data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; 'Zhang, Xian-Ming' School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; _publ_contact_author_phone '86-357-2051402' _publ_contact_author_fax '86-357-2051402' _publ_contact_author_email zhangxm@dns.sxnu.edu.cn _publ_requested_joiurnal 'ACS Appl. Mater. Interface' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a manuscript submitted to ACS Appl. Mater. Interface Xian-Ming Zhang ; #============================================================ # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; loop_ _publ_author_name _publ_author_address 'Yan-Wu Zhao' ; School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; 'Fu-Qiang Zhang' ; School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; 'Xian-Ming Zhang' ; School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; #====================================== data_1 _audit_creation_date 2015-09-13 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst., 40, 786-790; Palatinus, L. & van der Lee, A. (2008). J. Appl. Cryst. 41, 975-984; Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012). J. Appl. Cryst. 45, 575-580. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.25(C92 H68 Eu4 O40)' _chemical_formula_sum 'C23 H19 Eu O10' _chemical_formula_weight 607.34 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Eu' 'Eu' -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 12 _space_group_name_H-M_alt 'C 1 2/m 1' _space_group_name_Hall '-C 2y' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z' 5 '-x, -y, -z' 6 'x, -y, z' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z' _cell_length_a 13.780(9) _cell_length_b 24.104(14) _cell_length_c 8.437(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.833(11) _cell_angle_gamma 90.00 _cell_volume 2709(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 739 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 18.366 _cell_measurement_theta_min 2.498 _exptl_absorpt_coefficient_mu 2.363 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.479214 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; ? was used for absorption correction. R(int) was 0.0818 before and 0.0489 after correction. The Ratio of minimum to maximum transmission is 0.4792. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'block' _exptl_crystal_F_000 1200 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_unetI/netI 0.1070 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 6441 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 1.69 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71000 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 1746 _reflns_number_total 2465 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution ; Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008; Palatinus et al., 2012) ; _refine_diff_density_max 3.236 _refine_diff_density_min -1.152 _refine_diff_density_rms 0.269 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 161 _refine_ls_number_reflns 2465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0780 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2131 _refine_ls_wR_factor_ref 0.2289 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All O(H,H) groups 2. Others Fixed Sof: H1b(0.5) 3.a Rotating group: O1(H1a,H1b) 3.b Secondary CH2 refined with riding coordinates: C6(H6a,H6b) 3.c Aromatic/amide H refined with riding coordinates: C5(H5), C10(H10), C11(H11), C3(H3), C9(H9), C8(H8) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_site_symmetry_order _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Eu1 Eu 0.12596(7) 0.5000 0.33356(11) 0.0361(4) Uani 1 d . . 2 S T P O3 O 0.0636(8) 0.4250(4) 0.4461(14) 0.063(3) Uani 1 d . . 1 . . . O1 O -0.0449(12) 0.5000 0.1871(19) 0.063(4) Uani 1 d . . 2 S T P H1A H -0.0920 0.5000 0.2544 0.094 Uiso 1 d . . 2 GRS T P H1B H -0.0692 0.4657 0.1283 0.094 Uiso 0.50 d . . 1 GR . . O5 O 0.3848(9) 0.0626(5) -0.1049(14) 0.082(4) Uani 1 d . . 1 . . . O4 O 0.0989(7) 0.2206(3) 0.3145(11) 0.045(2) Uani 1 d . . 1 . . . O6 O 0.2473(8) 0.0662(4) -0.2958(14) 0.065(3) Uani 1 d . . 1 . . . O2 O 0.2375(18) 0.5000 0.605(2) 0.102(7) Uani 1 d . . 2 S T P C5 C 0.0000 0.2257(6) 0.5000 0.036(4) Uani 1 d . . 2 S T P H5 H 0.0000 0.1871 0.5000 0.043 Uiso 1 calc . . 2 RS T P C1 C 0.0000 0.4024(6) 0.5000 0.035(4) Uani 1 d . . 2 S T P C10 C 0.3168(12) 0.1432(6) 0.0814(19) 0.054(4) Uani 1 d . . 1 . . . H10 H 0.3802 0.1277 0.1211 0.065 Uiso 1 calc . . 1 R . . C12 C 0.2581(10) 0.1264(5) -0.0652(16) 0.040(3) Uani 1 d . . 1 . . . C2 C 0.0000 0.3386(6) 0.5000 0.031(4) Uani 1 d . . 2 S T P C6 C 0.1517(11) 0.2491(6) 0.2108(17) 0.050(4) Uani 1 d . . 1 . . . H6A H 0.2084 0.2696 0.2768 0.059 Uiso 1 calc . . 1 R . . H6B H 0.1073 0.2749 0.1386 0.059 Uiso 1 calc . . 1 R . . C7 C 0.1867(11) 0.2054(5) 0.1137(17) 0.042(3) Uani 1 d . . 1 . . . C13 C 0.2984(10) 0.0829(6) -0.1637(17) 0.044(3) Uani 1 d . . 1 . . . C11 C 0.1666(11) 0.1477(6) -0.1242(18) 0.052(4) Uani 1 d . . 1 . . . H11 H 0.1263 0.1356 -0.2241 0.063 Uiso 1 calc . . 1 R . . C3 C 0.0535(9) 0.3113(4) 0.4056(14) 0.032(3) Uani 1 d . . 1 . . . H3 H 0.0892 0.3311 0.3445 0.038 Uiso 1 calc . . 1 R . . C4 C 0.0528(9) 0.2534(5) 0.4040(15) 0.034(3) Uani 1 d . . 1 . . . C9 C 0.1323(11) 0.1882(6) -0.0344(19) 0.056(4) Uani 1 d . . 1 . . . H9 H 0.0695 0.2040 -0.0782 0.067 Uiso 1 calc . . 1 R . . C8 C 0.2829(13) 0.1837(6) 0.1736(18) 0.055(4) Uani 1 d . . 1 . . . H8 H 0.3238 0.1958 0.2730 0.066 Uiso 1 calc . . 1 R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0556(7) 0.0203(5) 0.0441(6) 0.000 0.0343(5) 0.000 O3 0.083(7) 0.022(4) 0.111(9) 0.013(5) 0.071(7) -0.009(5) O1 0.091(12) 0.043(8) 0.058(10) 0.000 0.027(8) 0.000 O5 0.077(8) 0.098(9) 0.068(8) -0.041(7) 0.012(6) 0.047(7) O4 0.074(7) 0.021(4) 0.056(6) -0.006(4) 0.045(5) -0.001(4) O6 0.064(7) 0.066(7) 0.065(7) -0.029(6) 0.019(6) 0.021(5) O2 0.18(2) 0.074(12) 0.051(11) 0.000 0.019(12) 0.000 C5 0.057(12) 0.015(8) 0.042(10) 0.000 0.027(9) 0.000 C1 0.047(11) 0.018(8) 0.041(10) 0.000 0.015(9) 0.000 C10 0.067(10) 0.043(8) 0.053(9) -0.011(7) 0.014(8) 0.020(7) C12 0.054(9) 0.033(7) 0.039(8) -0.012(6) 0.025(7) -0.004(6) C2 0.040(10) 0.015(7) 0.043(10) 0.000 0.017(8) 0.000 C6 0.068(10) 0.043(8) 0.048(9) -0.003(7) 0.034(8) 0.002(7) C7 0.062(9) 0.029(7) 0.047(8) -0.006(6) 0.035(7) -0.004(6) C13 0.043(8) 0.053(8) 0.042(8) -0.007(7) 0.024(7) 0.004(7) C11 0.048(8) 0.065(10) 0.043(8) -0.017(7) 0.011(7) 0.016(7) C3 0.047(7) 0.021(6) 0.035(7) -0.006(5) 0.026(6) -0.008(5) C4 0.044(7) 0.025(6) 0.039(7) -0.010(5) 0.022(6) 0.003(5) C9 0.050(9) 0.062(9) 0.064(11) 0.004(8) 0.028(8) 0.023(7) C8 0.079(11) 0.047(8) 0.044(9) -0.009(7) 0.023(8) 0.020(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O3 2.308(8) 6_565 ? Eu1 O3 2.308(8) . ? Eu1 O1 2.362(16) . ? Eu1 O5 2.424(10) 7 ? Eu1 O5 2.424(10) 4 ? Eu1 O6 2.447(9) 7 ? Eu1 O6 2.447(9) 4 ? Eu1 O2 2.411(18) . ? Eu1 C13 2.809(13) 4 ? Eu1 C13 2.809(13) 7 ? O3 C1 1.215(11) . ? O1 H1A 0.9655 . ? O1 H1B 0.9786 . ? O5 Eu1 2.424(10) 7 ? O5 C13 1.263(17) . ? O4 C6 1.446(15) . ? O4 C4 1.358(13) . ? O6 Eu1 2.447(9) 7 ? O6 C13 1.224(16) . ? C5 H5 0.9300 . ? C5 C4 1.390(14) . ? C5 C4 1.390(14) 2_556 ? C1 O3 1.215(11) 2_556 ? C1 C2 1.54(2) . ? C10 H10 0.9300 . ? C10 C12 1.355(19) . ? C10 C8 1.400(18) . ? C12 C13 1.530(17) . ? C12 C11 1.333(19) . ? C2 C3 1.382(13) . ? C2 C3 1.382(13) 2_556 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C7 1.487(17) . ? C7 C9 1.35(2) . ? C7 C8 1.40(2) . ? C13 Eu1 2.809(13) 7 ? C11 H11 0.9300 . ? C11 C9 1.392(19) . ? C3 H3 0.9300 . ? C3 C4 1.396(15) . ? C9 H9 0.9300 . ? C8 H8 0.9300 . ? 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 O3 Eu1 O3 103.1(5) 6_565 . ? O3 Eu1 O1 77.8(4) 6_565 . ? O3 Eu1 O1 77.8(4) . . ? O3 Eu1 O5 83.5(4) 6_565 4 ? O3 Eu1 O5 83.5(4) . 7 ? O3 Eu1 O5 149.5(4) 6_565 7 ? O3 Eu1 O5 149.5(4) . 4 ? O3 Eu1 O6 84.0(4) 6_565 4 ? O3 Eu1 O6 156.7(4) . 4 ? O3 Eu1 O6 84.0(4) . 7 ? O3 Eu1 O6 156.7(4) 6_565 7 ? O3 Eu1 O2 79.8(5) 6_565 . ? O3 Eu1 O2 79.8(5) . . ? O3 Eu1 C13 173.0(4) 6_565 7 ? O3 Eu1 C13 83.0(4) . 7 ? O3 Eu1 C13 173.0(4) . 4 ? O3 Eu1 C13 83.0(4) 6_565 4 ? O1 Eu1 O5 74.6(4) . 7 ? O1 Eu1 O5 74.6(4) . 4 ? O1 Eu1 O6 125.5(3) . 4 ? O1 Eu1 O6 125.5(3) . 7 ? O1 Eu1 O2 143.6(7) . . ? O1 Eu1 C13 100.6(4) . 7 ? O1 Eu1 C13 100.6(4) . 4 ? O5 Eu1 O5 77.0(7) 4 7 ? O5 Eu1 O6 101.7(5) 4 7 ? O5 Eu1 O6 52.4(3) 7 7 ? O5 Eu1 O6 52.4(3) 4 4 ? O5 Eu1 O6 101.7(5) 7 4 ? O5 Eu1 C13 89.5(5) 4 7 ? O5 Eu1 C13 89.5(5) 7 4 ? O5 Eu1 C13 26.7(4) 4 4 ? O5 Eu1 C13 26.7(4) 7 7 ? O6 Eu1 O6 81.5(6) 4 7 ? O6 Eu1 C13 25.8(4) 7 7 ? O6 Eu1 C13 25.8(4) 4 4 ? O6 Eu1 C13 91.6(4) 4 7 ? O6 Eu1 C13 91.6(4) 7 4 ? O2 Eu1 O5 130.6(4) . 7 ? O2 Eu1 O5 130.6(4) . 4 ? O2 Eu1 O6 79.7(5) . 7 ? O2 Eu1 O6 79.7(5) . 4 ? O2 Eu1 C13 104.8(5) . 4 ? O2 Eu1 C13 104.8(5) . 7 ? C13 Eu1 C13 90.6(6) 4 7 ? C1 O3 Eu1 152.4(9) . . ? Eu1 O1 H1A 115.0 . . ? Eu1 O1 H1B 115.6 . . ? H1A O1 H1B 96.0 . . ? C13 O5 Eu1 93.9(8) . 7 ? C4 O4 C6 116.1(10) . . ? C13 O6 Eu1 93.9(8) . 7 ? C4 C5 H5 118.7 . . ? C4 C5 H5 118.7 2_556 . ? C4 C5 C4 122.6(15) 2_556 . ? O3 C1 O3 126.6(16) . 2_556 ? O3 C1 C2 116.7(8) . . ? O3 C1 C2 116.7(8) 2_556 . ? C12 C10 H10 119.7 . . ? C12 C10 C8 120.6(14) . . ? C8 C10 H10 119.7 . . ? C10 C12 C13 119.0(13) . . ? C11 C12 C10 120.9(12) . . ? C11 C12 C13 120.1(12) . . ? C3 C2 C1 118.4(7) 2_556 . ? C3 C2 C1 118.4(7) . . ? C3 C2 C3 123.2(14) . 2_556 ? O4 C6 H6A 110.5 . . ? O4 C6 H6B 110.5 . . ? O4 C6 C7 106.4(10) . . ? H6A C6 H6B 108.7 . . ? C7 C6 H6A 110.5 . . ? C7 C6 H6B 110.5 . . ? C9 C7 C6 123.1(14) . . ? C9 C7 C8 118.2(12) . . ? C8 C7 C6 118.6(13) . . ? O5 C13 Eu1 59.4(7) . 7 ? O5 C13 C12 119.2(12) . . ? O6 C13 Eu1 60.3(7) . 7 ? O6 C13 O5 119.8(12) . . ? O6 C13 C12 121.0(12) . . ? C12 C13 Eu1 177.7(10) . 7 ? C12 C11 H11 120.4 . . ? C12 C11 C9 119.2(14) . . ? C9 C11 H11 120.4 . . ? C2 C3 H3 120.7 . . ? C2 C3 C4 118.5(11) . . ? C4 C3 H3 120.7 . . ? O4 C4 C5 115.7(11) . . ? O4 C4 C3 125.7(11) . . ? C5 C4 C3 118.6(11) . . ? C7 C9 C11 122.3(14) . . ? C7 C9 H9 118.8 . . ? C11 C9 H9 118.8 . . ? C10 C8 H8 120.6 . . ? C7 C8 C10 118.8(14) . . ? C7 C8 H8 120.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Eu1 O3 C1 O3 -21.5(15) . . . 2_556 ? Eu1 O3 C1 C2 158.5(15) . . . . ? Eu1 O5 C13 O6 0.0(16) 7 . . . ? Eu1 O5 C13 C12 177.8(11) 7 . . . ? Eu1 O6 C13 O5 0.0(16) 7 . . . ? Eu1 O6 C13 C12 -177.8(11) 7 . . . ? O3 Eu1 O3 C1 32(2) 6_565 . . . ? O3 C1 C2 C3 164.6(9) 2_556 . . . ? O3 C1 C2 C3 -15.4(9) . . . . ? O3 C1 C2 C3 -15.4(9) 2_556 . . 2_556 ? O3 C1 C2 C3 164.6(9) . . . 2_556 ? O1 Eu1 O3 C1 -42.4(19) . . . . ? O5 Eu1 O3 C1 -68(2) 4 . . . ? O5 Eu1 O3 C1 -117.9(19) 7 . . . ? O4 C6 C7 C9 91.1(16) . . . . ? O4 C6 C7 C8 -93.2(15) . . . . ? O6 Eu1 O3 C1 -170.7(19) 7 . . . ? O6 Eu1 O3 C1 137.5(17) 4 . . . ? O2 Eu1 O3 C1 109(2) . . . . ? C1 C2 C3 C4 -179.3(8) . . . . ? C10 C12 C13 Eu1 55(25) . . . 7 ? C10 C12 C13 O5 1(2) . . . . ? C10 C12 C13 O6 179.3(14) . . . . ? C10 C12 C11 C9 1(2) . . . . ? C12 C10 C8 C7 2(2) . . . . ? C12 C11 C9 C7 -3(2) . . . . ? C2 C3 C4 O4 178.0(10) . . . . ? C2 C3 C4 C5 -1.3(16) . . . . ? C6 O4 C4 C5 178.3(10) . . . . ? C6 O4 C4 C3 -1.0(19) . . . . ? C6 C7 C9 C11 179.4(14) . . . . ? C6 C7 C8 C10 -179.0(13) . . . . ? C13 Eu1 O3 C1 -120(3) 4 . . . ? C13 Eu1 O3 C1 -145(2) 7 . . . ? C13 C12 C11 C9 -178.5(13) . . . . ? C11 C12 C13 Eu1 -125(24) . . . 7 ? C11 C12 C13 O5 -179.1(15) . . . . ? C11 C12 C13 O6 -1(2) . . . . ? C3 C2 C3 C4 0.7(8) 2_556 . . . ? C4 O4 C6 C7 -174.4(11) . . . . ? C4 C5 C4 O4 -178.7(12) 2_556 . . . ? C4 C5 C4 C3 0.7(8) 2_556 . . . ? C9 C7 C8 C10 -3(2) . . . . ? C8 C10 C12 C13 178.9(14) . . . . ? C8 C10 C12 C11 0(2) . . . . ? C8 C7 C9 C11 4(2) . . . . ? _olex2_submission_special_instructions 'No special instructions were received' _platon_squeeze_details ; ; # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.017 296 86 ' ' 2 0.500 0.500 0.023 296 86 ' ' #============================================================ data_2 _audit_creation_date 2015-09-13 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst., 40, 786-790; Palatinus, L. & van der Lee, A. (2008). J. Appl. Cryst. 41, 975-984; Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012). J. Appl. Cryst. 45, 575-580. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.25(C92 H68 O40 Tb4)' _chemical_formula_sum 'C23 H19 O10 Tb' _chemical_formula_weight 614.30 _chemical_melting_point ? 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' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 12 _space_group_name_H-M_alt 'C 1 2/m 1' _space_group_name_Hall '-C 2y' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z' 5 '-x, -y, -z' 6 'x, -y, z' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z' _cell_length_a 13.8044(11) _cell_length_b 24.0322(19) _cell_length_c 8.4465(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.521(2) _cell_angle_gamma 90.00 _cell_volume 2712.6(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1192 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 20.137 _cell_measurement_theta_min 2.710 _exptl_absorpt_coefficient_mu 2.654 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.403634 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; ? was used for absorption correction. R(int) was 0.0494 before and 0.0376 after correction. The Ratio of minimum to maximum transmission is 0.4036. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'block' _exptl_crystal_F_000 1208 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_unetI/netI 0.0646 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 6559 _diffrn_reflns_theta_full 24.99 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_min 1.69 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71000 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 2043 _reflns_number_total 2463 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution ; Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008; Palatinus et al., 2012) ; _refine_diff_density_max 2.382 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.223 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 161 _refine_ls_number_reflns 2463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0578 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1682 _refine_ls_wR_factor_ref 0.1743 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All O(H,H) groups 2. Others Fixed Sof: H4a(0.5) H4b(0.5) 3.a Rotating group: O4(H4a,H4b) 3.b Secondary CH2 refined with riding coordinates: C7(H7a,H7b) 3.c Aromatic/amide H refined with riding coordinates: C6(H6), C10(H10), C12(H12), C4(H4), C13(H13), C9(H9) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_site_symmetry_order _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Tb1 Tb 0.12455(4) 0.5000 0.83258(7) 0.0317(3) Uani 1 d . . 2 S T P O5 O 0.0632(6) 0.5737(3) 0.9464(11) 0.059(2) Uani 1 d . . 1 . . . O1 O 0.1130(6) 0.5622(4) 0.6070(10) 0.079(3) Uani 1 d . . 1 . . . O4 O -0.0482(7) 0.5000 0.6900(13) 0.055(3) Uani 1 d . . 2 S T P H4A H -0.0957 0.5030 0.7531 0.082 Uiso 0.50 d . . 1 GR . . H4B H -0.0735 0.4655 0.6252 0.082 Uiso 0.50 d . . 1 GR . . O2 O 0.2527(6) 0.5650(3) 0.7969(10) 0.061(2) Uani 1 d . . 1 . . . O6 O 0.0999(5) 0.7791(3) 0.8154(8) 0.0418(17) Uani 1 d . . 1 . . . O3 O 0.2363(11) 0.5000 1.1027(14) 0.086(4) Uani 1 d . . 2 S T P C7 C 0.1522(8) 0.7512(4) 0.7110(13) 0.045(2) Uani 1 d . . 1 . . . H7A H 0.1075 0.7259 0.6378 0.054 Uiso 1 calc . . 1 R . . H7B H 0.2078 0.7299 0.7761 0.054 Uiso 1 calc . . 1 R . . C11 C 0.2599(7) 0.8747(4) 0.4346(11) 0.035(2) Uani 1 d . . 1 . . . C2 C 0.0000 0.5981(5) 1.0000 0.030(3) Uani 1 d . . 2 S T P C3 C 0.0000 0.6606(5) 1.0000 0.031(3) Uani 1 d . . 2 S T P C6 C 0.0000 0.7747(5) 1.0000 0.034(3) Uani 1 d . . 2 S T P H6 H 0.0000 0.8134 1.0000 0.040 Uiso 1 calc . . 2 RS T P C10 C 0.3187(8) 0.8569(4) 0.5854(13) 0.046(3) Uani 1 d . . 1 . . . H10 H 0.3821 0.8720 0.6273 0.055 Uiso 1 calc . . 1 R . . C1 C 0.2009(7) 0.5816(4) 0.6634(13) 0.038(2) Uani 1 d . . 1 . . . C12 C 0.1670(8) 0.8530(5) 0.3751(13) 0.049(3) Uani 1 d . . 1 . . . H12 H 0.1272 0.8649 0.2752 0.059 Uiso 1 calc . . 1 R . . C8 C 0.1896(7) 0.7953(4) 0.6146(12) 0.038(2) Uani 1 d . . 1 . . . C5 C 0.0512(6) 0.7465(4) 0.9052(11) 0.032(2) Uani 1 d . . 1 . . . C4 C 0.0537(6) 0.6886(3) 0.9054(10) 0.0291(19) Uani 1 d . . 1 . . . H4 H 0.0900 0.6692 0.8442 0.035 Uiso 1 calc . . 1 R . . C13 C 0.1323(8) 0.8126(4) 0.4657(14) 0.049(3) Uani 1 d . . 1 . . . H13 H 0.0692 0.7972 0.4246 0.059 Uiso 1 calc . . 1 R . . C9 C 0.2830(8) 0.8177(4) 0.6699(13) 0.048(3) Uani 1 d . . 1 . . . H9 H 0.3232 0.8056 0.7693 0.058 Uiso 1 calc . . 1 R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0449(4) 0.0234(4) 0.0354(4) 0.000 0.0260(3) 0.000 O5 0.077(5) 0.024(3) 0.092(6) -0.003(4) 0.055(5) 0.006(4) O1 0.069(6) 0.107(7) 0.057(5) 0.041(5) 0.007(4) -0.045(5) O4 0.050(6) 0.058(7) 0.057(7) 0.000 0.017(5) 0.000 O2 0.058(5) 0.068(5) 0.057(5) 0.027(4) 0.017(4) -0.018(4) O6 0.063(4) 0.025(3) 0.050(4) 0.006(3) 0.038(4) -0.007(3) O3 0.133(12) 0.082(9) 0.039(7) 0.000 0.012(7) 0.000 C7 0.059(6) 0.039(6) 0.049(6) 0.001(5) 0.037(5) -0.002(5) C11 0.044(5) 0.033(5) 0.032(5) 0.002(4) 0.018(4) -0.004(4) C2 0.039(7) 0.022(6) 0.035(7) 0.000 0.018(6) 0.000 C3 0.043(7) 0.021(6) 0.035(7) 0.000 0.022(6) 0.000 C6 0.044(8) 0.019(6) 0.039(8) 0.000 0.013(6) 0.000 C10 0.041(6) 0.047(6) 0.048(6) 0.009(5) 0.010(5) -0.018(5) C1 0.044(6) 0.034(5) 0.042(6) 0.002(4) 0.020(5) -0.006(4) C12 0.046(6) 0.063(7) 0.041(6) 0.013(5) 0.014(5) -0.013(5) C8 0.050(6) 0.035(5) 0.041(6) 0.001(4) 0.031(5) -0.002(4) C5 0.041(5) 0.029(5) 0.029(5) 0.001(4) 0.016(4) -0.008(4) C4 0.039(5) 0.023(4) 0.031(5) 0.000(3) 0.020(4) 0.002(4) C13 0.037(5) 0.056(6) 0.054(7) 0.007(5) 0.009(5) -0.014(5) C9 0.051(6) 0.049(6) 0.042(6) 0.013(5) 0.009(5) -0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O5 2.276(7) 6_565 ? Tb1 O5 2.276(6) . ? Tb1 O1 2.396(7) 6_565 ? Tb1 O1 2.396(7) . ? Tb1 O4 2.387(10) . ? Tb1 O2 2.436(7) 6_565 ? Tb1 O2 2.436(7) . ? Tb1 O3 2.412(12) . ? Tb1 C1 2.784(9) . ? Tb1 C1 2.784(9) 6_565 ? O5 C2 1.229(9) . ? O1 C1 1.275(12) . ? O4 H4A 0.9452 . ? O4 H4B 1.0066 . ? O2 C1 1.239(12) . ? O6 C7 1.438(10) . ? O6 C5 1.377(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.506(12) . ? C11 C10 1.395(14) . ? C11 C1 1.519(12) 7_566 ? C11 C12 1.358(14) . ? C2 O5 1.229(9) 2_557 ? C2 C3 1.502(16) . ? C3 C4 1.392(10) . ? C3 C4 1.392(10) 2_557 ? C6 H6 0.9300 . ? C6 C5 1.372(10) . ? C6 C5 1.372(10) 2_557 ? C10 H10 0.9300 . ? C10 C9 1.347(13) . ? C1 C11 1.519(12) 7_566 ? C12 H12 0.9300 . ? C12 C13 1.393(14) . ? C8 C13 1.372(14) . ? C8 C9 1.367(14) . ? C5 C4 1.392(11) . ? C4 H4 0.9300 . ? C13 H13 0.9300 . ? C9 H9 0.9300 . ? 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 Tb1 O5 102.1(4) 6_565 . ? O5 Tb1 O1 83.9(3) 6_565 6_565 ? O5 Tb1 O1 149.7(3) . 6_565 ? O5 Tb1 O1 149.7(3) 6_565 . ? O5 Tb1 O1 83.9(3) . . ? O5 Tb1 O4 77.5(3) 6_565 . ? O5 Tb1 O4 77.5(3) . . ? O5 Tb1 O2 155.5(3) . 6_565 ? O5 Tb1 O2 84.9(3) . . ? O5 Tb1 O2 84.9(3) 6_565 6_565 ? O5 Tb1 O2 155.5(3) 6_565 . ? O5 Tb1 O3 79.5(3) 6_565 . ? O5 Tb1 O3 79.5(3) . . ? O5 Tb1 C1 173.2(3) 6_565 . ? O5 Tb1 C1 84.2(3) . . ? O5 Tb1 C1 84.2(3) 6_565 6_565 ? O5 Tb1 C1 173.2(3) . 6_565 ? O1 Tb1 O1 77.2(5) 6_565 . ? O1 Tb1 O2 53.6(3) . . ? O1 Tb1 O2 53.6(3) 6_565 6_565 ? O1 Tb1 O2 102.0(3) . 6_565 ? O1 Tb1 O2 102.0(3) 6_565 . ? O1 Tb1 O3 130.7(3) 6_565 . ? O1 Tb1 O3 130.7(3) . . ? O1 Tb1 C1 27.2(3) 6_565 6_565 ? O1 Tb1 C1 89.4(3) . 6_565 ? O1 Tb1 C1 27.2(3) . . ? O1 Tb1 C1 89.4(3) 6_565 . ? O4 Tb1 O1 74.9(3) . . ? O4 Tb1 O1 74.9(3) . 6_565 ? O4 Tb1 O2 127.0(2) . . ? O4 Tb1 O2 127.0(2) . 6_565 ? O4 Tb1 O3 143.0(5) . . ? O4 Tb1 C1 101.5(3) . . ? O4 Tb1 C1 101.5(3) . 6_565 ? O2 Tb1 O2 79.8(4) . 6_565 ? O2 Tb1 C1 90.5(3) 6_565 . ? O2 Tb1 C1 90.5(3) . 6_565 ? O2 Tb1 C1 26.4(3) . . ? O2 Tb1 C1 26.4(3) 6_565 6_565 ? O3 Tb1 O2 78.8(3) . 6_565 ? O3 Tb1 O2 78.8(3) . . ? O3 Tb1 C1 104.5(3) . 6_565 ? O3 Tb1 C1 104.5(3) . . ? C1 Tb1 C1 89.5(4) 6_565 . ? C2 O5 Tb1 154.3(7) . . ? C1 O1 Tb1 93.6(6) . . ? Tb1 O4 H4A 117.5 . . ? Tb1 O4 H4B 116.2 . . ? H4A O4 H4B 100.1 . . ? C1 O2 Tb1 92.7(6) . . ? C5 O6 C7 117.5(7) . . ? O6 C7 H7A 110.3 . . ? O6 C7 H7B 110.3 . . ? O6 C7 C8 107.2(7) . . ? H7A C7 H7B 108.5 . . ? C8 C7 H7A 110.3 . . ? C8 C7 H7B 110.3 . . ? C10 C11 C1 120.3(8) . 7_566 ? C12 C11 C10 119.9(9) . . ? C12 C11 C1 119.8(9) . 7_566 ? O5 C2 O5 122.8(12) 2_557 . ? O5 C2 C3 118.6(6) . . ? O5 C2 C3 118.6(6) 2_557 . ? C4 C3 C2 118.9(5) . . ? C4 C3 C2 118.9(5) 2_557 . ? C4 C3 C4 122.2(11) 2_557 . ? C5 C6 H6 119.6 2_557 . ? C5 C6 H6 119.6 . . ? C5 C6 C5 120.8(11) 2_557 . ? C11 C10 H10 120.3 . . ? C9 C10 C11 119.4(9) . . ? C9 C10 H10 120.3 . . ? O1 C1 Tb1 59.2(5) . . ? O1 C1 C11 118.9(9) . 7_566 ? O2 C1 Tb1 60.9(5) . . ? O2 C1 O1 120.1(8) . . ? O2 C1 C11 121.0(9) . 7_566 ? C11 C1 Tb1 177.9(7) 7_566 . ? C11 C12 H12 120.4 . . ? C11 C12 C13 119.2(10) . . ? C13 C12 H12 120.4 . . ? C13 C8 C7 120.8(9) . . ? C9 C8 C7 121.0(9) . . ? C9 C8 C13 118.1(9) . . ? O6 C5 C4 123.6(8) . . ? C6 C5 O6 115.7(8) . . ? C6 C5 C4 120.6(8) . . ? C3 C4 H4 121.1 . . ? C5 C4 C3 117.9(8) . . ? C5 C4 H4 121.1 . . ? C12 C13 H13 119.5 . . ? C8 C13 C12 121.0(10) . . ? C8 C13 H13 119.5 . . ? C10 C9 C8 122.3(10) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Tb1 O5 C2 O5 24.5(12) . . . 2_557 ? Tb1 O5 C2 C3 -155.5(12) . . . . ? Tb1 O1 C1 O2 -1.7(11) . . . . ? Tb1 O1 C1 C11 178.9(7) . . . 7_566 ? Tb1 O2 C1 O1 1.6(11) . . . . ? Tb1 O2 C1 C11 -179.0(8) . . . 7_566 ? O5 Tb1 O5 C2 -35.3(17) 6_565 . . . ? O5 Tb1 O1 C1 89.1(7) . . . . ? O5 Tb1 O1 C1 -167.4(5) 6_565 . . . ? O5 Tb1 O2 C1 164.8(6) 6_565 . . . ? O5 Tb1 O2 C1 -87.0(7) . . . . ? O5 Tb1 C1 O1 69(3) 6_565 . . . ? O5 Tb1 C1 O1 -87.9(7) . . . . ? O5 Tb1 C1 O2 -113(2) 6_565 . . . ? O5 Tb1 C1 O2 90.4(7) . . . . ? O5 Tb1 C1 C11 -115(19) . . . 7_566 ? O5 Tb1 C1 C11 42(20) 6_565 . . 7_566 ? O5 C2 C3 C4 15.4(6) 2_557 . . 2_557 ? O5 C2 C3 C4 -164.6(6) 2_557 . . . ? O5 C2 C3 C4 -164.6(6) . . . 2_557 ? O5 C2 C3 C4 15.4(6) . . . . ? O1 Tb1 O5 C2 63.3(17) 6_565 . . . ? O1 Tb1 O5 C2 114.6(15) . . . . ? O1 Tb1 O1 C1 -114.7(6) 6_565 . . . ? O1 Tb1 O2 C1 -0.9(6) . . . . ? O1 Tb1 O2 C1 63.1(7) 6_565 . . . ? O1 Tb1 C1 O1 62.4(7) 6_565 . . . ? O1 Tb1 C1 O2 -119.2(7) 6_565 . . . ? O1 Tb1 C1 O2 178.3(11) . . . . ? O1 Tb1 C1 C11 36(19) 6_565 . . 7_566 ? O1 Tb1 C1 C11 -27(18) . . . 7_566 ? O4 Tb1 O5 C2 38.7(15) . . . . ? O4 Tb1 O1 C1 167.8(7) . . . . ? O4 Tb1 O2 C1 -16.9(8) . . . . ? O4 Tb1 C1 O1 -12.1(7) . . . . ? O4 Tb1 C1 O2 166.3(6) . . . . ? O4 Tb1 C1 C11 -39(19) . . . 7_566 ? O2 Tb1 O5 C2 168.4(15) . . . . ? O2 Tb1 O5 C2 -139.9(13) 6_565 . . . ? O2 Tb1 O1 C1 0.9(6) . . . . ? O2 Tb1 O1 C1 -66.7(7) 6_565 . . . ? O2 Tb1 O2 C1 112.3(6) 6_565 . . . ? O2 Tb1 C1 O1 116.0(7) 6_565 . . . ? O2 Tb1 C1 O1 -178.3(11) . . . . ? O2 Tb1 C1 O2 -65.6(7) 6_565 . . . ? O2 Tb1 C1 C11 155(19) . . . 7_566 ? O2 Tb1 C1 C11 89(19) 6_565 . . 7_566 ? O6 C7 C8 C13 -90.4(11) . . . . ? O6 C7 C8 C9 92.0(11) . . . . ? O6 C5 C4 C3 -179.1(7) . . . . ? O3 Tb1 O5 C2 -112.1(15) . . . . ? O3 Tb1 O1 C1 18.6(9) . . . . ? O3 Tb1 O2 C1 -167.3(7) . . . . ? O3 Tb1 C1 O1 -165.5(7) . . . . ? O3 Tb1 C1 O2 12.9(7) . . . . ? O3 Tb1 C1 C11 168(19) . . . 7_566 ? C7 O6 C5 C6 -178.4(8) . . . . ? C7 O6 C5 C4 2.8(13) . . . . ? C7 C8 C13 C12 -179.2(10) . . . . ? C7 C8 C9 C10 179.4(9) . . . . ? C11 C10 C9 C8 -1.3(17) . . . . ? C11 C12 C13 C8 1.0(17) . . . . ? C2 C3 C4 C5 179.0(6) . . . . ? C6 C5 C4 C3 2.1(12) . . . . ? C10 C11 C12 C13 -0.6(16) . . . . ? C1 Tb1 O5 C2 141.9(15) . . . . ? C1 Tb1 O5 C2 121(2) 6_565 . . . ? C1 Tb1 O1 C1 -90.1(8) 6_565 . . . ? C1 Tb1 O2 C1 88.0(7) 6_565 . . . ? C1 Tb1 C1 O1 89.6(7) 6_565 . . . ? C1 Tb1 C1 O2 -92.0(7) 6_565 . . . ? C1 Tb1 C1 C11 63(19) 6_565 . . 7_566 ? C1 C11 C10 C9 -179.4(9) 7_566 . . . ? C1 C11 C12 C13 179.5(10) 7_566 . . . ? C12 C11 C10 C9 0.7(16) . . . . ? C5 O6 C7 C8 174.4(8) . . . . ? C5 C6 C5 O6 -180.0(9) 2_557 . . . ? C5 C6 C5 C4 -1.1(6) 2_557 . . . ? C4 C3 C4 C5 -1.0(6) 2_557 . . . ? C13 C8 C9 C10 1.7(16) . . . . ? C9 C8 C13 C12 -1.6(16) . . . . ? _olex2_submission_special_instructions 'No special instructions were received' _platon_squeeze_details ; ; # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.033 296 77 ' ' 2 0.500 0.500 0.004 296 77 ' ' #============================================================ data_3 _audit_creation_date 2015-09-13 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G.L., De Caro, L., Giacovazzo, C., Polidori, G., Siliqi, D., Spagna, R. (2007). J. Appl. Cryst. 40, 609-613. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.25(C92 H60 Gd4 O40)' _chemical_formula_sum 'C23 H19 Gd O10' _chemical_formula_weight 612.63 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 12 _space_group_name_H-M_alt 'C 1 2/m 1' _space_group_name_Hall '-C 2y' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z' 5 '-x, -y, -z' 6 'x, -y, z' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z' _cell_length_a 13.8599(19) _cell_length_b 24.088(3) _cell_length_c 8.4281(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.557(2) _cell_angle_gamma 90.00 _cell_volume 2723.5(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2777 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 27.779 _cell_measurement_theta_min 2.497 _exptl_absorpt_coefficient_mu 2.482 _exptl_absorpt_correction_T_max 0.7894 _exptl_absorpt_correction_T_min 0.562957 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; ? was used for absorption correction. R(int) was 0.0689 before and 0.0331 after correction. The Ratio of minimum to maximum transmission is 0.5630. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'coloeless' _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'block' _exptl_crystal_F_000 1188 _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_unetI/netI 0.0435 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 5395 _diffrn_reflns_theta_full 24.99 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_min 1.69 _diffrn_ambient_temperature 298.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 2190 _reflns_number_total 2444 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XH (Sheldrick, 2008)' _computing_structure_solution 'SIR2004 (Burla et al., 2007)' _refine_diff_density_max 3.160 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.220 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 160 _refine_ls_number_reflns 2444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0531 _refine_ls_restrained_S_all 1.166 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1031P)^2^+8.6183P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1603 _refine_ls_wR_factor_ref 0.1647 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C35(H35A,H35B) 2.b Aromatic/amide H refined with riding coordinates: C12(H12A), C18(H18A), C31(H31A), C34(H34A), C37(H37A), C38(H38A) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_site_symmetry_order _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Gd1 Gd 0.12529(4) 0.0000 0.33248(6) 0.0299(3) Uani 1 d . . 2 S T P O1 O 0.2370(11) 0.0000 0.6038(13) 0.085(4) Uani 1 d . . 2 S T P O4 O 0.0620(6) 0.0740(2) 0.4441(10) 0.059(2) Uani 1 d . . 1 . . . O6 O 0.3848(5) 0.4375(3) -0.1051(9) 0.065(2) Uani 1 d . . 1 . . . O7 O 0.2477(5) 0.4341(3) -0.2963(8) 0.0573(19) Uani 1 d . . 1 . . . O12 O 0.0990(5) 0.2793(2) 0.3142(7) 0.0429(15) Uani 1 d . . 1 . . . C3 C 0.2983(6) 0.4182(4) -0.1622(10) 0.0351(18) Uani 1 d . . 1 . . . C9 C 0.2594(6) 0.3744(3) -0.0650(10) 0.0343(18) Uani 1 d . . 1 . . . C11 C 0.0000 0.0981(4) 0.5000 0.031(2) Uani 1 d . . 2 S T P C12 C 0.0532(5) 0.1886(3) 0.4057(9) 0.0285(16) Uani 1 d . . 1 . . . H12A H 0.0887 0.1690 0.3440 0.034 Uiso 1 calc . . 1 R . . C13 C 0.0522(6) 0.2465(3) 0.4056(9) 0.0307(17) Uani 1 d . . 1 . . . C18 C 0.1666(7) 0.3527(4) -0.1242(12) 0.047(2) Uani 1 d . . 1 . . . H18A H 0.1271 0.3647 -0.2244 0.057 Uiso 1 calc . . 1 R . . C30 C 0.0000 0.1613(4) 0.5000 0.028(2) Uani 1 d . . 2 S T P C31 C 0.2824(7) 0.3169(4) 0.1712(12) 0.050(2) Uani 1 d . . 1 . . . H31A H 0.3229 0.3044 0.2700 0.060 Uiso 1 calc . . 1 R . . C34 C 0.3170(7) 0.3565(4) 0.0852(12) 0.046(2) Uani 1 d . . 1 . . . H34A H 0.3799 0.3718 0.1274 0.056 Uiso 1 calc . . 1 R . . C35 C 0.1504(7) 0.2509(3) 0.2096(12) 0.043(2) Uani 1 d . . 1 . . . H35A H 0.1053 0.2260 0.1358 0.052 Uiso 1 calc . . 1 R . . H35B H 0.2054 0.2293 0.2746 0.052 Uiso 1 calc . . 1 R . . C36 C 0.1884(6) 0.2949(3) 0.1144(11) 0.0376(19) Uani 1 d . . 1 . . . C37 C 0.1311(7) 0.3127(4) -0.0354(12) 0.050(2) Uani 1 d . . 1 . . . H37A H 0.0680 0.2976 -0.0771 0.060 Uiso 1 calc . . 1 R . . C38 C 0.0000 0.2758(4) 0.5000 0.031(2) Uani 1 d . . 2 S T P H38A H 0.0000 0.3144 0.5000 0.037 Uiso 1 calc . . 2 RS T P O3 O -0.0473(7) 0.0000 0.1856(12) 0.053(2) Uani 1 d . . 2 S T 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 0.0414(4) 0.0193(3) 0.0368(4) 0.000 0.0244(3) 0.000 O1 0.127(11) 0.074(8) 0.048(7) 0.000 0.012(7) 0.000 O4 0.081(5) 0.020(3) 0.098(6) -0.008(3) 0.061(4) 0.002(3) O6 0.057(4) 0.081(5) 0.056(4) 0.030(4) 0.009(3) -0.036(4) O7 0.049(4) 0.067(5) 0.056(4) 0.025(4) 0.013(3) -0.021(3) O12 0.064(4) 0.024(3) 0.053(4) 0.005(2) 0.037(3) -0.004(3) C3 0.040(4) 0.038(5) 0.034(4) 0.005(4) 0.020(4) -0.003(4) C9 0.039(4) 0.034(4) 0.036(4) 0.004(3) 0.021(4) -0.002(3) C11 0.042(6) 0.019(5) 0.036(6) 0.000 0.018(5) 0.000 C12 0.035(4) 0.023(4) 0.032(4) 0.000(3) 0.017(3) 0.002(3) C13 0.039(4) 0.024(4) 0.034(4) 0.003(3) 0.018(3) -0.003(3) C18 0.041(5) 0.057(6) 0.045(5) 0.015(4) 0.014(4) -0.012(4) C30 0.039(6) 0.016(5) 0.034(6) 0.000 0.017(5) 0.000 C31 0.058(6) 0.052(6) 0.039(5) 0.013(4) 0.009(4) -0.010(5) C34 0.042(5) 0.047(5) 0.047(5) 0.009(4) 0.005(4) -0.015(4) C35 0.057(5) 0.033(5) 0.051(5) 0.000(4) 0.035(4) -0.005(4) C36 0.049(5) 0.029(4) 0.045(5) -0.003(4) 0.029(4) -0.005(4) C37 0.041(5) 0.062(6) 0.049(6) 0.005(5) 0.014(4) -0.017(4) C38 0.042(6) 0.016(5) 0.038(6) 0.000 0.014(5) 0.000 O3 0.054(5) 0.047(6) 0.060(6) 0.000 0.018(5) 0.000 _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 O1 2.418(11) . ? Gd1 O4 2.291(6) . ? Gd1 O4 2.291(6) 6 ? Gd1 O6 2.413(6) 4_545 ? Gd1 O6 2.413(6) 7 ? Gd1 O7 2.446(6) 7 ? Gd1 O7 2.446(6) 4_545 ? Gd1 C3 2.798(8) 4_545 ? Gd1 C3 2.798(8) 7 ? Gd1 O3 2.402(9) . ? O4 C11 1.225(8) . ? O6 Gd1 2.413(6) 7 ? O6 C3 1.264(10) . ? O7 Gd1 2.446(6) 7 ? O7 C3 1.232(11) . ? O12 C13 1.375(9) . ? O12 C35 1.438(9) . ? C3 Gd1 2.798(8) 7 ? C3 C9 1.516(11) . ? C9 C18 1.362(12) . ? C9 C34 1.384(13) . ? C11 O4 1.225(8) 2_556 ? C11 C30 1.522(14) . ? C12 H12A 0.9300 . ? C12 C13 1.393(11) . ? C12 C30 1.380(9) . ? C13 C38 1.394(9) . ? C18 H18A 0.9300 . ? C18 C37 1.385(12) . ? C30 C12 1.380(9) 2_556 ? C31 H31A 0.9300 . ? C31 C34 1.357(12) . ? C31 C36 1.377(12) . ? C34 H34A 0.9300 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 C36 1.502(11) . ? C36 C37 1.379(13) . ? C37 H37A 0.9300 . ? C38 C13 1.394(9) 2_556 ? C38 H38A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Gd1 O7 78.9(3) . 4_545 ? O1 Gd1 O7 78.9(3) . 7 ? O1 Gd1 C3 104.5(3) . 4_545 ? O1 Gd1 C3 104.5(3) . 7 ? O4 Gd1 O1 80.3(3) . . ? O4 Gd1 O1 80.3(3) 6 . ? O4 Gd1 O4 102.2(3) . 6 ? O4 Gd1 O6 149.3(3) 6 7 ? O4 Gd1 O6 149.3(3) . 4_545 ? O4 Gd1 O6 83.6(3) . 7 ? O4 Gd1 O6 83.6(3) 6 4_545 ? O4 Gd1 O7 156.7(3) 6 7 ? O4 Gd1 O7 156.7(3) . 4_545 ? O4 Gd1 O7 84.7(3) . 7 ? O4 Gd1 O7 84.7(3) 6 4_545 ? O4 Gd1 C3 172.8(2) . 4_545 ? O4 Gd1 C3 172.8(2) 6 7 ? O4 Gd1 C3 84.0(2) . 7 ? O4 Gd1 C3 84.0(2) 6 4_545 ? O4 Gd1 O3 77.1(2) . . ? O4 Gd1 O3 77.1(2) 6 . ? O6 Gd1 O1 130.3(3) 4_545 . ? O6 Gd1 O1 130.3(3) 7 . ? O6 Gd1 O6 77.2(4) 4_545 7 ? O6 Gd1 O7 101.9(3) 4_545 7 ? O6 Gd1 O7 52.9(2) 4_545 4_545 ? O6 Gd1 O7 101.9(3) 7 4_545 ? O6 Gd1 O7 52.9(2) 7 7 ? O6 Gd1 C3 89.2(3) 7 4_545 ? O6 Gd1 C3 89.2(3) 4_545 7 ? O6 Gd1 C3 26.8(2) 7 7 ? O6 Gd1 C3 26.8(2) 4_545 4_545 ? O7 Gd1 O7 81.0(4) 7 4_545 ? O7 Gd1 C3 90.9(2) 4_545 7 ? O7 Gd1 C3 26.1(2) 7 7 ? O7 Gd1 C3 26.1(2) 4_545 4_545 ? O7 Gd1 C3 90.9(2) 7 4_545 ? C3 Gd1 C3 89.5(3) 4_545 7 ? O3 Gd1 O1 143.7(4) . . ? O3 Gd1 O6 74.9(2) . 7 ? O3 Gd1 O6 74.9(2) . 4_545 ? O3 Gd1 O7 126.2(2) . 4_545 ? O3 Gd1 O7 126.2(2) . 7 ? O3 Gd1 C3 101.1(2) . 7 ? O3 Gd1 C3 101.1(2) . 4_545 ? C11 O4 Gd1 154.7(6) . . ? C3 O6 Gd1 93.8(5) . 7 ? C3 O7 Gd1 93.1(5) . 7 ? C13 O12 C35 116.5(6) . . ? O6 C3 Gd1 59.4(4) . 7 ? O6 C3 C9 118.9(7) . . ? O7 C3 Gd1 60.8(4) . 7 ? O7 C3 O6 120.1(7) . . ? O7 C3 C9 121.0(7) . . ? C9 C3 Gd1 178.1(6) . 7 ? C18 C9 C3 120.0(8) . . ? C18 C9 C34 119.4(8) . . ? C34 C9 C3 120.6(8) . . ? O4 C11 O4 123.5(11) 2_556 . ? O4 C11 C30 118.3(5) . . ? O4 C11 C30 118.3(5) 2_556 . ? C13 C12 H12A 120.9 . . ? C30 C12 H12A 120.9 . . ? C30 C12 C13 118.1(7) . . ? O12 C13 C12 124.7(7) . . ? O12 C13 C38 114.4(7) . . ? C12 C13 C38 120.8(7) . . ? C9 C18 H18A 120.0 . . ? C9 C18 C37 120.0(9) . . ? C37 C18 H18A 120.0 . . ? C12 C30 C11 118.5(5) . . ? C12 C30 C11 118.5(5) 2_556 . ? C12 C30 C12 122.9(10) . 2_556 ? C34 C31 H31A 119.5 . . ? C34 C31 C36 121.1(9) . . ? C36 C31 H31A 119.5 . . ? C9 C34 H34A 119.8 . . ? C31 C34 C9 120.5(8) . . ? C31 C34 H34A 119.8 . . ? O12 C35 H35A 110.4 . . ? O12 C35 H35B 110.4 . . ? O12 C35 C36 106.6(6) . . ? H35A C35 H35B 108.6 . . ? C36 C35 H35A 110.4 . . ? C36 C35 H35B 110.4 . . ? C31 C36 C35 120.9(8) . . ? C31 C36 C37 118.4(8) . . ? C37 C36 C35 120.6(8) . . ? C18 C37 H37A 119.7 . . ? C36 C37 C18 120.6(8) . . ? C36 C37 H37A 119.7 . . ? C13 C38 C13 119.1(10) 2_556 . ? C13 C38 H38A 120.4 . . ? C13 C38 H38A 120.4 2_556 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Gd1 O4 C11 O4 21.3(12) . . . 2_556 ? Gd1 O4 C11 C30 -158.7(12) . . . . ? Gd1 O6 C3 O7 2.2(10) 7 . . . ? Gd1 O6 C3 C9 -179.4(7) 7 . . . ? Gd1 O7 C3 O6 -2.2(10) 7 . . . ? Gd1 O7 C3 C9 179.5(7) 7 . . . ? Gd1 C3 C9 C18 164(18) 7 . . . ? Gd1 C3 C9 C34 -15(19) 7 . . . ? O1 Gd1 O4 C11 -108.5(15) . . . . ? O4 Gd1 O4 C11 -30.7(17) 6 . . . ? O4 C11 C30 C12 -165.6(6) 2_556 . . . ? O4 C11 C30 C12 14.4(6) 2_556 . . 2_556 ? O4 C11 C30 C12 14.4(6) . . . . ? O4 C11 C30 C12 -165.6(6) . . . 2_556 ? O6 Gd1 O4 C11 67.5(16) 4_545 . . . ? O6 Gd1 O4 C11 118.8(14) 7 . . . ? O6 C3 C9 C18 -179.6(9) . . . . ? O6 C3 C9 C34 1.2(13) . . . . ? O7 Gd1 O4 C11 -135.9(13) 4_545 . . . ? O7 Gd1 O4 C11 171.9(15) 7 . . . ? O7 C3 C9 C18 -1.3(13) . . . . ? O7 C3 C9 C34 179.5(9) . . . . ? O12 C13 C38 C13 178.5(8) . . . 2_556 ? O12 C35 C36 C31 92.0(10) . . . . ? O12 C35 C36 C37 -90.6(10) . . . . ? C3 Gd1 O4 C11 145.7(15) 7 . . . ? C3 Gd1 O4 C11 119.3(18) 4_545 . . . ? C3 C9 C18 C37 -179.9(9) . . . . ? C3 C9 C34 C31 -179.4(9) . . . . ? C9 C18 C37 C36 0.8(16) . . . . ? C12 C13 C38 C13 -0.4(5) . . . 2_556 ? C13 O12 C35 C36 175.9(7) . . . . ? C13 C12 C30 C11 179.6(5) . . . . ? C13 C12 C30 C12 -0.4(5) . . . 2_556 ? C18 C9 C34 C31 1.4(15) . . . . ? C30 C12 C13 O12 -178.0(6) . . . . ? C30 C12 C13 C38 0.9(10) . . . . ? C31 C36 C37 C18 -1.6(15) . . . . ? C34 C9 C18 C37 -0.7(15) . . . . ? C34 C31 C36 C35 179.8(9) . . . . ? C34 C31 C36 C37 2.3(14) . . . . ? C35 O12 C13 C12 1.4(12) . . . . ? C35 O12 C13 C38 -177.5(7) . . . . ? C35 C36 C37 C18 -179.1(9) . . . . ? C36 C31 C34 C9 -2.2(15) . . . . ? O3 Gd1 O4 C11 42.9(14) . . . . ? _olex2_submission_special_instructions 'No special instructions were received' _platon_squeeze_details ; ; # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 -0.018 298 67 ' ' 2 0.500 0.000 0.023 298 67 ' ' #============================================================ data_4 _audit_creation_date 2015-09-13 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst., 40, 786-790; Palatinus, L. & van der Lee, A. (2008). J. Appl. Cryst. 41, 975-984; Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012). J. Appl. Cryst. 45, 575-580. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.25(C92 H68 O40 Tm4)' _chemical_formula_sum 'C23 H19 O10 Tm' _chemical_formula_weight 624.31 _chemical_melting_point ? 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' _space_group_crystal_system 'monoclinic' _space_group_IT_number 12 _space_group_name_H-M_alt 'C 1 2/m 1' _space_group_name_Hall '-C 2y' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z' 5 '-x, -y, -z' 6 'x, -y, z' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z' _cell_length_a 13.7892(10) _cell_length_b 23.8999(18) _cell_length_c 8.4148(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.2550(10) _cell_angle_gamma 90.00 _cell_volume 2687.8(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2096 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.108 _cell_measurement_theta_min 2.498 _exptl_absorpt_coefficient_mu 3.349 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.718957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; ? was used for absorption correction. R(int) was 0.0676 before and 0.0431 after correction. The Ratio of minimum to maximum transmission is 0.7190. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'block' _exptl_crystal_F_000 1224 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_unetI/netI 0.0616 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 7036 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 1.70 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71000 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 2147 _reflns_number_total 2441 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution ; Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008; Palatinus et al., 2012) ; _refine_diff_density_max 3.368 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.247 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 161 _refine_ls_number_reflns 2441 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0559 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1070P)^2^+0.9280P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1648 _refine_ls_wR_factor_ref 0.1723 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All O(H,H) groups 2. Others Fixed Sof: H4a(0.5) H4b(0.5) 3.a Rotating group: O4(H4a,H4b) 3.b Secondary CH2 refined with riding coordinates: C7(H7a,H7b) 3.c Aromatic/amide H refined with riding coordinates: C5(H5), C12(H12), C4(H4), C10(H10), C13(H13), C9(H9) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_site_symmetry_order _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Tm1 Tm 0.37859(4) 0.5000 0.16927(6) 0.0326(3) Uani 1 d . . 2 S T P O5 O 0.4388(6) 0.4271(3) 0.0589(12) 0.062(2) Uani 1 d . . 1 . . . O4 O 0.5468(8) 0.5000 0.3076(14) 0.054(3) Uani 1 d . . 2 S T P H4A H 0.5823 0.4874 0.2445 0.081 Uiso 0.50 d . . 1 GR . . H4B H 0.5562 0.4791 0.3934 0.081 Uiso 0.50 d . . 1 GR . . O1 O 0.3895(6) 0.5609(4) 0.3915(10) 0.072(3) Uani 1 d . . 1 . . . O2 O 0.2514(6) 0.4358(3) 0.2021(10) 0.058(2) Uani 1 d . . 1 . . . O6 O 0.3997(5) 0.2206(3) 0.1850(8) 0.0435(17) Uani 1 d . . 1 . . . O3 O 0.2726(13) 0.5000 -0.0984(14) 0.086(4) Uani 1 d . . 2 S T P C7 C 0.3479(8) 0.2486(4) 0.2907(14) 0.045(2) Uani 1 d . . 1 . . . H7A H 0.2924 0.2702 0.2264 0.054 Uiso 1 calc . . 1 R . . H7B H 0.3929 0.2738 0.3642 0.054 Uiso 1 calc . . 1 R . . C3 C 0.5000 0.3399(5) 0.0000 0.030(3) Uani 1 d . . 2 S T P C5 C 0.5000 0.2245(5) 0.0000 0.035(3) Uani 1 d . . 2 S T P H5 H 0.5000 0.1855 0.0000 0.042 Uiso 1 calc . . 2 RS T P C1 C 0.3024(7) 0.4197(4) 0.3362(11) 0.035(2) Uani 1 d . . 1 . . . C2 C 0.5000 0.4036(5) 0.0000 0.034(3) Uani 1 d . . 2 S T P C12 C 0.3325(8) 0.1460(5) 0.6253(14) 0.051(3) Uani 1 d . . 1 . . . H12 H 0.3718 0.1339 0.7256 0.061 Uiso 1 calc . . 1 R . . C11 C 0.2375(7) 0.1242(4) 0.5663(11) 0.036(2) Uani 1 d . . 1 . . . C4 C 0.4461(6) 0.3115(4) 0.0959(11) 0.0319(19) Uani 1 d . . 1 . . . H4 H 0.4100 0.3309 0.1580 0.038 Uiso 1 calc . . 1 R . . C6 C 0.4485(7) 0.2534(4) 0.0950(11) 0.034(2) Uani 1 d . . 1 . . . C10 C 0.1801(7) 0.1435(4) 0.4178(13) 0.046(2) Uani 1 d . . 1 . . . H10 H 0.1161 0.1290 0.3776 0.055 Uiso 1 calc . . 1 R . . C8 C 0.3107(8) 0.2042(4) 0.3861(12) 0.042(2) Uani 1 d . . 1 . . . C13 C 0.3690(8) 0.1855(4) 0.5363(14) 0.050(3) Uani 1 d . . 1 . . . H13 H 0.4331 0.1999 0.5767 0.060 Uiso 1 calc . . 1 R . . C9 C 0.2141(8) 0.1825(4) 0.3297(13) 0.049(3) Uani 1 d . . 1 . . . H9 H 0.1733 0.1950 0.2311 0.059 Uiso 1 calc . . 1 R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tm1 0.0492(4) 0.0208(4) 0.0380(4) 0.000 0.0302(3) 0.000 O5 0.088(6) 0.021(4) 0.101(7) -0.014(4) 0.068(5) -0.001(4) O4 0.070(7) 0.042(6) 0.056(7) 0.000 0.027(5) 0.000 O1 0.073(5) 0.086(6) 0.056(5) -0.037(4) 0.011(4) 0.044(5) O2 0.058(4) 0.059(5) 0.059(5) 0.021(4) 0.019(4) -0.015(4) O6 0.066(4) 0.022(4) 0.056(4) 0.006(3) 0.040(4) 0.000(3) O3 0.164(13) 0.056(8) 0.039(7) 0.000 0.026(8) 0.000 C7 0.060(6) 0.030(5) 0.058(6) 0.003(4) 0.041(5) -0.001(5) C3 0.033(6) 0.021(6) 0.037(7) 0.000 0.014(5) 0.000 C5 0.053(8) 0.011(6) 0.045(7) 0.000 0.022(6) 0.000 C1 0.045(5) 0.029(5) 0.035(5) 0.003(4) 0.018(4) -0.003(4) C2 0.053(8) 0.015(6) 0.037(7) 0.000 0.014(6) 0.000 C12 0.051(6) 0.051(7) 0.053(6) 0.017(5) 0.017(5) -0.007(5) C11 0.046(5) 0.037(5) 0.035(5) -0.001(4) 0.026(4) -0.006(4) C4 0.040(5) 0.028(5) 0.035(5) -0.001(4) 0.023(4) 0.004(4) C6 0.044(5) 0.027(5) 0.039(5) 0.003(4) 0.023(4) -0.003(4) C10 0.045(5) 0.046(6) 0.049(6) 0.009(5) 0.017(5) -0.014(5) C8 0.064(6) 0.037(5) 0.039(5) 0.001(4) 0.039(5) -0.002(5) C13 0.050(6) 0.045(6) 0.061(7) 0.005(5) 0.023(5) -0.012(5) C9 0.056(6) 0.049(6) 0.045(6) 0.005(5) 0.017(5) -0.011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tm1 O5 2.229(7) 6_565 ? Tm1 O5 2.229(7) . ? Tm1 O4 2.325(10) . ? Tm1 O1 2.344(7) . ? Tm1 O1 2.344(7) 6_565 ? Tm1 O2 2.397(7) . ? Tm1 O2 2.397(7) 6_565 ? Tm1 O3 2.364(12) . ? Tm1 C1 2.737(9) 6_565 ? Tm1 C1 2.737(9) . ? O5 C2 1.216(9) . ? O4 H4A 0.8604 . ? O4 H4B 0.8608 . ? O1 C1 1.265(11) 6_565 ? O2 C1 1.235(12) . ? O6 C7 1.435(11) . ? O6 C6 1.374(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.497(12) . ? C3 C2 1.523(16) . ? C3 C4 1.399(10) 2_655 ? C3 C4 1.399(10) . ? C5 H5 0.9300 . ? C5 C6 1.379(11) 2_655 ? C5 C6 1.379(11) . ? C1 O1 1.265(11) 6_565 ? C1 C11 1.516(12) 7_556 ? C2 O5 1.216(9) 2_655 ? C12 H12 0.9300 . ? C12 C11 1.383(13) . ? C12 C13 1.376(14) . ? C11 C1 1.516(12) 7_556 ? C11 C10 1.383(14) . ? C4 H4 0.9300 . ? C4 C6 1.389(12) . ? C10 H10 0.9300 . ? C10 C9 1.345(14) . ? C8 C13 1.394(14) . ? C8 C9 1.399(14) . ? C13 H13 0.9300 . ? C9 H9 0.9300 . ? 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 Tm1 O5 102.8(4) 6_565 . ? O5 Tm1 O4 77.3(3) 6_565 . ? O5 Tm1 O4 77.3(3) . . ? O5 Tm1 O1 83.7(3) 6_565 . ? O5 Tm1 O1 83.7(3) . 6_565 ? O5 Tm1 O1 149.3(3) . . ? O5 Tm1 O1 149.3(3) 6_565 6_565 ? O5 Tm1 O2 155.1(3) 6_565 . ? O5 Tm1 O2 84.6(3) 6_565 6_565 ? O5 Tm1 O2 155.1(3) . 6_565 ? O5 Tm1 O2 84.6(3) . . ? O5 Tm1 O3 79.0(4) 6_565 . ? O5 Tm1 O3 79.0(4) . . ? O5 Tm1 C1 172.6(3) . 6_565 ? O5 Tm1 C1 84.0(3) 6_565 6_565 ? O5 Tm1 C1 84.0(3) . . ? O5 Tm1 C1 172.6(3) 6_565 . ? O4 Tm1 O1 74.9(3) . 6_565 ? O4 Tm1 O1 74.9(3) . . ? O4 Tm1 O2 127.6(2) . . ? O4 Tm1 O2 127.6(2) . 6_565 ? O4 Tm1 O3 141.6(5) . . ? O4 Tm1 C1 101.8(3) . 6_565 ? O4 Tm1 C1 101.8(3) . . ? O1 Tm1 O1 76.7(5) . 6_565 ? O1 Tm1 O2 102.2(3) . . ? O1 Tm1 O2 54.3(2) . 6_565 ? O1 Tm1 O2 54.3(2) 6_565 . ? O1 Tm1 O2 102.2(3) 6_565 6_565 ? O1 Tm1 O3 131.6(3) . . ? O1 Tm1 O3 131.6(3) 6_565 . ? O1 Tm1 C1 89.0(3) 6_565 6_565 ? O1 Tm1 C1 27.5(3) . 6_565 ? O1 Tm1 C1 27.5(3) 6_565 . ? O1 Tm1 C1 89.0(3) . . ? O2 Tm1 O2 79.7(4) . 6_565 ? O2 Tm1 C1 90.3(3) 6_565 . ? O2 Tm1 C1 26.8(3) 6_565 6_565 ? O2 Tm1 C1 90.3(3) . 6_565 ? O2 Tm1 C1 26.8(3) . . ? O3 Tm1 O2 79.1(4) . 6_565 ? O3 Tm1 O2 79.1(4) . . ? O3 Tm1 C1 105.3(3) . . ? O3 Tm1 C1 105.3(3) . 6_565 ? C1 Tm1 C1 89.1(4) . 6_565 ? C2 O5 Tm1 153.9(7) . . ? Tm1 O4 H4A 109.9 . . ? Tm1 O4 H4B 110.2 . . ? H4A O4 H4B 108.9 . . ? C1 O1 Tm1 93.8(6) 6_565 . ? C1 O2 Tm1 92.1(6) . . ? C6 O6 C7 117.5(8) . . ? O6 C7 H7A 110.3 . . ? O6 C7 H7B 110.3 . . ? O6 C7 C8 106.9(8) . . ? H7A C7 H7B 108.6 . . ? C8 C7 H7A 110.3 . . ? C8 C7 H7B 110.3 . . ? C4 C3 C2 119.0(6) . . ? C4 C3 C2 119.0(6) 2_655 . ? C4 C3 C4 122.0(11) . 2_655 ? C6 C5 H5 120.1 2_655 . ? C6 C5 H5 120.1 . . ? C6 C5 C6 119.8(11) 2_655 . ? O1 C1 Tm1 58.7(5) 6_565 . ? O1 C1 C11 119.6(8) 6_565 7_556 ? O2 C1 Tm1 61.1(5) . . ? O2 C1 O1 119.8(8) . 6_565 ? O2 C1 C11 120.6(8) . 7_556 ? C11 C1 Tm1 178.2(7) 7_556 . ? O5 C2 O5 125.0(13) 2_655 . ? O5 C2 C3 117.5(6) 2_655 . ? O5 C2 C3 117.5(6) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C13 C12 C11 120.3(10) . . ? C12 C11 C1 120.3(8) . 7_556 ? C10 C11 C1 121.1(8) . 7_556 ? C10 C11 C12 118.7(9) . . ? C3 C4 H4 121.1 . . ? C6 C4 C3 117.7(8) . . ? C6 C4 H4 121.1 . . ? O6 C6 C5 115.2(8) . . ? O6 C6 C4 123.5(8) . . ? C5 C6 C4 121.3(9) . . ? C11 C10 H10 119.1 . . ? C9 C10 C11 121.9(9) . . ? C9 C10 H10 119.1 . . ? C13 C8 C7 121.0(10) . . ? C13 C8 C9 118.6(9) . . ? C9 C8 C7 120.3(9) . . ? C12 C13 C8 120.4(10) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? C10 C9 C8 120.2(10) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Tm1 O5 C2 O5 -19.9(13) . . . 2_655 ? Tm1 O5 C2 C3 160.1(13) . . . . ? Tm1 O2 C1 O1 -2.2(11) . . . 6_565 ? Tm1 O2 C1 C11 179.3(8) . . . 7_556 ? O5 Tm1 O5 C2 29.0(19) 6_565 . . . ? O5 Tm1 O1 C1 89.1(7) 6_565 . . 6_565 ? O5 Tm1 O1 C1 -166.4(5) . . . 6_565 ? O5 Tm1 O2 C1 87.4(7) . . . . ? O5 Tm1 O2 C1 -163.7(6) 6_565 . . . ? O5 Tm1 C1 O1 -70(2) 6_565 . . 6_565 ? O5 Tm1 C1 O1 87.9(7) . . . 6_565 ? O5 Tm1 C1 O2 -89.9(7) . . . . ? O5 Tm1 C1 O2 112(2) 6_565 . . . ? O5 Tm1 C1 C11 -48(23) 6_565 . . 7_556 ? O5 Tm1 C1 C11 110(22) . . . 7_556 ? O4 Tm1 O5 C2 -44.7(16) . . . . ? O4 Tm1 O1 C1 167.6(8) . . . 6_565 ? O4 Tm1 O2 C1 18.0(8) . . . . ? O4 Tm1 C1 O1 12.2(8) . . . 6_565 ? O4 Tm1 C1 O2 -165.6(6) . . . . ? O4 Tm1 C1 C11 35(22) . . . 7_556 ? O1 Tm1 O5 C2 -120.6(16) 6_565 . . . ? O1 Tm1 O5 C2 -70.4(19) . . . . ? O1 Tm1 O1 C1 -114.7(6) 6_565 . . 6_565 ? O1 Tm1 O2 C1 1.3(6) 6_565 . . . ? O1 Tm1 O2 C1 -62.3(7) . . . . ? O1 Tm1 C1 O1 -62.2(7) . . . 6_565 ? O1 Tm1 C1 O2 -177.8(11) 6_565 . . . ? O1 Tm1 C1 O2 120.0(7) . . . . ? O1 Tm1 C1 C11 22(22) 6_565 . . 7_556 ? O1 Tm1 C1 C11 -40(22) . . . 7_556 ? O2 Tm1 O5 C2 134.0(14) 6_565 . . . ? O2 Tm1 O5 C2 -175.2(16) . . . . ? O2 Tm1 O1 C1 1.2(6) 6_565 . . 6_565 ? O2 Tm1 O1 C1 -66.4(7) . . . 6_565 ? O2 Tm1 O2 C1 -112.0(6) 6_565 . . . ? O2 Tm1 C1 O1 -116.4(7) 6_565 . . 6_565 ? O2 Tm1 C1 O1 177.8(11) . . . 6_565 ? O2 Tm1 C1 O2 65.8(7) 6_565 . . . ? O2 Tm1 C1 C11 -160(22) . . . 7_556 ? O2 Tm1 C1 C11 -94(22) 6_565 . . 7_556 ? O6 C7 C8 C13 89.9(12) . . . . ? O6 C7 C8 C9 -93.3(11) . . . . ? O3 Tm1 O5 C2 104.9(17) . . . . ? O3 Tm1 O1 C1 19.8(10) . . . 6_565 ? O3 Tm1 O2 C1 167.2(7) . . . . ? O3 Tm1 C1 O1 164.7(7) . . . 6_565 ? O3 Tm1 C1 O2 -13.0(7) . . . . ? O3 Tm1 C1 C11 -173(100) . . . 7_556 ? C7 O6 C6 C5 177.8(8) . . . . ? C7 O6 C6 C4 -3.1(13) . . . . ? C7 C8 C13 C12 177.8(10) . . . . ? C7 C8 C9 C10 -178.5(10) . . . . ? C3 C4 C6 O6 179.3(7) . . . . ? C3 C4 C6 C5 -1.6(12) . . . . ? C1 Tm1 O5 C2 -128.6(19) 6_565 . . . ? C1 Tm1 O5 C2 -148.2(17) . . . . ? C1 Tm1 O1 C1 -89.9(8) . . . 6_565 ? C1 Tm1 O2 C1 -87.3(7) 6_565 . . . ? C1 Tm1 C1 O1 -89.7(7) 6_565 . . 6_565 ? C1 Tm1 C1 O2 92.6(7) 6_565 . . . ? C1 Tm1 C1 C11 -67(22) 6_565 . . 7_556 ? C1 C11 C10 C9 179.9(10) 7_556 . . . ? C2 C3 C4 C6 -179.2(6) . . . . ? C12 C11 C10 C9 0.1(17) . . . . ? C11 C12 C13 C8 0.2(18) . . . . ? C11 C10 C9 C8 1.1(17) . . . . ? C4 C3 C2 O5 -13.2(7) . . . . ? C4 C3 C2 O5 -13.2(7) 2_655 . . 2_655 ? C4 C3 C2 O5 166.8(7) 2_655 . . . ? C4 C3 C2 O5 166.8(7) . . . 2_655 ? C4 C3 C4 C6 0.8(6) 2_655 . . . ? C6 O6 C7 C8 -174.4(8) . . . . ? C6 C5 C6 O6 -180.0(9) 2_655 . . . ? C6 C5 C6 C4 0.8(6) 2_655 . . . ? C13 C12 C11 C1 179.5(10) . . . 7_556 ? C13 C12 C11 C10 -0.7(17) . . . . ? C13 C8 C9 C10 -1.6(16) . . . . ? C9 C8 C13 C12 1.0(17) . . . . ? _olex2_submission_special_instructions 'No special instructions were received' _platon_squeeze_details ; ; # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 -0.032 303 78 ' ' 2 0.500 0.000 0.010 303 78 ' ' #============================================================