# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '- C2DT30085K_ccdc_808461_842877_cif.txt' _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 loop_ _publ_author_address ; School of Chemistry and Environment South China Normal University Guangzhou 510006 P.R. China ; #TrackingRef '- cifs.cif' #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Hong Deng School of Chemistry and Environment South China Nomal University Guangzhou 510006 P. R. China ; _publ_contact_author_email dh@scnu.edu.cn _publ_contact_author_fax '86 20 33381880' _publ_contact_author_phone '86 20 33381880' _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as supplmentary data for a manuscript submitted to Dalton Trans. Deng Hong ; _publ_requested_coeditor_name ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_contact_author_name 'Hong Deng' _publ_author_name 'Hong Deng' data_1 #TrackingRef '- C2DT30085K_ccdc_808461_842877_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 808461' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H34 Gd2 N16 O16, 4(H2 O)' _chemical_formula_sum 'C32 H42 Gd2 N16 O20' _chemical_formula_weight 1285.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.162(2) _cell_length_b 11.9463(12) _cell_length_c 12.1414(12) _cell_angle_alpha 117.0890(10) _cell_angle_beta 98.242(2) _cell_angle_gamma 99.395(2) _cell_volume 1130.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3975 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 634.0 _exptl_absorpt_coefficient_mu 3.003 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4663 _exptl_absorpt_correction_T_max 0.4871 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5793 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.20 _reflns_number_total 3975 _reflns_number_gt 3756 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0239P)^2^+0.5659P] 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 3975 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0492 _refine_ls_wR_factor_gt 0.0482 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7893(3) 0.6293(3) 0.3297(3) 0.0291(6) Uani 1 1 d . . . C2 C 0.8939(3) 0.5430(3) 0.2869(3) 0.0274(6) Uani 1 1 d . . . C3 C 0.9997(4) 0.5322(3) 0.3736(3) 0.0340(7) Uani 1 1 d . . . H3 H 1.0056 0.5790 0.4605 0.041 Uiso 1 1 calc R . . C4 C 1.0956(4) 0.4528(3) 0.3316(3) 0.0390(8) Uani 1 1 d . . . H8 H 1.1641 0.4443 0.3899 0.047 Uiso 1 1 calc R . . C5 C 1.0906(4) 0.3855(3) 0.2031(3) 0.0377(7) Uani 1 1 d . . . H5 H 1.1576 0.3338 0.1756 0.045 Uiso 1 1 calc R . . C6 C 0.9853(3) 0.3947(3) 0.1143(3) 0.0287(6) Uani 1 1 d . . . C7 C 0.8865(3) 0.4733(3) 0.1582(3) 0.0286(6) Uani 1 1 d . . . H7 H 0.8145 0.4788 0.0998 0.034 Uiso 1 1 calc R . . C8 C 0.9772(3) 0.3242(3) -0.0224(3) 0.0295(6) Uani 1 1 d . . . C9 C 0.4094(3) 0.9993(3) 0.3107(3) 0.0272(6) Uani 1 1 d . . . C10 C 0.3485(3) 0.9861(3) 0.1827(3) 0.0265(6) Uani 1 1 d . . . C11 C 0.2542(4) 1.0625(3) 0.1720(3) 0.0365(7) Uani 1 1 d . . . H11 H 0.2287 1.1215 0.2438 0.044 Uiso 1 1 calc R . . C12 C 0.1983(4) 1.0502(3) 0.0532(3) 0.0446(9) Uani 1 1 d . . . H12 H 0.1369 1.1026 0.0460 0.053 Uiso 1 1 calc R . . C13 C 0.2333(4) 0.9609(3) -0.0539(3) 0.0402(8) Uani 1 1 d . . . H13 H 0.1950 0.9529 -0.1330 0.048 Uiso 1 1 calc R . . C14 C 0.3257(3) 0.8825(3) -0.0442(3) 0.0289(6) Uani 1 1 d . . . C15 C 0.3827(3) 0.8960(3) 0.0748(3) 0.0269(6) Uani 1 1 d . . . H15 H 0.4445 0.8440 0.0820 0.032 Uiso 1 1 calc R . . C16 C 0.3590(3) 0.7870(3) -0.1599(3) 0.0291(6) Uani 1 1 d . . . Gd1 Gd 0.574434(15) 0.786564(13) 0.379689(12) 0.02472(6) Uani 1 1 d . . . N1 N 0.3088(3) 0.7670(3) -0.2766(2) 0.0385(6) Uani 1 1 d . . . N2 N 0.3677(4) 0.6728(3) -0.3536(2) 0.0431(7) Uani 1 1 d . . . N3 N 0.4518(3) 0.6355(3) -0.2884(2) 0.0392(6) Uani 1 1 d . . . N4 N 0.4466(3) 0.7065(2) -0.1673(2) 0.0330(6) Uani 1 1 d . . . H4 H 0.4928 0.7010 -0.1038 0.040 Uiso 1 1 calc R . . N5 N 0.8611(3) 0.3082(3) -0.1130(2) 0.0343(6) Uani 1 1 d . . . N6 N 0.8960(3) 0.2382(3) -0.2235(2) 0.0377(6) Uani 1 1 d . . . N7 N 1.0276(3) 0.2134(3) -0.2009(3) 0.0408(7) Uani 1 1 d . . . N8 N 1.0820(3) 0.2673(3) -0.0733(2) 0.0382(6) Uani 1 1 d . . . O7 O 0.4956(3) 0.9297(2) 0.31653(19) 0.0375(5) Uani 1 1 d . . . O8 O 0.3717(3) 1.0797(2) 0.40448(18) 0.0393(5) Uani 1 1 d . . . O9 O 0.6789(2) 0.6171(2) 0.24605(19) 0.0349(5) Uani 1 1 d . . . O10 O 0.80968(10) 0.71108(9) 0.44510(8) 0.0397(5) Uani 1 1 d . . . O1W O 0.88852(10) 0.14360(9) 0.40448(8) 0.0661(8) Uani 1 1 d R . . H1A H 0.9833 0.1806 0.4363 0.099 Uiso 1 1 d R . . H1B H 0.8556 0.1839 0.3684 0.099 Uiso 1 1 d R . . O2W O 0.39376(10) 0.36216(9) 1.01390(8) 0.0416(5) Uani 1 1 d R . . H2A H 0.3006 0.3218 0.9797 0.062 Uiso 1 1 d R . . H2B H 0.4332 0.3610 0.9551 0.062 Uiso 1 1 d R . . O3W O 0.79121(10) 0.90099(9) 0.35761(8) 0.0531(7) Uani 1 1 d R . . H3A H 0.8093 0.9773 0.3748 0.080 Uiso 1 1 d R . . H3B H 0.8482 0.8637 0.3162 0.080 Uiso 1 1 d R . . O4W O 0.40940(10) 0.64287(9) 0.16574(8) 0.0356(5) Uani 1 1 d R . . H4A H 0.3283 0.6545 0.1401 0.053 Uiso 1 1 d R . . H4B H 0.4042 0.5654 0.1363 0.053 Uiso 1 1 d R . . O5W O 0.32376(10) 0.79612(9) 0.42244(8) 0.0453(6) Uani 1 1 d R . . H5A H 0.2532 0.7819 0.3634 0.068 Uiso 1 1 d R . . H5B H 0.2973 0.8252 0.4896 0.068 Uiso 1 1 d R . . O6W O 0.47883(10) 0.61102(9) 0.41712(8) 0.0478(6) Uani 1 1 d R . . H6A H 0.4318 0.6238 0.4722 0.072 Uiso 1 1 d R . . H6B H 0.4939 0.5387 0.3870 0.072 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 C1 0.0299(16) 0.0256(15) 0.0312(16) 0.0129(14) 0.0091(13) 0.0070(12) C2 0.0272(15) 0.0236(15) 0.0311(15) 0.0121(13) 0.0093(12) 0.0080(12) C3 0.0389(18) 0.0322(17) 0.0298(16) 0.0137(14) 0.0084(14) 0.0115(14) C4 0.0370(18) 0.0436(19) 0.0375(18) 0.0189(16) 0.0051(14) 0.0194(15) C5 0.0353(18) 0.0355(18) 0.0415(18) 0.0145(15) 0.0108(15) 0.0196(15) C6 0.0238(15) 0.0260(15) 0.0321(16) 0.0106(13) 0.0070(12) 0.0071(12) C7 0.0250(15) 0.0274(15) 0.0309(15) 0.0120(13) 0.0057(12) 0.0090(12) C8 0.0243(15) 0.0265(15) 0.0334(16) 0.0111(13) 0.0065(13) 0.0072(12) C9 0.0276(15) 0.0239(15) 0.0228(14) 0.0064(12) 0.0041(12) 0.0059(12) C10 0.0269(15) 0.0234(15) 0.0247(14) 0.0084(12) 0.0067(12) 0.0060(12) C11 0.0453(19) 0.0312(17) 0.0281(16) 0.0078(14) 0.0092(14) 0.0181(15) C12 0.057(2) 0.042(2) 0.0370(18) 0.0165(16) 0.0071(16) 0.0296(17) C13 0.050(2) 0.044(2) 0.0284(16) 0.0182(16) 0.0060(15) 0.0200(16) C14 0.0316(16) 0.0268(15) 0.0247(14) 0.0095(13) 0.0070(12) 0.0080(13) C15 0.0281(15) 0.0263(15) 0.0255(14) 0.0115(13) 0.0066(12) 0.0086(12) C16 0.0313(16) 0.0278(16) 0.0262(15) 0.0118(13) 0.0077(12) 0.0065(13) Gd1 0.02746(9) 0.02596(9) 0.01833(8) 0.00712(6) 0.00671(6) 0.01157(6) N1 0.0524(17) 0.0355(15) 0.0243(13) 0.0108(12) 0.0091(12) 0.0156(13) N2 0.0616(19) 0.0404(16) 0.0265(14) 0.0133(13) 0.0159(13) 0.0168(14) N3 0.0524(18) 0.0375(15) 0.0280(14) 0.0122(13) 0.0174(13) 0.0180(13) N4 0.0396(15) 0.0351(14) 0.0234(12) 0.0119(11) 0.0090(11) 0.0142(12) N5 0.0285(14) 0.0343(15) 0.0323(14) 0.0095(12) 0.0074(11) 0.0094(11) N6 0.0309(15) 0.0382(15) 0.0339(14) 0.0095(13) 0.0078(12) 0.0084(12) N7 0.0327(15) 0.0454(17) 0.0359(15) 0.0109(13) 0.0108(12) 0.0148(13) N8 0.0329(15) 0.0416(16) 0.0347(14) 0.0108(13) 0.0110(12) 0.0177(13) O7 0.0452(13) 0.0424(13) 0.0308(11) 0.0186(10) 0.0101(10) 0.0233(11) O8 0.0473(14) 0.0411(13) 0.0209(10) 0.0052(10) 0.0073(10) 0.0220(11) O9 0.0326(12) 0.0371(12) 0.0296(11) 0.0093(10) 0.0069(9) 0.0186(10) O10 0.0436(13) 0.0399(13) 0.0283(11) 0.0084(10) 0.0067(10) 0.0201(11) O1W 0.0663(19) 0.0460(16) 0.0754(19) 0.0348(15) -0.0146(15) 0.0005(13) O2W 0.0348(13) 0.0528(15) 0.0340(12) 0.0194(11) 0.0062(10) 0.0110(11) O3W 0.0513(16) 0.0386(14) 0.0838(19) 0.0310(14) 0.0410(14) 0.0233(12) O4W 0.0297(11) 0.0337(12) 0.0314(11) 0.0067(10) 0.0006(9) 0.0127(9) O5W 0.0354(13) 0.0643(16) 0.0365(12) 0.0207(12) 0.0151(10) 0.0210(12) O6W 0.0641(16) 0.0385(13) 0.0574(15) 0.0261(12) 0.0400(13) 0.0255(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 C1 O10 1.254(3) . ? C1 O9 1.264(3) . ? C1 C2 1.493(4) . ? C2 C7 1.380(4) . ? C2 C3 1.392(4) . ? C3 C4 1.376(4) . ? C3 H3 0.9300 . ? C4 C5 1.381(4) . ? C4 H8 0.9300 . ? C5 C6 1.396(4) . ? C5 H5 0.9300 . ? C6 C7 1.395(4) . ? C6 C8 1.463(4) . ? C7 H7 0.9300 . ? C8 N8 1.329(4) . ? C8 N5 1.336(4) . ? C9 O8 1.251(3) . ? C9 O7 1.254(3) . ? C9 C10 1.499(4) . ? C10 C15 1.384(4) . ? C10 C11 1.389(4) . ? C11 C12 1.391(4) . ? C11 H11 0.9300 . ? C12 C13 1.379(5) . ? C12 H12 0.9300 . ? C13 C14 1.392(4) . ? C13 H13 0.9300 . ? C14 C15 1.389(4) . ? C14 C16 1.464(4) . ? C15 H15 0.9300 . ? C16 N1 1.321(4) . ? C16 N4 1.331(4) . ? Gd1 O8 2.2852(19) 2_676 ? Gd1 O7 2.339(2) . ? Gd1 O3W 2.3420 . ? Gd1 O9 2.3938(19) . ? Gd1 O6W 2.3988 . ? Gd1 O5W 2.4353 . ? Gd1 O4W 2.4385 . ? Gd1 O10 2.6240(9) . ? N1 N2 1.348(4) . ? N2 N3 1.296(4) . ? N3 N4 1.335(3) . ? N4 H4 0.8600 . ? N5 N6 1.338(4) . ? N6 N7 1.308(4) . ? N7 N8 1.353(4) . ? O8 Gd1 2.2852(19) 2_676 ? O1W H1A 0.8495 . ? O1W H1B 0.8468 . ? O2W H2A 0.8460 . ? O2W H2B 0.8412 . ? O3W H3A 0.8179 . ? O3W H3B 0.8191 . ? O4W H4A 0.8214 . ? O4W H4B 0.8159 . ? O5W H5A 0.8246 . ? O5W H5B 0.8194 . ? O6W H6A 0.8164 . ? O6W H6B 0.8157 . ? 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 O10 C1 O9 120.9(2) . . ? O10 C1 C2 121.1(2) . . ? O9 C1 C2 118.0(2) . . ? C7 C2 C3 119.3(3) . . ? C7 C2 C1 119.1(2) . . ? C3 C2 C1 121.6(3) . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.3(3) . . ? C3 C4 H8 119.8 . . ? C5 C4 H8 119.8 . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 118.6(3) . . ? C5 C6 C8 121.5(3) . . ? C7 C6 C8 119.9(3) . . ? C2 C7 C6 121.1(3) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? N8 C8 N5 111.0(3) . . ? N8 C8 C6 125.2(3) . . ? N5 C8 C6 123.7(3) . . ? O8 C9 O7 124.4(3) . . ? O8 C9 C10 117.8(2) . . ? O7 C9 C10 117.8(2) . . ? C15 C10 C11 119.8(3) . . ? C15 C10 C9 120.4(2) . . ? C11 C10 C9 119.8(3) . . ? C12 C11 C10 119.6(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 120.4(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 119.1(3) . . ? C13 C14 C16 119.2(3) . . ? C15 C14 C16 121.7(3) . . ? C10 C15 C14 120.7(3) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? N1 C16 N4 107.4(3) . . ? N1 C16 C14 125.7(3) . . ? N4 C16 C14 126.9(3) . . ? O8 Gd1 O7 97.96(7) 2_676 . ? O8 Gd1 O3W 93.53(7) 2_676 . ? O7 Gd1 O3W 73.12(6) . . ? O8 Gd1 O9 133.26(7) 2_676 . ? O7 Gd1 O9 121.42(7) . . ? O3W Gd1 O9 76.88(6) . . ? O8 Gd1 O6W 87.14(6) 2_676 . ? O7 Gd1 O6W 142.29(6) . . ? O3W Gd1 O6W 144.2 . . ? O9 Gd1 O6W 76.81(6) . . ? O8 Gd1 O5W 76.38(6) 2_676 . ? O7 Gd1 O5W 74.23(6) . . ? O3W Gd1 O5W 144.0 . . ? O9 Gd1 O5W 134.55(6) . . ? O6W Gd1 O5W 70.8 . . ? O8 Gd1 O4W 155.57(6) 2_676 . ? O7 Gd1 O4W 76.24(6) . . ? O3W Gd1 O4W 107.0 . . ? O9 Gd1 O4W 66.23(5) . . ? O6W Gd1 O4W 83.8 . . ? O5W Gd1 O4W 79.2 . . ? O8 Gd1 O10 81.88(6) 2_676 . ? O7 Gd1 O10 145.03(6) . . ? O3W Gd1 O10 72.00(3) . . ? O9 Gd1 O10 51.51(5) . . ? O6W Gd1 O10 72.65(3) . . ? O5W Gd1 O10 137.96(4) . . ? O4W Gd1 O10 116.59(3) . . ? C16 N1 N2 106.4(3) . . ? N3 N2 N1 110.6(2) . . ? N2 N3 N4 106.0(2) . . ? C16 N4 N3 109.6(2) . . ? C16 N4 H4 125.2 . . ? N3 N4 H4 125.2 . . ? C8 N5 N6 105.2(2) . . ? N7 N6 N5 109.6(2) . . ? N6 N7 N8 109.0(2) . . ? C8 N8 N7 105.1(2) . . ? C9 O7 Gd1 153.2(2) . . ? C9 O8 Gd1 148.46(19) . 2_676 ? C1 O9 Gd1 99.08(17) . . ? C1 O10 Gd1 88.50(14) . . ? H1A O1W H1B 105.3 . . ? H2A O2W H2B 106.7 . . ? Gd1 O3W H3A 125.6 . . ? Gd1 O3W H3B 121.9 . . ? H3A O3W H3B 111.2 . . ? Gd1 O4W H4A 123.2 . . ? Gd1 O4W H4B 116.2 . . ? H4A O4W H4B 111.2 . . ? Gd1 O5W H5A 117.6 . . ? Gd1 O5W H5B 131.3 . . ? H5A O5W H5B 109.9 . . ? Gd1 O6W H6A 119.1 . . ? Gd1 O6W H6B 128.7 . . ? H6A O6W H6B 111.8 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.639 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.072 data_4 #TrackingRef '- C2DT30085K_ccdc_808461_842877_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 808462' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H34 N16 O16 Tb2, 4(H2 O)' _chemical_formula_sum 'C32 H42 N16 O20 Tb2' _chemical_formula_weight 1288.68 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1459(18) _cell_length_b 11.9522(10) _cell_length_c 12.1423(10) _cell_angle_alpha 117.2750(10) _cell_angle_beta 98.1120(10) _cell_angle_gamma 99.4350(10) _cell_volume 1127.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3974 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 25.19 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636.0 _exptl_absorpt_coefficient_mu 3.206 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4471 _exptl_absorpt_correction_T_max 0.5019 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 5802 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.19 _reflns_number_total 3974 _reflns_number_gt 3744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0227P)^2^+0.9385P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3974 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0498 _refine_ls_wR_factor_gt 0.0489 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7891(4) 0.6297(3) -0.1689(3) 0.0292(7) Uani 1 1 d . . . C2 C 0.8942(4) 0.5432(3) -0.2121(3) 0.0271(7) Uani 1 1 d . . . C3 C 0.9999(4) 0.5327(3) -0.1260(3) 0.0316(7) Uani 1 1 d . . . C4 C 1.0962(4) 0.4527(3) -0.1688(3) 0.0385(8) Uani 1 1 d . . . C5 C 1.0898(4) 0.3857(3) -0.2976(3) 0.0361(8) Uani 1 1 d . . . C6 C 0.9855(4) 0.3949(3) -0.3855(3) 0.0282(7) Uani 1 1 d . . . C7 C 0.9757(3) 0.3241(3) -0.5229(3) 0.0282(7) Uani 1 1 d . . . C8 C 0.8865(4) 0.4734(3) -0.3413(3) 0.0274(7) Uani 1 1 d . . . C9 C 0.5901(3) 1.0012(3) 0.1877(3) 0.0266(7) Uani 1 1 d . . . C10 C 0.6519(3) 1.0143(3) 0.3156(3) 0.0251(6) Uani 1 1 d . . . C11 C 0.7458(4) 0.9377(3) 0.3260(3) 0.0360(8) Uani 1 1 d . . . C12 C 0.8018(5) 0.9494(4) 0.4440(4) 0.0445(9) Uani 1 1 d . . . C13 C 0.7672(4) 1.0389(3) 0.5526(3) 0.0380(8) Uani 1 1 d . . . C14 C 0.6740(4) 1.1174(3) 0.5430(3) 0.0264(6) Uani 1 1 d . . . C15 C 0.6157(4) 1.1031(3) 0.4240(3) 0.0253(6) Uani 1 1 d . . . C16 C 0.6407(4) 1.2126(3) 0.6593(3) 0.0276(7) Uani 1 1 d . . . N1 N 1.0820(3) 0.2672(3) -0.5746(3) 0.0374(7) Uani 1 1 d . . . N2 N 1.0271(3) 0.2139(3) -0.7017(3) 0.0395(7) Uani 1 1 d . . . N3 N 0.8961(3) 0.2386(3) -0.7243(3) 0.0367(7) Uani 1 1 d . . . N4 N 0.8608(3) 0.3091(3) -0.6126(3) 0.0332(6) Uani 1 1 d . . . N5 N 0.6913(4) 1.2323(3) 0.7760(2) 0.0371(7) Uani 1 1 d . . . N6 N 0.6319(4) 1.3263(3) 0.8536(3) 0.0425(7) Uani 1 1 d . . . N7 N 0.5476(4) 1.3639(3) 0.7889(3) 0.0383(7) Uani 1 1 d . . . N8 N 0.5522(3) 1.2934(3) 0.6668(2) 0.0313(6) Uani 1 1 d . . . H8 H 0.5058 1.2990 0.6035 0.038 Uiso 1 1 calc R . . O7 O 0.6786(3) 0.6178(2) -0.2528(2) 0.0340(5) Uani 1 1 d . . . O8 O 0.8099(3) 0.7126(2) -0.0530(2) 0.0396(6) Uani 1 1 d . . . O9 O 0.6283(3) 0.9209(2) 0.0933(2) 0.0382(6) Uani 1 1 d . . . O10 O 0.50400(11) 1.07089(9) 0.18234(9) 0.0360(5) Uani 1 1 d . . . O1W O 0.88573(11) 0.14359(9) 0.90388(9) 0.0642(8) Uani 1 1 d R . . H1A H 0.9416 0.1243 0.8522 0.096 Uiso 1 1 d R . . H1B H 0.9385 0.2151 0.9689 0.096 Uiso 1 1 d R . . O2W O 0.39406(11) 0.36203(9) 0.51361(9) 0.0394(6) Uani 1 1 d R . . H2A H 0.4287 0.3495 0.4495 0.059 Uiso 1 1 d R . . H2B H 0.2984 0.3298 0.4862 0.059 Uiso 1 1 d R . . O3W O 0.78894(11) 0.89928(9) -0.14307(9) 0.0509(7) Uani 1 1 d R . . H3B H 0.8254 0.9783 -0.1060 0.076 Uiso 1 1 d R . . H3A H 0.8463 0.8617 -0.1850 0.076 Uiso 1 1 d R . . O4W O 0.47906(11) 0.61204(9) -0.08294(9) 0.0473(7) Uani 1 1 d R . . H4B H 0.4423 0.6274 -0.0220 0.071 Uiso 1 1 d R . . H4A H 0.5036 0.5441 -0.1106 0.071 Uiso 1 1 d R . . O5W O 0.40970(11) 0.64279(9) -0.33436(9) 0.0346(5) Uani 1 1 d R . . H5A H 0.3247 0.6538 -0.3530 0.052 Uiso 1 1 d R . . H5B H 0.4031 0.5644 -0.3676 0.052 Uiso 1 1 d R . . O6W O 0.32472(11) 0.79538(9) -0.07788(9) 0.0433(6) Uani 1 1 d R . . H6A H 0.3019 0.8276 -0.0096 0.065 Uiso 1 1 d R . . H6B H 0.2512 0.7743 -0.1371 0.065 Uiso 1 1 d R . . Tb1 Tb 0.573695(16) 0.785879(13) -0.120737(12) 0.02412(6) Uani 1 1 d . . . H5 H 0.774(3) 0.886(3) 0.258(3) 0.019(8) Uiso 1 1 d . . . H9 H 0.551(4) 1.148(3) 0.412(3) 0.031(9) Uiso 1 1 d . . . H1 H 1.005(4) 0.580(3) -0.045(3) 0.023(8) Uiso 1 1 d . . . H2 H 1.165(4) 0.446(3) -0.106(4) 0.043(10) Uiso 1 1 d . . . H4 H 0.821(4) 0.484(3) -0.394(3) 0.029(9) Uiso 1 1 d . . . H7 H 0.812(5) 1.053(4) 0.638(4) 0.061(12) Uiso 1 1 d . . . H6 H 0.863(5) 0.904(4) 0.453(4) 0.056(12) Uiso 1 1 d . . . H3 H 1.148(4) 0.337(4) -0.324(4) 0.047(11) 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 C1 0.0304(17) 0.0265(17) 0.0342(18) 0.0150(15) 0.0130(15) 0.0117(14) C2 0.0286(16) 0.0209(15) 0.0309(16) 0.0111(13) 0.0093(13) 0.0074(13) C3 0.0375(19) 0.0294(18) 0.0249(17) 0.0101(15) 0.0064(15) 0.0121(15) C4 0.040(2) 0.039(2) 0.0362(19) 0.0172(17) 0.0029(16) 0.0187(17) C5 0.0356(19) 0.0331(19) 0.040(2) 0.0138(16) 0.0112(16) 0.0211(16) C6 0.0255(16) 0.0257(16) 0.0326(17) 0.0122(14) 0.0086(14) 0.0098(13) C7 0.0228(16) 0.0257(16) 0.0343(17) 0.0118(14) 0.0090(14) 0.0093(13) C8 0.0244(16) 0.0269(17) 0.0296(17) 0.0123(14) 0.0057(14) 0.0089(13) C9 0.0282(16) 0.0243(16) 0.0238(15) 0.0081(13) 0.0084(13) 0.0080(13) C10 0.0287(16) 0.0188(15) 0.0221(15) 0.0061(12) 0.0043(13) 0.0055(13) C11 0.045(2) 0.0315(19) 0.0256(17) 0.0052(15) 0.0088(16) 0.0217(16) C12 0.055(2) 0.041(2) 0.038(2) 0.0154(17) 0.0073(18) 0.031(2) C13 0.049(2) 0.040(2) 0.0252(17) 0.0154(16) 0.0039(16) 0.0194(17) C14 0.0305(17) 0.0245(16) 0.0214(15) 0.0089(13) 0.0074(13) 0.0067(13) C15 0.0283(16) 0.0223(16) 0.0238(16) 0.0089(13) 0.0076(13) 0.0095(13) C16 0.0307(17) 0.0261(16) 0.0242(16) 0.0108(13) 0.0082(13) 0.0066(14) N1 0.0344(16) 0.0386(16) 0.0351(16) 0.0109(14) 0.0117(13) 0.0187(13) N2 0.0366(16) 0.0411(17) 0.0336(16) 0.0090(14) 0.0139(13) 0.0169(14) N3 0.0282(15) 0.0382(16) 0.0336(15) 0.0095(13) 0.0081(12) 0.0083(13) N4 0.0303(15) 0.0348(16) 0.0302(15) 0.0099(13) 0.0109(12) 0.0135(12) N5 0.0533(18) 0.0340(16) 0.0226(14) 0.0113(12) 0.0088(13) 0.0164(14) N6 0.064(2) 0.0403(17) 0.0268(15) 0.0147(14) 0.0170(15) 0.0219(16) N7 0.0528(19) 0.0346(16) 0.0277(15) 0.0120(13) 0.0167(14) 0.0165(14) N8 0.0405(16) 0.0333(15) 0.0212(13) 0.0116(12) 0.0109(12) 0.0157(13) O7 0.0318(12) 0.0358(13) 0.0295(12) 0.0088(10) 0.0076(10) 0.0192(10) O8 0.0450(14) 0.0397(14) 0.0281(12) 0.0078(11) 0.0097(11) 0.0235(12) O9 0.0469(14) 0.0391(14) 0.0211(11) 0.0054(10) 0.0077(10) 0.0221(12) O10 0.0465(14) 0.0403(14) 0.0289(12) 0.0180(11) 0.0124(11) 0.0250(12) O1W 0.070(2) 0.0435(16) 0.065(2) 0.0272(15) -0.0084(16) 0.0001(15) O2W 0.0334(13) 0.0531(15) 0.0308(12) 0.0195(12) 0.0071(10) 0.0134(12) O3W 0.0484(16) 0.0357(14) 0.080(2) 0.0277(14) 0.0390(15) 0.0214(12) O4W 0.0652(18) 0.0400(14) 0.0541(16) 0.0255(13) 0.0403(14) 0.0284(13) O5W 0.0298(12) 0.0333(13) 0.0323(12) 0.0084(10) 0.0041(10) 0.0144(10) O6W 0.0376(14) 0.0599(17) 0.0338(13) 0.0197(12) 0.0150(11) 0.0212(13) Tb1 0.02945(9) 0.02460(9) 0.01712(8) 0.00671(6) 0.00794(6) 0.01327(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 C1 O8 1.258(4) . ? C1 O7 1.268(4) . ? C1 C2 1.497(4) . ? C2 C3 1.384(4) . ? C2 C8 1.383(4) . ? C3 C4 1.382(5) . ? C3 H1 0.87(3) . ? C4 C5 1.378(5) . ? C4 H2 0.96(4) . ? C5 C6 1.385(5) . ? C5 H3 0.83(4) . ? C6 C8 1.393(4) . ? C6 C7 1.465(4) . ? C7 N4 1.327(4) . ? C7 N1 1.342(4) . ? C8 H4 0.88(3) . ? C9 O10 1.252(3) . ? C9 O9 1.253(4) . ? C9 C10 1.501(4) . ? C10 C11 1.388(4) . ? C10 C15 1.388(4) . ? C11 C12 1.386(5) . ? C11 H5 0.88(3) . ? C12 C13 1.386(5) . ? C12 H6 0.87(4) . ? C13 C14 1.399(5) . ? C13 H7 0.98(4) . ? C14 C15 1.388(4) . ? C14 C16 1.464(4) . ? C15 H9 0.90(3) . ? C16 N5 1.324(4) . ? C16 N8 1.339(4) . ? N1 N2 1.347(4) . ? N2 N3 1.301(4) . ? N3 N4 1.349(4) . ? N5 N6 1.349(4) . ? N6 N7 1.297(4) . ? N7 N8 1.340(4) . ? N8 H8 0.8600 . ? O7 Tb1 2.375(2) . ? O8 Tb1 2.625(2) . ? O9 Tb1 2.266(2) . ? O10 Tb1 2.3275(9) 2_675 ? O1W H1A 0.8397 . ? O1W H1B 0.8521 . ? O2W H2A 0.8408 . ? O2W H2B 0.8448 . ? O3W Tb1 2.3235 . ? O3W H3B 0.8186 . ? O3W H3A 0.8244 . ? O4W Tb1 2.3818 . ? O4W H4B 0.8122 . ? O4W H4A 0.8087 . ? O5W Tb1 2.4286 . ? O5W H5A 0.8268 . ? O5W H5B 0.8199 . ? O6W Tb1 2.4153 . ? O6W H6A 0.8135 . ? O6W H6B 0.8208 . ? Tb1 O10 2.3275(9) 2_675 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 C1 O7 120.8(3) . . ? O8 C1 C2 121.2(3) . . ? O7 C1 C2 118.1(3) . . ? C3 C2 C8 119.4(3) . . ? C3 C2 C1 121.7(3) . . ? C8 C2 C1 118.9(3) . . ? C2 C3 C4 120.3(3) . . ? C2 C3 H1 118(2) . . ? C4 C3 H1 122(2) . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H2 123(2) . . ? C3 C4 H2 117(2) . . ? C4 C5 C6 120.9(3) . . ? C4 C5 H3 120(3) . . ? C6 C5 H3 119(3) . . ? C5 C6 C8 118.7(3) . . ? C5 C6 C7 121.9(3) . . ? C8 C6 C7 119.4(3) . . ? N4 C7 N1 111.0(3) . . ? N4 C7 C6 124.2(3) . . ? N1 C7 C6 124.7(3) . . ? C2 C8 C6 120.8(3) . . ? C2 C8 H4 118(2) . . ? C6 C8 H4 121(2) . . ? O10 C9 O9 124.4(3) . . ? O10 C9 C10 118.0(2) . . ? O9 C9 C10 117.6(3) . . ? C11 C10 C15 119.5(3) . . ? C11 C10 C9 120.1(3) . . ? C15 C10 C9 120.3(3) . . ? C12 C11 C10 120.0(3) . . ? C12 C11 H5 121(2) . . ? C10 C11 H5 119(2) . . ? C11 C12 C13 120.5(3) . . ? C11 C12 H6 121(3) . . ? C13 C12 H6 118(3) . . ? C12 C13 C14 119.8(3) . . ? C12 C13 H7 121(2) . . ? C14 C13 H7 119(2) . . ? C15 C14 C13 119.3(3) . . ? C15 C14 C16 121.9(3) . . ? C13 C14 C16 118.9(3) . . ? C14 C15 C10 120.8(3) . . ? C14 C15 H9 123(2) . . ? C10 C15 H9 116(2) . . ? N5 C16 N8 107.8(3) . . ? N5 C16 C14 125.7(3) . . ? N8 C16 C14 126.5(3) . . ? C7 N1 N2 104.8(3) . . ? N3 N2 N1 109.5(3) . . ? N2 N3 N4 109.4(3) . . ? C7 N4 N3 105.2(2) . . ? C16 N5 N6 106.2(3) . . ? N7 N6 N5 110.8(3) . . ? N6 N7 N8 106.3(3) . . ? C16 N8 N7 108.9(3) . . ? C16 N8 H8 125.6 . . ? N7 N8 H8 125.6 . . ? C1 O7 Tb1 99.43(18) . . ? C1 O8 Tb1 87.94(18) . . ? C9 O9 Tb1 148.6(2) . . ? C9 O10 Tb1 153.09(15) . 2_675 ? H1A O1W H1B 104.9 . . ? H2A O2W H2B 106.7 . . ? Tb1 O3W H3B 127.6 . . ? Tb1 O3W H3A 122.0 . . ? H3B O3W H3A 110.0 . . ? Tb1 O4W H4B 119.0 . . ? Tb1 O4W H4A 124.7 . . ? H4B O4W H4A 113.4 . . ? Tb1 O5W H5A 119.5 . . ? Tb1 O5W H5B 118.6 . . ? H5A O5W H5B 109.1 . . ? Tb1 O6W H6A 129.3 . . ? Tb1 O6W H6B 119.0 . . ? H6A O6W H6B 111.0 . . ? O9 Tb1 O3W 93.08(7) . . ? O9 Tb1 O10 97.20(6) . 2_675 ? O3W Tb1 O10 72.93(4) . 2_675 ? O9 Tb1 O7 133.14(8) . . ? O3W Tb1 O7 76.76(6) . . ? O10 Tb1 O7 121.83(6) 2_675 . ? O9 Tb1 O4W 87.59(7) . . ? O3W Tb1 O4W 144.1 . . ? O10 Tb1 O4W 142.560(18) 2_675 . ? O7 Tb1 O4W 76.84(6) . . ? O9 Tb1 O6W 76.58(6) . . ? O3W Tb1 O6W 144.0 . . ? O10 Tb1 O6W 74.33(4) 2_675 . ? O7 Tb1 O6W 134.74(6) . . ? O4W Tb1 O6W 70.7 . . ? O9 Tb1 O5W 155.96(7) . . ? O3W Tb1 O5W 106.7 . . ? O10 Tb1 O5W 76.39(4) 2_675 . ? O7 Tb1 O5W 66.53(6) . . ? O4W Tb1 O5W 84.3 . . ? O6W Tb1 O5W 79.4 . . ? O9 Tb1 O8 81.43(7) . . ? O3W Tb1 O8 72.04(6) . . ? O10 Tb1 O8 144.80(6) 2_675 . ? O7 Tb1 O8 51.80(7) . . ? O4W Tb1 O8 72.63(6) . . ? O6W Tb1 O8 137.67(6) . . ? O5W Tb1 O8 117.22(5) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.508 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.076 data_2 #TrackingRef '- C2DT30085K_ccdc_808461_842877_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 808463' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H34 Dy2 N16 O16, 4(H2 O)' _chemical_formula_sum 'C32 H42 Dy2 N16 O20' _chemical_formula_weight 1295.82 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' Dy Dy -0.1892 4.4098 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.164(3) _cell_length_b 11.9340(17) _cell_length_c 12.1166(17) _cell_angle_alpha 117.3780(10) _cell_angle_beta 98.139(2) _cell_angle_gamma 99.356(2) _cell_volume 1125.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3965 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.913 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 638.0 _exptl_absorpt_coefficient_mu 3.392 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4296 _exptl_absorpt_correction_T_max 0.4504 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5769 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.20 _reflns_number_total 3965 _reflns_number_gt 3786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0231P)^2^+1.3115P] 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 3965 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0591 _refine_ls_wR_factor_gt 0.0584 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4098(4) 0.4987(3) 0.3134(3) 0.0247(8) Uani 1 1 d . . . C2 C 0.3478(4) 0.4857(3) 0.1856(3) 0.0254(8) Uani 1 1 d . . . C3 C 0.2539(5) 0.5626(4) 0.1751(4) 0.0337(9) Uani 1 1 d . . . H8 H 0.2289 0.6223 0.2475 0.040 Uiso 1 1 calc R . . C4 C 0.1980(5) 0.5501(4) 0.0574(4) 0.0407(10) Uani 1 1 d . . . H7 H 0.1359 0.6024 0.0512 0.049 Uiso 1 1 calc R . . C5 C 0.2325(5) 0.4613(4) -0.0519(4) 0.0374(10) Uani 1 1 d . . . H6 H 0.1941 0.4539 -0.1309 0.045 Uiso 1 1 calc R . . C6 C 0.3259(4) 0.3827(3) -0.0423(3) 0.0249(8) Uani 1 1 d . . . C7 C 0.3833(4) 0.3962(3) 0.0764(3) 0.0239(7) Uani 1 1 d . . . H4 H 0.4464 0.3448 0.0832 0.029 Uiso 1 1 calc R . . C8 C 0.3600(4) 0.2880(4) -0.1584(3) 0.0266(8) Uani 1 1 d . . . C9 C 0.2125(4) 0.8702(4) 0.6692(4) 0.0275(8) Uani 1 1 d . . . C10 C 0.1067(4) 0.9568(3) 0.7125(3) 0.0262(8) Uani 1 1 d . . . C11 C 0.0006(2) 0.96650(19) 0.62540(18) 0.0311(8) Uani 1 1 d . . . H21 H -0.0053 0.9192 0.5381 0.037 Uiso 1 1 calc R . . O1W O 0.3925(2) 0.86184(19) 1.01346(18) 0.0373(7) Uani 1 1 d R . . H1B H 0.4326 0.8602 0.9545 0.056 Uiso 1 1 d R . . H1A H 0.3095 0.8024 0.9768 0.056 Uiso 1 1 d R . . O2W O 0.1116(2) 0.35945(19) 0.59801(18) 0.0652(10) Uani 1 1 d R . . H2B H 0.0221 0.3588 0.6095 0.098 Uiso 1 1 d R . . H2A H 0.1438 0.3118 0.6247 0.098 Uiso 1 1 d R . . C12 C -0.0961(5) 1.0463(4) 0.6683(4) 0.0362(9) Uani 1 1 d . . . H14 H -0.1652 1.0546 0.6101 0.043 Uiso 1 1 calc R . . C13 C -0.0897(4) 1.1139(4) 0.7979(4) 0.0337(9) Uani 1 1 d . . . H13 H -0.1566 1.1657 0.8264 0.040 Uiso 1 1 calc R . . C14 C 0.0155(4) 1.1050(3) 0.8859(3) 0.0256(8) Uani 1 1 d . . . C15 C 0.1145(4) 1.0268(3) 0.8419(3) 0.0260(8) Uani 1 1 d . . . H11 H 0.1869 1.0216 0.9003 0.031 Uiso 1 1 calc R . . C16 C 0.0242(4) 1.1759(4) 1.0237(4) 0.0273(8) Uani 1 1 d . . . Dy1 Dy 0.426767(18) 0.714686(15) 0.621247(14) 0.02224(7) Uani 1 1 d . . . N1 N 0.4479(4) 0.2075(3) -0.1663(3) 0.0301(7) Uani 1 1 d . . . H1 H 0.4943 0.2018 -0.1030 0.036 Uiso 1 1 calc R . . N2 N 0.4522(4) 0.1368(3) -0.2889(3) 0.0362(8) Uani 1 1 d . . . N3 N 0.3685(4) 0.1745(3) -0.3535(3) 0.0401(8) Uani 1 1 d . . . N4 N 0.3089(4) 0.2680(3) -0.2763(3) 0.0352(8) Uani 1 1 d . . . N5 N 0.1394(3) 1.1915(3) 1.1138(3) 0.0307(7) Uani 1 1 d . . . N6 N 0.1034(4) 1.2613(3) 1.2257(3) 0.0355(8) Uani 1 1 d . . . N7 N -0.0269(4) 1.2860(3) 1.2029(3) 0.0370(8) Uani 1 1 d . . . N8 N -0.0811(4) 1.2332(3) 1.0755(3) 0.0346(8) Uani 1 1 d . . . O7 O 0.4966(3) 0.4295(3) 0.3189(2) 0.0340(6) Uani 1 1 d . . . O8 O 0.3719(3) 0.5791(3) 0.4081(2) 0.0358(7) Uani 1 1 d . . . O9 O 0.1914(3) 0.7875(3) 0.5532(3) 0.0381(7) Uani 1 1 d . . . O10 O 0.32304(14) 0.88286(12) 0.75307(12) 0.0320(6) Uani 1 1 d . . . O3W O 0.21127(14) 0.60021(12) 0.64260(12) 0.0476(8) Uani 1 1 d R . . H3B H 0.1518 0.6312 0.6849 0.071 Uiso 1 1 d R . . H3A H 0.2935 0.6124 0.6887 0.071 Uiso 1 1 d R . . O5W O 0.52065(14) 0.88761(12) 0.58351(12) 0.0455(8) Uani 1 1 d R . . H5B H 0.5726 0.8744 0.5311 0.068 Uiso 1 1 d R . . H5A H 0.5069 0.9609 0.6119 0.068 Uiso 1 1 d R . . O6W O 0.67337(14) 0.70339(12) 0.57631(12) 0.0404(7) Uani 1 1 d R . . H6B H 0.7467 0.7174 0.6329 0.061 Uiso 1 1 d R . . H6A H 0.6932 0.6675 0.5061 0.061 Uiso 1 1 d R . . O4W O 0.59050(14) 0.85670(12) 0.83349(12) 0.0332(6) Uani 1 1 d R . . H4A H 0.6002 0.9356 0.8644 0.050 Uiso 1 1 d R . . H4B H 0.6725 0.8428 0.8537 0.050 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 C1 0.0282(18) 0.0247(19) 0.0172(17) 0.0070(15) 0.0056(14) 0.0071(15) C2 0.0296(18) 0.0233(19) 0.0197(18) 0.0073(15) 0.0062(14) 0.0081(15) C3 0.043(2) 0.031(2) 0.0230(19) 0.0056(17) 0.0080(17) 0.0214(18) C4 0.053(3) 0.039(2) 0.034(2) 0.016(2) 0.009(2) 0.029(2) C5 0.053(3) 0.038(2) 0.0218(19) 0.0137(18) 0.0050(18) 0.021(2) C6 0.0300(18) 0.0237(19) 0.0197(18) 0.0084(15) 0.0093(15) 0.0080(15) C7 0.0282(18) 0.0218(18) 0.0201(18) 0.0073(15) 0.0080(14) 0.0103(15) C8 0.0328(19) 0.0242(19) 0.0192(18) 0.0084(15) 0.0067(15) 0.0056(15) C9 0.032(2) 0.0243(19) 0.029(2) 0.0120(17) 0.0152(16) 0.0117(16) C10 0.0292(19) 0.0223(19) 0.0268(19) 0.0096(16) 0.0115(15) 0.0102(15) C11 0.035(2) 0.034(2) 0.0243(19) 0.0129(17) 0.0089(16) 0.0136(17) O1W 0.0327(15) 0.0503(18) 0.0270(14) 0.0175(13) 0.0080(12) 0.0101(13) O2W 0.069(2) 0.041(2) 0.076(3) 0.0332(19) -0.010(2) 0.0034(17) C12 0.041(2) 0.038(2) 0.032(2) 0.0170(19) 0.0059(18) 0.0189(19) C13 0.0282(19) 0.034(2) 0.040(2) 0.0151(19) 0.0125(17) 0.0183(17) C14 0.0263(18) 0.0218(18) 0.0269(19) 0.0091(15) 0.0093(15) 0.0085(15) C15 0.0277(18) 0.0266(19) 0.0258(19) 0.0118(16) 0.0100(15) 0.0131(15) C16 0.0254(18) 0.0258(19) 0.030(2) 0.0110(16) 0.0096(15) 0.0111(15) Dy1 0.02887(10) 0.02383(10) 0.01326(9) 0.00553(7) 0.00902(7) 0.01309(7) N1 0.0396(18) 0.0332(18) 0.0189(15) 0.0102(14) 0.0122(13) 0.0169(15) N2 0.054(2) 0.0354(19) 0.0218(17) 0.0116(15) 0.0183(15) 0.0193(17) N3 0.062(2) 0.037(2) 0.0215(17) 0.0114(15) 0.0161(16) 0.0187(18) N4 0.052(2) 0.0352(19) 0.0196(16) 0.0116(15) 0.0105(15) 0.0185(16) N5 0.0281(16) 0.0332(18) 0.0273(17) 0.0098(14) 0.0112(13) 0.0119(14) N6 0.0309(17) 0.0369(19) 0.0279(17) 0.0071(15) 0.0090(14) 0.0087(15) N7 0.0317(18) 0.040(2) 0.0318(18) 0.0085(16) 0.0136(14) 0.0150(15) N8 0.0331(18) 0.0389(19) 0.0276(17) 0.0094(15) 0.0111(14) 0.0180(15) O7 0.0467(16) 0.0398(16) 0.0250(14) 0.0181(12) 0.0132(12) 0.0252(14) O8 0.0483(17) 0.0382(16) 0.0149(12) 0.0035(12) 0.0105(12) 0.0237(13) O9 0.0453(16) 0.0419(17) 0.0253(14) 0.0095(13) 0.0132(12) 0.0254(14) O10 0.0330(14) 0.0346(15) 0.0267(14) 0.0097(12) 0.0090(11) 0.0200(12) O3W 0.0432(17) 0.0436(18) 0.070(2) 0.0287(17) 0.0382(16) 0.0244(14) O5W 0.064(2) 0.0375(17) 0.0509(19) 0.0240(15) 0.0396(16) 0.0253(15) O6W 0.0370(15) 0.060(2) 0.0276(15) 0.0179(14) 0.0169(12) 0.0245(14) O4W 0.0317(14) 0.0329(15) 0.0274(14) 0.0070(12) 0.0045(11) 0.0166(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 C1 O7 1.252(4) . ? C1 O8 1.251(4) . ? C1 C2 1.499(5) . ? C2 C7 1.390(5) . ? C2 C3 1.391(5) . ? C3 C4 1.376(6) . ? C3 H8 0.9300 . ? C4 C5 1.383(6) . ? C4 H7 0.9300 . ? C5 C6 1.400(5) . ? C5 H6 0.9300 . ? C6 C7 1.385(5) . ? C6 C8 1.460(5) . ? C7 H4 0.9300 . ? C8 N4 1.333(5) . ? C8 N1 1.330(5) . ? C9 O9 1.254(4) . ? C9 O10 1.265(4) . ? C9 C10 1.501(5) . ? C10 C15 1.381(5) . ? C10 C11 1.389(4) . ? C11 C12 1.383(4) . ? C11 H21 0.9300 . ? O1W H1B 0.8426 . ? O1W H1A 0.8469 . ? O2W H2B 0.8506 . ? O2W H2A 0.8443 . ? C12 C13 1.384(6) . ? C12 H14 0.9300 . ? C13 C14 1.387(5) . ? C13 H13 0.9300 . ? C14 C15 1.391(5) . ? C14 C16 1.467(5) . ? C15 H11 0.9300 . ? C16 N5 1.328(5) . ? C16 N8 1.335(5) . ? Dy1 O8 2.251(2) . ? Dy1 O7 2.318(3) 2_666 ? Dy1 O3W 2.3294(14) . ? Dy1 O10 2.3632(12) . ? Dy1 O5W 2.3685(13) . ? Dy1 O4W 2.4102(13) . ? Dy1 O6W 2.4086(14) . ? Dy1 O9 2.617(3) . ? Dy1 H3A 2.0891 . ? N1 N2 1.339(4) . ? N1 H1 0.8600 . ? N2 N3 1.292(5) . ? N3 N4 1.342(5) . ? N5 N6 1.348(4) . ? N6 N7 1.299(5) . ? N7 N8 1.346(5) . ? O7 Dy1 2.318(3) 2_666 ? O3W H3B 0.8161 . ? O3W H3A 0.8192 . ? O5W H5B 0.8200 . ? O5W H5A 0.8189 . ? O6W H6B 0.8228 . ? O6W H6A 0.8215 . ? O4W H4A 0.8204 . ? O4W H4B 0.8236 . ? 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 O7 C1 O8 124.3(3) . . ? O7 C1 C2 118.2(3) . . ? O8 C1 C2 117.5(3) . . ? C7 C2 C3 119.4(3) . . ? C7 C2 C1 120.2(3) . . ? C3 C2 C1 120.3(3) . . ? C4 C3 C2 119.8(3) . . ? C4 C3 H8 120.1 . . ? C2 C3 H8 120.1 . . ? C3 C4 C5 121.2(4) . . ? C3 C4 H7 119.4 . . ? C5 C4 H7 119.4 . . ? C4 C5 C6 119.3(4) . . ? C4 C5 H6 120.4 . . ? C6 C5 H6 120.4 . . ? C7 C6 C5 119.5(3) . . ? C7 C6 C8 121.6(3) . . ? C5 C6 C8 118.9(3) . . ? C6 C7 C2 120.8(3) . . ? C6 C7 H4 119.6 . . ? C2 C7 H4 119.6 . . ? N4 C8 N1 107.6(3) . . ? N4 C8 C6 125.6(3) . . ? N1 C8 C6 126.8(3) . . ? O9 C9 O10 121.0(3) . . ? O9 C9 C10 120.8(3) . . ? O10 C9 C10 118.1(3) . . ? C15 C10 C11 119.6(3) . . ? C15 C10 C9 118.8(3) . . ? C11 C10 C9 121.6(3) . . ? C12 C11 C10 120.1(3) . . ? C12 C11 H21 119.9 . . ? C10 C11 H21 119.9 . . ? H1B O1W H1A 106.2 . . ? H2B O2W H2A 106.1 . . ? C11 C12 C13 119.8(3) . . ? C11 C12 H14 120.1 . . ? C13 C12 H14 120.1 . . ? C12 C13 C14 120.6(3) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C15 119.0(3) . . ? C13 C14 C16 121.5(3) . . ? C15 C14 C16 119.5(3) . . ? C10 C15 C14 120.7(3) . . ? C10 C15 H11 119.6 . . ? C14 C15 H11 119.6 . . ? N5 C16 N8 111.0(3) . . ? N5 C16 C14 123.9(3) . . ? N8 C16 C14 125.0(3) . . ? O8 Dy1 O7 96.52(10) . 2_666 ? O8 Dy1 O3W 92.51(8) . . ? O7 Dy1 O3W 72.85(8) 2_666 . ? O8 Dy1 O10 133.23(7) . . ? O7 Dy1 O10 122.26(7) 2_666 . ? O3W Dy1 O10 77.11(4) . . ? O8 Dy1 O5W 87.89(8) . . ? O7 Dy1 O5W 142.66(8) 2_666 . ? O3W Dy1 O5W 144.21(6) . . ? O10 Dy1 O5W 76.76(4) . . ? O8 Dy1 O4W 155.78(8) . . ? O7 Dy1 O4W 76.67(8) 2_666 . ? O3W Dy1 O4W 107.2 . . ? O10 Dy1 O4W 66.80(4) . . ? O5W Dy1 O4W 84.3 . . ? O8 Dy1 O6W 76.19(8) . . ? O7 Dy1 O6W 74.34(8) 2_666 . ? O3W Dy1 O6W 143.70(6) . . ? O10 Dy1 O6W 135.06(6) . . ? O5W Dy1 O6W 70.8 . . ? O4W Dy1 O6W 79.6 . . ? O8 Dy1 O9 81.40(9) . . ? O7 Dy1 O9 144.64(10) 2_666 . ? O3W Dy1 O9 71.99(8) . . ? O10 Dy1 O9 51.92(7) . . ? O5W Dy1 O9 72.70(8) . . ? O4W Dy1 O9 117.62(7) . . ? O6W Dy1 O9 137.45(7) . . ? O8 Dy1 H3A 104.4 . . ? O7 Dy1 H3A 55.7 2_666 . ? O3W Dy1 H3A 20.4 . . ? O10 Dy1 H3A 81.2 . . ? O5W Dy1 H3A 157.6 . . ? O4W Dy1 H3A 91.0 . . ? O6W Dy1 H3A 129.9 . . ? O9 Dy1 H3A 90.4 . . ? C8 N1 N2 109.0(3) . . ? C8 N1 H1 125.5 . . ? N2 N1 H1 125.5 . . ? N3 N2 N1 106.5(3) . . ? N2 N3 N4 110.9(3) . . ? C8 N4 N3 106.1(3) . . ? C16 N5 N6 105.1(3) . . ? N7 N6 N5 109.4(3) . . ? N6 N7 N8 109.5(3) . . ? C16 N8 N7 105.0(3) . . ? C1 O7 Dy1 152.9(3) . 2_666 ? C1 O8 Dy1 148.7(2) . . ? C9 O9 Dy1 87.7(2) . . ? C9 O10 Dy1 99.34(17) . . ? Dy1 O3W H3B 126.9 . . ? Dy1 O3W H3A 63.0 . . ? H3B O3W H3A 111.4 . . ? Dy1 O5W H5B 118.1 . . ? Dy1 O5W H5A 130.7 . . ? H5B O5W H5A 111.1 . . ? Dy1 O6W H6B 120.0 . . ? Dy1 O6W H6A 128.1 . . ? H6B O6W H6A 109.7 . . ? Dy1 O4W H4A 117.8 . . ? Dy1 O4W H4B 119.9 . . ? H4A O4W H4B 109.9 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.671 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.101 data_6 #TrackingRef '- C2DT30085K_ccdc_808461_842877_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 842875' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H34 Er2 N16 O16, 4(H2 O)' _chemical_formula_sum 'C32 H42 Er2 N16 O20' _chemical_formula_weight 1305.34 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' Er Er -0.2586 4.9576 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.169(4) _cell_length_b 11.884(2) _cell_length_c 12.081(2) _cell_angle_alpha 117.455(2) _cell_angle_beta 98.129(3) _cell_angle_gamma 99.353(3) _cell_volume 1116.9(6) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4011 _cell_measurement_theta_min 0.33 _cell_measurement_theta_max 0.384 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.941 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 642.0 _exptl_absorpt_coefficient_mu 3.828 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.330 _exptl_absorpt_correction_T_max 0.384 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 5726 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.19 _reflns_number_total 4011 _reflns_number_gt 3638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0306P)^2^+0.7034P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3929 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0607 _refine_ls_wR_factor_gt 0.0594 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5903(4) 0.0014(4) 0.1850(4) 0.0237(8) Uani 1 1 d . . . C2 C 0.6516(4) 0.0134(4) 0.3130(3) 0.0241(8) Uani 1 1 d . . . C3 C 0.6159(5) 0.1022(4) 0.4222(4) 0.0247(8) Uani 1 1 d . . . C4 C 0.6742(4) 0.1166(4) 0.5415(4) 0.0252(8) Uani 1 1 d . . . C5 C 0.7670(5) 0.0380(4) 0.5505(4) 0.0354(10) Uani 1 1 d . . . C6 C 0.8021(6) -0.0512(5) 0.4410(4) 0.0429(12) Uani 1 1 d . . . C7 C 0.7476(5) -0.0617(4) 0.3232(4) 0.0349(10) Uani 1 1 d . . . C8 C 0.6404(5) 0.2113(4) 0.6586(4) 0.0268(9) Uani 1 1 d . . . C9 C 0.2134(5) 0.3693(4) 0.1687(4) 0.0282(9) Uani 1 1 d . . . C10 C 0.1088(4) 0.4567(4) 0.2123(4) 0.0252(8) Uani 1 1 d . . . C11 C 0.0023(5) 0.4659(4) 0.1249(4) 0.0310(9) Uani 1 1 d . . . C12 C -0.0953(5) 0.5451(4) 0.1681(4) 0.0369(10) Uani 1 1 d . . . C13 C -0.0905(5) 0.6123(4) 0.2978(4) 0.0350(10) Uani 1 1 d . . . C14 C 0.0167(5) 0.6047(4) 0.3868(4) 0.0264(9) Uani 1 1 d . . . C15 C 0.1166(5) 0.5279(4) 0.3422(4) 0.0271(9) Uani 1 1 d . . . C16 C 0.0250(4) 0.6760(4) 0.5250(4) 0.0280(9) Uani 1 1 d . . . Er1 Er 0.42761(2) 0.215334(17) 0.122349(15) 0.02326(7) Uani 1 1 d . . . H1 H -0.006(5) 0.413(5) 0.039(5) 0.043(13) Uiso 1 1 d . . . H2 H -0.171(5) 0.553(4) 0.103(4) 0.030(11) Uiso 1 1 d . . . H3 H -0.165(5) 0.649(5) 0.330(4) 0.042(13) Uiso 1 1 d . . . H4 H 0.175(5) 0.515(4) 0.395(4) 0.024(11) Uiso 1 1 d . . . H5 H 0.558(5) 0.139(4) 0.412(4) 0.020(11) Uiso 1 1 d . . . H6 H 0.779(5) -0.112(4) 0.253(4) 0.033(12) Uiso 1 1 d . . . H7 H 0.862(6) -0.097(5) 0.448(5) 0.053(15) Uiso 1 1 d . . . H8 H 0.802(6) 0.045(5) 0.628(5) 0.052(15) Uiso 1 1 d . . . N1 N 0.5521(4) 0.2923(3) 0.6670(3) 0.0305(8) Uani 1 1 d . . . H9 H 0.5056 0.2978 0.6033 0.037 Uiso 1 1 calc R . . N2 N 0.5469(4) 0.3639(4) 0.7897(3) 0.0363(9) Uani 1 1 d . . . N3 N 0.6316(5) 0.3256(4) 0.8547(3) 0.0398(9) Uani 1 1 d . . . N4 N 0.6906(4) 0.2309(4) 0.7762(3) 0.0365(9) Uani 1 1 d . . . N5 N -0.0808(4) 0.7324(4) 0.5763(3) 0.0351(8) Uani 1 1 d . . . N6 N -0.0274(4) 0.7860(4) 0.7044(3) 0.0375(9) Uani 1 1 d . . . N7 N 0.1040(4) 0.7612(4) 0.7269(3) 0.0361(8) Uani 1 1 d . . . N8 N 0.1389(4) 0.6919(3) 0.6157(3) 0.0314(8) Uani 1 1 d . . . O7 O 0.1937(4) 0.2868(3) 0.0525(3) 0.0386(7) Uani 1 1 d . . . O8 O 0.3245(3) 0.3827(3) 0.2530(3) 0.0330(7) Uani 1 1 d . . . O9 O 0.5018(3) 0.0698(3) 0.1794(3) 0.0337(7) Uani 1 1 d . . . O10 O 0.62904(13) -0.07900(12) 0.08945(11) 0.0355(7) Uani 1 1 d . . . O1W O 0.10848(13) 0.86239(12) 0.10205(11) 0.0687(12) Uani 1 1 d R . . H1A H 0.1488 0.8195 0.1314 0.103 Uiso 1 1 d R . . H1B H 0.0141 0.8234 0.0732 0.103 Uiso 1 1 d R . . O2W O 0.39242(13) 0.36258(12) 0.51419(11) 0.0386(7) Uani 1 1 d R . . H2A H 0.4381 0.3546 0.4565 0.058 Uiso 1 1 d R . . H2B H 0.3034 0.3134 0.4779 0.058 Uiso 1 1 d R . . O3W O 0.21569(13) 0.10343(12) 0.14409(11) 0.0483(9) Uani 1 1 d R . . H3A H 0.2039 0.0256 0.1222 0.072 Uiso 1 1 d R . . H3B H 0.1474 0.1305 0.1781 0.072 Uiso 1 1 d R . . O4W O 0.58898(13) 0.35453(12) 0.33227(11) 0.0329(7) Uani 1 1 d R . . H4A H 0.6710 0.3404 0.3498 0.049 Uiso 1 1 d R . . H4B H 0.5944 0.4330 0.3682 0.049 Uiso 1 1 d R . . O5W O 0.52143(13) 0.38684(12) 0.08520(11) 0.0433(8) Uani 1 1 d R . . H5A H 0.4951 0.4550 0.1113 0.065 Uiso 1 1 d R . . H5B H 0.5749 0.3787 0.0354 0.065 Uiso 1 1 d R . . O6W O 0.67114(13) 0.20341(12) 0.07517(11) 0.0403(8) Uani 1 1 d R . . H6A H 0.7434 0.2081 0.1273 0.060 Uiso 1 1 d R . . H6B H 0.6874 0.1725 0.0033 0.060 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 C1 0.023(2) 0.0221(19) 0.0207(19) 0.0071(17) 0.0053(16) 0.0019(17) C2 0.025(2) 0.0214(19) 0.0182(19) 0.0046(16) 0.0021(16) 0.0045(17) C3 0.026(2) 0.023(2) 0.025(2) 0.0108(18) 0.0065(17) 0.0099(18) C4 0.024(2) 0.023(2) 0.022(2) 0.0073(17) 0.0042(16) 0.0041(17) C5 0.043(3) 0.036(2) 0.024(2) 0.012(2) 0.004(2) 0.018(2) C6 0.049(3) 0.041(3) 0.034(3) 0.012(2) 0.002(2) 0.028(3) C7 0.042(3) 0.033(2) 0.024(2) 0.007(2) 0.010(2) 0.018(2) C8 0.029(2) 0.025(2) 0.023(2) 0.0102(18) 0.0059(17) 0.0055(18) C9 0.032(2) 0.025(2) 0.030(2) 0.0125(19) 0.0143(19) 0.0102(18) C10 0.024(2) 0.023(2) 0.026(2) 0.0089(17) 0.0071(17) 0.0064(17) C11 0.034(3) 0.029(2) 0.025(2) 0.010(2) 0.0065(19) 0.0089(19) C12 0.036(3) 0.039(3) 0.034(2) 0.016(2) 0.004(2) 0.014(2) C13 0.030(2) 0.035(2) 0.037(2) 0.013(2) 0.011(2) 0.017(2) C14 0.025(2) 0.0204(19) 0.028(2) 0.0079(17) 0.0063(17) 0.0046(17) C15 0.023(2) 0.029(2) 0.025(2) 0.0107(19) 0.0025(17) 0.0095(18) C16 0.022(2) 0.026(2) 0.032(2) 0.0106(19) 0.0070(18) 0.0079(17) Er1 0.02651(12) 0.02420(11) 0.01494(10) 0.00496(8) 0.00605(7) 0.01034(8) N1 0.036(2) 0.0336(19) 0.0201(17) 0.0108(16) 0.0083(15) 0.0127(17) N2 0.047(2) 0.035(2) 0.0248(19) 0.0099(17) 0.0162(17) 0.0158(18) N3 0.059(3) 0.037(2) 0.0214(18) 0.0094(17) 0.0128(18) 0.019(2) N4 0.047(2) 0.036(2) 0.0208(18) 0.0094(16) 0.0048(16) 0.0144(18) N5 0.030(2) 0.040(2) 0.0257(18) 0.0063(17) 0.0079(16) 0.0140(17) N6 0.031(2) 0.039(2) 0.032(2) 0.0079(18) 0.0108(17) 0.0124(17) N7 0.029(2) 0.037(2) 0.031(2) 0.0085(17) 0.0075(16) 0.0074(17) N8 0.0248(19) 0.034(2) 0.0300(19) 0.0106(17) 0.0086(15) 0.0091(16) O7 0.0420(19) 0.0384(17) 0.0282(16) 0.0077(15) 0.0097(14) 0.0198(15) O8 0.0318(17) 0.0349(16) 0.0266(15) 0.0083(13) 0.0055(13) 0.0173(14) O9 0.0414(18) 0.0398(17) 0.0257(15) 0.0167(14) 0.0113(13) 0.0213(15) O10 0.0395(18) 0.0363(17) 0.0177(14) 0.0016(13) 0.0062(13) 0.0150(14) O1W 0.067(3) 0.043(2) 0.080(3) 0.034(2) -0.021(2) -0.0043(19) O2W 0.0335(18) 0.0489(19) 0.0272(16) 0.0150(15) 0.0048(13) 0.0099(15) O3W 0.047(2) 0.0362(18) 0.073(2) 0.0269(18) 0.0379(19) 0.0208(16) O4W 0.0273(16) 0.0320(16) 0.0288(15) 0.0057(13) 0.0039(13) 0.0129(13) O5W 0.058(2) 0.0369(17) 0.0491(19) 0.0232(16) 0.0358(17) 0.0236(16) O6W 0.0361(18) 0.057(2) 0.0301(16) 0.0187(16) 0.0138(14) 0.0216(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 C1 O9 1.254(5) . ? C1 O10 1.257(4) . ? C1 C2 1.500(5) . ? C2 C3 1.382(5) . ? C2 C7 1.383(6) . ? C3 C4 1.385(5) . ? C3 H5 0.77(4) . ? C4 C5 1.391(6) . ? C4 C8 1.461(5) . ? C5 C6 1.383(6) . ? C5 H8 0.90(5) . ? C6 C7 1.381(6) . ? C6 H7 0.85(5) . ? C7 H6 0.91(4) . ? C8 N4 1.326(5) . ? C8 N1 1.334(5) . ? C9 O7 1.251(5) . ? C9 O8 1.266(5) . ? C9 C10 1.497(5) . ? C10 C15 1.382(5) . ? C10 C11 1.388(6) . ? C11 C12 1.384(6) . ? C11 H1 0.92(5) . ? C12 C13 1.382(6) . ? C12 H2 1.02(4) . ? C13 C14 1.397(6) . ? C13 H3 0.90(5) . ? C14 C15 1.385(5) . ? C14 C16 1.466(6) . ? C15 H4 0.86(4) . ? C16 N8 1.322(5) . ? C16 N5 1.332(5) . ? Er1 O10 2.2293(12) 2_655 ? Er1 O3W 2.2891(14) . ? Er1 O9 2.298(3) . ? Er1 O5W 2.3406(13) . ? Er1 O8 2.341(3) . ? Er1 O4W 2.3732(12) . ? Er1 O6W 2.3914(15) . ? Er1 O7 2.603(3) . ? N1 N2 1.339(5) . ? N1 H9 0.8600 . ? N2 N3 1.303(5) . ? N3 N4 1.348(5) . ? N5 N6 1.348(5) . ? N6 N7 1.307(5) . ? N7 N8 1.332(5) . ? O10 Er1 2.2293(12) 2_655 ? O1W H1A 0.8442 . ? O1W H1B 0.8489 . ? O2W H2A 0.8398 . ? O2W H2B 0.8414 . ? O3W H3A 0.8193 . ? O3W H3B 0.8251 . ? O4W H4A 0.8169 . ? O4W H4B 0.8161 . ? O5W H5A 0.8146 . ? O5W H5B 0.8111 . ? O6W H6A 0.8220 . ? O6W H6B 0.8188 . ? 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 O9 C1 O10 124.2(3) . . ? O9 C1 C2 118.3(3) . . ? O10 C1 C2 117.5(3) . . ? C3 C2 C7 119.5(4) . . ? C3 C2 C1 120.3(3) . . ? C7 C2 C1 120.2(3) . . ? C2 C3 C4 121.0(4) . . ? C2 C3 H5 117(3) . . ? C4 C3 H5 122(3) . . ? C3 C4 C5 119.2(4) . . ? C3 C4 C8 122.0(4) . . ? C5 C4 C8 118.7(4) . . ? C6 C5 C4 119.7(4) . . ? C6 C5 H8 121(3) . . ? C4 C5 H8 119(3) . . ? C7 C6 C5 120.7(4) . . ? C7 C6 H7 120(4) . . ? C5 C6 H7 119(4) . . ? C6 C7 C2 119.9(4) . . ? C6 C7 H6 121(3) . . ? C2 C7 H6 119(3) . . ? N4 C8 N1 107.5(3) . . ? N4 C8 C4 125.9(4) . . ? N1 C8 C4 126.5(3) . . ? O7 C9 O8 120.8(4) . . ? O7 C9 C10 121.3(4) . . ? O8 C9 C10 117.9(3) . . ? C15 C10 C11 119.4(4) . . ? C15 C10 C9 119.1(3) . . ? C11 C10 C9 121.5(4) . . ? C12 C11 C10 120.0(4) . . ? C12 C11 H1 122(3) . . ? C10 C11 H1 118(3) . . ? C13 C12 C11 120.2(4) . . ? C13 C12 H2 120(2) . . ? C11 C12 H2 119(2) . . ? C12 C13 C14 120.3(4) . . ? C12 C13 H3 124(3) . . ? C14 C13 H3 114(3) . . ? C15 C14 C13 118.6(4) . . ? C15 C14 C16 120.0(4) . . ? C13 C14 C16 121.3(4) . . ? C10 C15 C14 121.3(4) . . ? C10 C15 H4 119(3) . . ? C14 C15 H4 119(3) . . ? N8 C16 N5 110.8(4) . . ? N8 C16 C14 124.2(3) . . ? N5 C16 C14 125.0(4) . . ? O10 Er1 O3W 92.12(4) 2_655 . ? O10 Er1 O9 95.72(8) 2_655 . ? O3W Er1 O9 72.77(8) . . ? O10 Er1 O5W 88.40(4) 2_655 . ? O3W Er1 O5W 144.24(5) . . ? O9 Er1 O5W 142.74(8) . . ? O10 Er1 O8 132.88(7) 2_655 . ? O3W Er1 O8 76.78(8) . . ? O9 Er1 O8 122.83(10) . . ? O5W Er1 O8 76.86(8) . . ? O10 Er1 O4W 156.209(17) 2_655 . ? O3W Er1 O4W 106.8 . . ? O9 Er1 O4W 76.92(8) . . ? O5W Er1 O4W 84.5 . . ? O8 Er1 O4W 67.24(8) . . ? O10 Er1 O6W 76.14(5) 2_655 . ? O3W Er1 O6W 144.10(6) . . ? O9 Er1 O6W 74.79(8) . . ? O5W Er1 O6W 70.3 . . ? O8 Er1 O6W 135.38(8) . . ? O4W Er1 O6W 80.1 . . ? O10 Er1 O7 80.71(7) 2_655 . ? O3W Er1 O7 71.93(8) . . ? O9 Er1 O7 144.34(11) . . ? O5W Er1 O7 72.89(8) . . ? O8 Er1 O7 52.23(9) . . ? O4W Er1 O7 118.41(7) . . ? O6W Er1 O7 136.63(8) . . ? C8 N1 N2 109.6(3) . . ? C8 N1 H9 125.2 . . ? N2 N1 H9 125.2 . . ? N3 N2 N1 105.8(3) . . ? N2 N3 N4 110.7(3) . . ? C8 N4 N3 106.4(3) . . ? C16 N5 N6 105.1(3) . . ? N7 N6 N5 108.9(3) . . ? N6 N7 N8 109.3(3) . . ? C16 N8 N7 105.9(3) . . ? C9 O7 Er1 87.5(2) . . ? C9 O8 Er1 99.4(2) . . ? C1 O9 Er1 152.2(3) . . ? C1 O10 Er1 148.29(19) . 2_655 ? H1A O1W H1B 105.9 . . ? H2A O2W H2B 107.7 . . ? Er1 O3W H3A 119.9 . . ? Er1 O3W H3B 129.9 . . ? H3A O3W H3B 109.9 . . ? Er1 O4W H4A 118.7 . . ? Er1 O4W H4B 119.3 . . ? H4A O4W H4B 111.6 . . ? Er1 O5W H5A 124.7 . . ? Er1 O5W H5B 121.7 . . ? H5A O5W H5B 113.0 . . ? Er1 O6W H6A 121.2 . . ? Er1 O6W H6B 125.9 . . ? H6A O6W H6B 110.2 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.922 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.098 data_3 #TrackingRef '- C2DT30085K_ccdc_808461_842877_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 842876' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H34 Eu2 N16 O16, 4(H2 O)' _chemical_formula_sum 'C32 H42 Eu2 N16 O20' _chemical_formula_weight 1274.76 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.150(4) _cell_length_b 11.993(2) _cell_length_c 12.181(2) _cell_angle_alpha 117.270(2) _cell_angle_beta 98.188(3) _cell_angle_gamma 99.407(3) _cell_volume 1135.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4007 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.864 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632.0 _exptl_absorpt_coefficient_mu 2.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4846 _exptl_absorpt_correction_T_max 0.5387 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 5801 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4007 _reflns_number_gt 3750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0393P)^2^+0.7653P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4007 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.045 _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 C1 C 0.4102(4) 0.4997(4) 0.8098(3) 0.0270(8) Uani 1 1 d . . . C2 C 0.3476(4) 0.4853(4) 0.6817(4) 0.0256(8) Uani 1 1 d . . . C3 C 0.3828(4) 0.3964(4) 0.5740(4) 0.0263(8) Uani 1 1 d . . . C4 C 0.3251(4) 0.3817(4) 0.4556(4) 0.0274(8) Uani 1 1 d . . . C5 C 0.3588(4) 0.2868(4) 0.3399(4) 0.0276(8) Uani 1 1 d . . . C6 C 0.2336(6) 0.4605(5) 0.4458(4) 0.0382(10) Uani 1 1 d . . . C7 C 0.1991(6) 0.5499(5) 0.5531(4) 0.0441(12) Uani 1 1 d . . . C8 C 0.2547(5) 0.5625(4) 0.6712(4) 0.0354(10) Uani 1 1 d . . . C9 C 0.7908(4) 0.1298(4) 0.8307(4) 0.0281(8) Uani 1 1 d . . . C10 C 0.8955(4) 0.0426(4) 0.7872(4) 0.0270(8) Uani 1 1 d . . . C11 C 1.0012(5) 0.0315(4) 0.8740(4) 0.0332(9) Uani 1 1 d . . . C12 C 1.0958(5) -0.0481(4) 0.8314(4) 0.0377(10) Uani 1 1 d . . . C13 C 1.0912(5) -0.1151(4) 0.7029(4) 0.0373(10) Uani 1 1 d . . . C14 C 0.9859(4) -0.1046(4) 0.6149(4) 0.0283(8) Uani 1 1 d . . . C15 C 0.9772(4) -0.1759(4) 0.4778(4) 0.0290(8) Uani 1 1 d . . . C16 C 0.8877(4) -0.0271(4) 0.6585(4) 0.0283(8) Uani 1 1 d . . . Eu1 Eu 0.57485(2) 0.287281(17) 0.880537(15) 0.02436(8) Uani 1 1 d . . . H1 H 1.003(5) 0.080(4) 0.956(4) 0.029(11) Uiso 1 1 d . . . H2 H 1.163(6) -0.065(5) 0.885(5) 0.053(15) Uiso 1 1 d . . . H3 H 1.154(6) -0.163(5) 0.672(5) 0.048(14) Uiso 1 1 d . . . H4 H 0.824(5) -0.015(4) 0.598(4) 0.036(12) Uiso 1 1 d . . . H5 H 0.217(5) 0.613(4) 0.744(4) 0.030(11) Uiso 1 1 d . . . H6 H 0.136(6) 0.590(6) 0.547(5) 0.061(17) Uiso 1 1 d . . . H7 H 0.441(5) 0.342(4) 0.580(4) 0.021(10) Uiso 1 1 d . . . H8 H 0.192(6) 0.450(5) 0.362(5) 0.055(15) Uiso 1 1 d . . . N1 N 0.3091(4) 0.2668(4) 0.2235(3) 0.0377(8) Uani 1 1 d . . . N2 N 0.3678(5) 0.1731(4) 0.1468(3) 0.0427(9) Uani 1 1 d . . . N3 N 0.4517(4) 0.1367(4) 0.2117(3) 0.0386(9) Uani 1 1 d . . . N4 N 0.4463(4) 0.2061(3) 0.3327(3) 0.0316(8) Uani 1 1 d . . . N5 N 0.8613(4) -0.1910(3) 0.3881(3) 0.0325(8) Uani 1 1 d . . . N6 N 0.8960(4) -0.2613(4) 0.2785(3) 0.0374(8) Uani 1 1 d . . . N7 N 1.0266(4) -0.2872(4) 0.2998(3) 0.0386(9) Uani 1 1 d . . . N8 N 1.0824(4) -0.2332(4) 0.4267(3) 0.0375(8) Uani 1 1 d . . . O7 O 0.4950(3) 0.4286(3) 0.8150(3) 0.0371(7) Uani 1 1 d . . . O8 O 0.3727(3) 0.5802(3) 0.9035(2) 0.0384(7) Uani 1 1 d . . . O9 O 0.6800(3) 0.1175(3) 0.7469(3) 0.0347(7) Uani 1 1 d . . . O10 O 0.8113(3) 0.2116(3) 0.9455(3) 0.0395(7) Uani 1 1 d . . . O1W O 0.6054(4) 0.1381(4) 0.4859(3) 0.0416(8) Uani 1 1 d . . . H1A H 0.563(7) 0.132(6) 0.524(6) 0.062 Uiso 1 1 d . . . H1B H 0.687(7) 0.180(6) 0.516(6) 0.062 Uiso 1 1 d . . . O2W O 0.8850(5) 0.6454(4) 0.9066(4) 0.0619(11) Uani 1 1 d . . . H2A H 0.860(9) 0.686(8) 0.882(8) 0.093 Uiso 1 1 d . . . H2B H 0.970(9) 0.650(8) 0.894(8) 0.093 Uiso 1 1 d . . . O3W O 0.4093(4) 0.1420(3) 0.6647(3) 0.0351(7) Uani 1 1 d . . . H3A H 0.324(6) 0.151(5) 0.644(5) 0.053 Uiso 1 1 d . . . H3B H 0.404(6) 0.063(6) 0.635(5) 0.053 Uiso 1 1 d . . . O4W O 0.7935(5) 0.4024(3) 0.8589(4) 0.0530(10) Uani 1 1 d . . . H4B H 0.805(9) 0.459(7) 0.866(7) 0.079 Uiso 1 1 d . . . H4A H 0.861(7) 0.362(6) 0.812(6) 0.079 Uiso 1 1 d . . . O5W O 0.3216(4) 0.2969(4) 0.9215(3) 0.0452(9) Uani 1 1 d . . . H5A H 0.251(7) 0.293(6) 0.864(6) 0.068 Uiso 1 1 d . . . H5B H 0.303(7) 0.322(6) 0.977(6) 0.068 Uiso 1 1 d . . . O6W O 0.4791(5) 0.1112(3) 0.9182(4) 0.0477(9) Uani 1 1 d . . . H6B H 0.491(7) 0.041(6) 0.884(6) 0.072 Uiso 1 1 d . . . H6A H 0.437(7) 0.125(6) 0.971(6) 0.072 Uiso 1 1 d . . . H9 H 0.495(5) 0.192(5) 0.382(5) 0.037(14) 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 C1 0.031(2) 0.028(2) 0.0141(18) 0.0037(16) 0.0058(15) 0.0070(16) C2 0.0280(19) 0.0252(19) 0.0175(19) 0.0057(16) 0.0053(15) 0.0065(15) C3 0.031(2) 0.028(2) 0.0186(19) 0.0085(16) 0.0076(16) 0.0121(17) C4 0.033(2) 0.026(2) 0.0173(19) 0.0059(16) 0.0064(16) 0.0064(16) C5 0.034(2) 0.029(2) 0.0178(19) 0.0091(17) 0.0082(16) 0.0075(17) C6 0.052(3) 0.042(3) 0.022(2) 0.015(2) 0.006(2) 0.021(2) C7 0.058(3) 0.045(3) 0.031(2) 0.014(2) 0.010(2) 0.035(2) C8 0.042(2) 0.036(2) 0.023(2) 0.0066(19) 0.0098(19) 0.0204(19) C9 0.031(2) 0.028(2) 0.025(2) 0.0100(17) 0.0119(17) 0.0132(16) C10 0.029(2) 0.026(2) 0.025(2) 0.0101(17) 0.0109(16) 0.0109(16) C11 0.037(2) 0.037(2) 0.024(2) 0.0109(19) 0.0104(18) 0.0158(18) C12 0.044(3) 0.043(3) 0.026(2) 0.015(2) 0.0056(19) 0.022(2) C13 0.038(2) 0.038(2) 0.037(3) 0.014(2) 0.015(2) 0.024(2) C14 0.0268(19) 0.027(2) 0.028(2) 0.0097(17) 0.0093(16) 0.0086(16) C15 0.027(2) 0.028(2) 0.026(2) 0.0091(17) 0.0062(17) 0.0086(16) C16 0.028(2) 0.029(2) 0.024(2) 0.0089(17) 0.0053(17) 0.0110(16) Eu1 0.03024(13) 0.02891(13) 0.01138(12) 0.00499(9) 0.00820(8) 0.01399(8) N1 0.055(2) 0.038(2) 0.0180(17) 0.0097(16) 0.0119(16) 0.0185(17) N2 0.064(3) 0.042(2) 0.0202(18) 0.0101(17) 0.0165(18) 0.0199(19) N3 0.055(2) 0.040(2) 0.0230(19) 0.0126(17) 0.0180(17) 0.0176(18) N4 0.040(2) 0.0338(19) 0.0194(18) 0.0093(16) 0.0115(16) 0.0155(16) N5 0.0268(17) 0.038(2) 0.0258(18) 0.0090(16) 0.0099(14) 0.0108(15) N6 0.0330(19) 0.042(2) 0.0274(19) 0.0077(17) 0.0099(15) 0.0108(16) N7 0.0340(19) 0.044(2) 0.028(2) 0.0068(17) 0.0120(15) 0.0152(16) N8 0.0324(18) 0.047(2) 0.0273(19) 0.0092(17) 0.0121(15) 0.0193(17) O7 0.0492(18) 0.0416(17) 0.0263(15) 0.0157(14) 0.0135(13) 0.0255(15) O8 0.0493(17) 0.0420(17) 0.0124(13) 0.0007(13) 0.0083(12) 0.0219(14) O9 0.0337(15) 0.0411(17) 0.0227(14) 0.0067(13) 0.0077(12) 0.0203(13) O10 0.0466(17) 0.0441(18) 0.0231(15) 0.0077(14) 0.0112(13) 0.0251(14) O1W 0.0347(18) 0.058(2) 0.0264(18) 0.0174(16) 0.0055(13) 0.0091(16) O2W 0.065(2) 0.049(2) 0.064(3) 0.030(2) -0.007(2) 0.007(2) O3W 0.0327(15) 0.0355(17) 0.0258(16) 0.0051(13) 0.0041(13) 0.0145(14) O4W 0.055(2) 0.038(2) 0.081(3) 0.030(2) 0.044(2) 0.0241(18) O5W 0.0399(18) 0.068(2) 0.0308(19) 0.0213(18) 0.0169(15) 0.0250(17) O6W 0.070(2) 0.0403(19) 0.047(2) 0.0222(17) 0.0411(18) 0.0248(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O8 1.249(5) . ? C1 O7 1.258(5) . ? C1 C2 1.503(5) . ? C2 C3 1.383(5) . ? C2 C8 1.389(6) . ? C3 C4 1.383(5) . ? C3 H7 0.93(4) . ? C4 C6 1.393(6) . ? C4 C5 1.464(5) . ? C5 N1 1.320(5) . ? C5 N4 1.335(5) . ? C6 C7 1.378(6) . ? C6 H8 0.98(5) . ? C7 C8 1.385(6) . ? C7 H6 0.83(6) . ? C8 H5 0.97(4) . ? C9 O10 1.250(5) . ? C9 O9 1.269(5) . ? C9 C10 1.502(5) . ? C10 C16 1.383(5) . ? C10 C11 1.396(6) . ? C11 C12 1.368(6) . ? C11 H1 0.89(4) . ? C12 C13 1.384(6) . ? C12 H2 0.94(5) . ? C13 C14 1.401(6) . ? C13 H3 0.88(5) . ? C14 C16 1.381(5) . ? C14 C15 1.469(6) . ? C15 N5 1.333(5) . ? C15 N8 1.335(5) . ? C16 H4 0.95(5) . ? Eu1 O8 2.289(3) 2_667 ? Eu1 O7 2.351(3) . ? Eu1 O4W 2.358(4) . ? Eu1 O9 2.403(3) . ? Eu1 O6W 2.415(3) . ? Eu1 O5W 2.448(3) . ? Eu1 O3W 2.459(3) . ? Eu1 O10 2.635(3) . ? Eu1 H4B 2.77(7) . ? N1 N2 1.342(5) . ? N2 N3 1.287(5) . ? N3 N4 1.333(5) . ? N4 H9 0.79(5) . ? N5 N6 1.331(5) . ? N6 N7 1.304(5) . ? N7 N8 1.348(5) . ? O8 Eu1 2.289(3) 2_667 ? O1W H1A 0.66(6) . ? O1W H1B 0.76(6) . ? O2W H2A 0.72(7) . ? O2W H2B 0.81(8) . ? O3W H3A 0.83(5) . ? O3W H3B 0.84(6) . ? O4W H4B 0.63(7) . ? O4W H4A 0.94(7) . ? O5W H5A 0.86(6) . ? O5W H5B 0.67(6) . ? O6W H6B 0.79(6) . ? O6W H6A 0.77(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 C1 O7 124.6(4) . . ? O8 C1 C2 117.7(3) . . ? O7 C1 C2 117.7(3) . . ? C3 C2 C8 119.6(4) . . ? C3 C2 C1 120.4(3) . . ? C8 C2 C1 119.9(3) . . ? C4 C3 C2 121.0(4) . . ? C4 C3 H7 119(2) . . ? C2 C3 H7 120(3) . . ? C3 C4 C6 119.1(4) . . ? C3 C4 C5 122.0(4) . . ? C6 C4 C5 118.8(4) . . ? N1 C5 N4 107.5(3) . . ? N1 C5 C4 126.0(4) . . ? N4 C5 C4 126.5(4) . . ? C7 C6 C4 120.0(4) . . ? C7 C6 H8 120(3) . . ? C4 C6 H8 120(3) . . ? C6 C7 C8 120.7(4) . . ? C6 C7 H6 121(4) . . ? C8 C7 H6 118(4) . . ? C7 C8 C2 119.6(4) . . ? C7 C8 H5 122(2) . . ? C2 C8 H5 118(2) . . ? O10 C9 O9 120.8(3) . . ? O10 C9 C10 121.4(4) . . ? O9 C9 C10 117.8(3) . . ? C16 C10 C11 119.4(4) . . ? C16 C10 C9 119.1(4) . . ? C11 C10 C9 121.5(3) . . ? C12 C11 C10 120.1(4) . . ? C12 C11 H1 124(3) . . ? C10 C11 H1 116(3) . . ? C11 C12 C13 120.6(4) . . ? C11 C12 H2 123(3) . . ? C13 C12 H2 116(3) . . ? C12 C13 C14 119.9(4) . . ? C12 C13 H3 123(3) . . ? C14 C13 H3 117(3) . . ? C16 C14 C13 119.1(4) . . ? C16 C14 C15 119.9(4) . . ? C13 C14 C15 121.0(4) . . ? N5 C15 N8 111.3(4) . . ? N5 C15 C14 123.6(3) . . ? N8 C15 C14 125.2(4) . . ? C14 C16 C10 120.9(4) . . ? C14 C16 H4 118(3) . . ? C10 C16 H4 121(3) . . ? O8 Eu1 O7 98.92(10) 2_667 . ? O8 Eu1 O4W 93.95(14) 2_667 . ? O7 Eu1 O4W 73.13(12) . . ? O8 Eu1 O9 133.11(10) 2_667 . ? O7 Eu1 O9 120.97(10) . . ? O4W Eu1 O9 76.99(11) . . ? O8 Eu1 O6W 86.55(12) 2_667 . ? O7 Eu1 O6W 142.35(12) . . ? O4W Eu1 O6W 144.04(13) . . ? O9 Eu1 O6W 76.68(11) . . ? O8 Eu1 O5W 76.49(12) 2_667 . ? O7 Eu1 O5W 73.97(12) . . ? O4W Eu1 O5W 143.73(13) . . ? O9 Eu1 O5W 134.45(12) . . ? O6W Eu1 O5W 71.20(13) . . ? O8 Eu1 O3W 155.49(11) 2_667 . ? O7 Eu1 O3W 75.73(11) . . ? O4W Eu1 O3W 106.90(14) . . ? O9 Eu1 O3W 66.07(10) . . ? O6W Eu1 O3W 84.01(13) . . ? O5W Eu1 O3W 79.06(11) . . ? O8 Eu1 O10 82.00(10) 2_667 . ? O7 Eu1 O10 145.07(11) . . ? O4W Eu1 O10 71.98(12) . . ? O9 Eu1 O10 51.29(9) . . ? O6W Eu1 O10 72.50(12) . . ? O5W Eu1 O10 138.53(11) . . ? O3W Eu1 O10 116.26(10) . . ? O8 Eu1 H4B 90.2(16) 2_667 . ? O7 Eu1 H4B 64.0(15) . . ? O4W Eu1 H4B 10.5(15) . . ? O9 Eu1 H4B 86.7(16) . . ? O6W Eu1 H4B 153.6(15) . . ? O5W Eu1 H4B 133.2(15) . . ? O3W Eu1 H4B 108.0(16) . . ? O10 Eu1 H4B 81.1(15) . . ? C5 N1 N2 106.5(3) . . ? N3 N2 N1 110.5(3) . . ? N2 N3 N4 106.7(3) . . ? N3 N4 C5 108.8(4) . . ? N3 N4 H9 116(4) . . ? C5 N4 H9 136(4) . . ? N6 N5 C15 104.8(3) . . ? N7 N6 N5 110.2(3) . . ? N6 N7 N8 109.0(3) . . ? C15 N8 N7 104.7(3) . . ? C1 O7 Eu1 153.4(3) . . ? C1 O8 Eu1 148.6(3) . 2_667 ? C9 O9 Eu1 99.2(2) . . ? C9 O10 Eu1 88.7(2) . . ? H1A O1W H1B 118(7) . . ? H2A O2W H2B 100(8) . . ? Eu1 O3W H3A 121(4) . . ? Eu1 O3W H3B 116(4) . . ? H3A O3W H3B 109(5) . . ? Eu1 O4W H4B 126(7) . . ? Eu1 O4W H4A 124(4) . . ? H4B O4W H4A 107(8) . . ? Eu1 O5W H5A 119(4) . . ? Eu1 O5W H5B 129(6) . . ? H5A O5W H5B 109(7) . . ? Eu1 O6W H6B 126(5) . . ? Eu1 O6W H6A 118(5) . . ? H6B O6W H6A 116(7) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.181 _refine_diff_density_min -1.034 _refine_diff_density_rms 0.100 data_5 #TrackingRef '- C2DT30085K_ccdc_808461_842877_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 842877' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H34 N16 O16 Sm2, 4(H2 O)' _chemical_formula_sum 'C32 H42 N16 O20 Sm2' _chemical_formula_weight 1271.54 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.128(3) _cell_length_b 11.9957(15) _cell_length_c 12.2137(15) _cell_angle_alpha 117.2010(10) _cell_angle_beta 98.160(2) _cell_angle_gamma 99.347(2) _cell_volume 1137.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4004 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.856 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 630.0 _exptl_absorpt_coefficient_mu 2.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5037 _exptl_absorpt_correction_T_max 0.5572 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 5859 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4004 _reflns_number_gt 3756 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0357P)^2^+0.4705P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4004 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0905(4) 0.4989(3) 0.8081(3) 0.0269(7) Uani 1 1 d . . . C2 C -0.1518(4) 0.4857(3) 0.6803(3) 0.0256(7) Uani 1 1 d . . . C3 C -0.1165(4) 0.3954(3) 0.5731(3) 0.0265(7) Uani 1 1 d . . . H3 H -0.0535 0.3444 0.5807 0.032 Uiso 1 1 calc R . . C4 C -0.1750(4) 0.3809(3) 0.4543(3) 0.0257(7) Uani 1 1 d . . . C5 C -0.2671(5) 0.4597(4) 0.4445(3) 0.0365(8) Uani 1 1 d . . . H5 H -0.3056 0.4515 0.3658 0.044 Uiso 1 1 calc R . . C6 C -0.1413(4) 0.2866(3) 0.3399(3) 0.0274(7) Uani 1 1 d . . . C7 C -0.3010(5) 0.5495(4) 0.5511(4) 0.0443(10) Uani 1 1 d . . . H7 H -0.3617 0.6022 0.5441 0.053 Uiso 1 1 calc R . . C8 C -0.2449(4) 0.5620(3) 0.6696(3) 0.0351(8) Uani 1 1 d . . . H8 H -0.2700 0.6216 0.7411 0.042 Uiso 1 1 calc R . . C9 C 0.2916(4) 0.1299(3) 0.8309(3) 0.0285(7) Uani 1 1 d . . . C10 C 0.3958(4) 0.0427(3) 0.7876(3) 0.0268(7) Uani 1 1 d . . . C11 C 0.5005(4) 0.0312(3) 0.8740(3) 0.0331(8) Uani 1 1 d . . . H11 H 0.5064 0.0775 0.9605 0.040 Uiso 1 1 calc R . . C12 C 0.5962(5) -0.0497(4) 0.8304(4) 0.0375(9) Uani 1 1 d . . . H12 H 0.6644 -0.0593 0.8879 0.045 Uiso 1 1 calc R . . C13 C 0.5913(4) -0.1160(4) 0.7031(4) 0.0366(8) Uani 1 1 d . . . H13 H 0.6580 -0.1682 0.6753 0.044 Uiso 1 1 calc R . . C14 C 0.4866(4) -0.1054(3) 0.6154(3) 0.0279(7) Uani 1 1 d . . . C15 C 0.4778(4) -0.1755(3) 0.4789(3) 0.0277(7) Uani 1 1 d . . . C16 C 0.3892(4) -0.0258(3) 0.6596(3) 0.0279(7) Uani 1 1 d . . . H16 H 0.3184 -0.0186 0.6020 0.033 Uiso 1 1 calc R . . H1 H -0.005(6) 0.188(5) 0.386(5) 0.064(15) Uiso 1 1 d . . . H1A H 0.641(8) 0.324(6) 0.136(6) 0.096 Uiso 1 1 d . . . H2A H 0.191(8) 0.185(6) 0.523(6) 0.096 Uiso 1 1 d . . . H3A H -0.184(7) 0.156(6) 0.647(6) 0.096 Uiso 1 1 d . . . H4A H 0.315(8) 0.466(6) 0.884(7) 0.096 Uiso 1 1 d . . . H5A H -0.064(7) 0.126(6) 0.968(6) 0.096 Uiso 1 1 d . . . H6A H -0.222(7) 0.312(6) 0.969(6) 0.096 Uiso 1 1 d . . . H1B H 0.529(8) 0.320(7) 0.067(7) 0.096 Uiso 1 1 d . . . H2B H 0.069(8) 0.148(7) 0.531(6) 0.096 Uiso 1 1 d . . . H3B H -0.104(7) 0.065(6) 0.623(6) 0.096 Uiso 1 1 d . . . H4B H 0.358(7) 0.370(6) 0.806(6) 0.096 Uiso 1 1 d . . . H5B H -0.007(8) 0.047(6) 0.892(6) 0.096 Uiso 1 1 d . . . H6B H -0.257(7) 0.291(6) 0.862(6) 0.096 Uiso 1 1 d . . . N1 N -0.0536(4) 0.2058(3) 0.3328(3) 0.0308(6) Uani 1 1 d . . . N2 N -0.0484(4) 0.1349(3) 0.2118(3) 0.0384(7) Uani 1 1 d . . . N3 N -0.1317(4) 0.1721(3) 0.1467(3) 0.0422(8) Uani 1 1 d . . . N4 N -0.1916(4) 0.2658(3) 0.2234(3) 0.0364(7) Uani 1 1 d . . . N5 N 0.3613(3) -0.1910(3) 0.3898(3) 0.0325(7) Uani 1 1 d . . . N6 N 0.3964(4) -0.2617(3) 0.2792(3) 0.0361(7) Uani 1 1 d . . . N7 N 0.5276(4) -0.2866(3) 0.3016(3) 0.0382(7) Uani 1 1 d . . . N8 N 0.5823(4) -0.2333(3) 0.4275(3) 0.0370(7) Uani 1 1 d . . . O1 O -0.0051(3) 0.4285(2) 0.8133(2) 0.0368(6) Uani 1 1 d . . . O2 O -0.1271(3) 0.5806(2) 0.9011(2) 0.0387(6) Uani 1 1 d . . . O5 O 0.3128(3) 0.2116(2) 0.9458(2) 0.0381(6) Uani 1 1 d . . . O6 O 0.1807(3) 0.1177(2) 0.7477(2) 0.0346(6) Uani 1 1 d . . . O1W O 0.6161(4) 0.3529(3) 0.0924(4) 0.0568(9) Uani 1 1 d . . . O2W O 0.1051(3) 0.1385(3) 0.4862(3) 0.0396(7) Uani 1 1 d . . . O3W O -0.0909(3) 0.1414(3) 0.6641(2) 0.0344(6) Uani 1 1 d . . . O4W O 0.2952(4) 0.4025(3) 0.8584(4) 0.0516(8) Uani 1 1 d . . . O5W O -0.0228(4) 0.1108(3) 0.9180(3) 0.0492(8) Uani 1 1 d . . . O6W O -0.1791(3) 0.2981(3) 0.9206(3) 0.0472(7) Uani 1 1 d . . . Sm1 Sm 0.075312(18) 0.288643(15) 0.881626(13) 0.02404(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0287(18) 0.0294(17) 0.0221(16) 0.0102(14) 0.0093(14) 0.0108(14) C2 0.0268(17) 0.0258(16) 0.0236(16) 0.0108(14) 0.0065(14) 0.0092(13) C3 0.0294(18) 0.0284(17) 0.0242(16) 0.0120(14) 0.0097(14) 0.0144(14) C4 0.0294(17) 0.0277(17) 0.0210(16) 0.0110(14) 0.0095(14) 0.0100(14) C5 0.048(2) 0.041(2) 0.0230(17) 0.0164(16) 0.0047(16) 0.0210(18) C6 0.0324(18) 0.0269(17) 0.0231(16) 0.0117(14) 0.0080(14) 0.0089(14) C7 0.057(3) 0.047(2) 0.036(2) 0.0192(19) 0.0120(19) 0.037(2) C8 0.043(2) 0.0357(19) 0.0255(17) 0.0095(16) 0.0104(16) 0.0236(17) C9 0.0305(18) 0.0292(17) 0.0296(18) 0.0142(15) 0.0140(15) 0.0127(14) C10 0.0272(17) 0.0266(17) 0.0287(17) 0.0127(14) 0.0110(14) 0.0116(14) C11 0.039(2) 0.0362(19) 0.0299(18) 0.0176(16) 0.0121(16) 0.0168(16) C12 0.040(2) 0.043(2) 0.0344(19) 0.0201(17) 0.0052(17) 0.0224(17) C13 0.034(2) 0.038(2) 0.039(2) 0.0154(17) 0.0120(17) 0.0212(17) C14 0.0265(17) 0.0276(17) 0.0312(18) 0.0133(15) 0.0115(15) 0.0105(14) C15 0.0244(17) 0.0281(17) 0.0312(18) 0.0126(15) 0.0104(15) 0.0112(14) C16 0.0249(17) 0.0316(18) 0.0291(17) 0.0143(15) 0.0084(14) 0.0132(14) N1 0.0394(18) 0.0331(16) 0.0236(14) 0.0130(13) 0.0142(13) 0.0164(13) N2 0.054(2) 0.0382(17) 0.0265(15) 0.0129(14) 0.0219(15) 0.0209(15) N3 0.063(2) 0.0419(18) 0.0262(15) 0.0163(15) 0.0189(16) 0.0205(16) N4 0.051(2) 0.0393(17) 0.0224(14) 0.0140(13) 0.0126(14) 0.0200(15) N5 0.0276(16) 0.0365(16) 0.0317(16) 0.0125(14) 0.0119(13) 0.0134(13) N6 0.0293(17) 0.0420(18) 0.0324(16) 0.0125(14) 0.0115(13) 0.0117(14) N7 0.0324(17) 0.0438(18) 0.0330(17) 0.0113(15) 0.0129(14) 0.0160(14) N8 0.0335(17) 0.0443(18) 0.0316(16) 0.0125(15) 0.0127(14) 0.0212(14) O1 0.0474(16) 0.0434(15) 0.0289(13) 0.0190(12) 0.0141(12) 0.0273(13) O2 0.0483(16) 0.0430(15) 0.0192(12) 0.0062(11) 0.0102(11) 0.0238(13) O5 0.0438(15) 0.0426(15) 0.0267(13) 0.0107(12) 0.0120(11) 0.0246(12) O6 0.0338(14) 0.0405(14) 0.0285(12) 0.0120(11) 0.0090(11) 0.0216(11) O1W 0.057(2) 0.0470(18) 0.063(2) 0.0329(17) -0.0038(17) 0.0056(15) O2W 0.0331(15) 0.0549(17) 0.0312(14) 0.0202(14) 0.0095(12) 0.0139(13) O3W 0.0306(14) 0.0361(14) 0.0272(13) 0.0065(11) 0.0039(11) 0.0167(12) O4W 0.0508(18) 0.0384(16) 0.083(2) 0.0319(17) 0.0444(18) 0.0244(15) O5W 0.068(2) 0.0425(17) 0.0561(19) 0.0282(16) 0.0423(17) 0.0267(15) O6W 0.0348(16) 0.077(2) 0.0365(16) 0.0266(16) 0.0195(13) 0.0257(15) Sm1 0.02802(11) 0.02994(11) 0.01663(10) 0.00970(8) 0.00986(7) 0.01541(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.249(4) . ? C1 O1 1.254(4) . ? C1 C2 1.507(4) . ? C2 C8 1.381(5) . ? C2 C3 1.389(4) . ? C3 C4 1.393(4) . ? C3 H3 0.9300 . ? C4 C5 1.396(5) . ? C4 C6 1.455(4) . ? C5 C7 1.375(5) . ? C5 H5 0.9300 . ? C6 N4 1.323(4) . ? C6 N1 1.335(5) . ? C7 C8 1.394(5) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 O5 1.253(4) . ? C9 O6 1.266(4) . ? C9 C10 1.496(5) . ? C10 C16 1.380(5) . ? C10 C11 1.392(5) . ? C11 C12 1.387(5) . ? C11 H11 0.9300 . ? C12 C13 1.375(5) . ? C12 H12 0.9300 . ? C13 C14 1.397(5) . ? C13 H13 0.9300 . ? C14 C16 1.391(5) . ? C14 C15 1.466(5) . ? C15 N5 1.331(4) . ? C15 N8 1.332(4) . ? C16 H16 0.9300 . ? N1 N2 1.340(4) . ? N1 H1 0.86(5) . ? N2 N3 1.293(4) . ? N3 N4 1.350(4) . ? N5 N6 1.345(4) . ? N6 N7 1.302(4) . ? N7 N8 1.343(4) . ? O1 Sm1 2.357(2) . ? O2 Sm1 2.307(2) 2_567 ? O5 Sm1 2.645(3) . ? O6 Sm1 2.414(2) . ? O1W H1A 0.78(6) . ? O1W H1B 0.77(7) . ? O2W H2A 0.81(7) . ? O2W H2B 0.65(6) . ? O3W Sm1 2.485(2) . ? O3W H3A 0.91(6) . ? O3W H3B 0.80(6) . ? O4W Sm1 2.367(3) . ? O4W H4A 0.66(6) . ? O4W H4B 0.91(6) . ? O5W Sm1 2.431(3) . ? O5W H5A 0.73(6) . ? O5W H5B 0.73(6) . ? O6W Sm1 2.446(3) . ? O6W H6A 0.73(6) . ? O6W H6B 0.89(6) . ? Sm1 O2 2.307(2) 2_567 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 124.9(3) . . ? O2 C1 C2 117.3(3) . . ? O1 C1 C2 117.8(3) . . ? C8 C2 C3 120.0(3) . . ? C8 C2 C1 120.1(3) . . ? C3 C2 C1 119.9(3) . . ? C2 C3 C4 120.3(3) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C5 119.3(3) . . ? C3 C4 C6 121.8(3) . . ? C5 C4 C6 118.9(3) . . ? C7 C5 C4 120.1(3) . . ? C7 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? N4 C6 N1 107.4(3) . . ? N4 C6 C4 126.0(3) . . ? N1 C6 C4 126.6(3) . . ? C5 C7 C8 120.5(3) . . ? C5 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C2 C8 C7 119.7(3) . . ? C2 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? O5 C9 O6 121.1(3) . . ? O5 C9 C10 121.1(3) . . ? O6 C9 C10 117.7(3) . . ? C16 C10 C11 119.6(3) . . ? C16 C10 C9 119.2(3) . . ? C11 C10 C9 121.2(3) . . ? C12 C11 C10 119.6(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C11 120.7(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 120.3(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C16 C14 C13 118.7(3) . . ? C16 C14 C15 119.7(3) . . ? C13 C14 C15 121.6(3) . . ? N5 C15 N8 111.1(3) . . ? N5 C15 C14 123.8(3) . . ? N8 C15 C14 125.1(3) . . ? C10 C16 C14 121.1(3) . . ? C10 C16 H16 119.4 . . ? C14 C16 H16 119.4 . . ? C6 N1 N2 109.2(3) . . ? C6 N1 H1 135(3) . . ? N2 N1 H1 116(3) . . ? N3 N2 N1 106.4(3) . . ? N2 N3 N4 110.4(3) . . ? C6 N4 N3 106.7(3) . . ? C15 N5 N6 104.9(3) . . ? N7 N6 N5 109.6(3) . . ? N6 N7 N8 109.3(3) . . ? C15 N8 N7 105.2(3) . . ? C1 O1 Sm1 152.7(2) . . ? C1 O2 Sm1 148.3(2) . 2_567 ? C9 O5 Sm1 88.5(2) . . ? C9 O6 Sm1 99.1(2) . . ? H1A O1W H1B 102(6) . . ? H2A O2W H2B 104(7) . . ? Sm1 O3W H3A 117(4) . . ? Sm1 O3W H3B 128(5) . . ? H3A O3W H3B 105(5) . . ? Sm1 O4W H4A 123(6) . . ? Sm1 O4W H4B 129(4) . . ? H4A O4W H4B 108(7) . . ? Sm1 O5W H5A 116(5) . . ? Sm1 O5W H5B 128(5) . . ? H5A O5W H5B 115(7) . . ? Sm1 O6W H6A 144(5) . . ? Sm1 O6W H6B 122(4) . . ? H6A O6W H6B 94(6) . . ? O2 Sm1 O1 100.32(9) 2_567 . ? O2 Sm1 O4W 94.92(12) 2_567 . ? O1 Sm1 O4W 73.15(10) . . ? O2 Sm1 O6 132.78(9) 2_567 . ? O1 Sm1 O6 120.32(8) . . ? O4W Sm1 O6 76.74(10) . . ? O2 Sm1 O5W 86.14(10) 2_567 . ? O1 Sm1 O5W 142.02(11) . . ? O4W Sm1 O5W 144.11(11) . . ? O6 Sm1 O5W 76.47(9) . . ? O2 Sm1 O6W 76.80(10) 2_567 . ? O1 Sm1 O6W 73.92(10) . . ? O4W Sm1 O6W 143.88(11) . . ? O6 Sm1 O6W 134.10(10) . . ? O5W Sm1 O6W 71.26(11) . . ? O2 Sm1 O3W 155.53(10) 2_567 . ? O1 Sm1 O3W 75.38(9) . . ? O4W Sm1 O3W 106.45(11) . . ? O6 Sm1 O3W 65.61(9) . . ? O5W Sm1 O3W 83.45(11) . . ? O6W Sm1 O3W 78.89(10) . . ? O2 Sm1 O5 81.87(8) 2_567 . ? O1 Sm1 O5 145.07(9) . . ? O4W Sm1 O5 71.94(10) . . ? O6 Sm1 O5 51.16(8) . . ? O5W Sm1 O5 72.72(10) . . ? O6W Sm1 O5 138.98(10) . . ? O3W Sm1 O5 115.69(8) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.816 _refine_diff_density_min -0.937 _refine_diff_density_rms 0.098