# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_dd77 _database_code_depnum_ccdc_archive 'CCDC 194697' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7.50 H13.50 Er O12' _chemical_formula_weight 462.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4005(2) _cell_length_b 10.6486(2) _cell_length_c 13.6321(3) _cell_angle_alpha 105.3070(7) _cell_angle_beta 93.8350(8) _cell_angle_gamma 108.9350(12) _cell_volume 1358.02(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 890 _exptl_absorpt_coefficient_mu 6.240 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '4-circle diffractometer' _diffrn_measurement_method 'scintillation counter' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19707 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 30.03 _reflns_number_total 7905 _reflns_number_gt 6467 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius CAD4 software' _computing_cell_refinement 'Nonius CAD4 software' _computing_data_reduction 'XCAD (P.McArdle, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+2.7991P] 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 7905 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1278 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.52361(2) 0.58006(2) 0.188079(18) 0.01724(8) Uani 1 1 d . . . Er2 Er 1.01863(2) 1.05028(2) 0.186582(18) 0.01590(8) Uani 1 1 d . . . O1 O 0.5868(4) 0.7482(4) 0.0993(3) 0.0287(9) Uani 1 1 d . . . O2 O 1.1053(4) 1.2756(5) 0.1584(4) 0.0311(10) Uani 1 1 d . . . O3 O 1.2218(4) 1.1405(6) 0.3078(3) 0.0349(11) Uani 1 1 d . . . O4 O 0.6193(6) 0.5077(5) 0.3170(4) 0.0497(15) Uani 1 1 d . . . O5 O 0.3432(5) 0.4840(6) 0.2723(4) 0.0475(14) Uani 1 1 d . . . O6 O 0.4271(5) 0.7481(6) 0.2622(5) 0.0479(14) Uani 1 1 d . . . O1W O 1.1745(8) 1.7266(10) 0.3290(6) 0.088(3) Uani 1 1 d . . . O2W O 1.5723(9) 2.0352(9) 0.2992(8) 0.101(3) Uani 1 1 d . . . O3W O 0.8596(10) 0.4871(11) 0.4098(10) 0.137(4) Uani 1 1 d . . . O4W O 0.9441(12) 1.4271(11) 0.2234(8) 0.123(4) Uani 1 1 d . . . O5W O 0.6366(19) 1.392(3) 0.5221(10) 0.295(13) Uani 1 1 d . . . O6W O 1.3853(13) 2.203(5) 0.4893(9) 0.82(5) Uani 1 1 d . . . O1A O 0.8610(4) 1.0616(4) 0.0736(3) 0.0239(9) Uani 1 1 d . . . O2A O 1.1953(4) 1.0555(5) 0.0936(3) 0.0255(9) Uani 1 1 d . . . O3A O 0.4610(4) 0.3309(4) 0.1170(3) 0.0240(8) Uani 1 1 d . . . O4A O 0.4805(4) 0.2367(4) 0.2432(3) 0.0271(9) Uani 1 1 d . . . C1A C 0.5202(5) 0.8912(6) -0.0727(4) 0.0169(10) Uani 1 1 d . . . C2A C 0.6332(5) 0.9988(5) -0.0056(4) 0.0174(10) Uani 1 1 d . . . C3A C 0.6119(5) 1.1055(6) 0.0658(5) 0.0201(11) Uani 1 1 d . . . H3A H 0.6871 1.1769 0.1103 0.024 Uiso 1 1 calc R . . C4A C 0.4694(5) 0.2340(6) 0.1508(4) 0.0182(10) Uani 1 1 d . . . C5A C 0.7769(5) 1.0004(5) -0.0096(4) 0.0167(10) Uani 1 1 d . . . O1B O 0.3560(4) 0.5099(5) 0.0513(4) 0.0294(10) Uani 1 1 d . . . O2B O 0.7144(4) 0.5545(5) 0.1172(3) 0.0281(9) Uani 1 1 d . . . O3B O 0.9221(4) 0.8168(4) 0.0596(3) 0.0222(8) Uani 1 1 d . . . O4B O 1.0611(4) 0.8409(4) 0.1971(3) 0.0277(9) Uani 1 1 d . . . C1B C 0.0057(5) 0.3728(6) -0.0582(4) 0.0163(10) Uani 1 1 d . . . C2B C 0.1278(5) 0.4867(5) -0.0089(4) 0.0155(10) Uani 1 1 d . . . C3B C 0.1209(5) 0.6111(5) 0.0487(4) 0.0190(11) Uani 1 1 d . . . H3B H 0.2019 0.6854 0.0816 0.023 Uiso 1 1 calc R . . C4B C 0.9903(5) 0.7684(5) 0.1096(5) 0.0202(11) Uani 1 1 d . . . C5B C 0.2671(5) 0.4783(5) -0.0262(4) 0.0182(10) Uani 1 1 d . . . O1C O 0.8201(4) 0.9237(4) 0.2364(3) 0.0259(9) Uani 1 1 d . . . O2C O 0.7020(4) 0.7674(4) 0.3077(3) 0.0276(9) Uani 1 1 d . . . O3C O 0.9676(4) 1.2011(4) 0.3200(3) 0.0275(9) Uani 1 1 d . . . O4C O 0.8834(7) 1.2699(7) 0.4607(5) 0.0597(17) Uani 1 1 d . . . C1C C 0.9062(5) 0.9434(6) 0.4075(4) 0.0194(10) Uani 1 1 d . . . C2C C 1.0590(6) 1.1415(6) 0.5424(4) 0.0221(11) Uani 1 1 d . . . H2C H 1.0996 1.2376 0.5712 0.027 Uiso 1 1 calc R . . C3C C 0.9655(5) 1.0887(6) 0.4504(4) 0.0196(10) Uani 1 1 d . . . C4C C 0.8022(5) 0.8739(6) 0.3104(4) 0.0199(11) Uani 1 1 d . . . C5C C 0.9338(6) 1.1923(6) 0.4052(5) 0.0240(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01396(12) 0.01341(13) 0.01992(15) 0.00202(10) 0.00147(9) 0.00180(9) Er2 0.01320(12) 0.01195(13) 0.01991(15) 0.00262(9) 0.00122(9) 0.00311(8) O1 0.028(2) 0.018(2) 0.034(2) 0.0090(19) -0.0017(17) 0.0015(16) O2 0.032(2) 0.018(2) 0.036(3) 0.0073(19) 0.0069(18) 0.0004(17) O3 0.024(2) 0.046(3) 0.026(2) 0.004(2) -0.0034(17) 0.0075(19) O4 0.066(3) 0.019(2) 0.046(3) 0.012(2) -0.021(3) -0.004(2) O5 0.044(3) 0.028(3) 0.058(4) 0.005(3) 0.023(2) 0.000(2) O6 0.048(3) 0.037(3) 0.066(4) 0.011(3) 0.025(3) 0.025(3) O1W 0.090(5) 0.154(9) 0.080(5) 0.064(5) 0.040(4) 0.094(6) O2W 0.104(6) 0.062(5) 0.136(8) 0.034(5) -0.020(6) 0.034(5) O3W 0.111(7) 0.079(7) 0.206(12) 0.040(8) -0.030(7) 0.029(6) O4W 0.184(10) 0.114(9) 0.125(8) 0.052(7) 0.050(7) 0.105(8) O5W 0.240(18) 0.56(4) 0.090(10) 0.128(17) 0.045(10) 0.12(2) O6W 0.092(8) 1.66(11) 0.045(7) -0.12(2) 0.024(6) -0.24(2) O1A 0.0166(18) 0.020(2) 0.032(2) 0.0037(18) -0.0018(15) 0.0065(15) O2A 0.0161(18) 0.026(2) 0.030(2) 0.0039(18) 0.0057(15) 0.0051(16) O3A 0.029(2) 0.0099(18) 0.032(2) 0.0051(17) 0.0022(16) 0.0069(15) O4A 0.033(2) 0.021(2) 0.028(2) 0.0084(18) 0.0040(17) 0.0102(17) C1A 0.013(2) 0.015(2) 0.020(3) 0.003(2) 0.0013(18) 0.0038(18) C2A 0.013(2) 0.015(2) 0.025(3) 0.006(2) 0.0037(19) 0.0064(18) C3A 0.011(2) 0.015(2) 0.031(3) 0.002(2) -0.0001(19) 0.0045(18) C4A 0.011(2) 0.016(2) 0.025(3) 0.004(2) 0.0046(18) 0.0030(18) C5A 0.015(2) 0.010(2) 0.025(3) 0.005(2) 0.0021(19) 0.0047(17) O1B 0.0183(19) 0.026(2) 0.035(3) -0.0015(19) -0.0072(16) 0.0077(17) O2B 0.022(2) 0.029(2) 0.032(2) 0.0065(19) 0.0065(17) 0.0103(17) O3B 0.0238(19) 0.0146(19) 0.029(2) 0.0057(16) 0.0043(15) 0.0084(15) O4B 0.026(2) 0.020(2) 0.032(2) 0.0005(18) -0.0052(17) 0.0091(16) C1B 0.014(2) 0.014(2) 0.020(3) 0.004(2) 0.0008(18) 0.0059(18) C2B 0.010(2) 0.014(2) 0.021(3) 0.003(2) 0.0018(17) 0.0056(17) C3B 0.013(2) 0.011(2) 0.029(3) 0.000(2) -0.0002(19) 0.0032(18) C4B 0.016(2) 0.009(2) 0.033(3) 0.005(2) 0.004(2) 0.0020(18) C5B 0.014(2) 0.013(2) 0.028(3) 0.005(2) 0.0052(19) 0.0053(18) O1C 0.025(2) 0.023(2) 0.024(2) 0.0083(18) 0.0020(16) 0.0008(16) O2C 0.027(2) 0.017(2) 0.027(2) 0.0062(17) -0.0025(16) -0.0056(16) O3C 0.042(2) 0.018(2) 0.026(2) 0.0074(17) 0.0111(18) 0.0136(18) O4C 0.105(5) 0.060(4) 0.052(4) 0.027(3) 0.038(3) 0.067(4) C1C 0.017(2) 0.016(3) 0.023(3) 0.006(2) 0.0017(19) 0.0033(19) C2C 0.028(3) 0.018(3) 0.016(3) 0.003(2) -0.001(2) 0.005(2) C3C 0.020(2) 0.014(2) 0.023(3) 0.006(2) 0.003(2) 0.0032(19) C4C 0.015(2) 0.012(2) 0.026(3) 0.000(2) -0.0006(19) 0.0005(18) C5C 0.027(3) 0.019(3) 0.025(3) 0.005(2) 0.002(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O1B 2.249(4) . ? Er1 O2B 2.327(4) . ? Er1 O5 2.355(5) . ? Er1 O2C 2.357(4) . ? Er1 O6 2.362(5) . ? Er1 O1 2.365(4) . ? Er1 O4 2.378(5) . ? Er1 O3A 2.416(4) . ? Er2 O1A 2.228(4) . ? Er2 O2A 2.295(4) . ? Er2 O3C 2.304(4) . ? Er2 O1C 2.326(4) . ? Er2 O3 2.344(4) . ? Er2 O2 2.418(4) . ? Er2 O4B 2.447(4) . ? Er2 O3B 2.462(4) . ? Er2 C4B 2.814(5) . ? O1A C5A 1.258(7) . ? O2A C5A 1.243(7) 2_775 ? O3A C4A 1.261(7) . ? O4A C4A 1.249(7) . ? C1A C3A 1.394(7) 2_675 ? C1A C2A 1.399(7) . ? C1A C4A 1.511(7) 2_665 ? C2A C3A 1.377(7) . ? C2A C5A 1.494(7) . ? C3A C1A 1.394(7) 2_675 ? C4A C1A 1.511(7) 2_665 ? C5A O2A 1.243(7) 2_775 ? O1B C5B 1.250(7) . ? O2B C5B 1.243(7) 2_665 ? O3B C4B 1.261(7) . ? O4B C4B 1.260(7) . ? C1B C3B 1.392(7) 2_565 ? C1B C2B 1.411(7) . ? C1B C4B 1.497(7) 2_665 ? C2B C3B 1.378(7) . ? C2B C5B 1.510(7) . ? C3B C1B 1.392(7) 2_565 ? C4B C1B 1.497(7) 2_665 ? C5B O2B 1.243(7) 2_665 ? O1C C4C 1.255(7) . ? O2C C4C 1.257(6) . ? O3C C5C 1.254(7) . ? O4C C5C 1.238(7) . ? C1C C2C 1.386(8) 2_776 ? C1C C3C 1.404(7) . ? C1C C4C 1.497(7) . ? C2C C1C 1.386(8) 2_776 ? C2C C3C 1.394(7) . ? C3C C5C 1.508(8) . ? 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 O1B Er1 O2B 104.58(16) . . ? O1B Er1 O5 84.8(2) . . ? O2B Er1 O5 145.46(19) . . ? O1B Er1 O2C 147.33(17) . . ? O2B Er1 O2C 79.77(15) . . ? O5 Er1 O2C 110.25(17) . . ? O1B Er1 O6 86.00(18) . . ? O2B Er1 O6 142.61(18) . . ? O5 Er1 O6 69.98(19) . . ? O2C Er1 O6 73.22(17) . . ? O1B Er1 O1 73.30(16) . . ? O2B Er1 O1 74.56(16) . . ? O5 Er1 O1 139.23(18) . . ? O2C Er1 O1 76.94(14) . . ? O6 Er1 O1 74.50(18) . . ? O1B Er1 O4 144.15(18) . . ? O2B Er1 O4 81.4(2) . . ? O5 Er1 O4 72.8(2) . . ? O2C Er1 O4 68.27(16) . . ? O6 Er1 O4 110.9(2) . . ? O1 Er1 O4 140.56(16) . . ? O1B Er1 O3A 73.15(15) . . ? O2B Er1 O3A 76.03(15) . . ? O5 Er1 O3A 75.13(17) . . ? O2C Er1 O3A 137.77(14) . . ? O6 Er1 O3A 140.68(16) . . ? O1 Er1 O3A 127.28(15) . . ? O4 Er1 O3A 74.23(16) . . ? O1A Er2 O2A 101.09(15) . . ? O1A Er2 O3C 91.36(15) . . ? O2A Er2 O3C 137.47(15) . . ? O1A Er2 O1C 80.76(15) . . ? O2A Er2 O1C 149.71(16) . . ? O3C Er2 O1C 72.11(15) . . ? O1A Er2 O3 154.85(18) . . ? O2A Er2 O3 73.77(15) . . ? O3C Er2 O3 77.91(16) . . ? O1C Er2 O3 116.35(16) . . ? O1A Er2 O2 71.79(15) . . ? O2A Er2 O2 71.52(16) . . ? O3C Er2 O2 74.29(15) . . ? O1C Er2 O2 135.57(15) . . ? O3 Er2 O2 83.36(18) . . ? O1A Er2 O4B 126.82(14) . . ? O2A Er2 O4B 78.69(15) . . ? O3C Er2 O4B 124.70(15) . . ? O1C Er2 O4B 76.38(15) . . ? O3 Er2 O4B 77.06(17) . . ? O2 Er2 O4B 147.92(15) . . ? O1A Er2 O3B 74.36(14) . . ? O2A Er2 O3B 79.46(14) . . ? O3C Er2 O3B 142.91(14) . . ? O1C Er2 O3B 71.89(14) . . ? O3 Er2 O3B 127.01(16) . . ? O2 Er2 O3B 129.35(15) . . ? O4B Er2 O3B 53.07(13) . . ? O1A Er2 C4B 100.85(16) . . ? O2A Er2 C4B 76.27(16) . . ? O3C Er2 C4B 141.18(16) . . ? O1C Er2 C4B 73.72(16) . . ? O3 Er2 C4B 101.69(18) . . ? O2 Er2 C4B 144.53(16) . . ? O4B Er2 C4B 26.56(15) . . ? O3B Er2 C4B 26.59(14) . . ? C5A O1A Er2 146.8(4) . . ? C5A O2A Er2 143.1(4) 2_775 . ? C4A O3A Er1 135.6(4) . . ? C3A C1A C2A 119.2(5) 2_675 . ? C3A C1A C4A 116.7(5) 2_675 2_665 ? C2A C1A C4A 124.1(4) . 2_665 ? C3A C2A C1A 119.5(5) . . ? C3A C2A C5A 119.1(5) . . ? C1A C2A C5A 121.4(5) . . ? C2A C3A C1A 121.3(5) . 2_675 ? O4A C4A O3A 126.1(5) . . ? O4A C4A C1A 117.4(5) . 2_665 ? O3A C4A C1A 116.3(5) . 2_665 ? O2A C5A O1A 125.4(5) 2_775 . ? O2A C5A C2A 118.4(5) 2_775 . ? O1A C5A C2A 116.1(5) . . ? C5B O1B Er1 176.1(4) . . ? C5B O2B Er1 131.5(4) 2_665 . ? C4B O3B Er2 92.5(3) . . ? C4B O4B Er2 93.2(3) . . ? C3B C1B C2B 119.1(5) 2_565 . ? C3B C1B C4B 119.5(5) 2_565 2_665 ? C2B C1B C4B 121.0(4) . 2_665 ? C3B C2B C1B 120.1(4) . . ? C3B C2B C5B 119.0(4) . . ? C1B C2B C5B 120.7(4) . . ? C2B C3B C1B 120.8(5) . 2_565 ? O4B C4B O3B 120.9(5) . . ? O4B C4B C1B 120.9(5) . 2_665 ? O3B C4B C1B 118.0(5) . 2_665 ? O4B C4B Er2 60.2(3) . . ? O3B C4B Er2 60.9(3) . . ? C1B C4B Er2 170.1(4) 2_665 . ? O2B C5B O1B 125.2(5) 2_665 . ? O2B C5B C2B 116.7(5) 2_665 . ? O1B C5B C2B 118.0(5) . . ? C4C O1C Er2 131.9(3) . . ? C4C O2C Er1 140.1(4) . . ? C5C O3C Er2 132.5(4) . . ? C2C C1C C3C 119.5(5) 2_776 . ? C2C C1C C4C 117.5(5) 2_776 . ? C3C C1C C4C 122.9(5) . . ? C1C C2C C3C 122.7(5) 2_776 . ? C2C C3C C1C 117.8(5) . . ? C2C C3C C5C 117.4(5) . . ? C1C C3C C5C 124.8(5) . . ? O1C C4C O2C 123.8(5) . . ? O1C C4C C1C 118.7(5) . . ? O2C C4C C1C 117.5(5) . . ? O4C C5C O3C 124.9(6) . . ? O4C C5C C3C 115.5(6) . . ? O3C C5C C3C 119.4(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.647 _refine_diff_density_min -3.773 _refine_diff_density_rms 0.325 data_multiscan _database_code_depnum_ccdc_archive 'CCDC 862348' #TrackingRef 'C1-archive.cif' _audit_creation_date 2012-10-25T13:58:05-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H40 O41 Tm4' _chemical_formula_sum 'C30 H40 O41 Tm4' _chemical_formula_weight 1732.34 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 11.2874(4) _cell_length_b 17.5352(3) _cell_length_c 11.8917(4) _cell_angle_alpha 90 _cell_angle_beta 106.7230(10) _cell_angle_gamma 90 _cell_volume 2254.14(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 42564 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.923 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.2098 _exptl_absorpt_correction_T_max 0.2568 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_unetI/netI 0.0389 _diffrn_reflns_number 28697 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 5320 _reflns_number_gt 4432 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0509P)^2^+4.4560P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00097(11) _refine_ls_number_reflns 5320 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 2.732 _refine_diff_density_min -1.746 _refine_diff_density_rms 0.2 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Tm01 Tm 0.23855(2) 0.998254(12) 0.35657(2) 0.01927(9) Uani 1 1 d . . . Tm02 Tm -0.20569(2) 1.012803(13) 0.16784(2) 0.02055(9) Uani 1 1 d . . . O003 O 0.3798(4) 0.8946(2) 0.3911(3) 0.0274(9) Uani 1 1 d . . . O004 O -0.3541(4) 0.9733(2) 0.2554(4) 0.0350(10) Uani 1 1 d . . . O005 O -0.3176(4) 1.1280(2) 0.1631(4) 0.0378(10) Uani 1 1 d . . . O006 O -0.1105(4) 0.9500(2) 0.0359(4) 0.0342(10) Uani 1 1 d . . . O007 O 0.2801(4) 1.1101(2) 0.4754(4) 0.0317(9) Uani 1 1 d . . . O008 O 0.1070(4) 1.0519(2) 0.4684(3) 0.0271(8) Uani 1 1 d . . . O009 O 0.3461(4) 0.9426(2) 0.5479(3) 0.0280(9) Uani 1 1 d . . . O010 O -0.2523(4) 0.8878(2) 0.0931(3) 0.0259(8) Uani 1 1 d . . . O011 O -0.1359(4) 1.0793(2) 0.3511(4) 0.0311(9) Uani 1 1 d . . . O012 O 0.1877(5) 0.9330(3) 0.1731(4) 0.0419(11) Uani 1 1 d . . . O013 O -0.3534(5) 1.0233(3) -0.0159(4) 0.0418(11) Uani 1 1 d . . . O014 O 0.4305(5) 1.1036(2) 0.1489(4) 0.0387(11) Uani 1 1 d . . . C015 C -0.0455(5) 0.8191(3) 0.3946(5) 0.0219(11) Uani 1 1 d . . . O016 O 0.1104(5) 1.0735(2) 0.2252(4) 0.0393(11) Uani 1 1 d . . . O017 O -0.0814(4) 1.1000(2) 0.1219(4) 0.0313(9) Uani 1 1 d . . . O018 O 0.1213(4) 0.8970(2) 0.3858(4) 0.0314(9) Uani 1 1 d . . . C019 C 0.1330(5) 1.1804(3) 0.5419(5) 0.0226(11) Uani 1 1 d . . . C020 C 0.0069(6) 0.8912(3) 0.3563(5) 0.0226(11) Uani 1 1 d . . . O021 O 0.3925(4) 1.0542(2) 0.3066(4) 0.0313(9) Uani 1 1 d . . . C022 C 0.0751(5) 1.1813(3) 0.0994(4) 0.0206(10) Uani 1 1 d . . . O023 O -0.0669(4) 0.9382(2) 0.2932(4) 0.0315(9) Uani 1 1 d . . . C024 C 0.1416(5) 1.1810(3) 0.0167(5) 0.0221(11) Uani 1 1 d . . . O025 O 0.2746(12) 0.75 0.9815(10) 0.100(4) Uani 1 2 d S . . C026 C -0.0035(7) 0.75 0.3641(7) 0.0234(15) Uani 1 2 d S . . H026 H 0.0543 0.75 0.322 0.028 Uiso 1 2 calc SR . . C027 C 0.1754(5) 1.1100(3) 0.4948(5) 0.0228(11) Uani 1 1 d . . . C028 C 0.5538(5) 1.1802(3) 0.4352(4) 0.0208(10) Uani 1 1 d . . . C029 C 0.4374(8) 1.25 0.2630(7) 0.0236(15) Uani 1 2 d S . . H029 H 0.3857 1.25 0.1864 0.028 Uiso 1 2 calc SR . . C030 C 0.4290(5) 1.1075(3) 0.2525(5) 0.0226(11) Uani 1 1 d . . . O031 O 0.1828(11) 0.75 0.6851(8) 0.076(3) Uani 1 2 d S . . C032 C 0.0446(8) 1.25 0.1407(7) 0.0238(16) Uani 1 2 d S . . H032 H 0.0026 1.25 0.1975 0.029 Uiso 1 2 calc SR . . C033 C 0.0332(6) 1.1114(3) 0.1506(5) 0.0233(11) Uani 1 1 d . . . C034 C 0.4758(5) 1.1805(3) 0.3198(4) 0.0204(10) Uani 1 1 d . . . C035 C -0.1696(6) 0.8898(3) 0.0390(5) 0.0245(11) Uani 1 1 d . . . C037 C 0.1758(8) 1.25 0.5112(7) 0.0238(16) Uani 1 2 d S . . H037 H 0.2339 1.25 0.4694 0.029 Uiso 1 2 calc SR . . O038 O 0.4483(7) 0.1706(3) 0.7003(7) 0.075(2) Uani 1 1 d . . . O039 O 0.5019(6) 0.8456(4) 0.0611(7) 0.0746(19) Uani 1 1 d . . . C040 C 0.3907(5) 0.8896(3) 0.4989(5) 0.0220(11) Uani 1 1 d . . . C044 C 0.1750(8) 1.25 -0.0229(7) 0.0222(15) Uani 1 2 d S . . O045 O 0.204(2) 0.75 1.1783(16) 0.181(8) Uani 1 2 d S . . C046 C 0.5913(8) 1.25 0.4921(7) 0.0249(16) Uani 1 2 d S . . H046 H 0.642 1.25 0.5692 0.03 Uiso 1 2 calc SR . . 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 Tm01 0.02454(15) 0.01520(13) 0.01904(14) 0.00101(7) 0.00783(11) 0.00004(7) Tm02 0.02575(15) 0.01691(13) 0.02013(13) -0.00109(8) 0.00843(10) -0.00024(8) O003 0.038(3) 0.026(2) 0.0192(19) 0.0056(14) 0.0103(18) 0.0088(16) O004 0.042(3) 0.033(2) 0.038(2) -0.0077(18) 0.024(2) -0.0083(19) O005 0.036(3) 0.025(2) 0.050(3) -0.0106(18) 0.009(2) 0.0048(17) O006 0.052(3) 0.020(2) 0.041(2) -0.0052(16) 0.028(2) -0.0096(18) O007 0.032(2) 0.022(2) 0.045(3) -0.0092(17) 0.018(2) -0.0014(16) O008 0.034(2) 0.0191(19) 0.031(2) -0.0019(15) 0.0135(18) -0.0018(15) O009 0.037(2) 0.0217(19) 0.0245(19) -0.0019(14) 0.0085(18) 0.0058(16) O010 0.034(2) 0.0189(19) 0.030(2) -0.0033(14) 0.0183(19) 0.0010(15) O011 0.041(3) 0.028(2) 0.024(2) -0.0031(15) 0.0090(19) 0.0002(17) O012 0.058(3) 0.040(3) 0.027(2) -0.0075(18) 0.011(2) 0.000(2) O013 0.043(3) 0.032(2) 0.042(3) -0.0082(19) -0.002(2) 0.005(2) O014 0.067(3) 0.027(2) 0.021(2) -0.0058(15) 0.012(2) -0.011(2) C015 0.024(3) 0.016(2) 0.025(3) 0.0006(18) 0.007(2) -0.0012(19) O016 0.056(3) 0.029(2) 0.029(2) 0.0122(17) 0.006(2) 0.013(2) O017 0.033(3) 0.025(2) 0.041(2) -0.0008(17) 0.019(2) -0.0054(16) O018 0.027(2) 0.0188(19) 0.050(3) 0.0006(17) 0.015(2) -0.0044(15) C019 0.026(3) 0.019(3) 0.026(3) 0.0012(19) 0.011(2) -0.0003(19) C020 0.035(3) 0.014(2) 0.022(3) -0.0018(18) 0.014(2) 0.000(2) O021 0.040(3) 0.021(2) 0.037(2) -0.0031(16) 0.019(2) -0.0056(17) C022 0.026(3) 0.016(2) 0.021(3) 0.0019(17) 0.009(2) -0.0007(19) O023 0.043(3) 0.0194(19) 0.029(2) 0.0056(15) 0.0047(19) 0.0059(17) C024 0.028(3) 0.017(3) 0.023(3) -0.0007(18) 0.011(2) 0.0025(19) O025 0.110(10) 0.093(8) 0.085(8) 0 0.012(7) 0 C026 0.023(4) 0.023(4) 0.025(4) 0 0.010(3) 0 C027 0.031(3) 0.018(2) 0.020(3) -0.0002(18) 0.009(2) 0.003(2) C028 0.027(3) 0.017(2) 0.017(2) -0.0004(18) 0.005(2) -0.0008(19) C029 0.029(4) 0.022(4) 0.019(4) 0 0.006(3) 0 C030 0.024(3) 0.019(2) 0.024(3) -0.0020(19) 0.007(2) -0.0014(19) O031 0.108(9) 0.045(5) 0.067(6) 0 0.010(6) 0 C032 0.032(5) 0.018(4) 0.027(4) 0 0.016(3) 0 C033 0.036(3) 0.015(2) 0.021(2) -0.0020(18) 0.011(2) 0.000(2) C034 0.028(3) 0.015(2) 0.019(2) 0.0009(17) 0.008(2) -0.0005(19) C035 0.034(3) 0.019(3) 0.021(3) 0.0000(19) 0.007(2) 0.002(2) C037 0.025(4) 0.021(4) 0.028(4) 0 0.012(3) 0 O038 0.069(5) 0.056(4) 0.115(6) -0.021(4) 0.051(4) -0.007(3) O039 0.047(4) 0.075(4) 0.100(5) 0.031(4) 0.018(4) 0.001(3) C040 0.023(3) 0.020(2) 0.023(3) -0.0012(19) 0.005(2) 0.0003(19) C044 0.030(4) 0.016(3) 0.023(4) 0 0.012(3) 0 O045 0.20(2) 0.208(19) 0.150(16) 0 0.073(15) 0 C046 0.036(5) 0.019(4) 0.018(3) 0 0.004(3) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Tm01 O021 2.220(4) . ? Tm01 O016 2.230(4) . ? Tm01 O018 2.301(4) . ? Tm01 O003 2.374(4) . ? Tm01 O007 2.384(4) . ? Tm01 O012 2.382(4) . ? Tm01 O008 2.449(4) . ? Tm01 O009 2.453(4) . ? Tm01 C027 2.779(5) . ? Tm01 C040 2.787(5) . ? Tm02 O023 2.245(4) . ? Tm02 O017 2.247(4) . ? Tm02 O004 2.318(4) . ? Tm02 O013 2.343(5) . ? Tm02 O010 2.367(4) . ? Tm02 O005 2.374(4) . ? Tm02 O011 2.396(4) . ? Tm02 O006 2.408(4) . ? Tm02 C035 2.744(5) . ? O003 C040 1.256(6) . ? O006 C035 1.257(7) . ? O007 C027 1.268(7) . ? O008 C027 1.262(7) . ? O009 C040 1.274(6) . ? O010 C035 1.278(7) . ? O014 C030 1.238(6) . ? C015 C026 1.387(6) . ? C015 C019 1.405(7) 3_576 ? C015 C020 1.519(7) . ? O016 C033 1.242(7) . ? O017 C033 1.255(7) . ? O018 C020 1.241(7) . ? C019 C037 1.399(6) . ? C019 C015 1.405(7) 3_576 ? C019 C027 1.491(7) . ? C020 O023 1.256(7) . ? O021 C030 1.269(6) . ? C022 C032 1.382(6) . ? C022 C024 1.399(7) . ? C022 C033 1.504(7) . ? C024 C044 1.390(6) . ? C024 C035 1.482(7) 3_575 ? C026 C015 1.387(6) 4_575 ? C028 C046 1.404(6) . ? C028 C034 1.400(7) . ? C028 C040 1.491(7) 3_676 ? C029 C034 1.401(6) 4_585 ? C029 C034 1.401(6) . ? C030 C034 1.521(7) . ? C032 C022 1.382(6) 4_585 ? C035 C024 1.482(7) 3_575 ? C037 C019 1.399(6) 4_585 ? C040 C028 1.491(7) 3_676 ? C044 C024 1.390(6) 4_585 ? C046 C028 1.404(6) 4_585 ? 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 O021 Tm01 O016 87.20(17) . . ? O021 Tm01 O018 155.54(14) . . ? O016 Tm01 O018 106.08(17) . . ? O021 Tm01 O003 81.13(15) . . ? O016 Tm01 O003 147.32(15) . . ? O018 Tm01 O003 76.71(15) . . ? O021 Tm01 O007 76.07(14) . . ? O016 Tm01 O007 84.61(16) . . ? O018 Tm01 O007 124.71(15) . . ? O003 Tm01 O007 121.30(15) . . ? O021 Tm01 O012 88.16(16) . . ? O016 Tm01 O012 72.87(17) . . ? O018 Tm01 O012 76.72(16) . . ? O003 Tm01 O012 76.33(15) . . ? O007 Tm01 O012 153.15(16) . . ? O021 Tm01 O008 128.27(14) . . ? O016 Tm01 O008 77.34(15) . . ? O018 Tm01 O008 75.48(13) . . ? O003 Tm01 O008 133.03(13) . . ? O007 Tm01 O008 53.75(14) . . ? O012 Tm01 O008 131.13(16) . . ? O021 Tm01 O009 101.98(15) . . ? O016 Tm01 O009 159.02(15) . . ? O018 Tm01 O009 72.86(15) . . ? O003 Tm01 O009 53.59(12) . . ? O007 Tm01 O009 79.47(14) . . ? O012 Tm01 O009 125.66(15) . . ? O008 Tm01 O009 82.22(13) . . ? O021 Tm01 C027 101.58(15) . . ? O016 Tm01 C027 76.85(16) . . ? O018 Tm01 C027 101.42(15) . . ? O003 Tm01 C027 135.33(15) . . ? O007 Tm01 C027 27.07(15) . . ? O012 Tm01 C027 147.66(17) . . ? O008 Tm01 C027 27.00(15) . . ? O009 Tm01 C027 82.79(14) . . ? O021 Tm01 C040 94.11(16) . . ? O016 Tm01 C040 172.63(16) . . ? O018 Tm01 C040 70.20(16) . . ? O003 Tm01 C040 26.66(14) . . ? O007 Tm01 C040 102.75(15) . . ? O012 Tm01 C040 99.91(16) . . ? O008 Tm01 C040 107.25(14) . . ? O009 Tm01 C040 27.19(14) . . ? C027 Tm01 C040 109.91(15) . . ? O023 Tm02 O017 101.09(16) . . ? O023 Tm02 O004 89.10(17) . . ? O017 Tm02 O004 153.53(15) . . ? O023 Tm02 O013 146.95(15) . . ? O017 Tm02 O013 92.65(18) . . ? O004 Tm02 O013 91.73(18) . . ? O023 Tm02 O010 75.36(14) . . ? O017 Tm02 O010 128.76(14) . . ? O004 Tm02 O010 77.33(14) . . ? O013 Tm02 O010 72.62(15) . . ? O023 Tm02 O005 140.89(15) . . ? O017 Tm02 O005 77.33(16) . . ? O004 Tm02 O005 79.41(16) . . ? O013 Tm02 O005 71.33(16) . . ? O010 Tm02 O005 136.02(15) . . ? O023 Tm02 O011 72.28(15) . . ? O017 Tm02 O011 79.93(15) . . ? O004 Tm02 O011 80.07(15) . . ? O013 Tm02 O011 140.28(15) . . ? O010 Tm02 O011 140.48(13) . . ? O005 Tm02 O011 68.96(15) . . ? O023 Tm02 O006 79.00(16) . . ? O017 Tm02 O006 74.07(14) . . ? O004 Tm02 O006 132.22(14) . . ? O013 Tm02 O006 76.10(17) . . ? O010 Tm02 O006 54.89(13) . . ? O005 Tm02 O006 135.04(16) . . ? O011 Tm02 O006 136.34(16) . . ? O023 Tm02 C035 74.07(16) . . ? O017 Tm02 C035 101.31(16) . . ? O004 Tm02 C035 104.99(16) . . ? O013 Tm02 C035 73.82(16) . . ? O010 Tm02 C035 27.72(15) . . ? O005 Tm02 C035 145.00(16) . . ? O011 Tm02 C035 145.88(16) . . ? O006 Tm02 C035 27.25(15) . . ? C040 O003 Tm01 95.3(3) . . ? C035 O006 Tm02 91.4(3) . . ? C027 O007 Tm01 94.1(3) . . ? C027 O008 Tm01 91.3(3) . . ? C040 O009 Tm01 91.2(3) . . ? C035 O010 Tm02 92.8(3) . . ? C026 C015 C019 119.4(5) . 3_576 ? C026 C015 C020 117.2(5) . . ? C019 C015 C020 123.4(5) 3_576 . ? C033 O016 Tm01 175.7(4) . . ? C033 O017 Tm02 135.1(4) . . ? C020 O018 Tm01 128.1(4) . . ? C037 C019 C015 119.0(5) . 3_576 ? C037 C019 C027 116.9(5) . . ? C015 C019 C027 123.9(5) 3_576 . ? O018 C020 O023 124.9(5) . . ? O018 C020 C015 116.5(5) . . ? O023 C020 C015 118.5(5) . . ? C030 O021 Tm01 148.7(4) . . ? C032 C022 C024 119.5(5) . . ? C032 C022 C033 115.3(5) . . ? C024 C022 C033 125.2(4) . . ? C020 O023 Tm02 174.3(4) . . ? C044 C024 C022 119.2(5) . . ? C044 C024 C035 117.6(5) . 3_575 ? C022 C024 C035 123.0(5) . 3_575 ? C015 C026 C015 121.8(7) . 4_575 ? O008 C027 O007 119.5(5) . . ? O008 C027 C019 121.5(5) . . ? O007 C027 C019 118.9(5) . . ? O008 C027 Tm01 61.7(3) . . ? O007 C027 Tm01 58.8(3) . . ? C019 C027 Tm01 166.2(4) . . ? C046 C028 C034 119.1(5) . . ? C046 C028 C040 116.1(5) . 3_676 ? C034 C028 C040 124.7(4) . 3_676 ? C034 C029 C034 121.0(7) 4_585 . ? O014 C030 O021 124.3(5) . . ? O014 C030 C034 117.9(5) . . ? O021 C030 C034 117.8(5) . . ? C022 C032 C022 121.4(7) 4_585 . ? O016 C033 O017 124.4(5) . . ? O016 C033 C022 119.2(5) . . ? O017 C033 C022 116.1(5) . . ? C029 C034 C028 119.7(5) . . ? C029 C034 C030 117.7(5) . . ? C028 C034 C030 122.5(4) . . ? O006 C035 O010 120.6(5) . . ? O006 C035 C024 120.5(5) . 3_575 ? O010 C035 C024 118.9(5) . 3_575 ? O006 C035 Tm02 61.3(3) . . ? O010 C035 Tm02 59.5(3) . . ? C024 C035 Tm02 173.0(4) 3_575 . ? C019 C037 C019 121.4(7) . 4_585 ? O003 C040 O009 118.8(5) . . ? O003 C040 C028 119.8(5) . 3_676 ? O009 C040 C028 121.3(5) . 3_676 ? O003 C040 Tm01 58.0(3) . . ? O009 C040 Tm01 61.6(3) . . ? C028 C040 Tm01 166.6(4) 3_676 . ? C024 C044 C024 121.2(7) 4_585 . ? C028 C046 C028 121.3(7) 4_585 . ? # END of CIF data_shelxl _database_code_depnum_ccdc_archive 'CCDC 862350' #TrackingRef 'import.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H29 O25 Tm2' _chemical_formula_weight 947.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2850(2) _cell_length_b 11.5717(3) _cell_length_c 13.5114(4) _cell_angle_alpha 85.5810(10) _cell_angle_beta 69.2090(10) _cell_angle_gamma 63.7550(10) _cell_volume 1342.23(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 914 _exptl_absorpt_coefficient_mu 6.676 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30939 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 42.19 _reflns_number_total 18620 _reflns_number_gt 15066 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0063(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 18620 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1447 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.461 _refine_ls_restrained_S_all 1.461 _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 Tm1 Tm 0.555394(13) 0.275444(12) 0.320310(9) 0.01453(4) Uani 1 1 d . . . Tm2 Tm 0.531178(14) -0.203020(12) 0.309302(10) 0.01488(4) Uani 1 1 d . . . O03 O 0.3929(3) -0.0151(2) 0.43527(19) 0.0189(4) Uani 1 1 d . . . O04 O 0.6196(3) -0.0462(2) 0.23173(18) 0.0193(4) Uani 1 1 d . . . O05 O 0.4007(3) 0.4814(2) 0.4260(2) 0.0233(5) Uani 1 1 d . . . O06 O 0.7152(3) 0.3024(3) 0.3885(2) 0.0229(4) Uani 1 1 d . . . O07 O 0.7003(3) -0.2797(2) 0.13883(19) 0.0236(4) Uani 1 1 d . . . O08 O 0.2967(3) 0.4332(3) 0.3280(2) 0.0253(5) Uani 1 1 d . . . O09 O 0.6995(3) 0.0622(2) 0.3577(2) 0.0225(4) Uani 1 1 d . . . O10 O 0.2716(3) 0.2253(3) 0.6345(2) 0.0237(4) Uani 1 1 d . . . O11 O 0.5144(3) 0.1650(2) 0.2120(2) 0.0253(5) Uani 1 1 d . . . O12 O 0.5806(4) 0.4223(3) 0.1940(3) 0.0374(7) Uani 1 1 d . . . O13 O 0.8682(3) -0.2463(4) -0.0030(3) 0.0430(8) Uani 1 1 d . . . O14 O 0.5972(4) 0.2726(4) 0.7725(3) 0.0386(7) Uani 1 1 d . . . C15 C 0.1382(3) 0.2472(3) 0.5187(2) 0.0155(4) Uani 1 1 d . . . O16 O 0.6529(3) -0.4222(3) 0.3256(2) 0.0311(6) Uani 1 1 d . . . C17 C 0.8655(3) 0.2776(3) 0.4921(2) 0.0151(4) Uani 1 1 d . . . O18 O 0.7992(3) 0.1776(3) 0.1801(2) 0.0355(6) Uani 1 1 d . . . O19 O 0.3005(3) -0.0124(2) 0.3103(2) 0.0230(4) Uani 1 1 d . . . O20 O 0.6383(3) 0.2454(3) 0.5516(2) 0.0270(5) Uani 1 1 d . . . O22 O 0.3913(3) 0.2356(3) 0.4637(2) 0.0254(5) Uani 1 1 d . . . C23 C 0.5567(3) 0.0487(3) 0.1840(2) 0.0169(4) Uani 1 1 d . . . C24 C 0.1428(3) 0.1563(3) 0.4522(2) 0.0163(4) Uani 1 1 d . . . C25 C 0.1397(3) 0.6281(3) 0.4457(2) 0.0162(4) Uani 1 1 d . . . C26 C 1.0067(3) 0.1720(3) 0.4407(3) 0.0183(5) Uani 1 1 d . . . H26 H 1.0105 0.1106 0.3978 0.022 Uiso 1 1 calc R . . C28 C 0.2778(3) 0.2342(3) 0.5389(2) 0.0166(4) Uani 1 1 d . . . C30 C 0.5280(3) 0.0214(3) 0.0892(2) 0.0161(4) Uani 1 1 d . . . C31 C 0.4200(4) 0.1223(3) 0.0540(2) 0.0189(5) Uani 1 1 d . . . H31 H 0.3654 0.2039 0.0913 0.023 Uiso 1 1 calc R . . C32 C -0.0031(3) 0.3548(3) 0.5677(2) 0.0176(5) Uani 1 1 d . . . H32 H -0.0070 0.4167 0.6102 0.021 Uiso 1 1 calc R . . C33 C 0.7344(4) -0.2166(3) 0.0602(3) 0.0205(5) Uani 1 1 d . . . C38 C 0.6068(3) -0.1028(3) 0.0350(2) 0.0163(4) Uani 1 1 d . . . C39 C 0.7263(3) 0.2783(3) 0.4780(2) 0.0162(4) Uani 1 1 d . . . C40 C 0.2873(3) 0.5081(3) 0.3966(3) 0.0193(5) Uani 1 1 d . . . C41 C 0.2881(3) 0.0377(3) 0.3954(2) 0.0174(4) Uani 1 1 d . . . O44 O 0.9571(5) 0.4140(5) 0.2607(5) 0.0842(18) Uani 1 1 d . . . O43 O 0.0039(5) 0.7139(6) 0.1717(4) 0.0785(16) Uani 1 1 d . . . O34 O 0.0999(6) 0.0951(8) 0.1713(5) 0.116(3) Uani 1 1 d . . . O35 O 0.0799(8) 0.8704(7) 0.2790(6) 0.116(3) Uani 1 1 d . . . O36 O 0.8144(8) 0.1566(8) 0.9757(4) 0.104(2) Uani 1 1 d . . . O29 O 0.2264(6) 0.4470(5) 0.1487(4) 0.0692(13) Uani 1 1 d . . . O27 O 0.4808(6) 0.6329(5) 0.0229(3) 0.0630(12) Uani 1 1 d . . . O21 O 0.8281(4) 0.4518(3) 0.0585(3) 0.0476(9) 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 Tm1 0.01435(6) 0.01322(6) 0.01603(6) -0.00122(4) -0.00672(4) -0.00476(4) Tm2 0.01463(6) 0.01325(6) 0.01599(6) -0.00022(4) -0.00611(4) -0.00485(4) O03 0.0178(9) 0.0160(9) 0.0205(10) 0.0000(7) -0.0094(7) -0.0032(7) O04 0.0252(10) 0.0173(9) 0.0190(9) 0.0032(7) -0.0126(8) -0.0091(8) O05 0.0171(9) 0.0172(10) 0.0337(13) -0.0069(9) -0.0120(9) -0.0022(7) O06 0.0221(10) 0.0263(12) 0.0255(11) 0.0014(9) -0.0145(9) -0.0104(9) O07 0.0295(11) 0.0162(9) 0.0165(9) 0.0012(7) -0.0067(8) -0.0040(8) O08 0.0210(10) 0.0214(11) 0.0309(13) -0.0089(9) -0.0130(9) -0.0026(8) O09 0.0283(11) 0.0180(10) 0.0222(11) 0.0007(8) -0.0108(9) -0.0095(9) O10 0.0225(10) 0.0290(12) 0.0224(11) 0.0032(9) -0.0141(8) -0.0094(9) O11 0.0358(13) 0.0154(9) 0.0275(12) -0.0008(8) -0.0203(10) -0.0065(9) O12 0.0351(15) 0.0289(15) 0.0420(17) 0.0142(13) -0.0100(13) -0.0134(12) O13 0.0209(12) 0.0442(19) 0.0392(17) 0.0152(14) -0.0037(11) -0.0007(12) O14 0.0395(16) 0.046(2) 0.0410(17) -0.0033(14) -0.0234(14) -0.0197(15) C15 0.0138(9) 0.0162(11) 0.0167(10) 0.0001(8) -0.0059(8) -0.0063(8) O16 0.0320(13) 0.0160(10) 0.0378(16) 0.0043(10) -0.0081(11) -0.0079(10) C17 0.0121(9) 0.0153(10) 0.0166(10) -0.0009(8) -0.0052(8) -0.0046(8) O18 0.0230(11) 0.0420(17) 0.0258(13) 0.0003(12) -0.0028(9) -0.0054(11) O19 0.0199(9) 0.0221(11) 0.0231(11) -0.0062(8) -0.0093(8) -0.0036(8) O20 0.0230(10) 0.0263(12) 0.0307(13) 0.0010(10) -0.0043(9) -0.0140(10) O22 0.0178(9) 0.0245(12) 0.0328(13) 0.0039(10) -0.0063(9) -0.0108(9) C23 0.0188(11) 0.0171(11) 0.0160(11) 0.0001(8) -0.0078(8) -0.0076(9) C24 0.0128(9) 0.0141(10) 0.0188(11) -0.0023(8) -0.0066(8) -0.0020(8) C25 0.0112(9) 0.0149(10) 0.0195(11) -0.0023(8) -0.0054(8) -0.0027(8) C26 0.0146(10) 0.0172(11) 0.0220(12) -0.0036(9) -0.0072(9) -0.0047(9) C28 0.0151(10) 0.0144(10) 0.0205(12) 0.0013(9) -0.0095(9) -0.0042(8) C30 0.0195(11) 0.0140(10) 0.0149(10) 0.0005(8) -0.0082(8) -0.0057(9) C31 0.0282(14) 0.0138(11) 0.0151(11) -0.0019(8) -0.0106(10) -0.0069(10) C32 0.0155(10) 0.0166(11) 0.0222(12) -0.0029(9) -0.0092(9) -0.0058(9) C33 0.0209(12) 0.0184(12) 0.0196(12) 0.0019(10) -0.0104(10) -0.0041(10) C38 0.0186(10) 0.0132(10) 0.0153(10) -0.0005(8) -0.0071(8) -0.0045(8) C39 0.0142(9) 0.0136(10) 0.0211(12) -0.0014(8) -0.0073(8) -0.0051(8) C40 0.0159(10) 0.0144(11) 0.0231(13) -0.0032(9) -0.0065(9) -0.0027(8) C41 0.0147(10) 0.0148(11) 0.0192(12) -0.0013(9) -0.0064(8) -0.0030(8) O44 0.048(3) 0.059(3) 0.113(5) 0.026(3) -0.012(3) -0.012(2) O43 0.050(3) 0.106(5) 0.075(4) 0.014(3) -0.032(2) -0.025(3) O34 0.053(3) 0.202(8) 0.106(5) 0.106(5) -0.041(3) -0.072(4) O35 0.110(5) 0.105(6) 0.154(7) 0.039(5) -0.048(5) -0.069(5) O36 0.116(5) 0.145(7) 0.055(3) -0.002(4) -0.033(3) -0.058(5) O29 0.091(4) 0.068(3) 0.064(3) 0.013(2) -0.051(3) -0.032(3) O27 0.097(4) 0.066(3) 0.052(3) 0.017(2) -0.040(2) -0.050(3) O21 0.0392(17) 0.0313(17) 0.059(2) 0.0054(16) -0.0109(16) -0.0100(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tm1 O22 2.246(3) . ? Tm1 O11 2.270(2) . ? Tm1 O06 2.284(2) . ? Tm1 O12 2.345(3) . ? Tm1 O18 2.368(3) . ? Tm1 O09 2.376(3) . ? Tm1 O05 2.411(2) . ? Tm1 O08 2.442(2) . ? Tm1 C40 2.785(3) . ? Tm2 O20 2.259(3) 2_656 ? Tm2 O07 2.286(2) . ? Tm2 O16 2.313(3) . ? Tm2 O10 2.314(2) 2_656 ? Tm2 O04 2.389(2) . ? Tm2 O14 2.393(3) 2_656 ? Tm2 O03 2.401(2) . ? Tm2 O19 2.418(3) . ? Tm2 C41 2.764(3) . ? O03 C41 1.266(4) . ? O04 C23 1.264(4) . ? O05 C40 1.267(4) . ? O06 C39 1.253(4) . ? O07 C33 1.276(4) . ? O08 C40 1.267(4) . ? O10 C28 1.269(4) . ? O10 Tm2 2.314(2) 2_656 ? O11 C23 1.260(4) . ? O13 C33 1.238(4) . ? O14 Tm2 2.393(3) 2_656 ? C15 C32 1.394(4) . ? C15 C24 1.410(4) . ? C15 C28 1.497(4) . ? C17 C26 1.390(4) . ? C17 C25 1.399(4) 2_666 ? C17 C39 1.507(4) . ? O19 C41 1.268(4) . ? O20 C39 1.249(4) . ? O20 Tm2 2.259(3) 2_656 ? O22 C28 1.252(4) . ? C23 C30 1.497(4) . ? C24 C26 1.394(4) 1_455 ? C24 C41 1.497(4) . ? C25 C17 1.399(4) 2_666 ? C25 C32 1.405(4) 2_566 ? C25 C40 1.496(4) . ? C26 C24 1.394(4) 1_655 ? C30 C31 1.402(4) . ? C30 C38 1.403(4) . ? C31 C38 1.381(4) 2_655 ? C32 C25 1.405(4) 2_566 ? C33 C38 1.514(4) . ? C38 C31 1.381(4) 2_655 ? 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 O22 Tm1 O11 90.53(10) . . ? O22 Tm1 O06 102.47(10) . . ? O11 Tm1 O06 151.16(10) . . ? O22 Tm1 O12 145.40(10) . . ? O11 Tm1 O12 91.61(11) . . ? O06 Tm1 O12 91.88(11) . . ? O22 Tm1 O18 143.77(11) . . ? O11 Tm1 O18 76.54(11) . . ? O06 Tm1 O18 77.89(10) . . ? O12 Tm1 O18 69.74(11) . . ? O22 Tm1 O09 73.83(9) . . ? O11 Tm1 O09 81.50(9) . . ? O06 Tm1 O09 77.70(9) . . ? O12 Tm1 O09 140.55(10) . . ? O18 Tm1 O09 70.87(10) . . ? O22 Tm1 O05 76.60(10) . . ? O11 Tm1 O05 134.10(9) . . ? O06 Tm1 O05 74.46(9) . . ? O12 Tm1 O05 77.26(11) . . ? O18 Tm1 O05 135.71(10) . . ? O09 Tm1 O05 133.36(9) . . ? O22 Tm1 O08 75.14(10) . . ? O11 Tm1 O08 80.14(9) . . ? O06 Tm1 O08 127.87(9) . . ? O12 Tm1 O08 71.24(10) . . ? O18 Tm1 O08 133.42(10) . . ? O09 Tm1 O08 143.56(9) . . ? O05 Tm1 O08 54.03(8) . . ? O22 Tm1 C40 73.14(10) . . ? O11 Tm1 C40 107.09(9) . . ? O06 Tm1 C40 101.32(9) . . ? O12 Tm1 C40 73.24(10) . . ? O18 Tm1 C40 142.91(11) . . ? O09 Tm1 C40 145.88(9) . . ? O05 Tm1 C40 27.01(8) . . ? O08 Tm1 C40 27.05(8) . . ? O20 Tm2 O07 142.12(10) 2_656 . ? O20 Tm2 O16 73.50(10) 2_656 . ? O07 Tm2 O16 78.81(10) . . ? O20 Tm2 O10 105.61(10) 2_656 2_656 ? O07 Tm2 O10 91.98(9) . 2_656 ? O16 Tm2 O10 76.10(10) . 2_656 ? O20 Tm2 O04 146.20(9) 2_656 . ? O07 Tm2 O04 70.95(8) . . ? O16 Tm2 O04 134.46(9) . . ? O10 Tm2 O04 71.86(9) 2_656 . ? O20 Tm2 O14 76.57(11) 2_656 2_656 ? O07 Tm2 O14 74.32(10) . 2_656 ? O16 Tm2 O14 81.81(12) . 2_656 ? O10 Tm2 O14 155.95(11) 2_656 2_656 ? O04 Tm2 O14 119.80(10) . 2_656 ? O20 Tm2 O03 74.03(9) 2_656 . ? O07 Tm2 O03 142.99(9) . . ? O16 Tm2 O03 132.79(10) . . ? O10 Tm2 O03 80.74(9) 2_656 . ? O04 Tm2 O03 72.31(8) . . ? O14 Tm2 O03 122.03(10) 2_656 . ? O20 Tm2 O19 83.47(10) 2_656 . ? O07 Tm2 O19 110.46(9) . . ? O16 Tm2 O19 149.59(9) . . ? O10 Tm2 O19 130.33(9) 2_656 . ? O04 Tm2 O19 74.69(8) . . ? O14 Tm2 O19 73.60(10) 2_656 . ? O03 Tm2 O19 54.43(8) . . ? O20 Tm2 C41 75.66(10) 2_656 . ? O07 Tm2 C41 131.54(9) . . ? O16 Tm2 C41 148.49(10) . . ? O10 Tm2 C41 106.51(9) 2_656 . ? O04 Tm2 C41 73.10(8) . . ? O14 Tm2 C41 97.28(11) 2_656 . ? O03 Tm2 C41 27.23(8) . . ? O19 Tm2 C41 27.30(8) . . ? C41 O03 Tm2 92.54(18) . . ? C23 O04 Tm2 127.92(19) . . ? C40 O05 Tm1 93.20(18) . . ? C39 O06 Tm1 128.4(2) . . ? C33 O07 Tm2 129.0(2) . . ? C40 O08 Tm1 91.75(19) . . ? C28 O10 Tm2 124.8(2) . 2_656 ? C23 O11 Tm1 137.7(2) . . ? C32 C15 C24 118.5(2) . . ? C32 C15 C28 118.3(2) . . ? C24 C15 C28 123.2(3) . . ? C26 C17 C25 119.5(2) . 2_666 ? C26 C17 C39 115.6(2) . . ? C25 C17 C39 124.9(2) 2_666 . ? C41 O19 Tm2 91.71(18) . . ? C39 O20 Tm2 175.3(2) . 2_656 ? C28 O22 Tm1 167.6(2) . . ? O11 C23 O04 124.3(3) . . ? O11 C23 C30 117.9(3) . . ? O04 C23 C30 117.9(3) . . ? C26 C24 C15 119.9(3) 1_455 . ? C26 C24 C41 117.0(3) 1_455 . ? C15 C24 C41 123.0(2) . . ? C17 C25 C32 119.3(2) 2_666 2_566 ? C17 C25 C40 120.7(2) 2_666 . ? C32 C25 C40 120.0(3) 2_566 . ? C17 C26 C24 121.2(3) . 1_655 ? O22 C28 O10 123.3(3) . . ? O22 C28 C15 120.0(3) . . ? O10 C28 C15 116.6(3) . . ? C31 C30 C38 119.4(3) . . ? C31 C30 C23 119.1(2) . . ? C38 C30 C23 121.5(3) . . ? C38 C31 C30 121.2(3) 2_655 . ? C15 C32 C25 121.4(3) . 2_566 ? O13 C33 O07 124.1(3) . . ? O13 C33 C38 115.7(3) . . ? O07 C33 C38 120.1(3) . . ? C31 C38 C30 119.3(3) 2_655 . ? C31 C38 C33 116.1(3) 2_655 . ? C30 C38 C33 124.2(3) . . ? O20 C39 O06 124.8(3) . . ? O20 C39 C17 118.6(3) . . ? O06 C39 C17 116.3(3) . . ? O05 C40 O08 120.9(3) . . ? O05 C40 C25 119.2(3) . . ? O08 C40 C25 119.9(3) . . ? O05 C40 Tm1 59.79(16) . . ? O08 C40 Tm1 61.20(16) . . ? C25 C40 Tm1 175.4(2) . . ? O03 C41 O19 120.9(3) . . ? O03 C41 C24 120.1(3) . . ? O19 C41 C24 119.0(3) . . ? O03 C41 Tm2 60.23(16) . . ? O19 C41 Tm2 60.99(16) . . ? C24 C41 Tm2 170.8(2) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 42.19 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 7.397 _refine_diff_density_min -6.231 _refine_diff_density_rms 0.313 data_job _database_code_depnum_ccdc_archive 'CCDC 862351' #TrackingRef 'C6.cif' _audit_creation_date 2012-11-22T14:16:00-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H16.5 Gd2.5 O22' _chemical_formula_sum 'C20 H16.50 Gd2.50 O22' _chemical_formula_weight 1001.96 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.53380(10) _cell_length_b 11.7159(2) _cell_length_c 14.7503(3) _cell_angle_alpha 106.5050(10) _cell_angle_beta 97.6840(10) _cell_angle_gamma 101.9810(10) _cell_volume 1512.30(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7214 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 34.972 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 2.2 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 945 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.511 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; 'P. Coppens in Crystallographic Computing ed F.R. Ahmed, S.R. Hall and C.P. Huber, Copenhagen, Munksgaard, (1970) pp 255-270' ; _exptl_absorpt_correction_T_min 0.2696 _exptl_absorpt_correction_T_max 0.4783 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_unetI/netI 0.0635 _diffrn_reflns_number 27451 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 34.98 _diffrn_reflns_theta_full 34.98 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 13226 _reflns_number_gt 11315 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0641P)^2^+7.4945P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0025(3) _refine_ls_number_reflns 13226 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1399 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.649 _refine_diff_density_min -2.901 _refine_diff_density_rms 0.286 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.023823(19) 0.415410(16) 0.327461(13) 0.01291(6) Uani 1 1 d . . . Gd2 Gd 0.012283(18) 0.901921(16) 0.355409(13) 0.01247(6) Uani 1 1 d . . . Gd3 Gd -0.51525(5) 0.18134(4) 0.08933(3) 0.02157(9) Uani 0.5 1 d P . . O7 O 0.2655(4) 0.8844(4) 0.3697(3) 0.0256(7) Uani 1 1 d . . . O8 O 0.1338(3) 0.8089(3) 0.4608(2) 0.0166(5) Uani 1 1 d . . . C18 C -0.0058(6) -0.0189(4) 0.0877(3) 0.0211(8) Uani 1 1 d . . . O3A O 0.2790(10) 0.3941(7) 0.3596(6) 0.0219(3) Uani 0.5 1 d P . . O3B O 0.2650(10) 0.3668(7) 0.3461(6) 0.0219(3) Uani 0.5 1 d P . . O4 O 0.1337(4) 0.3087(3) 0.4430(2) 0.0219(3) Uani 1 1 d . . . O5 O 0.1374(4) 0.5620(3) 0.4770(2) 0.0209(6) Uani 1 1 d . . . O6 O -0.1875(3) 0.3097(3) 0.3730(2) 0.0189(5) Uani 1 1 d . . . O13 O 0.0929(4) 0.3135(3) 0.1699(2) 0.0219(3) Uani 1 1 d . . . C11 C 0.1034(6) 0.6101(4) 0.0495(3) 0.0240(8) Uani 1 1 d . . . H11 H 0.1727 0.6844 0.0825 0.029 Uiso 1 1 calc R . . O1 O 0.1280(3) 0.0750(3) 0.4978(2) 0.0195(6) Uani 1 1 d . . . O2 O 0.2178(3) 0.2232(3) 0.6343(2) 0.0209(6) Uani 1 1 d . . . O9 O -0.0103(4) 0.7014(3) 0.2392(3) 0.0248(7) Uani 1 1 d . . . O14 O -0.0384(4) 0.1937(3) 0.2360(2) 0.0219(3) Uani 1 1 d . . . OW1 O -0.1232(4) 1.0564(3) 0.3587(3) 0.0242(6) Uani 1 1 d . . . C17 C 0.0158(6) 0.0997(4) 0.0824(3) 0.0220(8) Uani 1 1 d . . . O11 O -0.1572(4) 0.4055(3) 0.1925(2) 0.0227(6) Uani 1 1 d . . . C2 C 0.3787(4) 0.2859(4) 0.4569(3) 0.0163(6) Uani 1 1 d . . . O10 O 0.1271(4) 0.5746(3) 0.2645(2) 0.0206(6) Uani 1 1 d . . . C5 C 0.3780(4) 0.7871(4) 0.4697(3) 0.0158(6) Uani 1 1 d . . . OW2 O -0.1295(4) 0.5574(3) 0.3695(3) 0.0244(7) Uani 1 1 d . . . C15 C 0.0450(5) 0.6124(4) 0.2101(3) 0.0170(6) Uani 1 1 d . . . O16 O -0.1170(4) 0.8853(3) 0.1917(2) 0.0227(6) Uani 1 1 d . . . O12A O -0.3159(12) 0.3058(10) 0.0489(7) 0.041(2) Uani 0.5 1 d P . . O12B O -0.2611(12) 0.2635(10) 0.0537(7) 0.041(2) Uani 0.5 1 d P . . OW4 O -0.3657(6) 0.1441(6) 0.2059(6) 0.0247(15) Uani 0.5 1 d P . . O15 O 0.1123(4) 0.9967(4) 0.2454(3) 0.0251(7) Uani 1 1 d . . . C4 C 0.3630(4) 0.7102(4) 0.5274(3) 0.0137(6) Uani 1 1 d . . . C6 C 0.4851(4) 0.1734(4) 0.5506(3) 0.0174(7) Uani 1 1 d . . . H6 H 0.4738 0.1212 0.5877 0.021 Uiso 1 1 calc R . . OW6 O -0.3737(10) 0.0459(10) 0.0143(7) 0.044(2) Uani 0.5 1 d P . . C9 C 0.2167(4) 0.6508(3) 0.5440(3) 0.0138(6) Uani 1 1 d . . . C19 C -0.0034(5) 0.9546(4) 0.1816(3) 0.0190(7) Uani 1 1 d . . . C1 C 0.3645(4) 0.2111(4) 0.5163(3) 0.0158(6) Uani 1 1 d . . . C12 C 0.0181(5) 0.5504(4) 0.1018(3) 0.0175(7) Uani 1 1 d . . . C7 C 0.2265(4) 0.1680(4) 0.5496(3) 0.0149(6) Uani 1 1 d . . . OW3 O -0.4427(7) 0.3808(8) 0.2257(6) 0.0306(16) Uani 0.5 1 d P . . C20 C 0.0269(5) 0.2088(4) 0.1683(3) 0.0210(7) Uani 1 1 d . . . C13 C -0.0866(5) 0.4395(4) 0.0509(3) 0.0214(8) Uani 1 1 d . . . C16 C 0.0226(6) 0.1184(4) -0.0054(3) 0.0248(9) Uani 1 1 d . . . H16 H 0.0385 0.1978 -0.0094 0.03 Uiso 1 1 calc R . . C10 C 0.2523(4) 0.8288(4) 0.4308(3) 0.0150(6) Uani 1 1 d . . . C14 C -0.1851(7) 0.3720(5) 0.1010(4) 0.0374(14) Uani 1 1 d . . . C3 C 0.5159(4) 0.3242(4) 0.4362(3) 0.0170(7) Uani 1 1 d . . . H3 H 0.5266 0.3739 0.397 0.02 Uiso 1 1 calc R . . OW7 O -0.6341(9) 0.0962(10) -0.0774(6) 0.040(2) Uani 0.5 1 d P . . OW5 O -0.6708(8) 0.1797(7) 0.2049(6) 0.0276(14) Uani 0.5 1 d P . . C8 C 0.2543(4) 0.3272(4) 0.4159(3) 0.0177(7) Uani 1 1 d . . . OW8 O -0.6602(14) 0.3065(10) 0.0505(11) 0.078(5) Uani 0.5 1 d P . . OW9 O -0.6463(12) -0.0251(8) 0.0777(9) 0.113(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01279(9) 0.01366(9) 0.01280(9) 0.00384(6) 0.00390(6) 0.00431(6) Gd2 0.01171(9) 0.01559(9) 0.01219(9) 0.00600(6) 0.00385(6) 0.00497(6) Gd3 0.01604(17) 0.0259(2) 0.02204(19) 0.00802(16) 0.00389(14) 0.00338(14) O7 0.0203(14) 0.0389(19) 0.0320(18) 0.0264(16) 0.0119(13) 0.0137(13) O8 0.0136(12) 0.0213(13) 0.0188(13) 0.0085(11) 0.0061(10) 0.0084(10) C18 0.036(2) 0.0191(17) 0.0122(16) 0.0079(14) 0.0095(15) 0.0095(16) O3A 0.0279(8) 0.0211(8) 0.0199(8) 0.0077(7) 0.0097(6) 0.0088(7) O3B 0.0279(8) 0.0211(8) 0.0199(8) 0.0077(7) 0.0097(6) 0.0088(7) O4 0.0279(8) 0.0211(8) 0.0199(8) 0.0077(7) 0.0097(6) 0.0088(7) O5 0.0212(14) 0.0178(13) 0.0188(14) 0.0037(11) 0.0001(11) 0.0001(10) O6 0.0178(13) 0.0225(14) 0.0172(13) 0.0067(11) 0.0080(10) 0.0038(10) O13 0.0279(8) 0.0211(8) 0.0199(8) 0.0077(7) 0.0097(6) 0.0088(7) C11 0.032(2) 0.0213(19) 0.0139(17) 0.0046(14) 0.0070(15) -0.0021(16) O1 0.0140(12) 0.0192(13) 0.0215(14) 0.0040(11) 0.0030(10) 0.0005(10) O2 0.0183(13) 0.0223(14) 0.0203(14) 0.0046(11) 0.0071(11) 0.0024(11) O9 0.0347(18) 0.0230(15) 0.0186(14) 0.0033(12) 0.0062(13) 0.0161(13) O14 0.0279(8) 0.0211(8) 0.0199(8) 0.0077(7) 0.0097(6) 0.0088(7) OW1 0.0340(18) 0.0245(15) 0.0201(15) 0.0083(12) 0.0084(13) 0.0167(13) C17 0.040(2) 0.0179(17) 0.0107(15) 0.0044(13) 0.0082(15) 0.0110(16) O11 0.0231(15) 0.0303(17) 0.0140(13) 0.0077(12) 0.0045(11) 0.0042(12) C2 0.0128(15) 0.0210(17) 0.0203(17) 0.0113(14) 0.0057(12) 0.0075(12) O10 0.0249(15) 0.0195(13) 0.0181(14) 0.0085(11) 0.0043(11) 0.0037(11) C5 0.0122(14) 0.0201(16) 0.0198(17) 0.0108(14) 0.0047(12) 0.0072(12) OW2 0.0363(18) 0.0224(15) 0.0211(15) 0.0079(12) 0.0099(13) 0.0177(13) C15 0.0199(17) 0.0156(15) 0.0150(16) 0.0050(13) 0.0052(13) 0.0023(12) O16 0.0253(15) 0.0256(15) 0.0169(14) 0.0086(12) 0.0028(11) 0.0044(12) O12A 0.044(5) 0.041(5) 0.021(2) 0.002(3) 0.009(3) -0.019(3) O12B 0.044(5) 0.041(5) 0.021(2) 0.002(3) 0.009(3) -0.019(3) OW4 0.003(2) 0.017(3) 0.037(4) -0.010(2) -0.007(2) -0.0005(17) O15 0.0260(16) 0.0326(18) 0.0195(15) 0.0132(13) 0.0072(12) 0.0049(13) C4 0.0104(13) 0.0181(15) 0.0146(15) 0.0074(12) 0.0030(11) 0.0044(11) C6 0.0104(14) 0.0228(17) 0.0240(19) 0.0124(15) 0.0042(13) 0.0074(12) OW6 0.036(4) 0.057(6) 0.039(5) 0.006(4) 0.016(4) 0.019(4) C9 0.0103(13) 0.0151(14) 0.0167(16) 0.0068(12) 0.0028(11) 0.0022(11) C19 0.030(2) 0.0184(17) 0.0131(15) 0.0058(13) 0.0084(14) 0.0112(15) C1 0.0109(14) 0.0177(16) 0.0188(17) 0.0049(13) 0.0052(12) 0.0035(12) C12 0.0233(18) 0.0162(16) 0.0124(15) 0.0032(13) 0.0052(13) 0.0048(13) C7 0.0100(14) 0.0169(15) 0.0202(17) 0.0075(13) 0.0052(12) 0.0051(11) OW3 0.012(3) 0.053(5) 0.029(4) 0.016(3) 0.009(2) 0.008(3) C20 0.032(2) 0.0184(17) 0.0134(16) 0.0034(13) 0.0076(15) 0.0095(15) C13 0.028(2) 0.0195(17) 0.0130(16) 0.0038(13) 0.0064(14) -0.0005(15) C16 0.044(3) 0.0198(18) 0.0169(18) 0.0106(15) 0.0116(17) 0.0112(17) C10 0.0135(15) 0.0178(16) 0.0160(16) 0.0078(13) 0.0031(12) 0.0055(12) C14 0.048(3) 0.032(3) 0.018(2) 0.0043(18) 0.010(2) -0.016(2) C3 0.0106(14) 0.0236(18) 0.0212(17) 0.0122(15) 0.0051(12) 0.0052(12) OW7 0.027(4) 0.068(6) 0.028(4) 0.018(4) 0.000(3) 0.017(4) OW5 0.020(3) 0.028(3) 0.029(4) 0.004(3) 0.009(3) -0.002(2) C8 0.0168(16) 0.0223(17) 0.0159(16) 0.0067(14) 0.0025(13) 0.0089(13) OW8 0.075(8) 0.037(5) 0.107(11) 0.017(6) -0.044(8) 0.030(5) OW9 0.129(8) 0.055(5) 0.157(10) 0.040(6) 0.055(7) 0.002(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O5 2.329(3) . ? Gd1 O10 2.403(3) . ? Gd1 O11 2.413(3) . ? Gd1 O6 2.417(3) . ? Gd1 OW2 2.441(3) . ? Gd1 O14 2.465(3) . ? Gd1 O3B 2.480(10) . ? Gd1 O3A 2.493(10) . ? Gd1 O13 2.534(3) . ? Gd1 O4 2.616(3) . ? Gd1 C20 2.862(4) . ? Gd1 C8 2.922(4) . ? Gd2 O1 2.402(3) 1_565 ? Gd2 O15 2.403(3) . ? Gd2 O2 2.422(3) 2_566 ? Gd2 OW1 2.426(3) . ? Gd2 O9 2.430(3) . ? Gd2 O8 2.440(3) . ? Gd2 O7 2.452(3) . ? Gd2 O16 2.495(3) . ? Gd2 O1 2.673(3) 2_566 ? Gd2 C19 2.795(4) . ? Gd2 C10 2.807(4) . ? Gd2 C7 2.924(4) 2_566 ? Gd3 OW4 2.282(7) . ? Gd3 OW8 2.345(8) . ? Gd3 OW7 2.391(9) . ? Gd3 O12A 2.396(10) . ? Gd3 OW5 2.406(7) . ? Gd3 OW6 2.420(9) . ? Gd3 OW9 2.427(8) . ? Gd3 OW3 2.504(9) . ? Gd3 OW6 2.575(11) 2_455 ? Gd3 O12B 2.595(10) . ? O7 C10 1.258(5) . ? O8 C10 1.268(5) . ? C18 C16 1.387(6) 2 ? C18 C17 1.387(6) . ? C18 C19 1.502(6) 1_545 ? O3A C8 1.305(10) . ? O3B C8 1.251(10) . ? O4 C8 1.265(5) . ? O5 C9 1.233(5) . ? O6 C9 1.270(5) 2_566 ? O13 C20 1.249(6) . ? C11 C13 1.403(6) 2_565 ? C11 C12 1.408(6) . ? C11 H11 0.93 . ? O1 C7 1.251(5) . ? O1 Gd2 2.402(3) 1_545 ? O1 Gd2 2.673(3) 2_566 ? O2 C7 1.255(5) . ? O2 Gd2 2.422(3) 2_566 ? O9 C15 1.259(5) . ? O14 C20 1.279(5) . ? C17 C16 1.381(6) . ? C17 C20 1.496(6) . ? O11 C14 1.267(6) . ? C2 C3 1.395(5) . ? C2 C1 1.405(6) . ? C2 C8 1.490(5) . ? O10 C15 1.278(5) . ? C5 C6 1.393(5) 2_666 ? C5 C4 1.405(5) . ? C5 C10 1.491(5) . ? C15 C12 1.516(6) . ? O16 C19 1.266(6) . ? O12A O12B 0.801(14) . ? O12A C14 1.323(12) . ? O12B C14 1.267(11) . ? O15 C19 1.256(6) . ? C4 C3 1.390(5) 2_666 ? C4 C9 1.508(5) . ? C6 C5 1.393(5) 2_666 ? C6 C1 1.399(5) . ? C6 H6 0.93 . ? OW6 OW9 1.356(14) 2_455 ? OW6 Gd3 2.575(11) 2_455 ? C9 O6 1.270(5) 2_566 ? C19 C18 1.502(6) 1_565 ? C1 C7 1.505(5) . ? C12 C13 1.399(6) . ? C7 Gd2 2.924(4) 2_566 ? C13 C11 1.403(6) 2_565 ? C13 C14 1.503(7) . ? C16 C18 1.387(6) 2 ? C16 H16 0.93 . ? C3 C4 1.390(5) 2_666 ? C3 H3 0.93 . ? OW9 OW6 1.356(14) 2_455 ? 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 O5 Gd1 O10 84.06(11) . . ? O5 Gd1 O11 135.05(12) . . ? O10 Gd1 O11 72.98(11) . . ? O5 Gd1 O6 99.03(11) . . ? O10 Gd1 O6 147.62(11) . . ? O11 Gd1 O6 82.82(11) . . ? O5 Gd1 OW2 71.70(12) . . ? O10 Gd1 OW2 78.59(12) . . ? O11 Gd1 OW2 66.25(12) . . ? O6 Gd1 OW2 72.03(12) . . ? O5 Gd1 O14 143.72(12) . . ? O10 Gd1 O14 123.64(11) . . ? O11 Gd1 O14 79.51(12) . . ? O6 Gd1 O14 70.62(11) . . ? OW2 Gd1 O14 131.61(12) . . ? O5 Gd1 O3B 80.7(2) . . ? O10 Gd1 O3B 88.8(2) . . ? O11 Gd1 O3B 135.0(2) . . ? O6 Gd1 O3B 123.6(2) . . ? OW2 Gd1 O3B 150.58(19) . . ? O14 Gd1 O3B 77.38(18) . . ? O5 Gd1 O3A 74.20(19) . . ? O10 Gd1 O3A 85.0(2) . . ? O11 Gd1 O3A 138.6(2) . . ? O6 Gd1 O3A 127.0(2) . . ? OW2 Gd1 O3A 143.36(19) . . ? O14 Gd1 O3A 84.61(18) . . ? O3B Gd1 O3A 7.2(2) . . ? O5 Gd1 O13 138.30(12) . . ? O10 Gd1 O13 72.09(11) . . ? O11 Gd1 O13 69.86(11) . . ? O6 Gd1 O13 119.49(11) . . ? OW2 Gd1 O13 132.54(11) . . ? O14 Gd1 O13 52.32(11) . . ? O3B Gd1 O13 65.4(2) . . ? O3A Gd1 O13 70.2(2) . . ? O5 Gd1 O4 70.31(11) . . ? O10 Gd1 O4 133.90(11) . . ? O11 Gd1 O4 149.86(12) . . ? O6 Gd1 O4 75.96(11) . . ? OW2 Gd1 O4 124.69(11) . . ? O14 Gd1 O4 73.43(11) . . ? O3B Gd1 O4 50.6(2) . . ? O3A Gd1 O4 51.9(2) . . ? O13 Gd1 O4 102.38(11) . . ? O5 Gd1 C20 150.05(13) . . ? O10 Gd1 C20 97.57(12) . . ? O11 Gd1 C20 72.69(13) . . ? O6 Gd1 C20 95.33(12) . . ? OW2 Gd1 C20 138.09(13) . . ? O14 Gd1 C20 26.45(12) . . ? O3B Gd1 C20 69.4(2) . . ? O3A Gd1 C20 76.1(2) . . ? O13 Gd1 C20 25.86(12) . . ? O4 Gd1 C20 88.08(12) . . ? O5 Gd1 C8 71.97(12) . . ? O10 Gd1 C8 110.63(12) . . ? O11 Gd1 C8 152.28(12) . . ? O6 Gd1 C8 100.84(12) . . ? OW2 Gd1 C8 141.19(12) . . ? O14 Gd1 C8 75.99(12) . . ? O3B Gd1 C8 25.1(2) . . ? O3A Gd1 C8 26.4(2) . . ? O13 Gd1 C8 84.85(11) . . ? O4 Gd1 C8 25.64(11) . . ? C20 Gd1 C8 79.60(13) . . ? O1 Gd2 O15 95.13(12) 1_565 . ? O1 Gd2 O2 114.75(11) 1_565 2_566 ? O15 Gd2 O2 138.98(12) . 2_566 ? O1 Gd2 OW1 72.82(12) 1_565 . ? O15 Gd2 OW1 78.41(13) . . ? O2 Gd2 OW1 84.14(12) 2_566 . ? O1 Gd2 O9 154.50(12) 1_565 . ? O15 Gd2 O9 88.88(13) . . ? O2 Gd2 O9 76.14(12) 2_566 . ? OW1 Gd2 O9 132.53(12) . . ? O1 Gd2 O8 77.22(11) 1_565 . ? O15 Gd2 O8 128.11(11) . . ? O2 Gd2 O8 87.32(11) 2_566 . ? OW1 Gd2 O8 141.71(11) . . ? O9 Gd2 O8 80.52(11) . . ? O1 Gd2 O7 80.08(13) 1_565 . ? O15 Gd2 O7 74.71(12) . . ? O2 Gd2 O7 135.19(12) 2_566 . ? OW1 Gd2 O7 139.57(13) . . ? O9 Gd2 O7 76.72(13) . . ? O8 Gd2 O7 53.41(10) . . ? O1 Gd2 O16 132.55(11) 1_565 . ? O15 Gd2 O16 53.55(12) . . ? O2 Gd2 O16 85.47(11) 2_566 . ? OW1 Gd2 O16 66.95(12) . . ? O9 Gd2 O16 68.78(12) . . ? O8 Gd2 O16 149.29(11) . . ? O7 Gd2 O16 116.35(12) . . ? O1 Gd2 O1 64.46(12) 1_565 2_566 ? O15 Gd2 O1 146.57(12) . 2_566 ? O2 Gd2 O1 50.30(10) 2_566 2_566 ? OW1 Gd2 O1 70.52(11) . 2_566 ? O9 Gd2 O1 121.23(12) . 2_566 ? O8 Gd2 O1 75.36(10) . 2_566 ? O7 Gd2 O1 123.04(11) . 2_566 ? O16 Gd2 O1 120.53(11) . 2_566 ? O1 Gd2 C19 115.09(12) 1_565 . ? O15 Gd2 C19 26.63(13) . . ? O2 Gd2 C19 112.37(13) 2_566 . ? OW1 Gd2 C19 70.38(12) . . ? O9 Gd2 C19 77.98(12) . . ? O8 Gd2 C19 145.98(11) . . ? O7 Gd2 C19 95.84(12) . . ? O16 Gd2 C19 26.93(12) . . ? O1 Gd2 C19 138.60(11) 2_566 . ? O1 Gd2 C10 77.85(11) 1_565 . ? O15 Gd2 C10 101.30(12) . . ? O2 Gd2 C10 111.64(12) 2_566 . ? OW1 Gd2 C10 150.48(12) . . ? O9 Gd2 C10 76.68(12) . . ? O8 Gd2 C10 26.82(10) . . ? O7 Gd2 C10 26.59(11) . . ? O16 Gd2 C10 136.36(12) . . ? O1 Gd2 C10 99.77(11) 2_566 . ? C19 Gd2 C10 121.10(12) . . ? O1 Gd2 C7 89.78(11) 1_565 2_566 ? O15 Gd2 C7 151.27(12) . 2_566 ? O2 Gd2 C7 24.97(11) 2_566 2_566 ? OW1 Gd2 C7 76.06(12) . 2_566 ? O9 Gd2 C7 98.73(12) . 2_566 ? O8 Gd2 C7 80.58(10) . 2_566 ? O7 Gd2 C7 133.98(11) . 2_566 ? O16 Gd2 C7 103.54(11) . 2_566 ? O1 Gd2 C7 25.32(10) 2_566 2_566 ? C19 Gd2 C7 128.50(12) . 2_566 ? C10 Gd2 C7 107.41(11) . 2_566 ? OW4 Gd3 OW8 147.5(4) . . ? OW4 Gd3 OW7 142.1(3) . . ? OW8 Gd3 OW7 70.3(4) . . ? OW4 Gd3 O12A 93.4(3) . . ? OW8 Gd3 O12A 87.8(5) . . ? OW7 Gd3 O12A 90.2(3) . . ? OW4 Gd3 OW5 80.2(3) . . ? OW8 Gd3 OW5 80.0(5) . . ? OW7 Gd3 OW5 116.5(3) . . ? O12A Gd3 OW5 144.0(3) . . ? OW4 Gd3 OW6 70.5(3) . . ? OW8 Gd3 OW6 139.7(5) . . ? OW7 Gd3 OW6 74.6(3) . . ? O12A Gd3 OW6 72.9(4) . . ? OW5 Gd3 OW6 134.8(3) . . ? OW4 Gd3 OW9 79.0(3) . . ? OW8 Gd3 OW9 115.9(4) . . ? OW7 Gd3 OW9 77.6(4) . . ? O12A Gd3 OW9 146.7(4) . . ? OW5 Gd3 OW9 67.0(3) . . ? OW6 Gd3 OW9 74.0(4) . . ? OW4 Gd3 OW3 76.2(2) . . ? OW8 Gd3 OW3 72.7(4) . . ? OW7 Gd3 OW3 140.7(3) . . ? O12A Gd3 OW3 75.5(3) . . ? OW5 Gd3 OW3 68.6(2) . . ? OW6 Gd3 OW3 131.9(3) . . ? OW9 Gd3 OW3 131.9(3) . . ? OW4 Gd3 OW6 96.3(3) . 2_455 ? OW8 Gd3 OW6 111.0(4) . 2_455 ? OW7 Gd3 OW6 50.8(4) . 2_455 ? O12A Gd3 OW6 120.4(3) . 2_455 ? OW5 Gd3 OW6 95.5(3) . 2_455 ? OW6 Gd3 OW6 56.1(4) . 2_455 ? OW9 Gd3 OW6 31.3(3) . 2_455 ? OW3 Gd3 OW6 163.1(3) . 2_455 ? OW4 Gd3 O12B 79.6(3) . . ? OW8 Gd3 O12B 105.6(5) . . ? OW7 Gd3 O12B 94.1(3) . . ? O12A Gd3 O12B 17.9(3) . . ? OW5 Gd3 O12B 148.6(3) . . ? OW6 Gd3 O12B 57.5(4) . . ? OW9 Gd3 O12B 131.2(4) . . ? OW3 Gd3 O12B 83.4(3) . . ? OW6 Gd3 O12B 110.4(3) 2_455 . ? C10 O7 Gd2 92.7(2) . . ? C10 O8 Gd2 93.0(2) . . ? C16 C18 C17 120.5(4) 2 . ? C16 C18 C19 116.9(4) 2 1_545 ? C17 C18 C19 122.5(4) . 1_545 ? C8 O3A Gd1 95.5(5) . . ? C8 O3B Gd1 97.6(5) . . ? C8 O4 Gd1 90.8(3) . . ? C9 O5 Gd1 165.6(3) . . ? C9 O6 Gd1 122.1(3) 2_566 . ? C20 O13 Gd1 91.9(3) . . ? C13 C11 C12 121.7(4) 2_565 . ? C13 C11 H11 119.1 2_565 . ? C12 C11 H11 119.1 . . ? C7 O1 Gd2 155.8(3) . 1_545 ? C7 O1 Gd2 88.6(2) . 2_566 ? Gd2 O1 Gd2 115.54(12) 1_545 2_566 ? C7 O2 Gd2 100.5(2) . 2_566 ? C15 O9 Gd2 148.1(3) . . ? C20 O14 Gd1 94.4(3) . . ? C16 C17 C18 119.5(4) . . ? C16 C17 C20 118.2(4) . . ? C18 C17 C20 122.3(4) . . ? C14 O11 Gd1 141.6(4) . . ? C3 C2 C1 118.5(3) . . ? C3 C2 C8 118.6(4) . . ? C1 C2 C8 123.0(4) . . ? C15 O10 Gd1 120.6(3) . . ? C6 C5 C4 118.8(3) 2_666 . ? C6 C5 C10 119.3(3) 2_666 . ? C4 C5 C10 121.9(3) . . ? O9 C15 O10 124.9(4) . . ? O9 C15 C12 117.0(4) . . ? O10 C15 C12 118.0(4) . . ? C19 O16 Gd2 89.8(3) . . ? O12B O12A C14 68.2(12) . . ? O12B O12A Gd3 95.3(13) . . ? C14 O12A Gd3 131.0(7) . . ? O12A O12B C14 75.9(13) . . ? O12A O12B Gd3 66.8(12) . . ? C14 O12B Gd3 120.2(7) . . ? C19 O15 Gd2 94.4(3) . . ? C3 C4 C5 119.9(3) 2_666 . ? C3 C4 C9 117.0(3) 2_666 . ? C5 C4 C9 122.8(3) . . ? C5 C6 C1 121.2(4) 2_666 . ? C5 C6 H6 119.4 2_666 . ? C1 C6 H6 119.4 . . ? OW9 OW6 Gd3 124.6(8) 2_455 . ? OW9 OW6 Gd3 68.4(5) 2_455 2_455 ? Gd3 OW6 Gd3 123.9(4) . 2_455 ? O5 C9 O6 124.6(4) . 2_566 ? O5 C9 C4 117.0(4) . . ? O6 C9 C4 118.2(3) 2_566 . ? O15 C19 O16 122.2(4) . . ? O15 C19 C18 119.4(4) . 1_565 ? O16 C19 C18 118.3(4) . 1_565 ? O15 C19 Gd2 59.0(2) . . ? O16 C19 Gd2 63.2(2) . . ? C18 C19 Gd2 177.5(3) 1_565 . ? C6 C1 C2 120.0(4) . . ? C6 C1 C7 115.1(4) . . ? C2 C1 C7 124.9(3) . . ? C13 C12 C11 118.4(4) . . ? C13 C12 C15 124.3(4) . . ? C11 C12 C15 117.3(4) . . ? O1 C7 O2 120.6(4) . . ? O1 C7 C1 121.5(4) . . ? O2 C7 C1 117.8(4) . . ? O1 C7 Gd2 66.1(2) . 2_566 ? O2 C7 Gd2 54.5(2) . 2_566 ? C1 C7 Gd2 171.0(3) . 2_566 ? O13 C20 O14 121.4(4) . . ? O13 C20 C17 119.2(4) . . ? O14 C20 C17 119.2(4) . . ? O13 C20 Gd1 62.2(2) . . ? O14 C20 Gd1 59.2(2) . . ? C17 C20 Gd1 175.4(3) . . ? C12 C13 C11 119.9(4) . 2_565 ? C12 C13 C14 121.6(4) . . ? C11 C13 C14 118.4(4) 2_565 . ? C17 C16 C18 120.0(4) . 2 ? C17 C16 H16 120 . . ? C18 C16 H16 120 2 . ? O7 C10 O8 120.9(4) . . ? O7 C10 C5 119.7(4) . . ? O8 C10 C5 119.4(3) . . ? O7 C10 Gd2 60.7(2) . . ? O8 C10 Gd2 60.2(2) . . ? C5 C10 Gd2 178.8(3) . . ? O12B C14 O11 119.2(6) . . ? O12B C14 O12A 35.9(6) . . ? O11 C14 O12A 122.2(6) . . ? O12B C14 C13 118.1(6) . . ? O11 C14 C13 118.9(4) . . ? O12A C14 C13 116.2(6) . . ? C4 C3 C2 121.6(4) 2_666 . ? C4 C3 H3 119.2 2_666 . ? C2 C3 H3 119.2 . . ? O3B C8 O4 120.2(6) . . ? O3B C8 O3A 13.9(5) . . ? O4 C8 O3A 121.2(5) . . ? O3B C8 C2 118.8(6) . . ? O4 C8 C2 120.5(4) . . ? O3A C8 C2 117.8(5) . . ? O3B C8 Gd1 57.3(5) . . ? O4 C8 Gd1 63.5(2) . . ? O3A C8 Gd1 58.1(4) . . ? C2 C8 Gd1 176.0(3) . . ? OW6 OW9 Gd3 80.4(6) 2_455 . ? # END of CIF data_job _database_code_depnum_ccdc_archive 'CCDC 862519' #TrackingRef 'C4.cif' _audit_creation_date 2012-11-22T13:51:24-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C15 H26 Er2 O23.5' _chemical_formula_sum 'C15 H26 Er2 O23.50' _chemical_formula_weight 916.88 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4135(2) _cell_length_b 10.5541(2) _cell_length_c 14.0372(4) _cell_angle_alpha 99.5950(10) _cell_angle_beta 99.6200(10) _cell_angle_gamma 108.8430(10) _cell_volume 1398.72(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 13261 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 32.032 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.056 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; 'P. Coppens in Crystallographic Computing ed F.R. Ahmed, S.R. Hall and C.P. Huber, Copenhagen, Munksgaard, (1970) pp 255-270' ; _exptl_absorpt_correction_T_min 0.105 _exptl_absorpt_correction_T_max 0.546 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_unetI/netI 0.0501 _diffrn_reflns_number 18410 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 32.04 _diffrn_reflns_theta_full 32.04 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 9635 _reflns_number_gt 8099 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0353P)^2^+6.7749P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9635 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.97 _refine_diff_density_min -3.51 _refine_diff_density_rms 0.26 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 1.035843(18) 0.535827(18) 0.178552(14) 0.01442(5) Uani 1 1 d . . . Er2 Er 0.458221(18) -0.065384(18) -0.181988(14) 0.01567(5) Uani 1 1 d . . . O1 O 0.4001(4) -0.2405(3) -0.0955(3) 0.0265(7) Uani 1 1 d . . . O2 O 1.2464(4) 0.6164(5) 0.3011(3) 0.0406(10) Uani 1 1 d . . . O3 O 0.6383(4) 0.0405(4) -0.2567(4) 0.0415(10) Uani 1 1 d . . . O4 O 0.3576(5) 0.0153(4) -0.3104(3) 0.0453(12) Uani 1 1 d . . . O5 O 0.5523(5) -0.2245(4) -0.2508(4) 0.0461(12) Uani 1 1 d . . . O6 O 1.1188(4) 0.7644(3) 0.1462(3) 0.0272(7) Uani 1 1 d . . . O1A O 0.6376(4) -0.0069(4) -0.0469(3) 0.0278(8) Uani 1 1 d . . . O2A O 0.2730(4) -0.0420(4) -0.1164(3) 0.0280(8) Uani 1 1 d . . . O3A O 0.9238(3) 0.3101(3) 0.0574(2) 0.0191(6) Uani 1 1 d . . . O4A O 1.0802(4) 0.3249(3) 0.1890(3) 0.0270(8) Uani 1 1 d . . . C1A C 0.9983(4) 0.1208(4) 0.0557(3) 0.0171(8) Uani 1 1 d . . . C2A C 0.8723(4) 0.0120(4) 0.0095(3) 0.0157(7) Uani 1 1 d . . . C3A C 1.1248(4) 0.1089(4) 0.0468(3) 0.0169(8) Uani 1 1 d . . . H3A H 1.2079 0.1817 0.0783 0.02 Uiso 1 1 calc R . . C4A C 0.9991(4) 0.2586(4) 0.1056(4) 0.0184(8) Uani 1 1 d . . . C5A C 0.7350(4) 0.0177(4) 0.0270(4) 0.0175(8) Uani 1 1 d . . . O1B O 0.8688(3) 0.5575(3) 0.0677(3) 0.0231(7) Uani 1 1 d . . . O2B O 1.2068(3) 0.5494(4) 0.0932(3) 0.0242(7) Uani 1 1 d . . . O3B O 0.5256(3) 0.1783(3) -0.1144(3) 0.0208(6) Uani 1 1 d . . . O4B O 0.4973(6) 0.2849(5) -0.2363(4) 0.0470(8) Uani 1 1 d . . . C1B C 0.5119(4) 0.3982(4) -0.0719(3) 0.0157(7) Uani 1 1 d . . . C2B C 0.6316(4) 0.4984(4) -0.0068(3) 0.0155(7) Uani 1 1 d . . . C3B C 0.6188(4) 0.5993(4) 0.0649(4) 0.0188(8) Uani 1 1 d . . . H3B H 0.6985 0.6655 0.1085 0.023 Uiso 1 1 calc R . . C4B C 0.5151(4) 0.2795(4) -0.1470(3) 0.0170(8) Uani 1 1 d . . . C5B C 0.7748(4) 0.5014(4) -0.0118(3) 0.0156(7) Uani 1 1 d . . . O1C O 0.8457(4) 0.4070(4) 0.2294(3) 0.0248(7) Uani 1 1 d . . . O2C O 0.2738(4) -0.2477(4) -0.2991(3) 0.0292(8) Uani 1 1 d . . . O3C O 0.9998(5) 0.6842(4) 0.2989(3) 0.0330(9) Uani 1 1 d . . . O4C O 0.8753(5) 0.7451(5) 0.3942(4) 0.0470(8) Uani 1 1 d . . . C1C C 0.9698(5) 0.5801(5) 0.4349(4) 0.0215(9) Uani 1 1 d . . . C2C C 0.9171(5) 0.4352(4) 0.4039(3) 0.0205(8) Uani 1 1 d . . . C3C C 0.9489(5) 0.3583(5) 0.4697(4) 0.0251(10) Uani 1 1 d . . . H3C H 0.9143 0.2627 0.4487 0.03 Uiso 1 1 calc R . . C4C C 0.9438(5) 0.6740(5) 0.3697(4) 0.0248(9) Uani 1 1 d . . . C5C C 0.8231(4) 0.3577(4) 0.3033(3) 0.0178(8) Uani 1 1 d . . . O2W O 0.9472(8) 0.9075(7) 0.2191(6) 0.084(2) Uani 1 1 d . . . O1W O 0.8041(7) 0.8132(7) 0.6929(5) 0.077(2) Uani 1 1 d . . . O3W O 0.5761(10) 0.5065(8) 0.3015(8) 0.122(4) Uani 1 1 d . . . O7W O 0.662(2) 0.712(3) 0.5006(11) 0.159(11) Uani 0.5 1 d P . . O4W O 0.6224(9) 0.2577(13) 0.4969(6) 0.142(5) Uani 1 1 d . . . O5W O 0.8659(15) 0.0005(12) 0.4450(14) 0.125(8) Uani 0.5 1 d P . . O6W O 0.631(2) 0.002(2) 0.5490(10) 0.119(7) Uani 0.5 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01289(9) 0.01235(9) 0.01529(10) 0.00060(6) 0.00287(7) 0.00253(6) Er2 0.01407(9) 0.01342(9) 0.01536(10) -0.00001(6) 0.00277(7) 0.00158(6) O1 0.0304(18) 0.0197(15) 0.0224(18) 0.0045(13) 0.0031(14) 0.0018(13) O2 0.0255(19) 0.051(3) 0.032(2) -0.0033(19) -0.0045(16) 0.0082(18) O3 0.036(2) 0.034(2) 0.046(3) 0.0019(19) 0.0221(19) -0.0023(17) O4 0.055(3) 0.0231(19) 0.038(3) 0.0085(17) -0.014(2) -0.0006(18) O5 0.050(3) 0.031(2) 0.064(3) 0.002(2) 0.030(2) 0.0192(19) O6 0.0297(18) 0.0190(16) 0.0260(19) 0.0027(13) 0.0061(14) 0.0011(13) O1A 0.0189(15) 0.0265(17) 0.033(2) -0.0008(15) -0.0023(14) 0.0094(13) O2A 0.0217(16) 0.0331(19) 0.030(2) 0.0048(15) 0.0122(14) 0.0087(14) O3A 0.0227(15) 0.0150(13) 0.0183(16) 0.0005(11) 0.0033(12) 0.0078(11) O4A 0.0291(17) 0.0192(15) 0.0254(19) -0.0045(13) -0.0061(14) 0.0101(13) C1A 0.0145(17) 0.0137(17) 0.022(2) 0.0036(15) 0.0036(15) 0.0043(14) C2A 0.0129(17) 0.0144(17) 0.019(2) 0.0022(14) 0.0042(15) 0.0051(13) C3A 0.0127(17) 0.0119(16) 0.022(2) -0.0002(15) 0.0021(15) 0.0020(13) C4A 0.0168(18) 0.0123(17) 0.024(2) 0.0020(15) 0.0043(16) 0.0041(14) C5A 0.0112(17) 0.0133(17) 0.026(2) 0.0030(15) 0.0044(15) 0.0033(13) O1B 0.0159(14) 0.0224(16) 0.0276(19) 0.0019(13) -0.0010(13) 0.0074(12) O2B 0.0179(15) 0.0282(17) 0.0243(18) -0.0006(14) 0.0080(13) 0.0073(13) O3B 0.0264(16) 0.0133(13) 0.0209(17) 0.0025(12) 0.0041(13) 0.0065(12) O4B 0.069(2) 0.0510(19) 0.044(2) 0.0217(16) 0.0261(17) 0.0402(18) C1B 0.0149(17) 0.0128(16) 0.018(2) 0.0005(14) 0.0038(15) 0.0044(13) C2B 0.0112(16) 0.0157(17) 0.017(2) 0.0005(14) 0.0029(14) 0.0038(13) C3B 0.0126(17) 0.0157(18) 0.023(2) -0.0018(15) 0.0027(15) 0.0028(14) C4B 0.0135(17) 0.0141(17) 0.020(2) 0.0014(15) 0.0033(15) 0.0028(13) C5B 0.0123(17) 0.0132(16) 0.021(2) 0.0040(15) 0.0045(15) 0.0046(13) O1C 0.0231(16) 0.0238(16) 0.0170(17) 0.0015(13) 0.0044(13) -0.0036(13) O2C 0.0308(18) 0.0207(16) 0.0205(18) 0.0032(13) 0.0005(14) -0.0074(13) O3C 0.055(2) 0.0221(17) 0.026(2) 0.0063(14) 0.0209(18) 0.0135(16) O4C 0.069(2) 0.0510(19) 0.044(2) 0.0217(16) 0.0261(17) 0.0402(18) C1C 0.020(2) 0.0179(19) 0.019(2) 0.0011(16) 0.0035(16) -0.0004(15) C2C 0.024(2) 0.0166(19) 0.014(2) 0.0003(15) 0.0039(16) 0.0010(15) C3C 0.035(3) 0.0131(19) 0.020(2) 0.0010(16) 0.0045(19) 0.0018(17) C4C 0.027(2) 0.027(2) 0.023(2) 0.0058(18) 0.0088(19) 0.0118(18) C5C 0.0188(19) 0.0137(17) 0.014(2) -0.0020(14) 0.0025(15) 0.0007(14) O2W 0.112(6) 0.083(5) 0.085(5) 0.047(4) 0.034(4) 0.056(4) O1W 0.081(4) 0.109(6) 0.080(5) 0.048(4) 0.030(4) 0.067(4) O3W 0.138(7) 0.054(4) 0.147(9) 0.029(5) -0.031(6) 0.027(5) O7W 0.120(14) 0.35(3) 0.040(9) 0.018(14) 0.027(9) 0.133(19) O4W 0.094(6) 0.218(12) 0.050(5) 0.002(6) 0.012(4) -0.008(7) O5W 0.089(9) 0.040(6) 0.185(17) -0.023(8) -0.095(11) 0.029(6) O6W 0.144(15) 0.21(2) 0.029(7) 0.039(9) 0.053(8) 0.076(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O1B 2.229(3) . ? Er1 O3C 2.271(4) . ? Er1 O2B 2.287(3) . ? Er1 O1C 2.310(3) . ? Er1 O2 2.353(4) . ? Er1 O6 2.433(3) . ? Er1 O4A 2.437(3) . ? Er1 O3A 2.474(3) . ? Er1 C4A 2.811(4) . ? Er2 O1A 2.269(4) . ? Er2 O2A 2.336(3) . ? Er2 O1 2.351(4) . ? Er2 O4 2.352(4) . ? Er2 O5 2.356(4) . ? Er2 O3 2.358(4) . ? Er2 O2C 2.366(3) . ? Er2 O3B 2.409(3) . ? O1A C5A 1.249(6) . ? O2A C5A 1.259(6) 2_655 ? O3A C4A 1.260(5) . ? O4A C4A 1.261(6) . ? C1A C3A 1.387(6) . ? C1A C2A 1.398(6) . ? C1A C4A 1.502(6) . ? C2A C3A 1.396(6) 2_755 ? C2A C5A 1.509(6) . ? C3A C2A 1.396(6) 2_755 ? C3A H3A 0.93 . ? C5A O2A 1.259(6) 2_655 ? O1B C5B 1.262(5) . ? O2B C5B 1.251(6) 2_765 ? O3B C4B 1.259(5) . ? O4B C4B 1.250(7) . ? C1B C3B 1.390(6) 2_665 ? C1B C2B 1.398(6) . ? C1B C4B 1.509(6) . ? C2B C3B 1.394(6) . ? C2B C5B 1.496(6) . ? C3B C1B 1.390(6) 2_665 ? C3B H3B 0.93 . ? C5B O2B 1.251(6) 2_765 ? O1C C5C 1.259(6) . ? O2C C5C 1.253(5) 2_655 ? O3C C4C 1.235(6) . ? O4C C4C 1.238(6) . ? C1C C3C 1.382(7) 2_766 ? C1C C2C 1.409(6) . ? C1C C4C 1.512(7) . ? C2C C3C 1.393(7) . ? C2C C5C 1.503(6) . ? C3C C1C 1.382(7) 2_766 ? C3C H3C 0.93 . ? C5C O2C 1.253(5) 2_655 ? 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 O1B Er1 O3C 89.72(14) . . ? O1B Er1 O2B 101.92(13) . . ? O3C Er1 O2B 134.76(14) . . ? O1B Er1 O1C 81.96(13) . . ? O3C Er1 O1C 73.85(13) . . ? O2B Er1 O1C 150.54(13) . . ? O1B Er1 O2 155.02(15) . . ? O3C Er1 O2 76.91(16) . . ? O2B Er1 O2 74.61(15) . . ? O1C Er1 O2 113.50(15) . . ? O1B Er1 O6 70.84(12) . . ? O3C Er1 O6 72.01(13) . . ? O2B Er1 O6 71.10(13) . . ? O1C Er1 O6 135.88(13) . . ? O2 Er1 O6 84.88(15) . . ? O1B Er1 O4A 126.67(12) . . ? O3C Er1 O4A 128.51(14) . . ? O2B Er1 O4A 77.72(13) . . ? O1C Er1 O4A 76.79(13) . . ? O2 Er1 O4A 77.40(14) . . ? O6 Er1 O4A 147.27(13) . . ? O1B Er1 O3A 73.91(11) . . ? O3C Er1 O3A 143.68(13) . . ? O2B Er1 O3A 81.05(11) . . ? O1C Er1 O3A 71.91(12) . . ? O2 Er1 O3A 128.46(13) . . ? O6 Er1 O3A 128.51(12) . . ? O4A Er1 O3A 53.12(11) . . ? O1B Er1 C4A 100.49(13) . . ? O3C Er1 C4A 144.45(14) . . ? O2B Er1 C4A 76.56(13) . . ? O1C Er1 C4A 74.03(13) . . ? O2 Er1 C4A 102.62(15) . . ? O6 Er1 C4A 143.50(13) . . ? O4A Er1 C4A 26.59(12) . . ? O3A Er1 C4A 26.61(12) . . ? O1A Er2 O2A 104.40(14) . . ? O1A Er2 O1 73.23(13) . . ? O2A Er2 O1 74.72(13) . . ? O1A Er2 O4 144.52(14) . . ? O2A Er2 O4 82.59(17) . . ? O1 Er2 O4 140.80(14) . . ? O1A Er2 O5 85.69(16) . . ? O2A Er2 O5 144.54(15) . . ? O1 Er2 O5 76.01(16) . . ? O4 Er2 O5 108.90(19) . . ? O1A Er2 O3 83.09(16) . . ? O2A Er2 O3 145.11(15) . . ? O1 Er2 O3 138.81(15) . . ? O4 Er2 O3 73.18(18) . . ? O5 Er2 O3 68.91(16) . . ? O1A Er2 O2C 145.99(13) . . ? O2A Er2 O2C 81.69(14) . . ? O1 Er2 O2C 76.41(12) . . ? O4 Er2 O2C 68.90(13) . . ? O5 Er2 O2C 72.30(16) . . ? O3 Er2 O2C 111.23(14) . . ? O1A Er2 O3B 73.24(12) . . ? O2A Er2 O3B 74.92(12) . . ? O1 Er2 O3B 126.61(12) . . ? O4 Er2 O3B 75.31(13) . . ? O5 Er2 O3B 139.92(14) . . ? O3 Er2 O3B 74.89(13) . . ? O2C Er2 O3B 139.26(13) . . ? C5A O1A Er2 176.6(3) . . ? C5A O2A Er2 129.5(3) 2_655 . ? C4A O3A Er1 91.8(3) . . ? C4A O4A Er1 93.5(3) . . ? C3A C1A C2A 120.7(4) . . ? C3A C1A C4A 118.3(4) . . ? C2A C1A C4A 120.6(4) . . ? C3A C2A C1A 119.1(4) 2_755 . ? C3A C2A C5A 119.4(4) 2_755 . ? C1A C2A C5A 121.3(4) . . ? C1A C3A C2A 120.2(4) . 2_755 ? C1A C3A H3A 119.9 . . ? C2A C3A H3A 119.9 2_755 . ? O3A C4A O4A 121.2(4) . . ? O3A C4A C1A 117.4(4) . . ? O4A C4A C1A 121.1(4) . . ? O3A C4A Er1 61.6(2) . . ? O4A C4A Er1 59.9(2) . . ? C1A C4A Er1 169.5(3) . . ? O1A C5A O2A 125.4(4) . 2_655 ? O1A C5A C2A 118.3(4) . . ? O2A C5A C2A 116.3(4) 2_655 . ? C5B O1B Er1 146.8(3) . . ? C5B O2B Er1 141.2(3) 2_765 . ? C4B O3B Er2 136.1(3) . . ? C3B C1B C2B 119.6(4) 2_665 . ? C3B C1B C4B 116.8(4) 2_665 . ? C2B C1B C4B 123.5(4) . . ? C3B C2B C1B 119.8(4) . . ? C3B C2B C5B 118.4(4) . . ? C1B C2B C5B 121.7(4) . . ? C1B C3B C2B 120.6(4) 2_665 . ? C1B C3B H3B 119.7 2_665 . ? C2B C3B H3B 119.7 . . ? O4B C4B O3B 125.4(4) . . ? O4B C4B C1B 118.1(4) . . ? O3B C4B C1B 116.3(4) . . ? O2B C5B O1B 125.1(4) 2_765 . ? O2B C5B C2B 118.5(4) 2_765 . ? O1B C5B C2B 116.4(4) . . ? C5C O1C Er1 137.5(3) . . ? C5C O2C Er2 140.5(3) 2_655 . ? C4C O3C Er1 135.8(3) . . ? C3C C1C C2C 118.7(4) 2_766 . ? C3C C1C C4C 117.3(4) 2_766 . ? C2C C1C C4C 124.0(4) . . ? C3C C2C C1C 119.4(4) . . ? C3C C2C C5C 117.6(4) . . ? C1C C2C C5C 123.0(4) . . ? C1C C3C C2C 121.9(4) 2_766 . ? C1C C3C H3C 119 2_766 . ? C2C C3C H3C 119 . . ? O3C C4C O4C 122.7(5) . . ? O3C C4C C1C 119.0(4) . . ? O4C C4C C1C 118.1(5) . . ? O2C C5C O1C 124.4(4) 2_655 . ? O2C C5C C2C 117.1(4) 2_655 . ? O1C C5C C2C 118.5(4) . . ? # END of CIF data_job _database_code_depnum_ccdc_archive 'CCDC 912312' #TrackingRef 'C5.cif' _audit_creation_date 2012-11-22T14:02:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C15 H31 Gd2 O26' _chemical_formula_sum 'C15 H31 Gd2 O26' _chemical_formula_weight 941.9 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.24350(10) _cell_length_b 11.47890(10) _cell_length_c 14.0150(2) _cell_angle_alpha 84.7630(10) _cell_angle_beta 78.6310(10) _cell_angle_gamma 63.8190(10) _cell_volume 1449.83(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9494 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 32.032 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.158 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 914 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6064 _exptl_absorpt_correction_T_max 0.6731 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_unetI/netI 0.0459 _diffrn_reflns_number 34688 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 32.06 _diffrn_reflns_theta_full 32.06 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 10014 _reflns_number_gt 8050 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0372P)^2^+2.9719P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10014 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.957 _refine_diff_density_min -1.697 _refine_diff_density_rms 0.173 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.682568(17) 0.921900(14) 0.053995(11) 0.01492(5) Uani 1 1 d . . . Gd2 Gd 0.354209(19) 0.712129(14) 0.372013(12) 0.01854(5) Uani 1 1 d . . . O1 O 0.4135(3) 1.0386(2) 0.09725(18) 0.0182(5) Uani 1 1 d . . . O2 O 0.5910(3) 0.7608(2) 0.05439(19) 0.0207(5) Uani 1 1 d . . . O3 O 0.6083(3) 1.1504(2) 0.0168(2) 0.0216(5) Uani 1 1 d . . . O5 O 0.5996(3) 0.8695(2) 0.22117(19) 0.0246(5) Uani 1 1 d . . . O7 O 0.5100(3) 0.5251(2) -0.3643(2) 0.0266(6) Uani 1 1 d . . . O9 O 0.8840(3) 0.9536(2) -0.0542(2) 0.0277(6) Uani 1 1 d . . . O14 O 0.7093(4) 0.4380(3) -0.2976(2) 0.0366(7) Uani 1 1 d . . . O10 O 0.4500(3) 1.3289(2) 0.53359(19) 0.0241(5) Uani 1 1 d . . . O13 O 0.7824(3) 0.7729(2) -0.1095(2) 0.0260(6) Uani 1 1 d . . . O12 O 0.3976(3) 0.8992(2) 0.3314(2) 0.0283(6) Uani 1 1 d . . . O15 O 0.1751(3) 0.7640(2) -0.0843(2) 0.0262(6) Uani 1 1 d . . . O16 O 0.1483(3) 0.7792(3) 0.0757(2) 0.0279(6) Uani 1 1 d . . . O17 O 0.6697(3) 1.1824(3) 0.4697(2) 0.0294(6) Uani 1 1 d . . . C10 C 0.4933(4) 0.6230(3) 0.0116(2) 0.0163(6) Uani 1 1 d . . . C11 C 0.4840(4) 0.9379(3) 0.2778(2) 0.0183(6) Uani 1 1 d . . . C12 C 0.6710(4) 0.8514(3) -0.1406(2) 0.0175(6) Uani 1 1 d . . . C14 C 0.6230(4) 0.5112(3) 0.0159(3) 0.0177(6) Uani 1 1 d . . . H14 H 0.7061 0.5183 0.0263 0.021 Uiso 1 1 calc R . . C15 C 0.4768(4) 1.2317(3) 0.3815(3) 0.0202(7) Uani 1 1 d . . . C16 C 0.3684(4) 0.6117(3) -0.0050(3) 0.0179(6) Uani 1 1 d . . . C17 C 0.4913(4) 0.7545(3) 0.0180(2) 0.0156(6) Uani 1 1 d . . . C18 C 0.5357(4) 1.2514(3) 0.4656(3) 0.0221(7) Uani 1 1 d . . . C20 C 0.4499(4) 1.0779(3) 0.2894(3) 0.0191(6) Uani 1 1 d . . . C21 C 0.2216(4) 0.7279(3) -0.0049(3) 0.0195(7) Uani 1 1 d . . . C23 C 0.6246(4) 0.8229(3) -0.2271(2) 0.0175(6) Uani 1 1 d . . . C24 C 0.5942(4) 0.6694(3) -0.3176(3) 0.0206(7) Uani 1 1 d . . . C25 C 0.4958(4) 1.1067(3) 0.3675(3) 0.0219(7) Uani 1 1 d . . . H25 H 0.5399 1.0412 0.411 0.026 Uiso 1 1 calc R . . C26 C 0.6478(4) 0.6969(3) -0.2427(3) 0.0210(7) Uani 1 1 d . . . H26 H 0.6998 0.6301 -0.2027 0.025 Uiso 1 1 calc R . . C27 C 0.6057(5) 0.5366(3) -0.3266(3) 0.0238(7) Uani 1 1 d . . . O101 O 0.7723(4) 1.0178(3) 0.1577(2) 0.0334(7) Uani 1 1 d . . . O102 O 0.8969(3) 0.7399(3) 0.0909(2) 0.0332(7) Uani 1 1 d . . . O103 O 0.2614(4) 0.6034(3) 0.5133(3) 0.0411(8) Uani 1 1 d . . . O104 O 0.2493(4) 0.8180(3) 0.2277(2) 0.0437(8) Uani 1 1 d . . . O105 O 0.5696(4) 0.6388(3) 0.2486(2) 0.0432(8) Uani 1 1 d . . . O106 O 0.0957(4) 0.8472(4) 0.4234(3) 0.0494(9) Uani 1 1 d . . . O107 O 0.2155(6) 0.6191(5) 0.7591(4) 0.0831(15) Uani 1 1 d . . . O108 O 0.7843(6) 0.7557(6) 0.4167(5) 0.0960(18) Uani 1 1 d . . . O109 O 0.0214(7) 0.5223(5) 0.8629(6) 0.119(3) Uani 1 1 d . . . O110 O 0.8589(7) 0.9876(9) 0.3359(5) 0.190(5) Uani 1 1 d . . . O111 O -0.0211(6) 0.4310(6) 0.6956(5) 0.107(2) Uani 1 1 d . . . O112 O -0.0296(9) 0.6411(10) 0.5706(7) 0.169(4) Uani 1 1 d . . . O113 O 0.9341(16) 0.8782(13) 0.6294(13) 0.126(5) Uani 0.5 1 d P . . O213 O 0.8620(15) 0.8720(13) 0.5591(13) 0.126(5) Uani 0.5 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01632(8) 0.01121(7) 0.01988(9) 0.00086(5) -0.00732(6) -0.00682(6) Gd2 0.02755(10) 0.01305(8) 0.01989(9) 0.00127(6) -0.00880(7) -0.01154(7) O1 0.0208(12) 0.0149(10) 0.0199(12) -0.0021(8) -0.0064(9) -0.0072(9) O2 0.0249(13) 0.0136(10) 0.0300(14) 0.0019(9) -0.0112(11) -0.0118(9) O3 0.0212(12) 0.0117(10) 0.0335(14) 0.0018(9) -0.0105(11) -0.0064(9) O5 0.0333(15) 0.0167(11) 0.0240(13) 0.0010(9) -0.0056(11) -0.0111(10) O7 0.0384(16) 0.0182(12) 0.0321(15) 0.0020(10) -0.0152(12) -0.0170(11) O9 0.0207(13) 0.0201(12) 0.0406(17) -0.0009(11) -0.0030(12) -0.0082(10) O14 0.0499(19) 0.0162(12) 0.054(2) 0.0036(12) -0.0324(16) -0.0147(12) O10 0.0320(15) 0.0212(12) 0.0225(13) -0.0033(9) -0.0090(11) -0.0123(11) O13 0.0250(14) 0.0204(12) 0.0310(15) -0.0032(10) -0.0129(11) -0.0043(10) O12 0.0384(16) 0.0166(12) 0.0330(15) -0.0003(10) 0.0006(12) -0.0175(11) O15 0.0254(14) 0.0195(12) 0.0330(15) 0.0019(10) -0.0162(12) -0.0051(10) O16 0.0215(13) 0.0269(13) 0.0313(15) -0.0073(11) -0.0032(11) -0.0062(11) O17 0.0301(15) 0.0320(14) 0.0273(15) -0.0083(11) -0.0097(12) -0.0113(12) C10 0.0163(15) 0.0120(13) 0.0225(16) -0.0009(11) -0.0052(12) -0.0070(11) C11 0.0294(18) 0.0144(14) 0.0162(15) 0.0014(11) -0.0094(13) -0.0121(13) C12 0.0217(16) 0.0159(14) 0.0179(15) -0.0016(11) -0.0030(13) -0.0108(12) C14 0.0150(15) 0.0135(13) 0.0283(18) -0.0005(12) -0.0044(13) -0.0091(12) C15 0.0283(18) 0.0177(15) 0.0197(16) -0.0008(12) -0.0066(14) -0.0135(13) C16 0.0171(15) 0.0142(14) 0.0232(17) -0.0006(11) -0.0069(13) -0.0060(12) C17 0.0176(15) 0.0103(12) 0.0195(15) -0.0007(10) -0.0037(12) -0.0063(11) C18 0.035(2) 0.0174(15) 0.0215(17) 0.0005(12) -0.0082(15) -0.0169(14) C20 0.0284(18) 0.0130(13) 0.0186(16) 0.0012(11) -0.0041(13) -0.0117(13) C21 0.0145(15) 0.0129(14) 0.0339(19) -0.0010(12) -0.0079(14) -0.0067(11) C23 0.0227(16) 0.0135(13) 0.0184(16) -0.0016(11) -0.0055(13) -0.0086(12) C24 0.0279(18) 0.0145(14) 0.0227(17) -0.0022(12) -0.0077(14) -0.0105(13) C25 0.036(2) 0.0147(14) 0.0186(16) 0.0010(12) -0.0099(15) -0.0129(14) C26 0.032(2) 0.0146(14) 0.0191(16) -0.0001(11) -0.0096(14) -0.0109(13) C27 0.038(2) 0.0144(14) 0.0235(18) 0.0009(12) -0.0120(16) -0.0135(14) O101 0.0519(19) 0.0344(15) 0.0306(15) 0.0060(12) -0.0187(14) -0.0302(14) O102 0.0223(14) 0.0234(13) 0.0508(19) 0.0101(12) -0.0131(13) -0.0063(11) O103 0.0438(19) 0.0325(16) 0.0449(19) 0.0075(13) -0.0046(15) -0.0176(14) O104 0.070(2) 0.0336(16) 0.0391(18) 0.0115(13) -0.0347(18) -0.0253(16) O105 0.063(2) 0.0215(14) 0.0354(17) 0.0006(12) 0.0106(16) -0.0177(14) O106 0.0293(18) 0.051(2) 0.055(2) 0.0086(17) -0.0096(16) -0.0056(15) O107 0.076(3) 0.074(3) 0.091(4) -0.039(3) -0.004(3) -0.023(3) O108 0.077(4) 0.119(5) 0.103(4) -0.015(4) 0.005(3) -0.059(4) O109 0.079(4) 0.038(2) 0.226(8) -0.011(3) -0.024(5) -0.012(2) O110 0.094(5) 0.241(9) 0.094(5) -0.107(5) -0.067(4) 0.096(5) O111 0.065(4) 0.112(5) 0.140(6) -0.041(4) 0.010(4) -0.039(3) O112 0.106(6) 0.207(9) 0.189(9) 0.056(7) -0.002(6) -0.083(6) O113 0.084(8) 0.082(5) 0.188(14) -0.022(8) 0.049(7) -0.042(5) O213 0.084(8) 0.082(5) 0.188(14) -0.022(8) 0.049(7) -0.042(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O102 2.378(3) . ? Gd1 O2 2.414(2) . ? Gd1 O3 2.424(2) . ? Gd1 O101 2.424(3) . ? Gd1 O1 2.433(2) 2_675 ? Gd1 O5 2.446(3) . ? Gd1 O1 2.448(2) . ? Gd1 O9 2.453(3) . ? Gd1 O13 2.733(3) . ? Gd1 C12 2.953(3) . ? Gd1 Gd1 3.9133(3) 2_675 ? Gd2 O12 2.378(2) . ? Gd2 O105 2.386(3) . ? Gd2 O106 2.401(3) . ? Gd2 O104 2.445(3) . ? Gd2 O7 2.453(3) 2_665 ? Gd2 O14 2.463(3) 2_665 ? Gd2 O10 2.468(3) 2_676 ? Gd2 O103 2.498(3) . ? Gd2 O17 2.542(3) 2_676 ? Gd2 C27 2.814(3) 2_665 ? Gd2 C18 2.868(4) 2_676 ? O1 C12 1.296(4) 2_675 ? O1 Gd1 2.433(2) 2_675 ? O2 C17 1.259(4) . ? O3 C17 1.259(4) 2_675 ? O5 C11 1.253(4) . ? O7 C27 1.259(5) . ? O7 Gd2 2.453(3) 2_665 ? O14 C27 1.265(5) . ? O14 Gd2 2.463(3) 2_665 ? O10 C18 1.267(4) . ? O10 Gd2 2.468(3) 2_676 ? O13 C12 1.234(4) . ? O12 C11 1.253(4) . ? O15 C21 1.261(4) . ? O16 C21 1.258(5) . ? O17 C18 1.256(5) . ? O17 Gd2 2.542(3) 2_676 ? C10 C14 1.389(4) . ? C10 C16 1.406(5) . ? C10 C17 1.511(4) . ? C11 C20 1.504(4) . ? C12 O1 1.296(4) 2_675 ? C12 C23 1.497(5) . ? C14 C16 1.395(4) 2_665 ? C14 H14 0.93 . ? C15 C25 1.388(5) . ? C15 C24 1.401(5) 2_675 ? C15 C18 1.501(5) . ? C16 C14 1.395(4) 2_665 ? C16 C21 1.507(5) . ? C17 O3 1.259(4) 2_675 ? C18 Gd2 2.869(4) 2_676 ? C20 C25 1.391(5) . ? C20 C23 1.399(5) 2_675 ? C23 C26 1.388(4) . ? C23 C20 1.399(5) 2_675 ? C24 C26 1.394(5) . ? C24 C15 1.401(5) 2_675 ? C24 C27 1.492(4) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C27 Gd2 2.814(3) 2_665 ? O113 O213 1.37(2) . ? 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 O102 Gd1 O2 83.00(9) . . ? O102 Gd1 O3 137.63(9) . . ? O2 Gd1 O3 139.04(8) . . ? O102 Gd1 O101 78.14(11) . . ? O2 Gd1 O101 141.92(9) . . ? O3 Gd1 O101 69.01(9) . . ? O102 Gd1 O1 126.58(10) . 2_675 ? O2 Gd1 O1 75.84(8) . 2_675 ? O3 Gd1 O1 73.81(8) . 2_675 ? O101 Gd1 O1 141.21(9) . 2_675 ? O102 Gd1 O5 77.55(10) . . ? O2 Gd1 O5 69.84(9) . . ? O3 Gd1 O5 116.11(9) . . ? O101 Gd1 O5 73.92(9) . . ? O1 Gd1 O5 134.86(9) 2_675 . ? O102 Gd1 O1 145.03(9) . . ? O2 Gd1 O1 74.39(8) . . ? O3 Gd1 O1 71.02(8) . . ? O101 Gd1 O1 103.78(10) . . ? O1 Gd1 O1 73.40(9) 2_675 . ? O5 Gd1 O1 69.82(9) . . ? O102 Gd1 O9 77.15(10) . . ? O2 Gd1 O9 131.36(9) . . ? O3 Gd1 O9 69.57(9) . . ? O101 Gd1 O9 75.84(10) . . ? O1 Gd1 O9 81.31(9) 2_675 . ? O5 Gd1 O9 143.79(10) . . ? O1 Gd1 O9 137.65(8) . . ? O102 Gd1 O13 76.61(10) . . ? O2 Gd1 O13 64.16(9) . . ? O3 Gd1 O13 112.54(9) . . ? O101 Gd1 O13 139.64(10) . . ? O1 Gd1 O13 49.99(8) 2_675 . ? O5 Gd1 O13 129.17(8) . . ? O1 Gd1 O13 114.95(8) . . ? O9 Gd1 O13 68.19(9) . . ? O102 Gd1 C12 101.20(10) . . ? O2 Gd1 C12 65.23(9) . . ? O3 Gd1 C12 95.34(9) . . ? O101 Gd1 C12 150.91(10) . . ? O1 Gd1 C12 25.59(8) 2_675 . ? O5 Gd1 C12 134.80(9) . . ? O1 Gd1 C12 93.24(9) . . ? O9 Gd1 C12 75.70(9) . . ? O13 Gd1 C12 24.67(8) . . ? O102 Gd1 Gd1 152.02(7) . 2_675 ? O2 Gd1 Gd1 71.32(6) . 2_675 ? O3 Gd1 Gd1 67.87(6) . 2_675 ? O101 Gd1 Gd1 129.32(8) . 2_675 ? O1 Gd1 Gd1 36.83(6) 2_675 2_675 ? O5 Gd1 Gd1 102.87(7) . 2_675 ? O1 Gd1 Gd1 36.57(6) . 2_675 ? O9 Gd1 Gd1 111.61(7) . 2_675 ? O13 Gd1 Gd1 82.19(5) . 2_675 ? C12 Gd1 Gd1 58.30(7) . 2_675 ? O12 Gd2 O105 75.83(10) . . ? O12 Gd2 O106 90.42(12) . . ? O105 Gd2 O106 150.50(12) . . ? O12 Gd2 O104 70.01(11) . . ? O105 Gd2 O104 78.76(13) . . ? O106 Gd2 O104 71.99(13) . . ? O12 Gd2 O7 139.45(10) . 2_665 ? O105 Gd2 O7 66.90(10) . 2_665 ? O106 Gd2 O7 130.06(12) . 2_665 ? O104 Gd2 O7 115.60(10) . 2_665 ? O12 Gd2 O14 139.99(10) . 2_665 ? O105 Gd2 O14 85.09(12) . 2_665 ? O106 Gd2 O14 89.43(13) . 2_665 ? O104 Gd2 O14 71.98(10) . 2_665 ? O7 Gd2 O14 53.06(9) 2_665 2_665 ? O12 Gd2 O10 79.09(9) . 2_676 ? O105 Gd2 O10 78.30(11) . 2_676 ? O106 Gd2 O10 125.18(11) . 2_676 ? O104 Gd2 O10 145.10(11) . 2_676 ? O7 Gd2 O10 78.33(8) 2_665 2_676 ? O14 Gd2 O10 131.24(9) 2_665 2_676 ? O12 Gd2 O103 141.43(10) . . ? O105 Gd2 O103 133.55(10) . . ? O106 Gd2 O103 72.06(12) . . ? O104 Gd2 O103 131.03(12) . . ? O7 Gd2 O103 67.71(10) 2_665 . ? O14 Gd2 O103 75.55(11) 2_665 . ? O10 Gd2 O103 83.56(10) 2_676 . ? O12 Gd2 O17 72.38(10) . 2_676 ? O105 Gd2 O17 124.56(12) . 2_676 ? O106 Gd2 O17 73.41(12) . 2_676 ? O104 Gd2 O17 127.76(10) . 2_676 ? O7 Gd2 O17 116.59(9) 2_665 2_676 ? O14 Gd2 O17 144.56(11) 2_665 2_676 ? O10 Gd2 O17 52.03(9) 2_676 2_676 ? O103 Gd2 O17 69.77(11) . 2_676 ? O12 Gd2 C27 150.73(11) . 2_665 ? O105 Gd2 C27 76.56(11) . 2_665 ? O106 Gd2 C27 109.40(13) . 2_665 ? O104 Gd2 C27 95.22(10) . 2_665 ? O7 Gd2 C27 26.55(10) 2_665 2_665 ? O14 Gd2 C27 26.68(10) 2_665 2_665 ? O10 Gd2 C27 104.56(10) 2_676 2_665 ? O103 Gd2 C27 67.21(11) . 2_665 ? O17 Gd2 C27 133.00(10) 2_676 2_665 ? O12 Gd2 C18 75.11(10) . 2_676 ? O105 Gd2 C18 102.22(12) . 2_676 ? O106 Gd2 C18 99.13(13) . 2_676 ? O104 Gd2 C18 143.75(10) . 2_676 ? O7 Gd2 C18 97.23(9) 2_665 2_676 ? O14 Gd2 C18 144.15(10) 2_665 2_676 ? O10 Gd2 C18 26.11(10) 2_676 2_676 ? O103 Gd2 C18 74.23(11) . 2_676 ? O17 Gd2 C18 25.96(10) 2_676 2_676 ? C27 Gd2 C18 120.50(10) 2_665 2_676 ? C12 O1 Gd1 100.2(2) 2_675 2_675 ? C12 O1 Gd1 131.7(2) 2_675 . ? Gd1 O1 Gd1 106.60(9) 2_675 . ? C17 O2 Gd1 134.5(2) . . ? C17 O3 Gd1 140.6(2) 2_675 . ? C11 O5 Gd1 127.3(2) . . ? C27 O7 Gd2 92.9(2) . 2_665 ? C27 O14 Gd2 92.3(2) . 2_665 ? C18 O10 Gd2 94.9(2) . 2_676 ? C12 O13 Gd1 87.7(2) . . ? C11 O12 Gd2 142.6(2) . . ? C18 O17 Gd2 91.7(2) . 2_676 ? C14 C10 C16 119.0(3) . . ? C14 C10 C17 119.8(3) . . ? C16 C10 C17 121.0(3) . . ? O12 C11 O5 126.3(3) . . ? O12 C11 C20 115.7(3) . . ? O5 C11 C20 117.8(3) . . ? O13 C12 O1 120.8(3) . 2_675 ? O13 C12 C23 122.0(3) . . ? O1 C12 C23 117.2(3) 2_675 . ? O13 C12 Gd1 67.62(19) . . ? O1 C12 Gd1 54.17(16) 2_675 . ? C23 C12 Gd1 165.0(2) . . ? C10 C14 C16 121.5(3) . 2_665 ? C10 C14 H14 119.2 . . ? C16 C14 H14 119.2 2_665 . ? C25 C15 C24 119.1(3) . 2_675 ? C25 C15 C18 116.8(3) . . ? C24 C15 C18 124.2(3) 2_675 . ? C14 C16 C10 119.4(3) 2_665 . ? C14 C16 C21 118.4(3) 2_665 . ? C10 C16 C21 122.1(3) . . ? O2 C17 O3 124.8(3) . 2_675 ? O2 C17 C10 118.2(3) . . ? O3 C17 C10 117.0(3) 2_675 . ? O17 C18 O10 121.2(3) . . ? O17 C18 C15 118.0(3) . . ? O10 C18 C15 120.6(3) . . ? O17 C18 Gd2 62.35(19) . 2_676 ? O10 C18 Gd2 59.03(18) . 2_676 ? C15 C18 Gd2 179.2(3) . 2_676 ? C25 C20 C23 120.0(3) . 2_675 ? C25 C20 C11 116.5(3) . . ? C23 C20 C11 123.5(3) 2_675 . ? O16 C21 O15 123.5(3) . . ? O16 C21 C16 117.9(3) . . ? O15 C21 C16 118.5(3) . . ? C26 C23 C20 119.2(3) . 2_675 ? C26 C23 C12 119.5(3) . . ? C20 C23 C12 121.2(3) 2_675 . ? C26 C24 C15 119.9(3) . 2_675 ? C26 C24 C27 120.1(3) . . ? C15 C24 C27 119.9(3) 2_675 . ? C15 C25 C20 120.9(3) . . ? C15 C25 H25 119.5 . . ? C20 C25 H25 119.5 . . ? C23 C26 C24 120.8(3) . . ? C23 C26 H26 119.6 . . ? C24 C26 H26 119.6 . . ? O7 C27 O14 120.9(3) . . ? O7 C27 C24 118.4(3) . . ? O14 C27 C24 120.7(3) . . ? O7 C27 Gd2 60.51(18) . 2_665 ? O14 C27 Gd2 61.01(18) . 2_665 ? C24 C27 Gd2 171.7(3) . 2_665 ? # END of CIF data_gaussian-iso _database_code_depnum_ccdc_archive 'CCDC 912314' #TrackingRef 'archive-iso-C7.cif' _audit_creation_date 2012-11-22T14:24:19-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H56 Gd5 K1 O56' _chemical_formula_sum 'C40 H56 Gd5 K O56' _chemical_formula_weight 2258.2 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.537(5) _cell_length_b 14.761(5) _cell_length_c 23.057(5) _cell_angle_alpha 107.218(5) _cell_angle_beta 96.735(5) _cell_angle_gamma 97.691(5) _cell_volume 3030(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 34568 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 32.032 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2166 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.6000 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; a grid of 8 x 8 x 8 = 512 sampling points was used ; _exptl_absorpt_correction_T_min 0.3504 _exptl_absorpt_correction_T_max 0.7764 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_unetI/netI 0.0584 _diffrn_reflns_number 41851 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 32.05 _diffrn_reflns_theta_full 32.05 _diffrn_measured_fraction_theta_full 0.972 _diffrn_measured_fraction_theta_max 0.972 _reflns_number_total 20544 _reflns_number_gt 14291 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0807P)^2^+32.7747P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 20544 _refine_ls_number_parameters 844 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1792 _refine_ls_wR_factor_gt 0.1625 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 4.56 _refine_diff_density_min -6.806 _refine_diff_density_rms 0.321 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.43113(3) 0.12874(2) 0.957775(13) 0.01013(7) Uani 1 1 d . . . Gd2 Gd -0.06339(3) -0.36819(2) 0.457588(13) 0.00930(7) Uani 1 1 d . . . Gd3 Gd 0.30877(3) -0.34636(2) 0.798810(14) 0.00987(7) Uani 1 1 d . . . Gd4 Gd 0.18644(3) -0.15516(2) 0.700924(13) 0.00917(7) Uani 1 1 d . . . Gd5 Gd 0.64369(4) 0.24825(3) 0.65928(2) 0.02807(10) Uani 1 1 d . . . K6 K 0.85240(19) 0.25034(14) 0.84090(9) 0.0298(4) Uani 1 1 d . . . O7 O -0.0959(5) -0.5314(3) 0.5936(2) 0.0132(8) Uani 1 1 d . . . O8 O 0.3393(5) -0.2901(4) 0.7127(2) 0.0164(9) Uani 1 1 d . . . O9 O 0.2681(5) -0.0389(3) 0.9043(2) 0.0165(9) Uani 1 1 d . . . O10 O 0.0190(5) -0.3069(3) 0.6539(2) 0.0139(9) Uani 1 1 d . . . O11 O 0.2267(5) -0.4608(3) 0.5957(2) 0.0157(9) Uani 1 1 d . . . O12 O 0.3773(6) 0.1104(4) 0.8471(2) 0.0210(10) Uani 1 1 d . . . O13 O 0.1419(5) -0.2720(4) 0.8620(2) 0.0204(10) Uani 1 1 d . . . O14 O 0.5703(5) -0.3225(3) 0.8061(3) 0.0207(10) Uani 1 1 d . . . O15 O -0.1075(5) -0.4451(4) 0.5298(2) 0.0176(9) Uani 1 1 d . . . O16 O 0.3081(5) 0.0027(4) 0.6943(2) 0.0195(10) Uani 1 1 d . . . O17 O 0.1052(6) 0.3880(4) 0.6535(2) 0.0186(10) Uani 1 1 d . . . O18 O 0.3060(6) 0.2350(4) 0.9078(2) 0.0218(10) Uani 1 1 d . . . O19 O 0.1757(5) 0.2615(4) 0.5939(2) 0.0184(9) Uani 1 1 d . . . O20 O 0.4771(4) -0.1941(3) 0.8455(2) 0.0128(8) Uani 1 1 d . . . O21 O 0.1570(5) -0.2109(4) 0.7870(2) 0.0170(9) Uani 1 1 d . . . O22 O 0.5887(5) 0.0311(3) 0.9034(2) 0.0164(9) Uani 1 1 d . . . O23 O 0.3540(5) -0.2275(4) 0.6384(2) 0.0185(10) Uani 1 1 d . . . O24 O -0.0760(5) -0.1775(4) 0.6905(3) 0.0228(11) Uani 1 1 d . . . O25 O 0.3958(5) 0.0527(4) 1.0314(2) 0.0180(9) Uani 1 1 d . . . O26 O 0.3293(5) -0.5879(3) 0.5636(3) 0.0201(10) Uani 1 1 d . . . O27 O -0.0863(5) -0.2268(3) 0.5379(2) 0.0174(9) Uani 1 1 d . . . O28 O 0.8832(5) 0.2375(3) 0.5464(2) 0.0179(9) Uani 1 1 d . . . O29 O 0.6081(6) 0.3598(4) 1.1005(3) 0.0253(11) Uani 1 1 d . . . O30 O 0.6049(5) 0.2586(3) 0.9521(2) 0.0189(10) Uani 1 1 d . . . O31 O 0.1620(5) -0.3405(4) 0.5283(2) 0.0194(10) Uani 1 1 d . . . O32 O 0.1889(6) -0.4995(4) 0.8086(2) 0.0221(10) Uani 1 1 d . . . O33 O 0.0972(5) -0.4201(4) 0.7218(2) 0.0204(10) Uani 1 1 d . . . O34 O 0.1660(5) 0.0862(4) 0.9436(3) 0.0248(12) Uani 1 1 d . . . O35 O 0.3976(5) -0.0801(4) 0.7782(2) 0.0201(10) Uani 1 1 d . . . O36 O 0.1123(6) -0.1384(4) 0.6007(2) 0.0215(10) Uani 1 1 d . . . O37 O 0.8114(7) 0.3932(5) 0.6794(3) 0.0381(15) Uani 1 1 d . . . O38 O 0.4076(6) 0.2732(4) 1.0377(2) 0.0214(10) Uani 1 1 d . . . C39 C -0.2373(6) -0.3261(4) 0.6429(3) 0.0115(11) Uani 1 1 d . . . O40 O 0.6558(6) 0.1586(4) 1.0286(2) 0.0217(10) Uani 1 1 d . . . O41 O 0.1306(5) 0.0002(3) 0.7474(2) 0.0188(10) Uani 1 1 d . . . O42 O 0.3585(5) -0.5059(4) 0.7511(2) 0.0198(10) Uani 1 1 d . . . C43 C 0.7317(6) -0.1736(5) 0.8550(3) 0.0137(11) Uani 1 1 d . . . O44 O 0.6119(8) 0.3390(6) 0.7625(4) 0.0496(18) Uiso 1 1 d . . . C45 C 0.2450(7) 0.3471(5) 0.7605(3) 0.0151(12) Uani 1 1 d . . . O46 O 0.7908(9) 0.1503(5) 0.6003(4) 0.050(2) Uani 1 1 d . . . C47 C 0.1613(7) 0.3122(4) 0.6464(3) 0.0133(11) Uani 1 1 d . . . C48 C 0.2767(8) 0.3131(5) 0.8099(3) 0.0186(13) Uani 1 1 d . . . H48 H 0.2995 0.3564 0.8497 0.022 Uiso 1 1 calc R . . C49 C 0.3190(7) 0.1846(5) 0.8547(3) 0.0171(12) Uani 1 1 d . . . C50 C 0.2748(7) 0.2166(5) 0.8010(3) 0.0164(12) Uani 1 1 d . . . C51 C -0.0114(7) -0.1600(5) 0.8550(3) 0.0135(11) Uani 1 1 d . . . O52 O 0.4868(7) 0.3646(5) 0.6602(3) 0.0379(15) Uani 1 1 d . . . C53 C 0.0648(7) -0.0781(5) 0.4717(3) 0.0153(12) Uani 1 1 d . . . C54 C 0.8660(8) 0.1607(5) 0.5607(3) 0.0189(13) Uani 1 1 d . . . O55 O 0.6189(7) 0.2859(5) 0.5619(3) 0.0400(15) Uani 1 1 d . . . O56 O 0.8536(9) 0.2409(6) 0.7276(4) 0.058(2) Uiso 1 1 d . . . C57 C 0.6039(9) 0.3292(6) 0.9319(4) 0.0257(15) Uani 1 1 d . . . C58 C 0.8938(7) -0.0240(5) 0.9116(3) 0.0148(12) Uani 1 1 d . . . H58 H 0.9083 0.0399 0.9365 0.018 Uiso 1 1 calc R . . C59 C 0.6381(6) -0.0313(4) 0.9231(3) 0.0111(11) Uani 1 1 d . . . C60 C 0.2622(7) -0.5464(4) 0.7738(3) 0.0149(12) Uani 1 1 d . . . C61 C 0.5071(6) -0.3396(5) 0.6441(3) 0.0132(11) Uani 1 1 d . . . C62 C 0.2048(7) 0.2816(4) 0.7003(3) 0.0129(11) Uani 1 1 d . . . C63 C -0.2604(6) -0.4223(4) 0.6039(3) 0.0112(11) Uani 1 1 d . . . C64 C -0.1438(6) -0.4679(4) 0.5744(3) 0.0106(10) Uani 1 1 d . . . O65 O 1.1415(14) 0.2647(10) 0.9891(6) 0.104(4) Uiso 1 1 d . . . C66 C 0.0102(6) -0.0648(5) 0.8926(3) 0.0136(11) Uani 1 1 d . . . O67 O 0.5668(8) 0.1271(6) 0.7039(4) 0.0520(19) Uani 1 1 d . . . C68 C 0.2359(7) 0.1513(5) 0.7412(3) 0.0159(12) Uani 1 1 d . . . C69 C -0.0564(7) 0.0032(5) 0.5533(3) 0.0165(12) Uani 1 1 d . . . H69 H -0.0939 0.0058 0.5891 0.02 Uiso 1 1 calc R . . C70 C 0.1047(6) -0.2161(4) 0.8340(3) 0.0121(11) Uani 1 1 d . . . C71 C 0.2027(7) 0.1843(5) 0.6914(3) 0.0172(12) Uani 1 1 d . . . H71 H 0.1789 0.1406 0.6518 0.021 Uiso 1 1 calc R . . O72 O 0.4347(11) 0.1415(9) 0.5945(5) 0.096(4) Uani 1 1 d . . . C73 C 0.5077(7) 0.3462(5) 1.0562(3) 0.0163(12) Uani 1 1 d . . . C74 C 0.4848(6) -0.4353(4) 0.6074(3) 0.0122(11) Uani 1 1 d . . . C75 C 0.3907(6) -0.2847(4) 0.6657(3) 0.0109(11) Uani 1 1 d . . . C76 C 0.7549(6) -0.0777(4) 0.8936(3) 0.0122(11) Uani 1 1 d . . . C77 C 0.5842(6) -0.2341(4) 0.8344(3) 0.0118(11) Uani 1 1 d . . . C78 C -0.0896(6) -0.2661(5) 0.6634(3) 0.0130(11) Uani 1 1 d . . . C79 C 0.5490(8) 0.4165(5) 0.9681(3) 0.0198(13) Uani 1 1 d . . . C80 C 0.5063(7) 0.4237(5) 1.0256(3) 0.0176(12) Uani 1 1 d . . . C81 C 0.0120(7) -0.1527(4) 0.5566(3) 0.0136(11) Uani 1 1 d . . . C82 C -0.3534(7) -0.2854(5) 0.6631(3) 0.0164(12) Uani 1 1 d . . . H82 H -0.3386 -0.2222 0.6892 0.02 Uiso 1 1 calc R . . C84 C 0.5427(8) 0.4928(5) 0.9439(3) 0.0222(14) Uani 1 1 d . . . H84 H 0.5722 0.4876 0.9062 0.027 Uiso 1 1 calc R . . O86 O 0.6425(9) 0.3279(6) 0.8817(4) 0.057(2) Uiso 1 1 d . . . C88 C -0.3997(6) -0.4764(5) 0.5868(3) 0.0133(11) Uani 1 1 d . . . H88 H -0.415 -0.5402 0.5615 0.016 Uiso 1 1 calc R . . C91 C 0.8499(6) -0.2138(5) 0.8361(3) 0.0155(12) Uani 1 1 d . . . H91 H 0.8359 -0.2773 0.8105 0.019 Uiso 1 1 calc R . . C92 C 0.0070(7) -0.0757(4) 0.5260(3) 0.0144(11) Uani 1 1 d . . . C93 C 0.1586(7) -0.0019(5) 0.9151(3) 0.0163(12) Uani 1 1 d . . . C97 C 0.3369(6) -0.4972(5) 0.5878(3) 0.0136(11) Uani 1 1 d . . . O98 O 0.6887(9) 0.1298(6) 0.8231(4) 0.055(2) Uiso 1 1 d . . . O100 O 0.3880(17) -0.0515(11) 0.5676(7) 0.128(6) Uani 1 1 d . . . C11 C 0.2263(7) 0.0456(4) 0.7275(3) 0.0139(11) Uani 1 1 d . . . O104 O 0.2743(13) 0.4730(9) 0.2100(6) 0.101(4) Uiso 1 1 d . . . O102 O 0.938(2) 0.3807(14) 0.8315(9) 0.157(7) Uiso 1 1 d . . . O103 O 0.893(2) 0.2228(16) 0.9573(10) 0.178(8) Uiso 1 1 d . . . OW1 O 0.3719(15) 0.1942(11) 0.4905(7) 0.116(5) Uiso 1 1 d . . . O105 O 0.867(2) 0.0622(15) 0.7378(9) 0.168(7) Uiso 1 1 d . . . OW2 O 0.866(2) 0.4462(14) 0.0555(9) 0.148(6) Uiso 1 1 d . . . O106 O 0.989(3) 0.131(2) 0.8289(15) 0.275(14) Uiso 1 1 d . . . OW3 O 0.692(3) -0.068(2) 0.6361(14) 0.266(13) Uiso 1 1 d . . . OW4 O 0.120(3) 0.374(2) 0.0839(15) 0.275(13) Uiso 1 1 d . . . OW5 O 1.107(4) 0.372(3) 0.9417(17) 0.322(17) 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 Gd1 0.01027(13) 0.00970(14) 0.01067(14) 0.00389(11) 0.00090(10) 0.00185(10) Gd2 0.00946(13) 0.00846(14) 0.01051(14) 0.00378(11) 0.00124(10) 0.00204(10) Gd3 0.00881(13) 0.00699(13) 0.01332(15) 0.00264(11) 0.00141(10) 0.00144(9) Gd4 0.00841(13) 0.00669(13) 0.01202(14) 0.00257(10) 0.00114(10) 0.00135(9) Gd5 0.02612(19) 0.0273(2) 0.0322(2) 0.00984(16) 0.00875(15) 0.00519(15) K6 0.0285(8) 0.0300(9) 0.0362(9) 0.0139(7) 0.0121(7) 0.0096(7) O7 0.014(2) 0.011(2) 0.018(2) 0.0061(17) 0.0050(16) 0.0088(16) O8 0.015(2) 0.019(2) 0.016(2) 0.0056(19) 0.0069(17) 0.0049(17) O9 0.0079(19) 0.017(2) 0.026(3) 0.007(2) 0.0056(17) 0.0027(16) O10 0.0109(19) 0.011(2) 0.019(2) 0.0045(17) 0.0010(16) 0.0010(15) O11 0.0094(19) 0.015(2) 0.021(2) 0.0033(19) 0.0011(16) 0.0021(16) O12 0.030(3) 0.016(2) 0.018(2) 0.005(2) -0.0014(19) 0.008(2) O13 0.020(2) 0.025(3) 0.024(3) 0.014(2) 0.0083(19) 0.010(2) O14 0.013(2) 0.010(2) 0.033(3) -0.002(2) 0.0029(19) 0.0020(17) O15 0.022(2) 0.016(2) 0.017(2) 0.0069(19) 0.0061(18) 0.0036(18) O16 0.024(2) 0.013(2) 0.023(3) 0.008(2) 0.0036(19) 0.0030(18) O17 0.031(3) 0.014(2) 0.014(2) 0.0067(19) 0.0002(19) 0.0102(19) O18 0.036(3) 0.018(2) 0.012(2) 0.0038(19) 0.003(2) 0.010(2) O19 0.026(2) 0.016(2) 0.014(2) 0.0059(19) 0.0010(18) 0.0051(19) O20 0.0065(18) 0.012(2) 0.020(2) 0.0044(17) 0.0027(15) 0.0021(15) O21 0.018(2) 0.019(2) 0.017(2) 0.0052(19) 0.0082(17) 0.0069(18) O22 0.017(2) 0.015(2) 0.021(2) 0.0072(19) 0.0062(18) 0.0092(17) O23 0.017(2) 0.019(2) 0.024(3) 0.009(2) 0.0063(18) 0.0087(18) O24 0.014(2) 0.011(2) 0.039(3) 0.000(2) 0.004(2) 0.0040(17) O25 0.023(2) 0.016(2) 0.016(2) 0.0056(19) 0.0060(18) 0.0040(18) O26 0.011(2) 0.012(2) 0.035(3) 0.005(2) 0.0001(19) 0.0005(16) O27 0.023(2) 0.013(2) 0.014(2) 0.0031(18) -0.0001(17) 0.0019(18) O28 0.019(2) 0.011(2) 0.027(3) 0.009(2) 0.0084(19) 0.0051(17) O29 0.031(3) 0.021(3) 0.023(3) 0.011(2) -0.007(2) 0.001(2) O30 0.022(2) 0.012(2) 0.026(3) 0.011(2) 0.0048(19) 0.0044(18) O31 0.021(2) 0.014(2) 0.019(2) 0.0040(19) -0.0046(18) 0.0016(18) O32 0.032(3) 0.010(2) 0.024(3) 0.004(2) 0.007(2) 0.0024(19) O33 0.019(2) 0.015(2) 0.025(3) 0.007(2) -0.0032(19) 0.0014(18) O34 0.012(2) 0.012(2) 0.044(3) 0.002(2) -0.001(2) 0.0005(17) O35 0.022(2) 0.015(2) 0.021(3) 0.008(2) -0.0073(19) -0.0016(18) O36 0.025(3) 0.019(2) 0.019(3) 0.008(2) -0.0057(19) -0.0001(19) O37 0.031(3) 0.043(4) 0.039(4) 0.019(3) 0.001(3) -0.006(3) O38 0.028(3) 0.016(2) 0.019(2) 0.004(2) 0.004(2) 0.0040(19) C39 0.010(2) 0.008(3) 0.014(3) 0.000(2) 0.002(2) 0.0015(19) O40 0.024(2) 0.015(2) 0.022(3) 0.007(2) -0.0084(19) 0.0006(19) O41 0.019(2) 0.010(2) 0.028(3) 0.008(2) 0.0059(19) 0.0030(17) O42 0.021(2) 0.013(2) 0.028(3) 0.007(2) 0.0062(19) 0.0039(18) C43 0.008(2) 0.014(3) 0.019(3) 0.005(2) 0.003(2) 0.004(2) C45 0.022(3) 0.008(3) 0.013(3) 0.003(2) -0.002(2) 0.004(2) O46 0.083(6) 0.037(4) 0.058(5) 0.028(4) 0.054(4) 0.037(4) C47 0.016(3) 0.007(3) 0.014(3) 0.002(2) -0.001(2) 0.000(2) C48 0.031(4) 0.009(3) 0.015(3) 0.004(2) -0.005(3) 0.006(2) C49 0.020(3) 0.016(3) 0.014(3) 0.008(2) -0.003(2) 0.002(2) C50 0.027(3) 0.010(3) 0.010(3) 0.004(2) -0.004(2) 0.002(2) C51 0.012(3) 0.016(3) 0.013(3) 0.005(2) 0.003(2) 0.002(2) O52 0.033(3) 0.041(4) 0.040(4) 0.012(3) 0.004(3) 0.014(3) C53 0.018(3) 0.009(3) 0.019(3) 0.005(2) 0.002(2) 0.004(2) C54 0.029(3) 0.015(3) 0.017(3) 0.006(3) 0.005(3) 0.010(3) O55 0.039(4) 0.044(4) 0.044(4) 0.018(3) 0.015(3) 0.015(3) C57 0.041(4) 0.019(4) 0.022(4) 0.011(3) 0.009(3) 0.008(3) C58 0.011(3) 0.011(3) 0.022(3) 0.003(2) 0.006(2) 0.005(2) C59 0.010(2) 0.010(3) 0.011(3) 0.001(2) 0.0005(19) 0.0009(19) C60 0.021(3) 0.008(3) 0.014(3) 0.002(2) -0.004(2) 0.004(2) C61 0.009(2) 0.011(3) 0.017(3) 0.002(2) 0.004(2) 0.000(2) C62 0.018(3) 0.006(2) 0.016(3) 0.004(2) 0.001(2) 0.003(2) C63 0.012(3) 0.009(3) 0.012(3) 0.002(2) 0.005(2) 0.003(2) C64 0.009(2) 0.010(3) 0.012(3) 0.002(2) 0.0000(19) 0.0046(19) C66 0.010(3) 0.010(3) 0.019(3) 0.004(2) 0.003(2) 0.000(2) O67 0.044(4) 0.046(4) 0.068(5) 0.025(4) 0.010(4) -0.002(3) C68 0.020(3) 0.011(3) 0.018(3) 0.007(2) -0.001(2) 0.006(2) C69 0.024(3) 0.016(3) 0.015(3) 0.008(2) 0.011(2) 0.009(2) C70 0.006(2) 0.011(3) 0.017(3) 0.001(2) 0.001(2) 0.0004(19) C71 0.024(3) 0.010(3) 0.013(3) 0.002(2) -0.005(2) 0.002(2) O72 0.068(6) 0.129(10) 0.062(6) 0.025(6) -0.010(5) -0.055(6) C73 0.026(3) 0.011(3) 0.016(3) 0.007(2) 0.005(2) 0.007(2) C74 0.011(3) 0.008(3) 0.017(3) 0.001(2) 0.003(2) 0.002(2) C75 0.008(2) 0.010(3) 0.014(3) 0.004(2) 0.0014(19) 0.0003(19) C76 0.011(2) 0.011(3) 0.014(3) 0.000(2) 0.004(2) 0.004(2) C77 0.012(3) 0.007(3) 0.016(3) 0.002(2) 0.001(2) 0.0017(19) C78 0.007(2) 0.011(3) 0.019(3) 0.004(2) 0.001(2) 0.000(2) C79 0.029(4) 0.015(3) 0.015(3) 0.003(3) 0.005(3) 0.008(3) C80 0.022(3) 0.019(3) 0.012(3) 0.006(2) 0.001(2) 0.002(2) C81 0.021(3) 0.006(3) 0.014(3) 0.003(2) 0.004(2) 0.004(2) C82 0.011(3) 0.014(3) 0.020(3) 0.000(2) 0.002(2) 0.000(2) C84 0.035(4) 0.016(3) 0.020(3) 0.010(3) 0.008(3) 0.009(3) C88 0.011(3) 0.009(3) 0.019(3) 0.001(2) 0.004(2) 0.003(2) C91 0.009(3) 0.014(3) 0.017(3) -0.003(2) 0.002(2) 0.002(2) C92 0.021(3) 0.007(3) 0.015(3) 0.002(2) 0.001(2) 0.004(2) C93 0.010(3) 0.016(3) 0.025(3) 0.010(3) 0.000(2) 0.002(2) C97 0.011(3) 0.018(3) 0.012(3) 0.005(2) 0.001(2) 0.001(2) O100 0.143(13) 0.115(11) 0.098(10) 0.001(8) 0.044(9) -0.023(9) C11 0.021(3) 0.007(3) 0.012(3) 0.001(2) -0.004(2) 0.003(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O25 2.328(5) . ? Gd1 O30 2.406(5) . ? Gd1 O22 2.420(5) . ? Gd1 O38 2.427(5) . ? Gd1 O40 2.440(5) . ? Gd1 O12 2.469(5) . ? Gd1 O34 2.481(5) . ? Gd1 O18 2.542(5) . ? Gd1 O9 2.603(5) . ? Gd1 C49 2.876(6) . ? Gd1 C93 2.895(7) . ? Gd2 O15 2.322(5) . ? Gd2 O27 2.400(5) . ? Gd2 O7 2.426(4) 2_546 ? Gd2 O28 2.437(5) 2_656 ? Gd2 O31 2.448(5) . ? Gd2 O17 2.469(5) 2_556 ? Gd2 O26 2.485(5) 2_546 ? Gd2 O19 2.509(5) 2_556 ? Gd2 O11 2.640(5) 2_546 ? Gd2 C47 2.856(6) 2_556 ? Gd2 C97 2.931(6) 2_546 ? Gd3 O8 2.400(5) . ? Gd3 O33 2.416(5) . ? Gd3 O42 2.423(5) . ? Gd3 O13 2.435(5) . ? Gd3 O29 2.438(5) 2_657 ? Gd3 O20 2.446(5) . ? Gd3 O14 2.451(5) . ? Gd3 O32 2.477(5) . ? Gd3 O21 2.679(5) . ? Gd3 C60 2.798(6) . ? Gd3 C77 2.800(6) . ? Gd3 C70 2.931(6) . ? Gd4 O41 2.387(5) . ? Gd4 O21 2.394(5) . ? Gd4 O35 2.418(5) . ? Gd4 O23 2.421(5) . ? Gd4 O36 2.431(5) . ? Gd4 O10 2.437(5) . ? Gd4 O24 2.454(5) . ? Gd4 O16 2.515(5) . ? Gd4 O8 2.678(5) . ? Gd4 C78 2.799(6) . ? Gd4 C11 2.806(6) . ? Gd4 C75 2.926(6) . ? Gd5 O37 2.382(6) . ? Gd5 O67 2.389(7) . ? Gd5 O46 2.395(6) . ? Gd5 O72 2.399(9) . ? Gd5 O52 2.421(6) . ? Gd5 O56 2.434(8) . ? Gd5 O44 2.438(8) . ? Gd5 O55 2.460(7) . ? Gd5 K6 4.410(2) . ? K6 O102 2.071(19) . ? K6 O98 2.108(9) . ? K6 O106 2.30(3) . ? K6 O86 2.573(9) . ? K6 O56 2.576(9) . ? K6 O103 2.82(2) . ? K6 OW5 3.09(4) . ? K6 O105 3.11(2) . ? K6 O44 3.386(8) . ? K6 C57 3.440(8) . ? O7 C64 1.263(7) . ? O7 Gd2 2.426(4) 2_546 ? O8 C75 1.260(7) . ? O9 C93 1.259(8) . ? O10 C78 1.274(7) . ? O11 C97 1.250(8) . ? O11 Gd2 2.640(5) 2_546 ? O12 C49 1.270(8) . ? O13 C70 1.250(8) . ? O14 C77 1.256(8) . ? O15 C64 1.244(8) . ? O16 C11 1.258(8) . ? O17 C47 1.280(8) . ? O17 Gd2 2.469(5) 2_556 ? O18 C49 1.260(8) . ? O19 C47 1.254(8) . ? O19 Gd2 2.509(5) 2_556 ? O20 C77 1.261(7) . ? O21 C70 1.263(8) . ? O22 C59 1.261(8) . ? O23 C75 1.255(8) . ? O24 C78 1.253(8) . ? O25 C59 1.246(8) 2_657 ? O26 C97 1.277(8) . ? O26 Gd2 2.485(5) 2_546 ? O27 C81 1.270(8) . ? O28 C54 1.266(8) . ? O28 Gd2 2.437(5) 2_656 ? O29 C73 1.264(8) . ? O29 Gd3 2.438(5) 2_657 ? O30 C57 1.262(8) . ? O32 C60 1.243(8) . ? O34 C93 1.261(9) . ? O36 C81 1.258(8) . ? O38 C73 1.270(9) . ? C39 C82 1.392(9) . ? C39 C63 1.410(8) . ? C39 C78 1.501(8) . ? O41 C11 1.268(8) . ? O42 C60 1.275(8) . ? C43 C91 1.397(8) . ? C43 C76 1.403(9) . ? C43 C77 1.503(8) . ? C45 C48 1.393(9) . ? C45 C62 1.411(9) . ? C45 C60 1.492(9) 1_565 ? O46 C54 1.257(9) . ? C47 C62 1.479(9) . ? C47 Gd2 2.856(6) 2_556 ? C48 C50 1.375(9) . ? C49 C50 1.487(9) . ? C50 C68 1.402(9) . ? C51 C66 1.389(9) . ? C51 C91 1.397(9) 1_455 ? C51 C70 1.510(9) . ? C53 C69 1.397(9) 2_556 ? C53 C92 1.418(9) . ? C53 C54 1.507(9) 2_656 ? C54 C53 1.507(9) 2_656 ? C57 O86 1.250(11) . ? C57 C79 1.509(10) . ? C58 C66 1.386(8) 1_655 ? C58 C76 1.396(9) . ? C59 O25 1.246(8) 2_657 ? C59 C76 1.510(8) . ? C60 C45 1.492(9) 1_545 ? C61 C74 1.388(9) . ? C61 C82 1.404(8) 1_655 ? C61 C75 1.506(8) . ? C62 C71 1.385(9) . ? C63 C88 1.402(8) . ? C63 C64 1.503(8) . ? C66 C58 1.386(8) 1_455 ? C66 C93 1.524(9) . ? C68 C71 1.394(9) . ? C68 C11 1.485(9) . ? C69 C53 1.397(9) 2_556 ? C69 C92 1.401(9) . ? C73 C80 1.511(9) . ? C74 C88 1.393(8) 1_655 ? C74 C97 1.513(8) . ? C79 C84 1.402(10) . ? C79 C80 1.411(9) . ? C80 C84 1.397(10) 2_667 ? C81 C92 1.508(9) . ? C82 C61 1.404(8) 1_455 ? C84 C80 1.397(10) 2_667 ? C88 C74 1.393(8) 1_455 ? C91 C51 1.397(9) 1_655 ? C97 Gd2 2.931(6) 2_546 ? 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 O25 Gd1 O30 134.71(18) . . ? O25 Gd1 O22 99.16(17) . . ? O30 Gd1 O22 82.61(17) . . ? O25 Gd1 O38 84.58(17) . . ? O30 Gd1 O38 72.74(18) . . ? O22 Gd1 O38 147.81(18) . . ? O25 Gd1 O40 70.90(18) . . ? O30 Gd1 O40 66.51(17) . . ? O22 Gd1 O40 72.74(18) . . ? O38 Gd1 O40 78.51(18) . . ? O25 Gd1 O12 144.12(18) . . ? O30 Gd1 O12 79.50(18) . . ? O22 Gd1 O12 70.87(17) . . ? O38 Gd1 O12 122.58(17) . . ? O40 Gd1 O12 132.56(19) . . ? O25 Gd1 O34 77.09(19) . . ? O30 Gd1 O34 137.16(17) . . ? O22 Gd1 O34 126.07(18) . . ? O38 Gd1 O34 86.02(18) . . ? O40 Gd1 O34 145.5(2) . . ? O12 Gd1 O34 81.66(19) . . ? O25 Gd1 O18 138.10(17) . . ? O30 Gd1 O18 70.32(18) . . ? O22 Gd1 O18 119.59(16) . . ? O38 Gd1 O18 71.34(17) . . ? O40 Gd1 O18 132.84(18) . . ? O12 Gd1 O18 52.06(16) . . ? O34 Gd1 O18 67.72(18) . . ? O25 Gd1 O9 71.15(17) . . ? O30 Gd1 O9 149.42(17) . . ? O22 Gd1 O9 76.06(16) . . ? O38 Gd1 O9 134.13(16) . . ? O40 Gd1 O9 125.28(16) . . ? O12 Gd1 O9 72.99(17) . . ? O34 Gd1 O9 51.46(16) . . ? O18 Gd1 O9 101.60(17) . . ? O25 Gd1 C49 150.21(19) . . ? O30 Gd1 C49 72.87(18) . . ? O22 Gd1 C49 95.24(18) . . ? O38 Gd1 C49 96.87(19) . . ? O40 Gd1 C49 138.67(19) . . ? O12 Gd1 C49 26.09(18) . . ? O34 Gd1 C49 73.3(2) . . ? O18 Gd1 C49 25.98(18) . . ? O9 Gd1 C49 87.38(18) . . ? O25 Gd1 C93 72.62(19) . . ? O30 Gd1 C93 151.96(18) . . ? O22 Gd1 C93 101.13(19) . . ? O38 Gd1 C93 110.40(19) . . ? O40 Gd1 C93 141.33(18) . . ? O12 Gd1 C93 75.69(19) . . ? O34 Gd1 C93 25.67(18) . . ? O18 Gd1 C93 84.09(18) . . ? O9 Gd1 C93 25.79(17) . . ? C49 Gd1 C93 79.10(19) . . ? O15 Gd2 O27 83.62(17) . . ? O15 Gd2 O7 98.14(16) . 2_546 ? O27 Gd2 O7 147.26(16) . 2_546 ? O15 Gd2 O28 135.24(18) . 2_656 ? O27 Gd2 O28 73.30(17) . 2_656 ? O7 Gd2 O28 83.24(16) 2_546 2_656 ? O15 Gd2 O31 72.58(17) . . ? O27 Gd2 O31 78.66(17) . . ? O7 Gd2 O31 70.89(17) 2_546 . ? O28 Gd2 O31 65.67(17) 2_656 . ? O15 Gd2 O17 143.50(17) . 2_556 ? O27 Gd2 O17 125.02(16) . 2_556 ? O7 Gd2 O17 70.41(16) 2_546 2_556 ? O28 Gd2 O17 79.24(17) 2_656 2_556 ? O31 Gd2 O17 129.86(18) . 2_556 ? O15 Gd2 O26 78.05(18) . 2_546 ? O27 Gd2 O26 88.27(17) . 2_546 ? O7 Gd2 O26 124.22(17) 2_546 2_546 ? O28 Gd2 O26 137.00(16) 2_656 2_546 ? O31 Gd2 O26 148.91(18) . 2_546 ? O17 Gd2 O26 80.60(18) 2_556 2_546 ? O15 Gd2 O19 139.20(17) . 2_556 ? O27 Gd2 O19 73.19(16) . 2_556 ? O7 Gd2 O19 119.52(16) 2_546 2_556 ? O28 Gd2 O19 69.21(16) 2_656 2_556 ? O31 Gd2 O19 131.87(17) . 2_556 ? O17 Gd2 O19 52.59(16) 2_556 2_556 ? O26 Gd2 O19 68.33(17) 2_546 2_556 ? O15 Gd2 O11 69.28(17) . 2_546 ? O27 Gd2 O11 133.87(16) . 2_546 ? O7 Gd2 O11 75.43(15) 2_546 2_546 ? O28 Gd2 O11 150.27(16) 2_656 2_546 ? O31 Gd2 O11 123.83(16) . 2_546 ? O17 Gd2 O11 74.26(16) 2_556 2_546 ? O26 Gd2 O11 50.84(15) 2_546 2_546 ? O19 Gd2 O11 103.68(16) 2_556 2_546 ? O15 Gd2 C47 150.65(18) . 2_556 ? O27 Gd2 C47 98.84(17) . 2_556 ? O7 Gd2 C47 95.24(17) 2_546 2_556 ? O28 Gd2 C47 72.20(17) 2_656 2_556 ? O31 Gd2 C47 136.71(17) . 2_556 ? O17 Gd2 C47 26.57(17) 2_556 2_556 ? O26 Gd2 C47 72.81(18) 2_546 2_556 ? O19 Gd2 C47 26.02(17) 2_556 2_556 ? O11 Gd2 C47 89.18(16) 2_546 2_556 ? O15 Gd2 C97 71.26(18) . 2_546 ? O27 Gd2 C97 111.43(18) . 2_546 ? O7 Gd2 C97 99.90(18) 2_546 2_546 ? O28 Gd2 C97 152.98(17) 2_656 2_546 ? O31 Gd2 C97 140.84(17) . 2_546 ? O17 Gd2 C97 76.68(17) 2_556 2_546 ? O26 Gd2 C97 25.61(17) 2_546 2_546 ? O19 Gd2 C97 86.36(17) 2_556 2_546 ? O11 Gd2 C97 25.25(16) 2_546 2_546 ? C47 Gd2 C97 80.78(17) 2_556 2_546 ? O8 Gd3 O33 73.07(17) . . ? O8 Gd3 O42 95.50(17) . . ? O33 Gd3 O42 77.75(17) . . ? O8 Gd3 O13 114.74(16) . . ? O33 Gd3 O13 84.62(19) . . ? O42 Gd3 O13 138.66(17) . . ? O8 Gd3 O29 152.84(18) . 2_657 ? O33 Gd3 O29 133.93(18) . 2_657 ? O42 Gd3 O29 89.27(19) . 2_657 ? O13 Gd3 O29 76.58(19) . 2_657 ? O8 Gd3 O20 77.00(16) . . ? O33 Gd3 O20 141.74(16) . . ? O42 Gd3 O20 128.94(16) . . ? O13 Gd3 O20 86.79(17) . . ? O29 Gd3 O20 79.24(17) 2_657 . ? O8 Gd3 O14 78.89(18) . . ? O33 Gd3 O14 138.85(18) . . ? O42 Gd3 O14 75.60(16) . . ? O13 Gd3 O14 135.16(18) . . ? O29 Gd3 O14 76.44(19) 2_657 . ? O20 Gd3 O14 53.34(15) . . ? O8 Gd3 O32 133.56(17) . . ? O33 Gd3 O32 67.49(18) . . ? O42 Gd3 O32 53.41(17) . . ? O13 Gd3 O32 85.32(18) . . ? O29 Gd3 O32 69.33(18) 2_657 . ? O20 Gd3 O32 148.56(17) . . ? O14 Gd3 O32 116.98(18) . . ? O8 Gd3 O21 64.42(15) . . ? O33 Gd3 O21 70.57(16) . . ? O42 Gd3 O21 146.15(17) . . ? O13 Gd3 O21 50.32(15) . . ? O29 Gd3 O21 121.35(18) 2_657 . ? O20 Gd3 O21 75.31(15) . . ? O14 Gd3 O21 122.38(16) . . ? O32 Gd3 O21 120.55(17) . . ? O8 Gd3 C60 116.01(18) . . ? O33 Gd3 C60 70.04(18) . . ? O42 Gd3 C60 27.06(18) . . ? O13 Gd3 C60 111.63(19) . . ? O29 Gd3 C60 78.47(19) 2_657 . ? O20 Gd3 C60 146.59(17) . . ? O14 Gd3 C60 97.14(18) . . ? O32 Gd3 C60 26.36(18) . . ? O21 Gd3 C60 137.97(17) . . ? O8 Gd3 C77 77.02(17) . . ? O33 Gd3 C77 149.92(18) . . ? O42 Gd3 C77 102.21(17) . . ? O13 Gd3 C77 111.27(19) . . ? O29 Gd3 C77 75.84(19) 2_657 . ? O20 Gd3 C77 26.74(16) . . ? O14 Gd3 C77 26.61(16) . . ? O32 Gd3 C77 136.55(18) . . ? O21 Gd3 C77 99.37(17) . . ? C60 Gd3 C77 122.21(18) . . ? O8 Gd3 C70 89.93(17) . . ? O33 Gd3 C70 76.22(17) . . ? O42 Gd3 C70 150.54(17) . . ? O13 Gd3 C70 24.81(17) . . ? O29 Gd3 C70 98.97(19) 2_657 . ? O20 Gd3 C70 80.50(16) . . ? O14 Gd3 C70 133.80(16) . . ? O32 Gd3 C70 103.19(17) . . ? O21 Gd3 C70 25.52(16) . . ? C60 Gd3 C70 127.45(18) . . ? C77 Gd3 C70 107.23(17) . . ? O41 Gd4 O21 95.11(17) . . ? O41 Gd4 O35 78.66(18) . . ? O21 Gd4 O35 72.99(17) . . ? O41 Gd4 O23 139.36(17) . . ? O21 Gd4 O23 114.93(16) . . ? O35 Gd4 O23 84.52(18) . . ? O41 Gd4 O36 88.63(18) . . ? O21 Gd4 O36 155.21(17) . . ? O35 Gd4 O36 131.66(17) . . ? O23 Gd4 O36 75.48(18) . . ? O41 Gd4 O10 127.44(16) . . ? O21 Gd4 O10 77.45(17) . . ? O35 Gd4 O10 142.26(16) . . ? O23 Gd4 O10 87.21(17) . . ? O36 Gd4 O10 80.84(17) . . ? O41 Gd4 O24 73.83(16) . . ? O21 Gd4 O24 80.96(18) . . ? O35 Gd4 O24 139.91(19) . . ? O23 Gd4 O24 134.78(18) . . ? O36 Gd4 O24 76.57(19) . . ? O10 Gd4 O24 53.62(16) . . ? O41 Gd4 O16 53.38(17) . . ? O21 Gd4 O16 131.77(17) . . ? O35 Gd4 O16 66.14(17) . . ? O23 Gd4 O16 85.99(17) . . ? O36 Gd4 O16 68.90(17) . . ? O10 Gd4 O16 149.73(16) . . ? O24 Gd4 O16 115.59(17) . . ? O41 Gd4 O8 147.03(17) . . ? O21 Gd4 O8 64.51(15) . . ? O35 Gd4 O8 70.85(16) . . ? O23 Gd4 O8 50.43(15) . . ? O36 Gd4 O8 121.02(17) . . ? O10 Gd4 O8 75.55(15) . . ? O24 Gd4 O8 123.76(16) . . ? O16 Gd4 O8 120.57(16) . . ? O41 Gd4 C78 100.40(18) . . ? O21 Gd4 C78 78.32(18) . . ? O35 Gd4 C78 151.04(18) . . ? O23 Gd4 C78 111.59(18) . . ? O36 Gd4 C78 76.90(18) . . ? O10 Gd4 C78 27.05(17) . . ? O24 Gd4 C78 26.57(17) . . ? O16 Gd4 C78 136.08(17) . . ? O8 Gd4 C78 100.27(17) . . ? O41 Gd4 C11 26.75(18) . . ? O21 Gd4 C11 114.95(18) . . ? O35 Gd4 C11 70.20(17) . . ? O23 Gd4 C11 112.62(18) . . ? O36 Gd4 C11 77.69(18) . . ? O10 Gd4 C11 145.58(17) . . ? O24 Gd4 C11 95.05(18) . . ? O16 Gd4 C11 26.64(18) . . ? O8 Gd4 C11 138.81(17) . . ? C78 Gd4 C11 120.41(18) . . ? O41 Gd4 C75 151.98(17) . . ? O21 Gd4 C75 90.00(16) . . ? O35 Gd4 C75 76.56(18) . . ? O23 Gd4 C75 24.94(16) . . ? O36 Gd4 C75 98.14(18) . . ? O10 Gd4 C75 80.56(16) . . ? O24 Gd4 C75 134.18(16) . . ? O16 Gd4 C75 103.85(17) . . ? O8 Gd4 C75 25.50(15) . . ? C78 Gd4 C75 107.61(18) . . ? C11 Gd4 C75 128.80(18) . . ? O37 Gd5 O67 142.0(3) . . ? O37 Gd5 O46 93.4(3) . . ? O67 Gd5 O46 92.1(3) . . ? O37 Gd5 O72 147.0(3) . . ? O67 Gd5 O72 70.5(3) . . ? O46 Gd5 O72 89.2(4) . . ? O37 Gd5 O52 78.2(2) . . ? O67 Gd5 O52 115.3(3) . . ? O46 Gd5 O52 145.3(2) . . ? O72 Gd5 O52 81.1(4) . . ? O37 Gd5 O56 72.3(3) . . ? O67 Gd5 O56 74.3(3) . . ? O46 Gd5 O56 70.8(3) . . ? O72 Gd5 O56 138.5(4) . . ? O52 Gd5 O56 134.9(3) . . ? O37 Gd5 O44 78.4(3) . . ? O67 Gd5 O44 75.8(3) . . ? O46 Gd5 O44 145.2(3) . . ? O72 Gd5 O44 116.0(3) . . ? O52 Gd5 O44 66.6(2) . . ? O56 Gd5 O44 74.5(3) . . ? O37 Gd5 O55 75.2(2) . . ? O67 Gd5 O55 142.3(3) . . ? O46 Gd5 O55 76.6(2) . . ? O72 Gd5 O55 73.5(3) . . ? O52 Gd5 O55 68.6(2) . . ? O56 Gd5 O55 131.7(3) . . ? O44 Gd5 O55 131.6(2) . . ? O37 Gd5 K6 84.17(16) . . ? O67 Gd5 K6 57.9(2) . . ? O46 Gd5 K6 96.2(2) . . ? O72 Gd5 K6 128.2(3) . . ? O52 Gd5 K6 116.03(17) . . ? O56 Gd5 K6 29.2(2) . . ? O44 Gd5 K6 49.64(18) . . ? O55 Gd5 K6 157.57(17) . . ? O102 K6 O98 153.2(6) . . ? O102 K6 O106 119.0(10) . . ? O98 K6 O106 80.4(8) . . ? O102 K6 O86 88.4(5) . . ? O98 K6 O86 77.5(3) . . ? O106 K6 O86 151.1(8) . . ? O102 K6 O56 67.4(6) . . ? O98 K6 O56 96.3(3) . . ? O106 K6 O56 89.7(8) . . ? O86 K6 O56 110.9(3) . . ? O102 K6 O103 119.8(7) . . ? O98 K6 O103 81.3(5) . . ? O106 K6 O103 75.6(9) . . ? O86 K6 O103 82.8(5) . . ? O56 K6 O103 165.3(5) . . ? O102 K6 OW5 64.7(9) . . ? O98 K6 OW5 140.0(7) . . ? O106 K6 OW5 84.3(11) . . ? O86 K6 OW5 101.1(7) . . ? O56 K6 OW5 120.4(7) . . ? O103 K6 OW5 59.1(8) . . ? O102 K6 O105 118.2(6) . . ? O98 K6 O105 61.4(4) . . ? O106 K6 O105 44.0(8) . . ? O86 K6 O105 132.9(4) . . ? O56 K6 O105 56.6(4) . . ? O103 K6 O105 110.5(6) . . ? OW5 K6 O105 124.9(8) . . ? O102 K6 O44 67.3(5) . . ? O98 K6 O44 86.1(3) . . ? O106 K6 O44 142.7(8) . . ? O86 K6 O44 53.6(2) . . ? O56 K6 O44 57.4(2) . . ? O103 K6 O44 136.3(4) . . ? OW5 K6 O44 125.7(7) . . ? O105 K6 O44 99.3(4) . . ? O102 K6 C57 98.5(5) . . ? O98 K6 C57 74.3(3) . . ? O106 K6 C57 136.0(8) . . ? O86 K6 C57 17.4(2) . . ? O56 K6 C57 128.0(2) . . ? O103 K6 C57 65.5(4) . . ? OW5 K6 C57 92.5(7) . . ? O105 K6 C57 135.3(4) . . ? O44 K6 C57 70.88(19) . . ? O102 K6 Gd5 74.3(5) . . ? O98 K6 Gd5 81.8(2) . . ? O106 K6 Gd5 109.9(8) . . ? O86 K6 Gd5 85.1(2) . . ? O56 K6 Gd5 27.44(19) . . ? O103 K6 Gd5 161.0(4) . . ? OW5 K6 Gd5 138.2(7) . . ? O105 K6 Gd5 68.2(4) . . ? O44 K6 Gd5 33.27(13) . . ? C57 K6 Gd5 101.45(14) . . ? C64 O7 Gd2 123.5(4) . 2_546 ? C75 O8 Gd3 156.3(4) . . ? C75 O8 Gd4 88.3(4) . . ? Gd3 O8 Gd4 115.43(17) . . ? C93 O9 Gd1 90.2(4) . . ? C78 O10 Gd4 92.5(4) . . ? C97 O11 Gd2 90.5(4) . 2_546 ? C49 O12 Gd1 95.2(4) . . ? C70 O13 Gd3 100.4(4) . . ? C77 O14 Gd3 92.4(4) . . ? C64 O15 Gd2 165.6(4) . . ? C11 O16 Gd4 89.7(4) . . ? C47 O17 Gd2 93.8(4) . 2_556 ? C49 O18 Gd1 91.9(4) . . ? C47 O19 Gd2 92.6(4) . 2_556 ? C77 O20 Gd3 92.5(4) . . ? C70 O21 Gd4 155.8(4) . . ? C70 O21 Gd3 88.5(4) . . ? Gd4 O21 Gd3 115.64(17) . . ? C59 O22 Gd1 121.3(4) . . ? C75 O23 Gd4 100.7(4) . . ? C78 O24 Gd4 92.2(4) . . ? C59 O25 Gd1 164.5(4) 2_657 . ? C97 O26 Gd2 97.1(4) . 2_546 ? C81 O27 Gd2 121.4(4) . . ? C54 O28 Gd2 143.6(5) . 2_656 ? C73 O29 Gd3 149.7(5) . 2_657 ? C57 O30 Gd1 136.7(5) . . ? C60 O32 Gd3 91.4(4) . . ? C93 O34 Gd1 95.8(4) . . ? C81 O36 Gd4 147.2(5) . . ? C73 O38 Gd1 120.8(4) . . ? C82 C39 C63 119.6(5) . . ? C82 C39 C78 119.0(6) . . ? C63 C39 C78 121.4(5) . . ? C11 O41 Gd4 95.4(4) . . ? C60 O42 Gd3 93.1(4) . . ? C91 C43 C76 118.7(6) . . ? C91 C43 C77 119.5(6) . . ? C76 C43 C77 121.8(5) . . ? Gd5 O44 K6 97.1(2) . . ? C48 C45 C62 119.8(6) . . ? C48 C45 C60 117.6(6) . 1_565 ? C62 C45 C60 122.5(6) . 1_565 ? C54 O46 Gd5 133.5(5) . . ? O19 C47 O17 121.0(6) . . ? O19 C47 C62 119.3(6) . . ? O17 C47 C62 119.6(6) . . ? O19 C47 Gd2 61.4(3) . 2_556 ? O17 C47 Gd2 59.6(3) . 2_556 ? C62 C47 Gd2 177.3(4) . 2_556 ? C50 C48 C45 121.2(6) . . ? O18 C49 O12 120.8(6) . . ? O18 C49 C50 119.3(6) . . ? O12 C49 C50 119.7(6) . . ? O18 C49 Gd1 62.1(3) . . ? O12 C49 Gd1 58.8(3) . . ? C50 C49 Gd1 174.8(5) . . ? C48 C50 C68 119.1(6) . . ? C48 C50 C49 119.2(6) . . ? C68 C50 C49 121.7(6) . . ? C66 C51 C91 119.8(6) . 1_455 ? C66 C51 C70 125.9(5) . . ? C91 C51 C70 114.2(6) 1_455 . ? C69 C53 C92 119.8(6) 2_556 . ? C69 C53 C54 118.6(6) 2_556 2_656 ? C92 C53 C54 121.6(6) . 2_656 ? O46 C54 O28 122.1(6) . . ? O46 C54 C53 118.7(6) . 2_656 ? O28 C54 C53 119.2(6) . 2_656 ? Gd5 O56 K6 123.4(3) . . ? O86 C57 O30 122.0(8) . . ? O86 C57 C79 118.9(7) . . ? O30 C57 C79 119.1(7) . . ? O86 C57 K6 38.0(5) . . ? O30 C57 K6 90.3(5) . . ? C79 C57 K6 145.1(5) . . ? C66 C58 C76 120.8(6) 1_655 . ? O25 C59 O22 124.2(6) 2_657 . ? O25 C59 C76 117.0(6) 2_657 . ? O22 C59 C76 118.6(5) . . ? O32 C60 O42 122.1(6) . . ? O32 C60 C45 119.9(6) . 1_545 ? O42 C60 C45 117.9(6) . 1_545 ? O32 C60 Gd3 62.3(3) . . ? O42 C60 Gd3 59.8(3) . . ? C45 C60 Gd3 177.2(5) 1_545 . ? C74 C61 C82 120.3(6) . 1_655 ? C74 C61 C75 125.1(5) . . ? C82 C61 C75 114.6(6) 1_655 . ? C71 C62 C45 118.9(6) . . ? C71 C62 C47 118.4(6) . . ? C45 C62 C47 122.6(5) . . ? C88 C63 C39 119.6(5) . . ? C88 C63 C64 117.3(5) . . ? C39 C63 C64 122.8(5) . . ? O15 C64 O7 124.2(6) . . ? O15 C64 C63 117.5(5) . . ? O7 C64 C63 118.1(5) . . ? C58 C66 C51 119.7(6) 1_455 . ? C58 C66 C93 117.6(6) 1_455 . ? C51 C66 C93 122.6(6) . . ? C71 C68 C50 120.3(6) . . ? C71 C68 C11 116.9(6) . . ? C50 C68 C11 122.8(6) . . ? C53 C69 C92 121.8(6) 2_556 . ? O13 C70 O21 120.8(6) . . ? O13 C70 C51 118.5(6) . . ? O21 C70 C51 120.6(6) . . ? O13 C70 Gd3 54.8(3) . . ? O21 C70 Gd3 66.0(3) . . ? C51 C70 Gd3 172.0(4) . . ? C62 C71 C68 120.6(6) . . ? O29 C73 O38 123.5(6) . . ? O29 C73 C80 117.2(6) . . ? O38 C73 C80 119.2(6) . . ? C61 C74 C88 119.9(6) . 1_655 ? C61 C74 C97 122.0(5) . . ? C88 C74 C97 118.2(5) 1_655 . ? O23 C75 O8 120.6(6) . . ? O23 C75 C61 118.0(5) . . ? O8 C75 C61 121.2(6) . . ? O23 C75 Gd4 54.4(3) . . ? O8 C75 Gd4 66.2(3) . . ? C61 C75 Gd4 171.2(4) . . ? C58 C76 C43 120.0(5) . . ? C58 C76 C59 116.8(5) . . ? C43 C76 C59 122.9(5) . . ? O14 C77 O20 121.7(6) . . ? O14 C77 C43 119.4(5) . . ? O20 C77 C43 118.8(5) . . ? O14 C77 Gd3 61.0(3) . . ? O20 C77 Gd3 60.8(3) . . ? C43 C77 Gd3 178.7(4) . . ? O24 C78 O10 121.6(6) . . ? O24 C78 C39 119.2(5) . . ? O10 C78 C39 119.2(6) . . ? O24 C78 Gd4 61.2(3) . . ? O10 C78 Gd4 60.4(3) . . ? C39 C78 Gd4 179.6(5) . . ? C84 C79 C80 119.6(6) . . ? C84 C79 C57 118.5(6) . . ? C80 C79 C57 121.9(6) . . ? C84 C80 C79 118.1(6) 2_667 . ? C84 C80 C73 117.5(6) 2_667 . ? C79 C80 C73 124.3(6) . . ? O36 C81 O27 123.6(6) . . ? O36 C81 C92 117.6(6) . . ? O27 C81 C92 118.7(6) . . ? C39 C82 C61 120.2(6) . 1_455 ? C80 C84 C79 122.3(7) 2_667 . ? C57 O86 K6 124.6(7) . . ? C74 C88 C63 120.4(6) 1_455 . ? C51 C91 C43 121.0(6) 1_655 . ? C69 C92 C53 118.4(6) . . ? C69 C92 C81 118.0(6) . . ? C53 C92 C81 123.6(6) . . ? O9 C93 O34 122.5(6) . . ? O9 C93 C66 119.6(6) . . ? O34 C93 C66 117.9(6) . . ? O9 C93 Gd1 64.1(3) . . ? O34 C93 Gd1 58.5(3) . . ? C66 C93 Gd1 176.1(4) . . ? O11 C97 O26 121.5(6) . . ? O11 C97 C74 121.1(6) . . ? O26 C97 C74 117.4(5) . . ? O11 C97 Gd2 64.3(3) . 2_546 ? O26 C97 Gd2 57.3(3) . 2_546 ? C74 C97 Gd2 174.4(5) . 2_546 ? O16 C11 O41 121.6(6) . . ? O16 C11 C68 119.6(6) . . ? O41 C11 C68 118.8(6) . . ? O16 C11 Gd4 63.7(3) . . ? O41 C11 Gd4 57.9(3) . . ? C68 C11 Gd4 175.9(5) . . ? # END of CIF