . ? C18 C28 1.490(12) . ? C19 C24 1.396(13) . ? C19 C20 1.409(12) . ? C20 C21 1.368(13) . ? C20 H20 0.9500 . ? C21 C22 1.407(14) . ? C21 H21 0.9500 . ? C22 C23 1.355(14) . ? C22 H22 0.9500 . ? C23 C24 1.419(13) . ? C23 H23 0.9500 . ? C25 O27 1.211(10) . ? C25 O26 1.270(10) . ? C28 O29 1.225(9) . ? C28 O30 1.291(10) . ? C28 Gd 2.870(8) 3_757 ? O29 Gd 2.423(6) 3_757 ? O30 Gd 2.572(5) 3_757 ? O31 H31A 0.9063 . ? O31 H31B 0.9043 . ? N32 C33 1.358(11) . ? N32 C37 1.360(11) . ? N32 H32 1.0203 . ? C33 C34 1.353(11) . ? C33 H33 0.9500 . ? C34 C35 1.383(12) . ? C34 H34 0.9500 . ? C35 C36 1.403(12) . ? C35 C38 1.484(11) . ? C36 C37 1.352(12) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C38 1.305(18) 3_655 ? C38 H38 0.9500 . ? O39 H39A 0.9140 . ? O39 H39B 0.8965 . ? O40 H40A 0.9015 . ? O40 H40B 0.9167 . ? O41 H41A 0.9034 . ? O41 H41B 0.9005 . ? 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 O26 Gd O11 83.7(2) . . ? O26 Gd O14 93.0(2) . 3_756 ? O11 Gd O14 144.42(18) . 3_756 ? O26 Gd O15 87.56(19) . . ? O11 Gd O15 71.45(19) . . ? O14 Gd O15 73.02(19) 3_756 . ? O26 Gd O31 100.4(2) . . ? O11 Gd O31 70.74(19) . . ? O14 Gd O31 144.08(19) 3_756 . ? O15 Gd O31 140.1(2) . . ? O26 Gd O30 73.16(19) . . ? O11 Gd O30 133.61(19) . . ? O14 Gd O30 77.69(19) 3_756 . ? O15 Gd O30 143.9(2) . . ? O31 Gd O30 74.7(2) . . ? O26 Gd O29 168.73(18) . 3_757 ? O11 Gd O29 92.2(2) . 3_757 ? O14 Gd O29 84.3(2) 3_756 3_757 ? O15 Gd O29 81.18(19) . 3_757 ? O31 Gd O29 88.0(2) . 3_757 ? O30 Gd O29 116.68(19) . 3_757 ? O26 Gd O30 138.22(18) . 3_757 ? O11 Gd O30 128.36(19) . 3_757 ? O14 Gd O30 75.32(19) 3_756 3_757 ? O15 Gd O30 124.78(18) . 3_757 ? O31 Gd O30 72.51(19) . 3_757 ? O30 Gd O30 65.2(2) . 3_757 ? O29 Gd O30 51.52(18) 3_757 3_757 ? O26 Gd C28 163.4(2) . 3_757 ? O11 Gd C28 112.4(2) . 3_757 ? O14 Gd C28 76.6(2) 3_756 3_757 ? O15 Gd C28 101.5(2) . 3_757 ? O31 Gd C28 81.7(2) . 3_757 ? O30 Gd C28 91.7(2) . 3_757 ? O29 Gd C28 25.0(2) 3_757 3_757 ? O30 Gd C28 26.73(19) 3_757 3_757 ? C9 O1 C2 105.0(7) . . ? C3 C2 O1 113.0(8) . . ? C3 C2 C10 135.7(8) . . ? O1 C2 C10 111.3(8) . . ? C2 C3 C13 129.9(8) . . ? C2 C3 C4 105.0(8) . . ? C13 C3 C4 124.9(8) . . ? C5 C4 C9 120.5(9) . . ? C5 C4 C3 135.1(9) . . ? C9 C4 C3 104.2(8) . . ? C4 C5 C6 116.9(10) . . ? C4 C5 H5 121.5 . . ? C6 C5 H5 121.5 . . ? C7 C6 C5 121.7(10) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C8 C7 C6 122.2(10) . . ? C8 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? C7 C8 C9 116.2(10) . . ? C7 C8 H8 121.9 . . ? C9 C8 H8 121.9 . . ? O1 C9 C4 112.8(8) . . ? O1 C9 C8 124.6(9) . . ? C4 C9 C8 122.4(9) . . ? O12 C10 O11 124.1(8) . . ? O12 C10 C2 119.2(8) . . ? O11 C10 C2 116.5(8) . . ? C10 O11 Gd 143.0(6) . . ? O15 C13 O14 124.8(8) . . ? O15 C13 C3 120.2(8) . . ? O14 C13 C3 114.9(7) . . ? C13 O14 Gd 137.4(5) . 3_756 ? C13 O15 Gd 136.2(5) . . ? C17 O16 C24 105.7(6) . . ? C18 C17 O16 111.2(7) . . ? C18 C17 C25 137.2(8) . . ? O16 C17 C25 111.6(7) . . ? C17 C18 C19 107.1(8) . . ? C17 C18 C28 132.0(7) . . ? C19 C18 C28 120.9(7) . . ? C24 C19 C20 116.6(8) . . ? C24 C19 C18 104.8(7) . . ? C20 C19 C18 138.5(9) . . ? C21 C20 C19 118.3(9) . . ? C21 C20 H20 120.9 . . ? C19 C20 H20 120.9 . . ? C20 C21 C22 121.8(10) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C23 C22 C21 124.0(10) . . ? C23 C22 H22 118.0 . . ? C21 C22 H22 118.0 . . ? C22 C23 C24 112.3(10) . . ? C22 C23 H23 123.9 . . ? C24 C23 H23 123.9 . . ? O16 C24 C19 111.2(7) . . ? O16 C24 C23 121.8(9) . . ? C19 C24 C23 127.0(8) . . ? O27 C25 O26 127.5(8) . . ? O27 C25 C17 114.9(8) . . ? O26 C25 C17 117.6(8) . . ? C25 O26 Gd 158.4(5) . . ? O29 C28 O30 119.6(8) . . ? O29 C28 C18 119.2(8) . . ? O30 C28 C18 121.2(7) . . ? O29 C28 Gd 56.6(4) . 3_757 ? O30 C28 Gd 63.6(4) . 3_757 ? C18 C28 Gd 171.1(6) . 3_757 ? C28 O29 Gd 98.4(5) . 3_757 ? C28 O30 Gd 154.5(5) . . ? C28 O30 Gd 89.6(4) . 3_757 ? Gd O30 Gd 114.8(2) . 3_757 ? Gd O31 H31A 110.8 . . ? Gd O31 H31B 123.7 . . ? H31A O31 H31B 125.4 . . ? C33 N32 C37 120.7(7) . . ? C33 N32 H32 114.7 . . ? C37 N32 H32 123.7 . . ? C34 C33 N32 121.4(8) . . ? C34 C33 H33 119.3 . . ? N32 C33 H33 119.3 . . ? C33 C34 C35 119.6(8) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C36 117.8(8) . . ? C34 C35 C38 122.9(8) . . ? C36 C35 C38 119.3(8) . . ? C37 C36 C35 121.7(9) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C36 C37 N32 118.8(9) . . ? C36 C37 H37 120.6 . . ? N32 C37 H37 120.6 . . ? C38 C38 C35 123.5(11) 3_655 . ? C38 C38 H38 118.2 3_655 . ? C35 C38 H38 118.2 . . ? H39A O39 H39B 130.7 . . ? H40A O40 H40B 95.3 . . ? H41A O41 H41B 117.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O31 H31A O14 0.91 1.84 2.746(8) 179 1_556 O31 H31B O39 0.90 1.74 2.645(10) 179 . N32 H32 O27 1.02 1.62 2.616(9) 165 . O39 H39A O12 0.91 1.89 2.801(10) 179 . O39 H39B O41 0.90 1.75 2.647(13) 179 . O40 H40A O12 0.90 1.97 2.867(11) 179 . O40 H40B O1 0.92 2.43 3.022(10) 122 . O41 H41A O27 0.90 1.91 2.810(12) 180 3_657 O41 H41B O40 0.90 1.88 2.778(14) 180 1_556 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.263 _refine_diff_density_min -1.026 _refine_diff_density_rms 0.150 #===================END========================= data_12 _database_code_depnum_ccdc_archive 'CCDC 775261' #TrackingRef '- ti7-19.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H13 Cd O9, C10 H5 O5, H2 O' _chemical_formula_sum 'C20 H20 Cd O15' _chemical_formula_weight 612.76 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.37680(10) _cell_length_b 17.9573(4) _cell_length_c 16.5245(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.2846(8) _cell_angle_gamma 90.00 _cell_volume 2175.80(9) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4880 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.90 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 1.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7729 _exptl_absorpt_correction_T_max 0.8120 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f & \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18674 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.90 _reflns_number_total 5145 _reflns_number_gt 3640 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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. Due to partial disorder of one of the phenyl rings, several ISOR restraints were applied in order to avoid unreasonable ADP parameters of the disordered fragments. ; _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^)+(0.0902P)^2^+0.9733P] 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 5145 _refine_ls_number_parameters 325 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1361 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.25981(4) -0.04098(2) 0.19226(2) 0.01968(14) Uani 1 1 d . . . O12 O 0.2133(4) 0.06819(19) 0.1160(2) 0.0215(7) Uani 1 1 d . . . C10 C 0.1754(6) 0.1304(3) 0.1446(3) 0.0203(10) Uani 1 1 d . . . O1 O 0.2778(4) 0.18640(18) 0.02463(19) 0.0186(7) Uani 1 1 d . . . C2 C 0.2211(6) 0.1984(3) 0.0995(3) 0.0176(9) Uani 1 1 d . . . C3 C 0.2226(6) 0.2731(3) 0.1189(3) 0.0160(9) Uani 1 1 d . . . C4 C 0.2867(6) 0.3110(3) 0.0493(3) 0.0180(10) Uani 1 1 d . . . C5 C 0.3234(6) 0.3856(3) 0.0296(3) 0.0200(10) Uani 1 1 d . . . H5 H 0.3069 0.4252 0.0662 0.024 Uiso 1 1 calc R . . C6 C 0.3843(6) 0.3987(3) -0.0452(3) 0.0230(11) Uani 1 1 d . . . H6 H 0.4103 0.4483 -0.0600 0.028 Uiso 1 1 calc R . . C7 C 0.4091(6) 0.3408(3) -0.1001(3) 0.0227(11) Uani 1 1 d . . . H7 H 0.4486 0.3524 -0.1514 0.027 Uiso 1 1 calc R . . C8 C 0.3775(6) 0.2675(3) -0.0811(3) 0.0214(10) Uani 1 1 d . . . H8 H 0.3964 0.2279 -0.1173 0.026 Uiso 1 1 calc R . . C9 C 0.3169(6) 0.2554(3) -0.0063(3) 0.0183(10) Uani 1 1 d . . . O11 O 0.1031(4) 0.1403(2) 0.2097(2) 0.0248(8) Uani 1 1 d . . . C13 C 0.1770(6) 0.3112(3) 0.1926(3) 0.0202(10) Uani 1 1 d . . . O14 O 0.1148(4) 0.2734(2) 0.2514(2) 0.0243(8) Uani 1 1 d . . . H14 H 0.0955 0.2188 0.2378 0.036 Uiso 1 1 d . . . O15 O 0.1980(5) 0.3794(2) 0.1988(2) 0.0257(8) Uani 1 1 d . . . O16 O 0.0127(4) -0.1053(2) 0.1367(2) 0.0274(8) Uani 1 1 d . . . H16A H -0.0341 -0.1325 0.1743 0.041 Uiso 1 1 d . . . H16B H -0.0823 -0.0825 0.1076 0.041 Uiso 1 1 d . . . O17 O 0.3972(5) -0.0911(2) 0.0873(2) 0.0310(9) Uani 1 1 d . . . H17A H 0.5083 -0.0829 0.0790 0.047 Uiso 1 1 d . . . H17B H 0.3250 -0.1175 0.0401 0.047 Uiso 1 1 d . . . O18 O 0.0825(4) 0.0078(2) 0.2841(2) 0.0256(8) Uani 1 1 d . . . H18A H 0.0353 0.0521 0.2718 0.038 Uiso 1 1 d . . . H18B H -0.0224 -0.0129 0.2950 0.038 Uiso 1 1 d . . . O19 O 0.5347(4) 0.0077(2) 0.2366(2) 0.0292(8) Uani 1 1 d . . . H19A H 0.5817 0.0367 0.1909 0.044 Uiso 1 1 d . . . H19B H 0.6204 -0.0225 0.2628 0.044 Uiso 1 1 d . . . O20 O 0.7866(5) 0.2111(2) 0.0253(2) 0.0328(9) Uani 1 1 d . . . C21 C 0.7351(6) 0.2312(3) 0.0996(3) 0.0253(11) Uani 1 1 d U . . C22 C 0.7389(6) 0.3053(3) 0.1156(4) 0.0299(13) Uani 1 1 d . . . C23 C 0.8034(6) 0.3393(3) 0.0396(3) 0.0282(12) Uani 1 1 d . . . C24 C 0.8347(7) 0.4100(4) 0.0137(4) 0.0360(14) Uani 1 1 d . . . H24 H 0.8201 0.4520 0.0472 0.043 Uiso 1 1 calc R . . C25 C 0.8863(7) 0.4174(3) -0.0602(4) 0.0359(14) Uani 1 1 d . . . H25 H 0.9074 0.4663 -0.0790 0.043 Uiso 1 1 calc R . . C26 C 0.9113(6) 0.3590(4) -0.1115(3) 0.0322(13) Uani 1 1 d . . . H26 H 0.9472 0.3688 -0.1640 0.039 Uiso 1 1 calc R . . C27 C 0.8850(7) 0.2858(3) -0.0878(3) 0.0333(13) Uani 1 1 d U . . H27 H 0.9044 0.2442 -0.1213 0.040 Uiso 1 1 calc R . . C28 C 0.8263(6) 0.2787(3) -0.0086(3) 0.0283(12) Uani 1 1 d U . . C29 C 0.6780(7) 0.1636(3) 0.1485(4) 0.0287(12) Uani 1 1 d U . . O30 O 0.6833(5) 0.1009(2) 0.1187(3) 0.0418(10) Uani 1 1 d . . . O31 O 0.6275(5) 0.1779(2) 0.2173(3) 0.0411(10) Uani 1 1 d . . . C32 C 0.6886(7) 0.3463(3) 0.1855(4) 0.0328(13) Uani 1 1 d . . . O33 O 0.6295(5) 0.3112(2) 0.2425(2) 0.0371(10) Uani 1 1 d . . . H33 H 0.6157 0.2597 0.2596 0.056 Uiso 1 1 d . . . O34 O 0.7056(5) 0.4165(2) 0.1837(3) 0.0396(10) Uani 1 1 d . . . O35 O 0.7254(5) 0.9638(2) 0.0469(2) 0.0259(8) Uani 1 1 d . . . H35A H 0.6953 1.0088 0.0702 0.039 Uiso 1 1 d . . . H35B H 0.7498 0.9520 -0.0039 0.039 Uiso 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 Cd 0.0211(2) 0.0161(2) 0.0229(2) 0.00192(15) 0.00674(13) 0.00023(14) O12 0.0266(17) 0.0146(18) 0.0242(18) 0.0000(14) 0.0075(13) 0.0014(14) C10 0.016(2) 0.021(3) 0.024(3) 0.003(2) 0.0030(18) -0.0019(18) O1 0.0198(16) 0.0168(18) 0.0197(17) -0.0001(14) 0.0046(12) 0.0009(13) C2 0.018(2) 0.016(3) 0.018(2) 0.0013(19) 0.0018(17) 0.0019(17) C3 0.015(2) 0.012(2) 0.021(2) -0.0019(18) 0.0018(16) 0.0000(16) C4 0.018(2) 0.017(2) 0.020(2) 0.0034(19) 0.0023(17) 0.0029(17) C5 0.018(2) 0.019(3) 0.023(3) 0.002(2) 0.0022(17) -0.0009(18) C6 0.014(2) 0.022(3) 0.033(3) 0.007(2) 0.0024(18) -0.0028(18) C7 0.018(2) 0.026(3) 0.025(3) 0.008(2) 0.0064(18) 0.0033(19) C8 0.019(2) 0.024(3) 0.022(3) -0.002(2) 0.0041(18) 0.0017(19) C9 0.015(2) 0.013(2) 0.026(3) 0.0015(19) 0.0014(17) -0.0008(17) O11 0.0321(18) 0.019(2) 0.0251(19) 0.0003(15) 0.0115(14) 0.0014(14) C13 0.019(2) 0.022(3) 0.020(3) 0.000(2) 0.0024(17) 0.0023(19) O14 0.0330(19) 0.0199(19) 0.0213(19) -0.0007(15) 0.0091(14) 0.0015(14) O15 0.0344(18) 0.018(2) 0.0256(19) -0.0052(15) 0.0090(14) -0.0012(15) O16 0.0248(17) 0.021(2) 0.036(2) 0.0012(16) 0.0012(14) 0.0000(14) O17 0.0300(19) 0.028(2) 0.038(2) -0.0088(17) 0.0188(16) -0.0030(16) O18 0.0293(18) 0.0172(19) 0.033(2) 0.0026(15) 0.0158(15) 0.0022(14) O19 0.0231(18) 0.028(2) 0.035(2) 0.0095(17) -0.0019(15) -0.0036(15) O20 0.032(2) 0.032(2) 0.035(2) -0.0013(18) 0.0066(16) 0.0017(17) C21 0.0207(19) 0.034(2) 0.022(2) -0.0052(18) 0.0041(16) 0.0065(17) C22 0.011(2) 0.030(3) 0.047(3) 0.012(3) -0.002(2) -0.0028(19) C23 0.017(2) 0.039(3) 0.027(3) -0.004(2) -0.0039(19) 0.008(2) C24 0.021(3) 0.032(3) 0.054(4) -0.002(3) -0.003(2) -0.001(2) C25 0.021(3) 0.028(3) 0.057(4) 0.009(3) 0.000(2) 0.002(2) C26 0.014(2) 0.052(4) 0.030(3) 0.009(3) 0.0027(19) 0.001(2) C27 0.027(2) 0.035(2) 0.037(2) -0.014(2) -0.0037(18) 0.0079(19) C28 0.0215(19) 0.023(2) 0.039(2) 0.0077(19) -0.0039(17) -0.0023(17) C29 0.0242(19) 0.020(2) 0.039(2) -0.0085(19) -0.0073(17) 0.0058(17) O30 0.043(2) 0.029(2) 0.054(3) 0.002(2) 0.0058(19) -0.0012(18) O31 0.039(2) 0.039(3) 0.047(3) 0.008(2) 0.0105(18) 0.0003(18) C32 0.022(2) 0.033(4) 0.042(4) -0.008(3) 0.000(2) 0.002(2) O33 0.038(2) 0.045(3) 0.028(2) -0.0041(19) 0.0025(16) 0.0100(18) O34 0.037(2) 0.030(3) 0.052(3) -0.006(2) 0.0052(18) -0.0017(18) O35 0.0307(19) 0.024(2) 0.0242(19) -0.0045(15) 0.0081(14) 0.0050(15) _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 Cd O19 2.256(3) . ? Cd O16 2.265(3) . ? Cd O18 2.284(3) . ? Cd O17 2.288(3) . ? Cd O15 2.293(3) 2_545 ? Cd O12 2.336(3) . ? O12 C10 1.257(6) . ? C10 O11 1.265(6) . ? C10 C2 1.487(7) . ? O1 C2 1.367(6) . ? O1 C9 1.382(6) . ? C2 C3 1.379(7) . ? C3 C4 1.459(6) . ? C3 C13 1.468(7) . ? C4 C9 1.392(7) . ? C4 C5 1.413(7) . ? C5 C6 1.380(7) . ? C5 H5 0.9500 . ? C6 C7 1.405(7) . ? C6 H6 0.9500 . ? C7 C8 1.378(7) . ? C7 H7 0.9500 . ? C8 C9 1.377(7) . ? C8 H8 0.9500 . ? C13 O15 1.237(6) . ? C13 O14 1.309(6) . ? O14 H14 1.0125 . ? O15 Cd 2.293(3) 2 ? O16 H16A 0.8896 . ? O16 H16B 0.9031 . ? O17 H17A 0.8581 . ? O17 H17B 1.0124 . ? O18 H18A 0.8837 . ? O18 H18B 0.8943 . ? O19 H19A 1.0082 . ? O19 H19B 0.9066 . ? O20 C21 1.374(6) . ? O20 C28 1.382(7) . ? C21 C22 1.357(8) . ? C21 C29 1.541(8) . ? C22 C32 1.451(8) . ? C22 C23 1.520(8) . ? C23 C24 1.367(8) . ? C23 C28 1.370(8) . ? C24 C25 1.325(9) . ? C24 H24 0.9500 . ? C25 C26 1.372(9) . ? C25 H25 0.9500 . ? C26 C27 1.392(8) . ? C26 H26 0.9500 . ? C27 C28 1.428(8) . ? C27 H27 0.9500 . ? C29 O30 1.230(7) . ? C29 O31 1.261(7) . ? C32 O33 1.250(7) . ? C32 O34 1.268(7) . ? O33 H33 0.9759 . ? O35 H35A 0.9330 . ? O35 H35B 0.9022 . ? 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 O19 Cd O16 169.75(13) . . ? O19 Cd O18 101.29(13) . . ? O16 Cd O18 88.32(13) . . ? O19 Cd O17 86.64(13) . . ? O16 Cd O17 84.03(13) . . ? O18 Cd O17 171.30(13) . . ? O19 Cd O15 86.96(13) . 2_545 ? O16 Cd O15 91.97(13) . 2_545 ? O18 Cd O15 75.86(13) . 2_545 ? O17 Cd O15 108.46(13) . 2_545 ? O19 Cd O12 85.62(12) . . ? O16 Cd O12 98.33(12) . . ? O18 Cd O12 88.62(12) . . ? O17 Cd O12 88.40(13) . . ? O15 Cd O12 161.13(12) 2_545 . ? C10 O12 Cd 124.7(3) . . ? O12 C10 O11 125.2(4) . . ? O12 C10 C2 118.0(4) . . ? O11 C10 C2 116.8(4) . . ? C2 O1 C9 106.9(4) . . ? O1 C2 C3 111.6(4) . . ? O1 C2 C10 115.6(4) . . ? C3 C2 C10 132.7(4) . . ? C2 C3 C4 105.4(4) . . ? C2 C3 C13 130.5(4) . . ? C4 C3 C13 124.1(4) . . ? C9 C4 C5 118.6(4) . . ? C9 C4 C3 106.0(4) . . ? C5 C4 C3 135.4(4) . . ? C6 C5 C4 117.2(5) . . ? C6 C5 H5 121.4 . . ? C4 C5 H5 121.4 . . ? C5 C6 C7 122.0(5) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C6 121.5(5) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C9 C8 C7 115.8(5) . . ? C9 C8 H8 122.1 . . ? C7 C8 H8 122.1 . . ? C8 C9 O1 125.1(4) . . ? C8 C9 C4 124.8(5) . . ? O1 C9 C4 110.1(4) . . ? O15 C13 O14 120.2(4) . . ? O15 C13 C3 119.5(4) . . ? O14 C13 C3 120.3(4) . . ? C13 O14 H14 113.0 . . ? C13 O15 Cd 133.4(3) . 2 ? Cd O16 H16A 110.7 . . ? Cd O16 H16B 121.9 . . ? H16A O16 H16B 106.4 . . ? Cd O17 H17A 124.3 . . ? Cd O17 H17B 121.9 . . ? H17A O17 H17B 112.9 . . ? Cd O18 H18A 115.6 . . ? Cd O18 H18B 123.1 . . ? H18A O18 H18B 95.3 . . ? Cd O19 H19A 109.1 . . ? Cd O19 H19B 118.5 . . ? H19A O19 H19B 112.9 . . ? C21 O20 C28 102.9(4) . . ? C22 C21 O20 115.5(5) . . ? C22 C21 C29 132.1(5) . . ? O20 C21 C29 112.3(5) . . ? C21 C22 C32 130.6(5) . . ? C21 C22 C23 103.6(5) . . ? C32 C22 C23 125.7(5) . . ? C24 C23 C28 121.3(5) . . ? C24 C23 C22 135.4(5) . . ? C28 C23 C22 103.3(5) . . ? C25 C24 C23 117.2(6) . . ? C25 C24 H24 121.4 . . ? C23 C24 H24 121.4 . . ? C24 C25 C26 124.4(6) . . ? C24 C25 H25 117.8 . . ? C26 C25 H25 117.8 . . ? C25 C26 C27 121.0(5) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C28 114.1(5) . . ? C26 C27 H27 123.0 . . ? C28 C27 H27 123.0 . . ? C23 C28 O20 114.7(5) . . ? C23 C28 C27 122.1(5) . . ? O20 C28 C27 123.2(5) . . ? O30 C29 O31 124.9(6) . . ? O30 C29 C21 119.2(5) . . ? O31 C29 C21 115.9(5) . . ? O33 C32 O34 124.2(6) . . ? O33 C32 C22 119.0(5) . . ? O34 C32 C22 116.8(6) . . ? C32 O33 H33 138.7 . . ? H35A O35 H35B 132.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H14 O11 1.01 1.49 2.486(5) 168 . O16 H16A O33 0.89 1.90 2.791(5) 178 2_545 O16 H16B O35 0.90 1.84 2.747(5) 179 1_445 O17 H17A O35 0.86 1.93 2.763(5) 162 1_545 O17 H17B O20 1.01 2.12 3.064(5) 155 3_655 O18 H18A O11 0.88 1.98 2.691(5) 136 . O18 H18B O34 0.89 1.91 2.781(5) 163 2_545 O19 H19A O30 1.01 1.87 2.874(6) 171 . O19 H19B O34 0.91 1.84 2.745(5) 180 2_645 O33 H33 O31 0.98 1.63 2.430(6) 136 . O35 H35A O30 0.93 1.84 2.766(6) 169 1_565 O35 H35B O12 0.90 1.94 2.836(5) 175 3_665 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.234 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.149 #=======================END========================= data_13 _database_code_depnum_ccdc_archive 'CCDC 775262' #TrackingRef '- ti7-19.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H13 Mn O9, C10 H5 O5, H2 O' _chemical_formula_sum 'C20 H20 Mn O15' _chemical_formula_weight 555.30 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' Mn Mn 0.3368 0.7283 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.3730(2) _cell_length_b 17.9140(4) _cell_length_c 16.3998(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.2068(9) _cell_angle_gamma 90.00 _cell_volume 2153.39(10) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4857 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 26.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 0.697 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8732 _exptl_absorpt_correction_T_max 0.8732 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f & \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18336 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4213 _reflns_number_gt 3343 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Noniusa B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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. Due to partial disorder of one of the phenyl rings, several ISOR restraints were applied in order to avoid unreasonable ADP parameters of the disordered fragments. ; _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^)+(0.0991P)^2^+1.1522P] 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 4213 _refine_ls_number_parameters 325 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.2365 _refine_ls_wR_factor_gt 0.2234 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.074 _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 Mn Mn 0.25992(11) 0.04065(4) 0.19197(5) 0.0214(3) Uani 1 1 d . . . O1 O 0.2233(5) 0.31419(19) 0.4700(2) 0.0209(8) Uani 1 1 d . . . C2 C 0.2828(7) 0.3025(3) 0.3945(3) 0.0192(10) Uani 1 1 d . . . C3 C 0.2794(7) 0.2281(3) 0.3750(3) 0.0193(10) Uani 1 1 d . . . C4 C 0.2144(7) 0.1893(3) 0.4439(3) 0.0195(10) Uani 1 1 d . . . C5 C 0.1791(7) 0.1144(3) 0.4634(3) 0.0240(11) Uani 1 1 d . . . H5 H 0.1970 0.0750 0.4264 0.029 Uiso 1 1 calc R . . C6 C 0.1179(7) 0.1008(3) 0.5380(3) 0.0256(11) Uani 1 1 d . . . H6 H 0.0929 0.0508 0.5525 0.031 Uiso 1 1 calc R . . C7 C 0.0907(7) 0.1584(3) 0.5940(3) 0.0249(11) Uani 1 1 d . . . H7 H 0.0490 0.1463 0.6452 0.030 Uiso 1 1 calc R . . C8 C 0.1235(7) 0.2323(3) 0.5758(3) 0.0233(11) Uani 1 1 d . . . H8 H 0.1058 0.2718 0.6128 0.028 Uiso 1 1 calc R . . C9 C 0.1837(7) 0.2446(3) 0.5003(3) 0.0203(10) Uani 1 1 d . . . C10 C 0.3278(7) 0.3712(3) 0.3504(3) 0.0195(10) Uani 1 1 d . . . O11 O 0.4060(5) 0.36191(19) 0.2862(2) 0.0248(8) Uani 1 1 d . . . O12 O 0.2854(5) 0.43337(19) 0.3782(2) 0.0224(8) Uani 1 1 d . . . C13 C 0.3281(7) 0.1908(3) 0.2994(3) 0.0207(11) Uani 1 1 d . . . O14 O 0.3982(5) 0.2291(2) 0.2430(2) 0.0253(8) Uani 1 1 d . . . H14 H 0.4063 0.2837 0.2556 0.038 Uiso 1 1 d . . . O15 O 0.3004(6) 0.1233(2) 0.2912(2) 0.0283(9) Uani 1 1 d . . . O16 O 0.5242(5) -0.0044(2) 0.2356(3) 0.0309(9) Uani 1 1 d . . . H16A H 0.6129 0.0247 0.2608 0.050 Uiso 1 1 d . . . H16B H 0.5738 -0.0343 0.1994 0.050 Uiso 1 1 d . . . O17 O 0.3921(6) 0.0880(2) 0.0898(3) 0.0315(9) Uani 1 1 d . . . H17A H 0.3109 0.1128 0.0449 0.050 Uiso 1 1 d . . . H17B H 0.5179 0.0760 0.0742 0.050 Uiso 1 1 d . . . O18 O 0.0224(5) 0.1005(2) 0.1370(3) 0.0299(9) Uani 1 1 d . . . H18A H -0.0715 0.0773 0.1055 0.050 Uiso 1 1 d . . . H18B H -0.0180 0.1136 0.1894 0.050 Uiso 1 1 d . . . O19 O 0.0913(5) -0.0042(2) 0.2830(2) 0.0277(9) Uani 1 1 d . . . H19A H 0.0332 -0.0497 0.2622 0.050 Uiso 1 1 d . . . H19B H 0.0029 0.0296 0.2831 0.050 Uiso 1 1 d . . . O20 O -0.2865(6) 0.2902(2) 0.4729(3) 0.0365(10) Uani 1 1 d . . . C21 C -0.2338(8) 0.2710(3) 0.3982(3) 0.0312(13) Uani 1 1 d DU . . C22 C -0.2383(8) 0.1952(3) 0.3819(4) 0.0323(14) Uani 1 1 d D . . C23 C -0.3026(8) 0.1614(4) 0.4569(4) 0.0323(13) Uani 1 1 d D . . C24 C -0.3341(9) 0.0912(4) 0.4833(5) 0.0423(16) Uani 1 1 d . . . H24 H -0.3196 0.0492 0.4493 0.051 Uiso 1 1 calc R . . C25 C -0.3854(8) 0.0830(4) 0.5575(5) 0.0405(16) Uani 1 1 d . . . H25 H -0.4047 0.0337 0.5760 0.049 Uiso 1 1 calc R . . C26 C -0.4128(8) 0.1406(4) 0.6093(4) 0.0376(15) Uani 1 1 d . . . H26 H -0.4505 0.1300 0.6616 0.045 Uiso 1 1 calc R . . C27 C -0.3865(8) 0.2150(4) 0.5870(4) 0.0427(17) Uani 1 1 d . . . H27 H -0.4057 0.2563 0.6213 0.051 Uiso 1 1 calc R . . C28 C -0.3267(8) 0.2221(3) 0.5057(4) 0.0349(15) Uani 1 1 d . . . C29 C -0.1758(8) 0.3373(3) 0.3499(4) 0.0346(14) Uani 1 1 d DU . . O30 O -0.1803(7) 0.4009(2) 0.3792(3) 0.0445(12) Uani 1 1 d . . . O31 O -0.1256(7) 0.3243(3) 0.2800(3) 0.0459(12) Uani 1 1 d . . . C32 C -0.1863(9) 0.1548(4) 0.3113(4) 0.0378(15) Uani 1 1 d . . . O33 O -0.1272(6) 0.1906(3) 0.2540(3) 0.0430(11) Uani 1 1 d . . . H33 H -0.1122 0.2427 0.2376 0.064 Uiso 1 1 d R . . O34 O -0.2046(7) 0.0849(3) 0.3129(3) 0.0434(11) Uani 1 1 d . . . O35 O 0.2243(6) 0.4630(2) 0.5459(2) 0.0283(9) Uani 1 1 d . . . H35A H 0.2255 0.4544 0.4888 0.050 Uiso 1 1 d . . . H35B H 0.2204 0.5119 0.5614 0.050 Uiso 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 Mn 0.0270(5) 0.0151(4) 0.0232(5) -0.0023(3) 0.0070(3) -0.0007(3) O1 0.0291(19) 0.0137(17) 0.0207(18) 0.0001(14) 0.0070(15) -0.0018(14) C2 0.023(3) 0.019(2) 0.016(2) -0.0006(19) 0.0032(19) -0.0002(19) C3 0.021(3) 0.016(2) 0.021(3) 0.0014(19) 0.002(2) 0.0003(18) C4 0.021(2) 0.017(2) 0.021(3) 0.0011(19) 0.001(2) 0.0003(18) C5 0.029(3) 0.019(3) 0.024(3) -0.001(2) 0.005(2) 0.000(2) C6 0.029(3) 0.018(3) 0.031(3) 0.005(2) 0.008(2) -0.001(2) C7 0.027(3) 0.027(3) 0.022(3) 0.006(2) 0.010(2) 0.000(2) C8 0.026(3) 0.021(3) 0.023(3) 0.000(2) 0.005(2) 0.001(2) C9 0.021(2) 0.016(2) 0.024(3) 0.0004(19) 0.002(2) 0.0007(19) C10 0.023(3) 0.016(2) 0.019(2) -0.0010(19) 0.002(2) -0.0022(19) O11 0.037(2) 0.0139(17) 0.0252(19) 0.0010(14) 0.0126(16) 0.0003(15) O12 0.031(2) 0.0156(17) 0.0219(18) 0.0017(14) 0.0080(15) 0.0013(14) C13 0.025(3) 0.017(3) 0.021(3) 0.0004(19) 0.003(2) 0.0013(19) O14 0.038(2) 0.0177(18) 0.0218(19) -0.0015(14) 0.0098(16) 0.0014(15) O15 0.041(2) 0.019(2) 0.026(2) -0.0054(15) 0.0086(17) -0.0035(16) O16 0.029(2) 0.029(2) 0.035(2) -0.0093(17) 0.0034(17) 0.0023(16) O17 0.038(2) 0.023(2) 0.037(2) 0.0040(17) 0.0188(18) 0.0017(16) O18 0.030(2) 0.024(2) 0.036(2) 0.0010(16) 0.0031(17) -0.0007(16) O19 0.035(2) 0.0163(18) 0.034(2) -0.0015(15) 0.0127(17) 0.0010(15) O20 0.041(2) 0.034(2) 0.035(2) -0.0032(18) 0.0088(19) 0.0005(18) C21 0.023(3) 0.047(3) 0.023(3) -0.015(2) -0.001(2) 0.009(2) C22 0.021(3) 0.025(3) 0.050(4) 0.015(3) 0.001(2) 0.000(2) C23 0.023(3) 0.046(4) 0.027(3) -0.012(3) -0.003(2) 0.010(2) C24 0.031(3) 0.039(4) 0.056(4) -0.006(3) -0.002(3) -0.004(3) C25 0.026(3) 0.030(3) 0.064(5) 0.003(3) -0.001(3) -0.001(2) C26 0.025(3) 0.062(4) 0.026(3) 0.012(3) 0.004(2) -0.002(3) C27 0.025(3) 0.051(4) 0.050(4) -0.031(3) -0.010(3) 0.011(3) C28 0.022(3) 0.022(3) 0.058(4) 0.013(3) -0.009(3) -0.005(2) C29 0.030(3) 0.021(2) 0.049(3) -0.015(2) -0.016(2) 0.007(2) O30 0.053(3) 0.031(2) 0.051(3) -0.003(2) 0.009(2) -0.004(2) O31 0.049(3) 0.041(3) 0.049(3) 0.010(2) 0.012(2) -0.001(2) C32 0.029(3) 0.038(4) 0.047(4) -0.008(3) 0.005(3) 0.002(3) O33 0.046(3) 0.053(3) 0.030(2) -0.009(2) 0.002(2) 0.013(2) O34 0.049(3) 0.032(3) 0.051(3) -0.009(2) 0.010(2) -0.002(2) O35 0.038(2) 0.024(2) 0.024(2) -0.0038(15) 0.0063(17) 0.0033(16) _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 Mn O16 2.159(4) . ? Mn O18 2.165(4) . ? Mn O19 2.196(4) . ? Mn O15 2.196(4) . ? Mn O17 2.197(4) . ? Mn O12 2.246(4) 2_545 ? O1 C2 1.374(6) . ? O1 C9 1.384(6) . ? C2 C3 1.371(7) . ? C2 C10 1.483(7) . ? C3 C4 1.452(7) . ? C3 C13 1.486(7) . ? C4 C9 1.390(7) . ? C4 C5 1.410(7) . ? C5 C6 1.370(8) . ? C5 H5 0.9500 . ? C6 C7 1.409(8) . ? C6 H6 0.9500 . ? C7 C8 1.385(7) . ? C7 H7 0.9500 . ? C8 C9 1.378(7) . ? C8 H8 0.9500 . ? C10 O12 1.255(6) . ? C10 O11 1.265(6) . ? O12 Mn 2.246(4) 2 ? C13 O15 1.232(6) . ? C13 O14 1.303(6) . ? O14 H14 1.0002 . ? O16 H16A 0.9016 . ? O16 H16B 0.9047 . ? O17 H17A 1.0014 . ? O17 H17B 1.0120 . ? O18 H18A 0.9176 . ? O18 H18B 0.9678 . ? O19 H19A 0.9665 . ? O19 H19B 0.8893 . ? O20 C21 1.368(7) . ? O20 C28 1.378(7) . ? C21 C22 1.383(9) . ? C21 C29 1.515(9) . ? C22 C32 1.452(9) . ? C22 C23 1.493(8) . ? C23 C24 1.358(10) . ? C23 C28 1.374(9) . ? C24 C25 1.321(10) . ? C24 H24 0.9500 . ? C25 C26 1.365(10) . ? C25 H25 0.9500 . ? C26 C27 1.400(10) . ? C26 H26 0.9500 . ? C27 C28 1.455(10) . ? C27 H27 0.9500 . ? C29 O30 1.238(7) . ? C29 O31 1.264(8) . ? C32 O34 1.260(8) . ? C32 O33 1.253(8) . ? O33 H33 0.9822 . ? O35 H35A 0.9497 . ? O35 H35B 0.9140 . ? 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 O16 Mn O18 169.66(16) . . ? O16 Mn O19 101.26(16) . . ? O18 Mn O19 88.41(15) . . ? O16 Mn O15 87.78(15) . . ? O18 Mn O15 90.78(15) . . ? O19 Mn O15 77.51(14) . . ? O16 Mn O17 86.45(16) . . ? O18 Mn O17 84.07(16) . . ? O19 Mn O17 171.88(16) . . ? O15 Mn O17 105.59(15) . . ? O16 Mn O12 85.90(14) . 2_545 ? O18 Mn O12 98.16(15) . 2_545 ? O19 Mn O12 88.38(13) . 2_545 ? O15 Mn O12 163.10(14) . 2_545 ? O17 Mn O12 89.65(14) . 2_545 ? C2 O1 C9 106.6(4) . . ? C3 C2 O1 111.1(4) . . ? C3 C2 C10 133.8(5) . . ? O1 C2 C10 115.0(4) . . ? C2 C3 C4 106.4(4) . . ? C2 C3 C13 129.2(5) . . ? C4 C3 C13 124.4(4) . . ? C9 C4 C5 118.7(5) . . ? C9 C4 C3 105.5(4) . . ? C5 C4 C3 135.8(5) . . ? C6 C5 C4 117.3(5) . . ? C6 C5 H5 121.4 . . ? C4 C5 H5 121.4 . . ? C5 C6 C7 122.4(5) . . ? C5 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C8 C7 C6 121.3(5) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C9 C8 C7 115.3(5) . . ? C9 C8 H8 122.3 . . ? C7 C8 H8 122.3 . . ? C8 C9 O1 124.5(5) . . ? C8 C9 C4 125.1(5) . . ? O1 C9 C4 110.4(4) . . ? O12 C10 O11 124.9(4) . . ? O12 C10 C2 118.8(4) . . ? O11 C10 C2 116.3(4) . . ? C10 O12 Mn 127.1(3) . 2 ? O15 C13 O14 120.9(5) . . ? O15 C13 C3 118.7(5) . . ? O14 C13 C3 120.4(4) . . ? C13 O14 H14 112.8 . . ? C13 O15 Mn 138.6(4) . . ? Mn O16 H16A 121.3 . . ? Mn O16 H16B 114.7 . . ? H16A O16 H16B 108.6 . . ? Mn O17 H17A 116.9 . . ? Mn O17 H17B 127.2 . . ? H17A O17 H17B 113.5 . . ? Mn O18 H18A 122.5 . . ? Mn O18 H18B 93.6 . . ? H18A O18 H18B 108.9 . . ? Mn O19 H19A 109.3 . . ? Mn O19 H19B 102.8 . . ? H19A O19 H19B 106.1 . . ? C21 O20 C28 102.8(5) . . ? O20 C21 C22 114.6(6) . . ? O20 C21 C29 113.2(5) . . ? C22 C21 C29 132.2(5) . . ? C21 C22 C32 129.8(6) . . ? C21 C22 C23 104.0(5) . . ? C32 C22 C23 126.2(5) . . ? C24 C23 C28 120.7(6) . . ? C24 C23 C22 135.9(6) . . ? C28 C23 C22 103.4(5) . . ? C25 C24 C23 118.2(7) . . ? C25 C24 H24 120.9 . . ? C23 C24 H24 120.9 . . ? C24 C25 C26 124.4(7) . . ? C24 C25 H25 117.8 . . ? C26 C25 H25 117.8 . . ? C25 C26 C27 121.5(6) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C26 C27 C28 112.8(5) . . ? C26 C27 H27 123.6 . . ? C28 C27 H27 123.6 . . ? C23 C28 O20 115.2(6) . . ? C23 C28 C27 122.4(6) . . ? O20 C28 C27 122.4(6) . . ? O30 C29 O31 123.0(6) . . ? O30 C29 C21 119.9(6) . . ? O31 C29 C21 117.1(5) . . ? O34 C32 O33 124.8(6) . . ? O34 C32 C22 116.1(6) . . ? O33 C32 C22 119.1(6) . . ? C32 O33 H33 138.6 . . ? H35A O35 H35B 115.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H14 O11 1.00 1.49 2.481(5) 171 . O16 H16A O34 0.90 1.86 2.760(6) 180 1_655 O16 H16B O30 0.90 1.96 2.866(6) 180 2_545 O17 H17B O35 1.01 1.78 2.781(6) 169 4_665 O17 H17A O20 1.00 2.18 3.103(6) 153 4_665 O18 H18B O33 0.97 1.96 2.820(6) 146 . O18 H18A O35 0.92 1.85 2.765(6) 174 4_565 O19 H19B O34 0.89 1.93 2.789(6) 162 . O19 H19A O11 0.97 1.85 2.656(5) 139 2_545 O33 H33 O31 0.98 1.62 2.433(7) 136 . O35 H35B O30 0.91 1.88 2.765(6) 162 3_566 O35 H35A O12 0.95 1.95 2.884(5) 167 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.477 _refine_diff_density_min -0.723 _refine_diff_density_rms 0.138 #=====================END================================= data_14 _database_code_depnum_ccdc_archive 'CCDC 775263' #TrackingRef '- ti7-19.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 Ag N2, C10 H5 O5, H2 O' _chemical_formula_sum 'C20 H15 Ag N2 O6' _chemical_formula_weight 487.21 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' _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 7.9192(2) _cell_length_b 9.8162(2) _cell_length_c 12.2465(4) _cell_angle_alpha 71.9123(15) _cell_angle_beta 76.5751(12) _cell_angle_gamma 79.4170(14) _cell_volume 873.79(4) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3559 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.852 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 1.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7956 _exptl_absorpt_correction_T_max 0.8896 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13146 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3790 _reflns_number_gt 3406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+0.8473P] 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 3790 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.39374(3) 0.86363(2) 0.036758(17) 0.01687(8) Uani 1 1 d . . . O1 O 0.1769(2) -0.0212(2) 0.56327(15) 0.0162(4) Uani 1 1 d . . . C2 C 0.2416(3) -0.0883(3) 0.4761(2) 0.0152(5) Uani 1 1 d . . . C3 C 0.3513(3) -0.0078(3) 0.3856(2) 0.0149(5) Uani 1 1 d . . . C4 C 0.3598(3) 0.1201(3) 0.4183(2) 0.0151(5) Uani 1 1 d . . . C5 C 0.4491(4) 0.2427(3) 0.3683(2) 0.0180(5) Uani 1 1 d . . . H5 H 0.5266 0.2550 0.2950 0.022 Uiso 1 1 calc R . . C6 C 0.4210(4) 0.3443(3) 0.4290(3) 0.0212(6) Uani 1 1 d . . . H6 H 0.4809 0.4275 0.3967 0.025 Uiso 1 1 calc R . . C7 C 0.3065(4) 0.3284(3) 0.5369(2) 0.0207(6) Uani 1 1 d . . . H7 H 0.2886 0.4020 0.5752 0.025 Uiso 1 1 calc R . . C8 C 0.2185(4) 0.2075(3) 0.5893(2) 0.0186(5) Uani 1 1 d . . . H8 H 0.1416 0.1950 0.6629 0.022 Uiso 1 1 calc R . . C9 C 0.2502(3) 0.1061(3) 0.5269(2) 0.0153(5) Uani 1 1 d . . . C10 C 0.1818(4) -0.2332(3) 0.5028(2) 0.0192(6) Uani 1 1 d . . . O11 O 0.2289(3) -0.2951(2) 0.41962(17) 0.0239(4) Uani 1 1 d . . . O12 O 0.0949(3) -0.2846(2) 0.59899(17) 0.0248(4) Uani 1 1 d . . . C13 C 0.4464(4) -0.0376(3) 0.2735(2) 0.0173(5) Uani 1 1 d . . . O14 O 0.4271(3) -0.1579(2) 0.25610(16) 0.0211(4) Uani 1 1 d . . . H14 H 0.3665 -0.2072 0.3161 0.032 Uiso 1 1 calc R . . O15 O 0.5364(3) 0.0512(2) 0.20139(16) 0.0221(4) Uani 1 1 d . . . N16 N 0.5778(3) 0.6705(2) 0.04089(19) 0.0136(4) Uani 1 1 d . . . C17 C 0.6277(3) 0.5852(3) 0.1401(2) 0.0163(5) Uani 1 1 d . . . H17 H 0.5826 0.6126 0.2102 0.020 Uiso 1 1 calc R . . C18 C 0.7420(3) 0.4589(3) 0.1450(2) 0.0146(5) Uani 1 1 d . . . H18 H 0.7746 0.4025 0.2171 0.018 Uiso 1 1 calc R . . C19 C 0.8088(3) 0.4152(3) 0.0437(2) 0.0127(5) Uani 1 1 d . . . C20 C 0.7575(3) 0.5050(3) -0.0601(2) 0.0143(5) Uani 1 1 d . . . H20 H 0.7999 0.4804 -0.1316 0.017 Uiso 1 1 calc R . . C21 C 0.6443(3) 0.6301(3) -0.0572(2) 0.0162(5) Uani 1 1 d . . . H21 H 0.6121 0.6904 -0.1283 0.019 Uiso 1 1 calc R . . C22 C 0.9333(3) 0.2811(3) 0.0439(2) 0.0130(5) Uani 1 1 d . . . C23 C 0.9683(3) 0.1814(3) 0.1483(2) 0.0162(5) Uani 1 1 d . . . H23 H 0.9076 0.1951 0.2214 0.019 Uiso 1 1 calc R . . C24 C 1.0919(3) 0.0628(3) 0.1443(2) 0.0164(5) Uani 1 1 d . . . H24 H 1.1135 -0.0042 0.2159 0.020 Uiso 1 1 calc R . . N25 N 1.1834(3) 0.0376(2) 0.04329(19) 0.0141(4) Uani 1 1 d . . . C26 C 1.0228(3) 0.2516(3) -0.0602(2) 0.0146(5) Uani 1 1 d . . . H26 H 0.9990 0.3138 -0.1331 0.018 Uiso 1 1 calc R . . C27 C 1.1462(3) 0.1316(3) -0.0571(2) 0.0147(5) Uani 1 1 d . . . H27 H 1.2075 0.1147 -0.1291 0.018 Uiso 1 1 calc R . . O28 O 0.9361(3) 1.4560(2) -0.31400(17) 0.0229(4) Uani 1 1 d . . . H28A H 0.9729 1.5421 -0.3569 0.034 Uiso 1 1 d . . . H28B H 0.8784 1.4339 -0.3659 0.034 Uiso 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 Ag 0.01672(12) 0.01174(11) 0.02081(12) -0.00581(8) -0.00489(8) 0.00555(7) O1 0.0170(9) 0.0160(9) 0.0154(9) -0.0061(7) -0.0008(7) -0.0013(7) C2 0.0158(13) 0.0166(13) 0.0151(12) -0.0077(10) -0.0062(10) 0.0035(10) C3 0.0126(12) 0.0169(13) 0.0153(12) -0.0053(10) -0.0058(10) 0.0036(10) C4 0.0138(12) 0.0146(12) 0.0162(12) -0.0043(10) -0.0065(10) 0.0042(10) C5 0.0172(13) 0.0178(13) 0.0167(12) -0.0013(10) -0.0051(10) 0.0001(10) C6 0.0222(14) 0.0160(13) 0.0256(14) -0.0040(11) -0.0083(12) -0.0011(11) C7 0.0222(14) 0.0178(14) 0.0263(14) -0.0106(12) -0.0130(12) 0.0053(11) C8 0.0198(14) 0.0197(14) 0.0166(13) -0.0080(11) -0.0044(11) 0.0033(11) C9 0.0150(12) 0.0149(12) 0.0161(12) -0.0035(10) -0.0056(10) 0.0000(10) C10 0.0199(14) 0.0196(14) 0.0205(14) -0.0050(11) -0.0108(11) -0.0002(11) O11 0.0304(11) 0.0202(10) 0.0256(10) -0.0110(9) -0.0074(9) -0.0034(9) O12 0.0301(11) 0.0231(11) 0.0213(10) -0.0038(8) -0.0035(9) -0.0096(9) C13 0.0178(13) 0.0185(13) 0.0154(12) -0.0068(11) -0.0076(10) 0.0079(11) O14 0.0267(11) 0.0201(10) 0.0167(9) -0.0089(8) -0.0052(8) 0.0041(8) O15 0.0236(10) 0.0223(10) 0.0157(9) -0.0045(8) 0.0000(8) 0.0027(8) N16 0.0131(10) 0.0093(10) 0.0181(11) -0.0050(8) -0.0042(8) 0.0029(8) C17 0.0170(13) 0.0151(13) 0.0168(12) -0.0067(10) -0.0021(10) 0.0003(10) C18 0.0161(12) 0.0130(12) 0.0138(12) -0.0034(10) -0.0030(10) 0.0005(10) C19 0.0113(12) 0.0107(12) 0.0168(12) -0.0033(10) -0.0032(10) -0.0032(9) C20 0.0144(12) 0.0133(12) 0.0147(12) -0.0056(10) -0.0016(10) 0.0009(10) C21 0.0164(13) 0.0149(13) 0.0168(12) -0.0040(10) -0.0055(10) 0.0016(10) C22 0.0121(12) 0.0115(12) 0.0165(12) -0.0039(10) -0.0042(10) -0.0019(9) C23 0.0165(13) 0.0148(13) 0.0161(12) -0.0046(10) -0.0032(10) 0.0020(10) C24 0.0161(13) 0.0147(13) 0.0166(12) -0.0033(10) -0.0048(10) 0.0031(10) N25 0.0135(10) 0.0108(10) 0.0179(11) -0.0055(9) -0.0046(8) 0.0034(8) C26 0.0140(12) 0.0131(12) 0.0178(12) -0.0047(10) -0.0061(10) 0.0005(10) C27 0.0137(12) 0.0139(12) 0.0162(12) -0.0057(10) -0.0026(10) 0.0017(10) O28 0.0311(11) 0.0198(10) 0.0176(9) -0.0049(8) -0.0061(8) -0.0013(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N25 2.162(2) 1_465 ? Ag N16 2.163(2) . ? Ag Ag 3.2039(4) 2_675 ? O1 C9 1.378(3) . ? O1 C2 1.377(3) . ? C2 C3 1.367(4) . ? C2 C10 1.496(4) . ? C3 C4 1.449(4) . ? C3 C13 1.491(4) . ? C4 C9 1.392(4) . ? C4 C5 1.406(4) . ? C5 C6 1.378(4) . ? C5 H5 0.9500 . ? C6 C7 1.401(4) . ? C6 H6 0.9500 . ? C7 C8 1.389(4) . ? C7 H7 0.9500 . ? C8 C9 1.388(4) . ? C8 H8 0.9500 . ? C10 O12 1.224(3) . ? C10 O11 1.293(3) . ? C13 O15 1.227(3) . ? C13 O14 1.304(3) . ? O14 H14 0.8400 . ? N16 C21 1.342(3) . ? N16 C17 1.343(3) . ? C17 C18 1.388(4) . ? C17 H17 0.9500 . ? C18 C19 1.395(4) . ? C18 H18 0.9500 . ? C19 C20 1.404(4) . ? C19 C22 1.492(4) . ? C20 C21 1.385(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C26 1.396(4) . ? C22 C23 1.399(4) . ? C23 C24 1.382(4) . ? C23 H23 0.9500 . ? C24 N25 1.350(3) . ? C24 H24 0.9500 . ? N25 C27 1.347(3) . ? N25 Ag 2.162(2) 1_645 ? C26 C27 1.382(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? O28 H28A 0.9051 . ? O28 H28B 0.9573 . ? 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 N25 Ag N16 172.39(8) 1_465 . ? N25 Ag Ag 78.56(6) 1_465 2_675 ? N16 Ag Ag 108.94(6) . 2_675 ? C9 O1 C2 106.04(19) . . ? C3 C2 O1 111.6(2) . . ? C3 C2 C10 134.6(2) . . ? O1 C2 C10 113.7(2) . . ? C2 C3 C4 106.0(2) . . ? C2 C3 C13 129.6(2) . . ? C4 C3 C13 124.4(2) . . ? C9 C4 C5 118.6(2) . . ? C9 C4 C3 105.6(2) . . ? C5 C4 C3 135.8(2) . . ? C6 C5 C4 118.0(3) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? C5 C6 C7 121.8(3) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C8 C7 C6 121.4(2) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C7 C8 C9 115.6(2) . . ? C7 C8 H8 122.2 . . ? C9 C8 H8 122.2 . . ? O1 C9 C8 124.9(2) . . ? O1 C9 C4 110.7(2) . . ? C8 C9 C4 124.4(2) . . ? O12 C10 O11 124.9(3) . . ? O12 C10 C2 119.4(2) . . ? O11 C10 C2 115.7(2) . . ? O15 C13 O14 122.8(2) . . ? O15 C13 C3 119.6(2) . . ? O14 C13 C3 117.6(2) . . ? C13 O14 H14 109.5 . . ? C21 N16 C17 117.3(2) . . ? C21 N16 Ag 120.42(17) . . ? C17 N16 Ag 122.23(17) . . ? N16 C17 C18 123.0(2) . . ? N16 C17 H17 118.5 . . ? C18 C17 H17 118.5 . . ? C17 C18 C19 119.8(2) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C20 117.1(2) . . ? C18 C19 C22 121.9(2) . . ? C20 C19 C22 121.0(2) . . ? C21 C20 C19 119.2(2) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? N16 C21 C20 123.5(2) . . ? N16 C21 H21 118.2 . . ? C20 C21 H21 118.2 . . ? C26 C22 C23 117.2(2) . . ? C26 C22 C19 121.3(2) . . ? C23 C22 C19 121.5(2) . . ? C24 C23 C22 119.5(2) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? N25 C24 C23 123.2(2) . . ? N25 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? C27 N25 C24 117.2(2) . . ? C27 N25 Ag 119.52(17) . 1_645 ? C24 N25 Ag 123.13(17) . 1_645 ? C27 C26 C22 119.9(2) . . ? C27 C26 H26 120.1 . . ? C22 C26 H26 120.1 . . ? N25 C27 C26 123.0(2) . . ? N25 C27 H27 118.5 . . ? C26 C27 H27 118.5 . . ? H28A O28 H28B 102.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H14 O11 0.84 1.60 2.435(3) 172 . O28 H28A O12 0.91 1.98 2.841(3) 159 1_674 O28 H28B O11 0.96 2.06 2.947(3) 153 2_665 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.414 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.097 #===========================END=============================