# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Dominique Luneau' ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Francois Baril-Robert' ; ? # Address 2 ; ; ? # Footnote 2 ; 'Sarah Petit' '' '' 'Guillaume Pilet' '' '' 'Christian Reber' '' '' _publ_contact_author_name 'Dominique Luneau' _publ_contact_author_email DOMINIQUE.LUNEAU@UNIV-LYON1.FR _publ_section_title ; Luminescence spectroscopy of europium(III) and terbium(III) penta-, octa- and nonanuclear clusters with beta-diketonate ligands ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? # PROCESSING SUMMARY (IUCr Office Use Only): _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? _publ_contact_author_address ; Groupe de Cristallographie et Ing\'enierie Mol\'eculaire Laboratoire des Multimat\'eriaux et Interfaces UMR 5615 CNRS-Universit\'e Claude Bernard Lyon 1 B\^at. Jules Raulin 43 bd du 11 Novembre 1918 69622 Villeurbanne cedex FRANCE ; _publ_contact_author_fax '(+33)4 72 43 11 60' _publ_contact_author_phone '(+33)4 72 44 82 20' # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; Please consider this CIF submission for publication as a Short Format Paper in Acta Crystallographica E. The figures have been sent by mail. ; _publ_requested_category CO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Sarah Petit' # Attachment 'Eu9-Revised.cif' data_I _database_code_depnum_ccdc_archive 'CCDC 711968' _audit_creation_date 06-02-23 _audit_creation_method CRYSTALS_ver_12.82 _oxford_structure_analysis_title 'import in P 4/n' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 19.1714(7) _cell_length_b 19.1714(7) _cell_length_c 15.5661(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5721.2(4) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 4/n ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -y+1/2,x,z y+1/2,-x,-z -x+1/2,-y+1/2,z x+1/2,y+1/2,-z y,-x+1/2,z -y,x+1/2,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Eu -0.1578 3.6682 24.6274 2.3879 19.0886 0.1942 13.7603 13.7546 2.9227 123.1740 2.5745 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C80 H123 Eu9 O43 # Dc = 1.82 Fooo = 2900.00 Mu = 49.29 M = 785.12 # Found Formula = C80 H124.25 Eu8.25 O40.75 # Dc = 1.82 FOOO = 2900.00 Mu = 49.29 M = 785.62 _chemical_formula_sum 'C80 H123 O43 Eu9' _chemical_formula_moiety 'C80 H123 O43 Eu9' _chemical_compound_source ? _chemical_formula_weight 3140.5 _cell_measurement_reflns_used 6359 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 293 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_min 0.07 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_max 0.13 _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2900 _exptl_absorpt_coefficient_mu 4.929 # Sheldrick geometric approximatio 0.54 0.72 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.5374 _exptl_absorpt_correction_T_max 0.7223 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _computing_data_collection 'COLLECT. Nonius (1997-2001).' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 12096 _reflns_number_total 6798 _diffrn_reflns_av_R_equivalents 0.046 # Number of reflections with Friedels Law is 6798 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6811 _diffrn_reflns_theta_min 1.308 _diffrn_reflns_theta_max 27.878 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.320 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.21 _refine_diff_density_max 2.18 _refine_ls_number_reflns 2514 _refine_ls_number_restraints 0 _refine_ls_number_parameters 300 #_refine_ls_R_factor_ref 0.0522 _refine_ls_wR_factor_ref 0.0566 _refine_ls_goodness_of_fit_ref 1.1312 #_reflns_number_all 6774 _refine_ls_R_factor_all 0.1628 _refine_ls_wR_factor_all 0.1794 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 2514 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_gt 0.0566 _refine_ls_shift/su_max 0.000164 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.284 0.820E-01 0.419E-01 ; _publ_section_abstract # Text of the abstract ; ? ; _publ_section_comment # Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures ; ? ; _publ_section_exptl_refinement # Some potentially useful phrases are: ; Because the data were collected with molybdenum radiation, there were no measurable anomalous differences, as a consequence of which it was admissible to merge Friedel pairs of reflections. All hydrogen atoms were found in difference density syntheses. Hydrogen atoms were placed geometrically after each cycle. Hydrogen atoms were placed geometrically after each cycle, the preferred orientations of those groups whose conformations could not be assigned unambiguously having been previously identified by examination of a difference Fourier map. Hydrogen atoms were seen in a difference density synthesis. Those attached to carbon atoms were repositioned geometrically. Hydrogen were initially refined with soft restraints on the bonds to regularise their geometry (bond lengths to accepted values, angles either set by symmetry or to accepted values, and U[iso] dependent upon the adjacent bonded atom), after which they were refined with riding constraints only. donated by Bill Clegg: The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93-98, O---N in the range 0.86-0.89 and O---H = 0.82 \%A) and isotropic adps (U(H) in the range 1.2-1.5 times U~equiv~ of the adjacent atom), after which they were refined with riding constraints. . ; _publ_section_exptl_prep ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Eu1 Eu 0.2500 0.2500 -0.14030(11) 0.0338 1.0000 Uani S T . . . . Eu2 Eu 0.35172(5) 0.33918(5) -0.31720(6) 0.0388 1.0000 Uani . . . . . . Eu3 Eu 0.38646(4) 0.24521(4) 0.03431(5) 0.0361 1.0000 Uani . . . . . . O1 O 0.2500 0.2500 0.0551(14) 0.0287 1.0000 Uani S T . . . . O2 O 0.2500 0.2500 -0.3346(15) 0.0404 1.0000 Uani S T . . . . O3 O 0.3259(5) 0.1690(5) -0.0577(6) 0.0314 1.0000 Uani . . . . . . O4 O 0.3598(5) 0.2434(6) -0.2241(6) 0.0368 1.0000 Uani . . . . . . O10 O 0.3759(6) 0.2440(6) -0.4141(7) 0.0403 1.0000 Uani . . . . . . C11 C 0.4230(13) 0.2371(10) -0.4785(11) 0.0622 1.0000 Uani . . . . . . C12 C 0.4837(12) 0.2721(12) -0.4772(14) 0.0672 1.0000 Uani . . . . . . C13 C 0.5096(11) 0.3131(12) -0.4139(12) 0.0599 1.0000 Uani . . . . . . O14 O 0.4728(7) 0.3346(7) -0.3516(10) 0.0689 1.0000 Uani . . . . . . C15 C 0.4034(12) 0.1855(13) -0.5456(14) 0.0772 1.0000 Uani . . . . . . C16 C 0.5846(13) 0.3358(16) -0.4138(19) 0.1051 1.0000 Uani . . . . . . O17 O 0.3791(7) 0.4521(7) -0.3585(9) 0.0650 1.0000 Uani . . . . . . C18 C 0.4175(11) 0.5002(11) -0.3256(14) 0.0603 1.0000 Uani . . . . . . C19 C 0.4438(9) 0.5006(10) -0.2448(14) 0.0551 1.0000 Uani . . . . . . C20 C 0.4331(9) 0.4518(10) -0.1800(13) 0.0512 1.0000 Uani . . . . . . O21 O 0.4007(6) 0.3935(6) -0.1931(8) 0.0530 1.0000 Uani . . . . . . C22 C 0.4336(17) 0.5620(14) -0.3857(18) 0.1090 1.0000 Uani . . . . . . C23 C 0.4593(10) 0.4628(11) -0.0907(14) 0.0630 1.0000 Uani . . . . . . O24 O 0.4595(6) 0.2433(6) -0.0880(8) 0.0474 1.0000 Uani . . . . . . C25 C 0.5220(8) 0.2561(10) -0.1045(14) 0.0494 1.0000 Uani . . . . . . C26 C 0.5637(10) 0.2858(10) -0.0399(14) 0.0557 1.0000 Uani . . . . . . C27 C 0.5462(10) 0.3115(10) 0.0396(15) 0.0591 1.0000 Uani . . . . . . O28 O 0.4834(7) 0.3140(6) 0.0680(9) 0.0544 1.0000 Uani . . . . . . C29 C 0.5520(10) 0.2424(10) -0.1903(12) 0.0519 1.0000 Uani . . . . . . C30 C 0.6010(12) 0.3430(13) 0.0988(17) 0.0838 1.0000 Uani . . . . . . O31 O 0.4745(7) 0.1702(7) 0.0872(9) 0.0600 1.0000 Uani . . . . . . C32 C 0.4852(10) 0.1438(11) 0.1584(14) 0.0568 1.0000 Uani . . . . . . C33 C 0.4336(10) 0.1223(10) 0.2145(12) 0.0515 1.0000 Uani . . . . . . C34 C 0.3640(8) 0.1264(10) 0.2002(10) 0.0408 1.0000 Uani . . . . . . O35 O 0.3360(6) 0.1570(6) 0.1325(7) 0.0445 1.0000 Uani . . . . . . C36 C 0.5623(11) 0.1298(12) 0.1851(16) 0.0721 1.0000 Uani . . . . . . C37 C 0.3128(11) 0.0956(14) 0.2606(14) 0.0749 1.0000 Uani . . . . . . O40 O 0.2500 0.7500 0.0000 0.1390 1.0000 Uani S T . . . . H371 H 0.2617 0.1055 0.2414 0.0747 1.0000 Uiso . . . . . . H372 H 0.3169 0.1198 0.3195 0.0747 1.0000 Uiso . . . . . . H373 H 0.3189 0.0458 0.2672 0.0747 1.0000 Uiso . . . . . . H361 H 0.5899 0.1495 0.1280 0.0832 1.0000 Uiso . . . . . . H362 H 0.5716 0.1583 0.2301 0.0832 1.0000 Uiso . . . . . . H363 H 0.5685 0.0812 0.1853 0.0832 1.0000 Uiso . . . . . . H331 H 0.4483 0.1034 0.2702 0.0534 1.0000 Uiso . . . . . . H291 H 0.5104 0.2205 -0.2228 0.0707 1.0000 Uiso . . . . . . H292 H 0.5651 0.2855 -0.2132 0.0707 1.0000 Uiso . . . . . . H293 H 0.5876 0.2075 -0.1812 0.0707 1.0000 Uiso . . . . . . H301 H 0.5735 0.3587 0.1590 0.0936 1.0000 Uiso . . . . . . H302 H 0.6193 0.3828 0.0754 0.0936 1.0000 Uiso . . . . . . H303 H 0.6315 0.3057 0.1180 0.0936 1.0000 Uiso . . . . . . H261 H 0.6150 0.2895 -0.0499 0.0622 1.0000 Uiso . . . . . . H151 H 0.3525 0.1642 -0.5308 0.0871 1.0000 Uiso . . . . . . H152 H 0.3968 0.2102 -0.6004 0.0871 1.0000 Uiso . . . . . . H153 H 0.4351 0.1476 -0.5468 0.0871 1.0000 Uiso . . . . . . H161 H 0.5892 0.3677 -0.3539 0.1028 1.0000 Uiso . . . . . . H162 H 0.5903 0.3667 -0.4590 0.1028 1.0000 Uiso . . . . . . H163 H 0.6112 0.2965 -0.4051 0.1028 1.0000 Uiso . . . . . . H121 H 0.5102 0.2698 -0.5293 0.0716 1.0000 Uiso . . . . . . H221 H 0.4071 0.5442 -0.4481 0.1278 1.0000 Uiso . . . . . . H222 H 0.4829 0.5565 -0.4022 0.1278 1.0000 Uiso . . . . . . H223 H 0.4142 0.5987 -0.3676 0.1278 1.0000 Uiso . . . . . . H231 H 0.4444 0.4214 -0.0530 0.0775 1.0000 Uiso . . . . . . H232 H 0.5099 0.4664 -0.0912 0.0775 1.0000 Uiso . . . . . . H233 H 0.4364 0.5054 -0.0683 0.0775 1.0000 Uiso . . . . . . H191 H 0.4772 0.5370 -0.2315 0.0662 1.0000 Uiso . . . . . . H3 H 0.2500 0.2500 -0.3868 0.0500 0.5000 Uiso . . . . . . H8 H 0.3914 0.2408 -0.1835 0.0500 1.0000 Uiso . . . . . . H12 H 0.2500 0.2500 0.1058 0.0500 0.5000 Uiso . . . . . . H99 H 0.2301 0.7220 -0.0271 0.0500 0.5000 Uiso . . . . . . H32 H 0.3566 0.1278 -0.0717 0.0378 1.0000 Uiso . . . . . . 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 0.0331(6) 0.0331(6) 0.0353(9) 0.0000 0.0000 0.0000 Eu2 0.0395(5) 0.0399(5) 0.0370(4) 0.0032(4) 0.0017(4) -0.0023(4) Eu3 0.0340(5) 0.0370(5) 0.0374(4) 0.0009(4) -0.0029(4) -0.0006(4) O1 0.011(6) 0.011(6) 0.065(15) 0.0000 0.0000 0.0000 O2 0.031(7) 0.031(7) 0.060(16) 0.0000 0.0000 0.0000 O3 0.030(6) 0.032(6) 0.031(5) 0.002(4) 0.003(5) 0.003(4) O4 0.043(7) 0.041(6) 0.027(5) 0.006(5) 0.004(5) 0.002(5) O10 0.045(7) 0.039(7) 0.037(6) 0.009(5) 0.018(5) 0.006(5) C11 0.112(18) 0.045(11) 0.030(11) 0.005(9) -0.003(11) 0.003(12) C12 0.063(14) 0.079(16) 0.059(14) 0.012(12) 0.026(12) -0.005(12) C13 0.057(13) 0.087(16) 0.035(11) 0.007(11) 0.007(10) -0.004(12) O14 0.041(8) 0.079(10) 0.086(11) -0.008(8) 0.011(8) -0.013(7) C15 0.083(16) 0.097(18) 0.051(13) -0.016(13) 0.032(12) -0.017(13) C16 0.060(16) 0.14(3) 0.11(2) -0.01(2) 0.033(15) -0.024(16) O17 0.058(9) 0.066(9) 0.071(9) 0.012(8) -0.016(8) -0.013(7) C18 0.058(13) 0.057(13) 0.066(14) 0.011(11) -0.002(11) -0.012(10) C19 0.030(10) 0.055(12) 0.081(15) 0.005(11) 0.000(10) -0.014(9) C20 0.039(10) 0.054(12) 0.061(12) -0.021(10) 0.012(9) -0.015(9) O21 0.040(7) 0.053(8) 0.066(9) -0.008(7) -0.012(6) -0.006(6) C22 0.16(3) 0.072(17) 0.10(2) 0.038(15) -0.026(19) -0.035(18) C23 0.053(13) 0.074(15) 0.063(13) -0.011(11) -0.005(11) -0.014(11) O24 0.038(7) 0.050(7) 0.055(8) -0.002(6) -0.004(6) 0.000(5) C25 0.018(9) 0.051(11) 0.080(14) 0.010(10) -0.009(9) 0.001(7) C26 0.041(11) 0.056(12) 0.070(13) 0.027(11) 0.019(11) 0.006(9) C27 0.045(12) 0.045(11) 0.087(16) 0.005(12) -0.009(12) 0.001(9) O28 0.050(8) 0.042(7) 0.071(9) -0.008(6) -0.002(7) 0.002(6) C29 0.053(11) 0.064(12) 0.040(10) 0.010(9) 0.020(9) 0.002(9) C30 0.067(15) 0.083(17) 0.102(19) -0.032(15) -0.029(14) 0.001(13) O31 0.044(8) 0.073(10) 0.063(9) 0.011(8) -0.003(7) 0.003(7) C32 0.054(12) 0.060(13) 0.056(14) 0.010(10) 0.000(10) 0.002(10) C33 0.063(13) 0.046(11) 0.046(11) 0.010(9) -0.016(10) 0.001(9) C34 0.032(9) 0.066(12) 0.024(9) 0.004(8) -0.003(7) -0.015(8) O35 0.033(6) 0.056(8) 0.045(7) -0.001(6) -0.002(6) -0.007(6) C36 0.052(13) 0.075(15) 0.089(17) 0.017(14) -0.006(12) 0.012(11) C37 0.050(13) 0.12(2) 0.052(13) 0.021(13) -0.007(10) 0.032(13) O40 0.12(2) 0.12(2) 0.18(5) 0.0000 0.0000 0.0000 _refine_ls_extinction_method None _oxford_refine_ls_scale 0.03587(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Eu1 . O3 3_555 2.486(10) yes Eu1 . O3 5_555 2.486(10) yes Eu1 . O3 7_555 2.486(10) yes Eu1 . O4 3_555 2.479(10) yes Eu1 . O4 5_555 2.479(10) yes Eu1 . O4 7_555 2.479(10) yes Eu1 . O3 . 2.486(10) yes Eu1 . O4 . 2.479(10) yes Eu2 . O10 3_555 2.477(10) yes Eu2 . O4 3_555 2.363(11) yes Eu2 . O2 . 2.608(3) yes Eu2 . O4 . 2.345(10) yes Eu2 . O10 . 2.412(11) yes Eu2 . O14 . 2.384(13) yes Eu2 . O17 . 2.318(14) yes Eu2 . C20 . 3.414(18) yes Eu2 . O21 . 2.387(12) yes Eu3 . O35 3_555 2.461(11) yes Eu3 . O3 3_555 2.362(10) yes Eu3 . O1 . 2.638(3) yes Eu3 . O3 . 2.352(10) yes Eu3 . O24 . 2.364(12) yes Eu3 . O28 . 2.338(12) yes Eu3 . O31 . 2.366(13) yes Eu3 . O35 . 2.477(11) yes O1 . H12 . 0.837 no O2 . H3 . 0.813 no O3 . H32 . 0.789 no O4 . H8 . 0.878 no O10 . C11 . 1.36(2) yes C11 . C12 . 1.34(3) yes C11 . C15 . 1.49(3) yes C12 . C13 . 1.35(3) yes C12 . H121 . 0.958 no C13 . O14 . 1.27(2) yes C13 . C16 . 1.50(3) yes C15 . H151 . 1.083 no C15 . H152 . 0.984 no C15 . H153 . 0.946 no C16 . H161 . 1.118 no C16 . H162 . 0.926 no C16 . H163 . 0.920 no O17 . C18 . 1.29(2) yes C18 . C19 . 1.35(3) yes C18 . C22 . 1.54(3) yes C19 . C20 . 1.39(3) yes C19 . H191 . 0.970 no C20 . O21 . 1.30(2) yes C20 . C23 . 1.49(3) yes C22 . H221 . 1.148 no C22 . H222 . 0.985 no C22 . H223 . 0.842 no C23 . H231 . 1.027 no C23 . H232 . 0.971 no C23 . H233 . 0.991 no O24 . C25 . 1.249(19) yes C25 . C26 . 1.40(3) yes C25 . C29 . 1.48(3) yes C26 . C27 . 1.37(3) yes C26 . H261 . 0.998 no C27 . O28 . 1.28(2) yes C27 . C30 . 1.52(3) yes C29 . H291 . 1.032 no C29 . H292 . 0.935 no C29 . H293 . 0.968 no C30 . H301 . 1.116 no C30 . H302 . 0.915 no C30 . H303 . 0.971 no O31 . C32 . 1.23(2) yes C32 . C33 . 1.38(3) yes C32 . C36 . 1.56(3) yes C33 . C34 . 1.36(2) yes C33 . H331 . 0.982 no C34 . O35 . 1.320(19) yes C34 . C37 . 1.48(3) yes C36 . H361 . 1.101 no C36 . H362 . 0.907 no C36 . H363 . 0.938 no C37 . H371 . 1.043 no C37 . H372 . 1.030 no C37 . H373 . 0.967 no O40 . H99 4_566 0.791 no O40 . H99 5_655 0.791 no O40 . H99 8_646 0.791 no O40 . H99 . 0.791 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 3_555 Eu1 . O3 5_555 74.5(2) yes O3 3_555 Eu1 . O3 7_555 117.7(5) yes O3 5_555 Eu1 . O3 7_555 74.5(2) yes O3 3_555 Eu1 . O4 3_555 75.1(3) yes O3 5_555 Eu1 . O4 3_555 76.8(3) yes O3 7_555 Eu1 . O4 3_555 143.2(3) yes O3 3_555 Eu1 . O4 5_555 140.6(3) yes O3 5_555 Eu1 . O4 5_555 75.1(3) yes O3 7_555 Eu1 . O4 5_555 76.8(3) yes O4 3_555 Eu1 . O4 5_555 73.9(2) yes O3 3_555 Eu1 . O4 7_555 143.2(3) yes O3 5_555 Eu1 . O4 7_555 140.6(3) yes O3 7_555 Eu1 . O4 7_555 75.1(3) yes O4 3_555 Eu1 . O4 7_555 116.5(5) yes O4 5_555 Eu1 . O4 7_555 73.9(2) yes O3 3_555 Eu1 . O3 . 74.5(2) yes O3 5_555 Eu1 . O3 . 117.7(5) yes O3 7_555 Eu1 . O3 . 74.5(2) yes O4 3_555 Eu1 . O3 . 140.6(3) yes O4 5_555 Eu1 . O3 . 143.2(3) yes O3 3_555 Eu1 . O4 . 76.8(3) yes O3 5_555 Eu1 . O4 . 143.2(3) yes O3 7_555 Eu1 . O4 . 140.6(3) yes O4 3_555 Eu1 . O4 . 73.9(2) yes O4 5_555 Eu1 . O4 . 116.5(5) yes O4 7_555 Eu1 . O3 . 76.8(3) yes O4 7_555 Eu1 . O4 . 73.9(2) yes O3 . Eu1 . O4 . 75.1(3) yes O10 3_555 Eu2 . O4 3_555 75.8(4) yes O10 3_555 Eu2 . O2 . 64.5(4) yes O4 3_555 Eu2 . O2 . 66.2(4) yes O10 3_555 Eu2 . O4 . 130.4(4) yes O4 3_555 Eu2 . O4 . 78.6(5) yes O2 . Eu2 . O4 . 66.4(4) yes O10 3_555 Eu2 . O10 . 88.7(5) yes O4 3_555 Eu2 . O10 . 131.1(4) yes O2 . Eu2 . O10 . 65.3(4) yes O4 . Eu2 . O10 . 77.4(4) yes O10 3_555 Eu2 . O14 . 126.5(5) yes O4 3_555 Eu2 . O14 . 153.6(4) yes O2 . Eu2 . O14 . 132.9(4) yes O4 . Eu2 . O14 . 92.6(4) yes O10 . Eu2 . O14 . 69.2(4) yes O10 3_555 Eu2 . O17 . 74.6(4) yes O4 3_555 Eu2 . O17 . 100.9(4) yes O2 . Eu2 . O17 . 138.9(4) yes O4 . Eu2 . O17 . 152.6(4) yes O10 . Eu2 . O17 . 119.3(4) yes O10 3_555 Eu2 . C20 . 122.7(4) yes O4 3_555 Eu2 . C20 . 82.2(4) yes O2 . Eu2 . C20 . 145.2(6) yes O4 . Eu2 . C20 . 94.5(4) yes O10 . Eu2 . C20 . 141.4(4) yes O10 3_555 Eu2 . O21 . 131.3(4) yes O4 3_555 Eu2 . O21 . 74.6(4) yes O2 . Eu2 . O21 . 131.6(6) yes O4 . Eu2 . O21 . 79.4(4) yes O10 . Eu2 . O21 . 139.5(4) yes O14 . Eu2 . O17 . 75.6(5) yes O14 . Eu2 . C20 . 73.7(5) yes O17 . Eu2 . C20 . 58.6(5) yes O14 . Eu2 . O21 . 79.3(5) yes O17 . Eu2 . O21 . 74.2(5) yes C20 . Eu2 . O21 . 15.9(5) yes O35 3_555 Eu3 . O3 3_555 76.2(4) yes O35 3_555 Eu3 . O1 . 64.1(4) yes O3 3_555 Eu3 . O1 . 66.7(4) yes O35 3_555 Eu3 . O3 . 130.6(4) yes O3 3_555 Eu3 . O3 . 79.3(4) yes O1 . Eu3 . O3 . 66.8(4) yes O35 3_555 Eu3 . O24 . 135.4(4) yes O3 3_555 Eu3 . O24 . 77.8(4) yes O1 . Eu3 . O24 . 133.4(5) yes O3 . Eu3 . O24 . 78.0(4) yes O35 3_555 Eu3 . O28 . 74.4(4) yes O3 3_555 Eu3 . O28 . 97.1(4) yes O1 . Eu3 . O28 . 137.8(4) yes O3 . Eu3 . O28 . 151.5(4) yes O24 . Eu3 . O28 . 73.6(4) yes O35 3_555 Eu3 . O31 . 117.1(4) yes O3 3_555 Eu3 . O31 . 158.6(4) yes O1 . Eu3 . O31 . 133.3(4) yes O3 . Eu3 . O31 . 100.7(4) yes O24 . Eu3 . O31 . 81.3(4) yes O35 3_555 Eu3 . O35 . 88.1(5) yes O3 3_555 Eu3 . O35 . 130.2(3) yes O1 . Eu3 . O35 . 63.9(4) yes O3 . Eu3 . O35 . 76.0(4) yes O24 . Eu3 . O35 . 135.9(4) yes O28 . Eu3 . O31 . 72.4(4) yes O28 . Eu3 . O35 . 123.9(4) yes O31 . Eu3 . O35 . 69.4(4) yes Eu3 . O1 . Eu3 3_555 89.14(11) yes Eu3 . O1 . Eu3 5_555 165.9(9) yes Eu3 3_555 O1 . Eu3 5_555 89.14(11) yes Eu3 . O1 . Eu3 7_555 89.14(11) yes Eu3 3_555 O1 . Eu3 7_555 165.9(9) yes Eu3 5_555 O1 . Eu3 7_555 89.14(11) yes Eu3 . O1 . H12 . 97.0 no Eu3 3_555 O1 . H12 . 97.0 no Eu3 5_555 O1 . H12 . 97.0 no Eu3 7_555 O1 . H12 . 97.0 no Eu2 . O2 . Eu2 3_555 89.38(10) yes Eu2 . O2 . Eu2 5_555 168.1(10) yes Eu2 3_555 O2 . Eu2 5_555 89.38(10) yes Eu2 . O2 . Eu2 7_555 89.38(10) yes Eu2 3_555 O2 . Eu2 7_555 168.1(10) yes Eu2 5_555 O2 . Eu2 7_555 89.38(10) yes Eu2 . O2 . H3 . 95.9 no Eu2 3_555 O2 . H3 . 95.9 no Eu2 5_555 O2 . H3 . 95.9 no Eu2 7_555 O2 . H3 . 95.9 no Eu1 . O3 . Eu3 7_555 102.2(4) yes Eu1 . O3 . Eu3 . 102.5(4) yes Eu3 7_555 O3 . Eu3 . 103.5(4) yes Eu1 . O3 . H32 . 136.0 no Eu3 7_555 O3 . H32 . 99.2 no Eu3 . O3 . H32 . 109.3 no Eu1 . O4 . Eu2 7_555 102.7(4) yes Eu1 . O4 . Eu2 . 103.3(4) yes Eu2 7_555 O4 . Eu2 . 102.4(4) yes Eu1 . O4 . H8 . 102.2 no Eu2 7_555 O4 . H8 . 120.9 no Eu2 . O4 . H8 . 122.4 no Eu2 7_555 O10 . Eu2 . 97.2(3) yes Eu2 7_555 O10 . C11 . 124.5(10) yes Eu2 . O10 . C11 . 131.6(11) yes O10 . C11 . C12 . 121.1(18) yes O10 . C11 . C15 . 114.6(19) yes C12 . C11 . C15 . 124(2) yes C11 . C12 . C13 . 128.3(20) yes C11 . C12 . H121 . 115.0 no C13 . C12 . H121 . 116.6 no C12 . C13 . O14 . 122.7(20) yes C12 . C13 . C16 . 121(2) yes O14 . C13 . C16 . 116(2) yes C13 . O14 . Eu2 . 136.5(14) yes C11 . C15 . H151 . 109.2 no C11 . C15 . H152 . 108.6 no H151 . C15 . H152 . 104.5 no C11 . C15 . H153 . 111.2 no H151 . C15 . H153 . 107.1 no H152 . C15 . H153 . 115.8 no C13 . C16 . H161 . 103.6 no C13 . C16 . H162 . 107.2 no H161 . C16 . H162 . 106.0 no C13 . C16 . H163 . 107.1 no H161 . C16 . H163 . 106.3 no H162 . C16 . H163 . 124.8 no Eu2 . O17 . C18 . 133.5(13) yes O17 . C18 . C19 . 125.9(18) yes O17 . C18 . C22 . 115.1(20) yes C19 . C18 . C22 . 119.0(19) yes C18 . C19 . C20 . 127.9(18) yes C18 . C19 . H191 . 116.6 no C20 . C19 . H191 . 115.2 no C19 . C20 . Eu2 . 92.3(12) yes C19 . C20 . O21 . 122.5(18) yes Eu2 . C20 . O21 . 30.3(9) yes C19 . C20 . C23 . 122.1(17) yes Eu2 . C20 . C23 . 145.6(13) yes O21 . C20 . C23 . 115.4(18) yes C20 . O21 . Eu2 . 133.8(13) yes C18 . C22 . H221 . 101.3 no C18 . C22 . H222 . 105.4 no H221 . C22 . H222 . 99.9 no C18 . C22 . H223 . 110.6 no H221 . C22 . H223 . 109.7 no H222 . C22 . H223 . 126.8 no C20 . C23 . H231 . 109.1 no C20 . C23 . H232 . 109.8 no H231 . C23 . H232 . 109.8 no C20 . C23 . H233 . 107.1 no H231 . C23 . H233 . 108.2 no H232 . C23 . H233 . 112.8 no Eu3 . O24 . C25 . 137.0(13) yes O24 . C25 . C26 . 118.5(18) yes O24 . C25 . C29 . 121.6(17) yes C26 . C25 . C29 . 119.9(16) yes C25 . C26 . C27 . 130.7(18) yes C25 . C26 . H261 . 118.5 no C27 . C26 . H261 . 110.8 no C26 . C27 . O28 . 123.5(19) yes C26 . C27 . C30 . 121.3(20) yes O28 . C27 . C30 . 115(2) yes C27 . O28 . Eu3 . 130.3(12) yes C25 . C29 . H291 . 102.4 no C25 . C29 . H292 . 107.0 no H291 . C29 . H292 . 112.3 no C25 . C29 . H293 . 105.3 no H291 . C29 . H293 . 109.6 no H292 . C29 . H293 . 118.5 no C27 . C30 . H301 . 106.8 no C27 . C30 . H302 . 110.8 no H301 . C30 . H302 . 106.9 no C27 . C30 . H303 . 108.0 no H301 . C30 . H303 . 103.0 no H302 . C30 . H303 . 120.2 no Eu3 . O31 . C32 . 132.8(13) yes O31 . C32 . C33 . 124.7(19) yes O31 . C32 . C36 . 117.9(18) yes C33 . C32 . C36 . 117.3(18) yes C32 . C33 . C34 . 125.7(17) yes C32 . C33 . H331 . 117.5 no C34 . C33 . H331 . 116.7 no C33 . C34 . O35 . 123.9(15) yes C33 . C34 . C37 . 121.7(16) yes O35 . C34 . C37 . 114.5(14) yes C34 . O35 . Eu3 . 129.6(10) yes C34 . O35 . Eu3 7_555 129.3(10) yes Eu3 . O35 . Eu3 7_555 97.1(4) yes C32 . C36 . H361 . 100.4 no C32 . C36 . H362 . 106.7 no H361 . C36 . H362 . 108.9 no C32 . C36 . H363 . 107.0 no H361 . C36 . H363 . 106.4 no H362 . C36 . H363 . 124.8 no C34 . C37 . H371 . 111.6 no C34 . C37 . H372 . 109.7 no H371 . C37 . H372 . 104.2 no C34 . C37 . H373 . 112.4 no H371 . C37 . H373 . 108.8 no H372 . C37 . H373 . 109.9 no H99 4_566 O40 . H99 5_655 121.5 no H99 4_566 O40 . H99 8_646 87.5 no H99 5_655 O40 . H99 8_646 121.5 no H99 4_566 O40 . H99 . 121.5 no H99 5_655 O40 . H99 . 87.5 no H99 8_646 O40 . H99 . 121.5 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O4 . H8 . O24 . 174.7 0.878 1.979 2.854 yes O3 . H32 . O21 7_555 126.6 1.009 2.090 2.811 yes # Attachment 'Y9-Revised.cif' data_IV _database_code_depnum_ccdc_archive 'CCDC 711969' _audit_creation_date 06-02-13 _audit_creation_method CRYSTALS_ver_12.82 _oxford_structure_analysis_title 'import in P 4/n' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 19.151(2) _cell_length_b 19.151(2) _cell_length_c 15.5247(18) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5693.6(12) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 4/n ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -y+1/2,x,z y+1/2,-x,-z -x+1/2,-y+1/2,z x+1/2,y+1/2,-z y,-x+1/2,z -y,x+1/2,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Y -2.7962 3.5667 17.7760 1.4029 10.2946 12.8006 5.7263 0.1256 3.2659 104.3540 1.9121 'International Tables Vol C 4.2.6.8 and 6.1.1.4' C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C50 H76.25 O26.25 Y6.25 # Dc = 1.93 Fooo = 2500.00 Mu = 63.83 M = 826.52 # Found Formula = C40 H61.12 O20.38 Y4.12 # Dc = 1.50 FOOO = 2500.00 Mu = 46.05 M = 643.24 _chemical_formula_sum 'C80 H123 O43 Y9' _chemical_formula_moiety 'C80 H123 O43 Y9' _chemical_compound_source ? _chemical_formula_weight 2573.0 _cell_measurement_reflns_used 7005 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 290 _exptl_crystal_description cubic _exptl_crystal_colour colourless _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_max 0.02 _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2500 _exptl_absorpt_coefficient_mu 4.605 # Sheldrick geometric approximatio 0.91 0.91 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.9078 _exptl_absorpt_correction_T_max 0.9120 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _computing_data_collection 'COLLECT. Nonius (1997-2001).' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 290 _diffrn_reflns_number 7251 _reflns_number_total 7005 _diffrn_reflns_av_R_equivalents 0.050 # Number of reflections with Friedels Law is 7005 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6390 _diffrn_reflns_theta_min 1.312 _diffrn_reflns_theta_max 28.883 _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 27.150 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -17 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.63 _refine_diff_density_max 0.98 _refine_ls_number_reflns 3232 _refine_ls_number_restraints 0 _refine_ls_number_parameters 300 #_refine_ls_R_factor_ref 0.0350 _refine_ls_wR_factor_ref 0.0364 _refine_ls_goodness_of_fit_ref 1.1002 #_reflns_number_all 6988 _refine_ls_R_factor_all 0.1048 _refine_ls_wR_factor_all 0.0673 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3232 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_gt 0.0364 _refine_ls_shift/su_max 0.000526 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.47 -0.387 1.05 ; _publ_section_abstract # Text of the abstract ; ? ; _publ_section_comment # Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures ; ? ; _publ_section_exptl_refinement # Some potentially useful phrases are: ; Because the data were collected with molybdenum radiation, there were no measurable anomalous differences, as a consequence of which it was admissible to merge Friedel pairs of reflections. All hydrogen atoms were found in difference density syntheses. Hydrogen atoms were placed geometrically after each cycle. Hydrogen atoms were placed geometrically after each cycle, the preferred orientations of those groups whose conformations could not be assigned unambiguously having been previously identified by examination of a difference Fourier map. Hydrogen atoms were seen in a difference density synthesis. Those attached to carbon atoms were repositioned geometrically. Hydrogen were initially refined with soft restraints on the bonds to regularise their geometry (bond lengths to accepted values, angles either set by symmetry or to accepted values, and U[iso] dependent upon the adjacent bonded atom), after which they were refined with riding constraints only. donated by Bill Clegg: The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93-98, O---N in the range 0.86-0.89 and O---H = 0.82 \%A) and isotropic adps (U(H) in the range 1.2-1.5 times U~equiv~ of the adjacent atom), after which they were refined with riding constraints. . ; _publ_section_exptl_prep ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Y1 Y 0.2500 0.2500 -0.13853(5) 0.0275 1.0000 Uani S T . . . . Y2 Y 0.34900(2) 0.33735(2) -0.31278(3) 0.0331 1.0000 Uani . . . . . . Y3 Y 0.38316(2) 0.24549(2) 0.03435(2) 0.0302 1.0000 Uani . . . . . . O1 O 0.2500 0.2500 0.0526(4) 0.0335 1.0000 Uani S T . . . . O2 O 0.2500 0.2500 -0.3292(4) 0.0357 1.0000 Uani S T . . . . O3 O 0.32371(15) 0.17177(15) -0.05607(17) 0.0313 1.0000 Uani . . . . . . O4 O 0.35661(15) 0.24469(15) -0.22076(18) 0.0325 1.0000 Uani . . . . . . O10 O 0.37192(18) 0.24340(17) -0.41127(19) 0.0427 1.0000 Uani . . . . . . C11 C 0.4180(3) 0.2382(3) -0.4732(3) 0.0508 1.0000 Uani . . . . . . C12 C 0.4793(3) 0.2736(3) -0.4753(4) 0.0616 1.0000 Uani . . . . . . C13 C 0.5049(3) 0.3158(3) -0.4064(4) 0.0561 1.0000 Uani . . . . . . O14 O 0.4677(2) 0.3338(2) -0.3439(2) 0.0586 1.0000 Uani . . . . . . C15 C 0.3991(4) 0.1872(4) -0.5436(4) 0.0712 1.0000 Uani . . . . . . C16 C 0.5800(4) 0.3386(5) -0.4062(5) 0.0839 1.0000 Uani . . . . . . O17 O 0.3751(2) 0.44735(19) -0.3561(2) 0.0563 1.0000 Uani . . . . . . C18 C 0.4160(3) 0.4941(3) -0.3280(4) 0.0574 1.0000 Uani . . . . . . C19 C 0.4446(3) 0.4963(3) -0.2462(4) 0.0545 1.0000 Uani . . . . . . C20 C 0.4316(2) 0.4478(3) -0.1819(3) 0.0436 1.0000 Uani . . . . . . O21 O 0.39752(17) 0.39113(17) -0.1929(2) 0.0414 1.0000 Uani . . . . . . C22 C 0.4295(5) 0.5538(4) -0.3916(5) 0.1067 1.0000 Uani . . . . . . C23 C 0.4576(3) 0.4607(3) -0.0918(4) 0.0618 1.0000 Uani . . . . . . O24 O 0.45514(16) 0.24344(18) -0.0855(2) 0.0430 1.0000 Uani . . . . . . C25 C 0.5193(2) 0.2566(3) -0.0972(3) 0.0433 1.0000 Uani . . . . . . C26 C 0.5630(3) 0.2860(3) -0.0349(4) 0.0499 1.0000 Uani . . . . . . C27 C 0.5415(3) 0.3120(3) 0.0445(4) 0.0504 1.0000 Uani . . . . . . O28 O 0.47795(18) 0.31336(19) 0.0698(2) 0.0518 1.0000 Uani . . . . . . C29 C 0.5485(3) 0.2411(3) -0.1842(4) 0.0592 1.0000 Uani . . . . . . C30 C 0.5958(3) 0.3416(4) 0.1035(5) 0.0780 1.0000 Uani . . . . . . O31 O 0.46989(18) 0.1705(2) 0.0816(2) 0.0547 1.0000 Uani . . . . . . C32 C 0.4836(3) 0.1433(3) 0.1531(4) 0.0491 1.0000 Uani . . . . . . C33 C 0.4321(3) 0.1229(3) 0.2126(3) 0.0460 1.0000 Uani . . . . . . C34 C 0.3617(3) 0.1279(2) 0.1985(3) 0.0419 1.0000 Uani . . . . . . O35 O 0.33357(16) 0.15928(16) 0.13265(19) 0.0385 1.0000 Uani . . . . . . C36 C 0.5593(3) 0.1319(4) 0.1755(4) 0.0699 1.0000 Uani . . . . . . C37 C 0.3117(3) 0.0972(3) 0.2618(4) 0.0598 1.0000 Uani . . . . . . O40 O 0.2500 0.7500 0.0000 0.1390 1.0000 Uani DS T . . . . H371 H 0.2617 0.1055 0.2414 0.0747 1.0000 Uiso . . . . . . H372 H 0.3169 0.1198 0.3195 0.0747 1.0000 Uiso . . . . . . H373 H 0.3189 0.0458 0.2672 0.0747 1.0000 Uiso . . . . . . H361 H 0.5899 0.1495 0.1280 0.0832 1.0000 Uiso . . . . . . H362 H 0.5716 0.1583 0.2301 0.0832 1.0000 Uiso . . . . . . H363 H 0.5685 0.0812 0.1853 0.0832 1.0000 Uiso . . . . . . H331 H 0.4483 0.1034 0.2702 0.0534 1.0000 Uiso . . . . . . H291 H 0.5104 0.2205 -0.2228 0.0707 1.0000 Uiso . . . . . . H292 H 0.5651 0.2855 -0.2132 0.0707 1.0000 Uiso . . . . . . H293 H 0.5876 0.2075 -0.1812 0.0707 1.0000 Uiso . . . . . . H301 H 0.5735 0.3587 0.1590 0.0936 1.0000 Uiso . . . . . . H302 H 0.6193 0.3828 0.0754 0.0936 1.0000 Uiso . . . . . . H303 H 0.6315 0.3057 0.1180 0.0936 1.0000 Uiso . . . . . . H261 H 0.6150 0.2895 -0.0499 0.0622 1.0000 Uiso . . . . . . H151 H 0.3525 0.1642 -0.5308 0.0871 1.0000 Uiso . . . . . . H152 H 0.3968 0.2102 -0.6004 0.0871 1.0000 Uiso . . . . . . H153 H 0.4351 0.1476 -0.5468 0.0871 1.0000 Uiso . . . . . . H161 H 0.5892 0.3677 -0.3539 0.1028 1.0000 Uiso . . . . . . H162 H 0.5903 0.3667 -0.4590 0.1028 1.0000 Uiso . . . . . . H163 H 0.6112 0.2965 -0.4051 0.1028 1.0000 Uiso . . . . . . H121 H 0.5102 0.2698 -0.5293 0.0716 1.0000 Uiso . . . . . . H221 H 0.4071 0.5442 -0.4481 0.1278 1.0000 Uiso . . . . . . H222 H 0.4829 0.5565 -0.4022 0.1278 1.0000 Uiso . . . . . . H223 H 0.4142 0.5987 -0.3676 0.1278 1.0000 Uiso . . . . . . H231 H 0.4444 0.4214 -0.0530 0.0775 1.0000 Uiso . . . . . . H232 H 0.5099 0.4664 -0.0912 0.0775 1.0000 Uiso . . . . . . H233 H 0.4364 0.5054 -0.0683 0.0775 1.0000 Uiso . . . . . . H191 H 0.4772 0.5370 -0.2315 0.0662 1.0000 Uiso . . . . . . H3 H 0.2500 0.2500 -0.3908 0.0500 0.5000 Uiso . . . . . . H8 H 0.3914 0.2408 -0.1835 0.0500 1.0000 Uiso . . . . . . H12 H 0.2500 0.2500 0.1088 0.0500 0.5000 Uiso . . . . . . H99 H 0.2301 0.7220 -0.0271 0.0500 0.5000 Uiso D . . . . . H33 H 0.3520 0.1282 -0.0655 0.0379 1.0000 Uiso . . . . . . 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 Y1 0.0303(3) 0.0303(3) 0.0218(4) 0.0000 0.0000 0.0000 Y2 0.0368(2) 0.0373(2) 0.0251(2) 0.00406(18) 0.00143(18) -0.00244(19) Y3 0.0317(2) 0.0334(2) 0.02560(19) 0.00061(17) -0.00204(18) -0.00009(18) O1 0.0312(19) 0.0312(19) 0.038(3) 0.0000 0.0000 0.0000 O2 0.039(2) 0.039(2) 0.029(3) 0.0000 0.0000 0.0000 O3 0.0338(16) 0.0328(16) 0.0273(14) 0.0021(12) -0.0006(12) 0.0006(12) O4 0.0356(16) 0.0372(16) 0.0246(14) 0.0021(13) 0.0007(12) 0.0015(13) O10 0.0490(19) 0.0487(19) 0.0304(15) 0.0027(14) 0.0059(14) 0.0027(15) C11 0.062(3) 0.057(3) 0.033(3) 0.005(2) 0.010(2) 0.006(3) C12 0.062(3) 0.080(4) 0.043(3) 0.010(3) 0.024(3) 0.002(3) C13 0.057(3) 0.061(4) 0.050(3) 0.015(3) 0.003(3) 0.000(3) O14 0.047(2) 0.073(3) 0.055(2) -0.0034(19) 0.0087(18) -0.0023(18) C15 0.096(5) 0.079(4) 0.038(3) -0.006(3) 0.022(3) -0.003(4) C16 0.053(4) 0.121(6) 0.078(4) 0.007(4) 0.017(3) -0.009(4) O17 0.068(2) 0.050(2) 0.051(2) 0.0156(17) -0.0135(19) -0.0130(19) C18 0.068(4) 0.045(3) 0.059(3) 0.014(3) -0.002(3) -0.013(3) C19 0.058(3) 0.053(3) 0.053(3) 0.004(3) -0.004(3) -0.017(3) C20 0.036(2) 0.050(3) 0.044(3) -0.004(2) -0.002(2) -0.006(2) O21 0.0459(18) 0.0458(18) 0.0326(16) 0.0014(14) -0.0012(14) -0.0097(15) C22 0.153(8) 0.083(5) 0.084(5) 0.038(4) -0.021(5) -0.056(6) C23 0.071(4) 0.066(4) 0.048(3) -0.001(3) -0.014(3) -0.021(3) O24 0.0364(18) 0.058(2) 0.0345(17) 0.0042(15) 0.0024(14) -0.0018(15) C25 0.039(3) 0.042(3) 0.049(3) 0.010(2) 0.007(2) 0.002(2) C26 0.035(2) 0.055(3) 0.060(3) 0.008(3) -0.004(2) -0.004(2) C27 0.040(3) 0.046(3) 0.065(4) -0.003(3) 0.001(2) -0.004(2) O28 0.044(2) 0.056(2) 0.056(2) -0.0111(17) -0.0030(17) -0.0071(16) C29 0.043(3) 0.082(4) 0.052(3) 0.010(3) 0.010(3) 0.002(3) C30 0.056(4) 0.085(5) 0.093(5) -0.031(4) -0.010(3) -0.010(3) O31 0.046(2) 0.058(2) 0.060(2) 0.0189(19) 0.0041(17) 0.0101(17) C32 0.048(3) 0.040(3) 0.060(3) 0.004(2) -0.008(3) 0.007(2) C33 0.050(3) 0.051(3) 0.037(3) 0.004(2) -0.012(2) 0.004(2) C34 0.057(3) 0.040(3) 0.029(2) -0.0005(19) -0.003(2) 0.000(2) O35 0.0418(17) 0.0410(17) 0.0327(15) 0.0057(14) -0.0063(14) 0.0014(14) C36 0.051(3) 0.077(4) 0.083(4) 0.017(3) -0.010(3) 0.013(3) C37 0.057(3) 0.082(4) 0.041(3) 0.020(3) -0.003(2) -0.005(3) O40 0.217(12) 0.217(12) 0.159(15) 0.0000 0.0000 0.0000 _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2366(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Y1 . O3 3_555 2.424(3) yes Y1 . O3 5_555 2.424(3) yes Y1 . O3 7_555 2.424(3) yes Y1 . O4 3_555 2.410(3) yes Y1 . O4 5_555 2.410(3) yes Y1 . O4 7_555 2.410(3) yes Y1 . O3 . 2.424(3) yes Y1 . O4 . 2.410(3) yes Y2 . O10 3_555 2.430(3) yes Y2 . O4 3_555 2.323(3) yes Y2 . O2 . 2.5410(7) yes Y2 . O4 . 2.283(3) yes Y2 . O10 . 2.402(3) yes Y2 . O14 . 2.325(4) yes Y2 . O17 . 2.267(3) yes Y2 . O21 . 2.321(3) yes Y3 . O35 3_555 2.416(3) yes Y3 . O3 3_555 2.307(3) yes Y3 . O1 . 2.5673(8) yes Y3 . O3 . 2.293(3) yes Y3 . O24 . 2.316(3) yes Y3 . O28 . 2.300(3) yes Y3 . O31 . 2.315(3) yes Y3 . O35 . 2.441(3) yes O1 . H12 . 0.873 no O2 . H3 . 0.956 no O3 . H33 . 1.005 no O4 . H8 . 0.886 no O10 . C11 . 1.309(6) yes C11 . C12 . 1.357(8) yes C11 . C15 . 1.509(8) yes C12 . C13 . 1.428(9) yes C12 . H121 . 1.028 no C13 . O14 . 1.252(7) yes C13 . C16 . 1.503(9) yes C15 . H151 . 1.015 no C15 . H152 . 0.988 no C15 . H153 . 1.025 no C16 . H161 . 1.001 no C16 . H162 . 1.001 no C16 . H163 . 1.004 no O17 . C18 . 1.267(6) yes C18 . C19 . 1.382(8) yes C18 . C22 . 1.534(8) yes C19 . C20 . 1.387(7) yes C19 . H191 . 1.025 no C20 . O21 . 1.278(6) yes C20 . C23 . 1.505(7) yes C22 . H221 . 0.993 no C22 . H222 . 1.036 no C22 . H223 . 0.981 no C23 . H231 . 0.996 no C23 . H232 . 1.007 no C23 . H233 . 1.017 no O24 . C25 . 1.268(6) yes C25 . C26 . 1.397(7) yes C25 . C29 . 1.491(7) yes C26 . C27 . 1.392(8) yes C26 . H261 . 1.025 no C27 . O28 . 1.279(6) yes C27 . C30 . 1.497(8) yes C29 . H291 . 1.023 no C29 . H292 . 1.014 no C29 . H293 . 0.989 no C30 . H301 . 1.015 no C30 . H302 . 1.007 no C30 . H303 . 0.995 no O31 . C32 . 1.254(6) yes C32 . C33 . 1.407(8) yes C32 . C36 . 1.505(8) yes C33 . C34 . 1.370(7) yes C33 . H331 . 1.018 no C34 . O35 . 1.303(5) yes C34 . C37 . 1.492(7) yes C36 . H361 . 1.000 no C36 . H362 . 1.014 no C36 . H363 . 0.999 no C37 . H371 . 1.022 no C37 . H372 . 1.000 no C37 . H373 . 0.997 no O40 . H99 4_566 0.791 no O40 . H99 5_655 0.791 no O40 . H99 8_646 0.791 no O40 . H99 . 0.791 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 3_555 Y1 . O3 5_555 73.81(6) yes O3 3_555 Y1 . O3 7_555 116.25(13) yes O3 5_555 Y1 . O3 7_555 73.81(6) yes O3 3_555 Y1 . O4 3_555 76.13(9) yes O3 5_555 Y1 . O4 3_555 77.33(10) yes O3 7_555 Y1 . O4 3_555 143.05(10) yes O3 3_555 Y1 . O4 5_555 141.14(10) yes O3 5_555 Y1 . O4 5_555 76.13(9) yes O3 7_555 Y1 . O4 5_555 77.33(10) yes O4 3_555 Y1 . O4 5_555 73.70(6) yes O3 3_555 Y1 . O4 7_555 143.05(10) yes O3 5_555 Y1 . O4 7_555 141.14(10) yes O3 7_555 Y1 . O4 7_555 76.13(9) yes O4 3_555 Y1 . O4 7_555 116.03(13) yes O4 5_555 Y1 . O4 7_555 73.71(6) yes O3 3_555 Y1 . O3 . 73.81(6) yes O3 5_555 Y1 . O3 . 116.25(13) yes O3 7_555 Y1 . O3 . 73.81(6) yes O4 3_555 Y1 . O3 . 141.14(10) yes O4 5_555 Y1 . O3 . 143.05(10) yes O3 3_555 Y1 . O4 . 77.33(10) yes O3 5_555 Y1 . O4 . 143.05(10) yes O3 7_555 Y1 . O4 . 141.14(10) yes O4 3_555 Y1 . O4 . 73.70(6) yes O4 5_555 Y1 . O4 . 116.03(13) yes O4 7_555 Y1 . O3 . 77.33(10) yes O4 7_555 Y1 . O4 . 73.71(6) yes O3 . Y1 . O4 . 76.13(9) yes O10 3_555 Y2 . O4 3_555 77.37(10) yes O10 3_555 Y2 . O2 . 64.73(11) yes O4 3_555 Y2 . O2 . 65.79(11) yes O10 3_555 Y2 . O4 . 130.69(11) yes O4 3_555 Y2 . O4 . 77.75(13) yes O2 . Y2 . O4 . 66.33(12) yes O10 3_555 Y2 . O10 . 86.37(15) yes O4 3_555 Y2 . O10 . 130.67(11) yes O2 . Y2 . O10 . 65.13(11) yes O4 . Y2 . O10 . 78.72(10) yes O10 3_555 Y2 . O14 . 126.11(12) yes O4 3_555 Y2 . O14 . 152.57(12) yes O2 . Y2 . O14 . 133.57(11) yes O4 . Y2 . O14 . 92.55(12) yes O10 . Y2 . O14 . 70.55(13) yes O10 3_555 Y2 . O17 . 73.79(12) yes O4 3_555 Y2 . O17 . 101.85(13) yes O2 . Y2 . O17 . 138.29(12) yes O4 . Y2 . O17 . 153.36(12) yes O10 . Y2 . O17 . 117.82(13) yes O10 3_555 Y2 . O21 . 132.46(12) yes O4 3_555 Y2 . O21 . 75.26(11) yes O2 . Y2 . O21 . 132.14(15) yes O4 . Y2 . O21 . 79.48(11) yes O10 . Y2 . O21 . 140.33(12) yes O14 . Y2 . O17 . 75.53(14) yes O14 . Y2 . O21 . 77.77(13) yes O17 . Y2 . O21 . 74.78(12) yes O35 3_555 Y3 . O3 3_555 77.14(10) yes O35 3_555 Y3 . O1 . 64.68(11) yes O3 3_555 Y3 . O1 . 65.95(12) yes O35 3_555 Y3 . O3 . 130.50(10) yes O3 3_555 Y3 . O3 . 78.51(13) yes O1 . Y3 . O3 . 66.13(12) yes O35 3_555 Y3 . O24 . 136.03(12) yes O3 3_555 Y3 . O24 . 78.09(11) yes O1 . Y3 . O24 . 132.90(15) yes O3 . Y3 . O24 . 78.07(11) yes O35 3_555 Y3 . O28 . 73.72(12) yes O3 3_555 Y3 . O28 . 97.97(12) yes O1 . Y3 . O28 . 137.61(11) yes O3 . Y3 . O28 . 152.42(12) yes O24 . Y3 . O28 . 74.46(12) yes O35 3_555 Y3 . O31 . 118.33(12) yes O3 3_555 Y3 . O31 . 157.35(12) yes O1 . Y3 . O31 . 134.29(12) yes O3 . Y3 . O31 . 99.67(12) yes O24 . Y3 . O31 . 79.46(12) yes O35 3_555 Y3 . O35 . 86.93(14) yes O3 3_555 Y3 . O35 . 129.97(10) yes O1 . Y3 . O35 . 64.35(11) yes O3 . Y3 . O35 . 76.89(10) yes O24 . Y3 . O35 . 136.26(12) yes O28 . Y3 . O31 . 73.06(13) yes O28 . Y3 . O35 . 122.67(12) yes O31 . Y3 . O35 . 70.20(11) yes Y3 5_555 O1 . Y3 . 167.3(3) yes Y3 5_555 O1 . Y3 3_555 89.30(3) yes Y3 . O1 . Y3 3_555 89.30(3) yes Y3 5_555 O1 . Y3 7_555 89.30(3) yes Y3 . O1 . Y3 7_555 89.30(3) yes Y3 3_555 O1 . Y3 7_555 167.3(3) yes Y3 5_555 O1 . H12 . 96.4 no Y3 . O1 . H12 . 96.4 no Y3 3_555 O1 . H12 . 96.4 no Y3 7_555 O1 . H12 . 96.4 no Y2 7_555 O2 . Y2 3_555 168.5(3) yes Y2 7_555 O2 . Y2 5_555 89.43(3) yes Y2 3_555 O2 . Y2 5_555 89.43(3) yes Y2 7_555 O2 . Y2 . 89.43(3) yes Y2 3_555 O2 . Y2 . 89.43(3) yes Y2 5_555 O2 . Y2 . 168.5(3) yes Y2 7_555 O2 . H3 . 95.7 no Y2 3_555 O2 . H3 . 95.7 no Y2 5_555 O2 . H3 . 95.7 no Y2 . O2 . H3 . 95.7 no Y1 . O3 . Y3 7_555 103.00(11) yes Y1 . O3 . Y3 . 103.41(11) yes Y3 7_555 O3 . Y3 . 103.33(11) yes Y1 . O3 . H33 . 138.6 no Y3 7_555 O3 . H33 . 93.5 no Y3 . O3 . H33 . 109.4 no Y1 . O4 . Y2 7_555 102.93(11) yes Y1 . O4 . Y2 . 104.16(11) yes Y2 7_555 O4 . Y2 . 101.85(11) yes Y1 . O4 . H8 . 107.1 no Y2 7_555 O4 . H8 . 117.1 no Y2 . O4 . H8 . 121.5 no Y2 7_555 O10 . Y2 . 95.46(10) yes Y2 7_555 O10 . C11 . 126.2(3) yes Y2 . O10 . C11 . 130.4(3) yes O10 . C11 . C12 . 124.3(5) yes O10 . C11 . C15 . 114.8(5) yes C12 . C11 . C15 . 120.9(5) yes C11 . C12 . C13 . 124.2(5) yes C11 . C12 . H121 . 118.8 no C13 . C12 . H121 . 117.0 no C12 . C13 . O14 . 122.8(5) yes C12 . C13 . C16 . 119.6(6) yes O14 . C13 . C16 . 117.5(6) yes C13 . O14 . Y2 . 136.4(4) yes C11 . C15 . H151 . 110.4 no C11 . C15 . H152 . 111.6 no H151 . C15 . H152 . 109.2 no C11 . C15 . H153 . 110.6 no H151 . C15 . H153 . 106.4 no H152 . C15 . H153 . 108.5 no C13 . C16 . H161 . 109.5 no C13 . C16 . H162 . 110.0 no H161 . C16 . H162 . 109.3 no C13 . C16 . H163 . 109.8 no H161 . C16 . H163 . 109.1 no H162 . C16 . H163 . 109.1 no Y2 . O17 . C18 . 133.7(3) yes O17 . C18 . C19 . 125.7(5) yes O17 . C18 . C22 . 114.1(5) yes C19 . C18 . C22 . 120.1(5) yes C18 . C19 . C20 . 124.7(5) yes C18 . C19 . H191 . 118.1 no C20 . C19 . H191 . 117.2 no C19 . C20 . O21 . 124.4(5) yes C19 . C20 . C23 . 120.0(5) yes O21 . C20 . C23 . 115.6(4) yes C20 . O21 . Y2 . 133.5(3) yes C18 . C22 . H221 . 110.9 no C18 . C22 . H222 . 107.8 no H221 . C22 . H222 . 107.2 no C18 . C22 . H223 . 111.0 no H221 . C22 . H223 . 111.7 no H222 . C22 . H223 . 108.1 no C20 . C23 . H231 . 110.7 no C20 . C23 . H232 . 110.9 no H231 . C23 . H232 . 109.3 no C20 . C23 . H233 . 109.9 no H231 . C23 . H233 . 108.5 no H232 . C23 . H233 . 107.6 no Y3 . O24 . C25 . 133.6(3) yes O24 . C25 . C26 . 124.1(5) yes O24 . C25 . C29 . 117.0(5) yes C26 . C25 . C29 . 118.9(4) yes C25 . C26 . C27 . 125.5(5) yes C25 . C26 . H261 . 116.8 no C27 . C26 . H261 . 117.8 no C26 . C27 . O28 . 124.1(5) yes C26 . C27 . C30 . 118.2(5) yes O28 . C27 . C30 . 117.7(5) yes C27 . O28 . Y3 . 131.8(3) yes C25 . C29 . H291 . 109.9 no C25 . C29 . H292 . 110.7 no H291 . C29 . H292 . 106.6 no C25 . C29 . H293 . 111.8 no H291 . C29 . H293 . 108.5 no H292 . C29 . H293 . 109.2 no C27 . C30 . H301 . 110.5 no C27 . C30 . H302 . 110.0 no H301 . C30 . H302 . 107.7 no C27 . C30 . H303 . 110.7 no H301 . C30 . H303 . 108.6 no H302 . C30 . H303 . 109.3 no Y3 . O31 . C32 . 133.5(3) yes O31 . C32 . C33 . 123.3(5) yes O31 . C32 . C36 . 117.8(5) yes C33 . C32 . C36 . 118.9(5) yes C32 . C33 . C34 . 124.5(4) yes C32 . C33 . H331 . 117.7 no C34 . C33 . H331 . 117.8 no C33 . C34 . O35 . 124.3(4) yes C33 . C34 . C37 . 119.9(4) yes O35 . C34 . C37 . 115.7(4) yes Y3 . O35 . Y3 7_555 95.99(10) yes Y3 . O35 . C34 . 130.0(3) yes Y3 7_555 O35 . C34 . 129.0(3) yes C32 . C36 . H361 . 110.2 no C32 . C36 . H362 . 110.1 no H361 . C36 . H362 . 108.3 no C32 . C36 . H363 . 110.2 no H361 . C36 . H363 . 109.5 no H362 . C36 . H363 . 108.4 no C34 . C37 . H371 . 109.6 no C34 . C37 . H372 . 110.9 no H371 . C37 . H372 . 107.7 no C34 . C37 . H373 . 110.8 no H371 . C37 . H373 . 107.9 no H372 . C37 . H373 . 109.7 no H99 4_566 O40 . H99 5_655 121.4 no H99 4_566 O40 . H99 8_646 87.6 no H99 5_655 O40 . H99 8_646 121.4 no H99 4_566 O40 . H99 . 121.4 no H99 5_655 O40 . H99 . 87.6 no H99 8_646 O40 . H99 . 121.4 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O4 . H8 . O24 . 167.9 0.886 1.951 2.823 yes O3 . H33 . O21 7_555 120.5 1.005 2.171 2.818 yes # Attachment 'Y8-Revised.cif' data_III _database_code_depnum_ccdc_archive 'CCDC 711970' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 18.2366(10) _cell_length_b 27.6109(10) _cell_length_c 31.2719(17) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 15746.3(13) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c n b ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y,z+1/2 x+1/2,-y,-z+1/2 x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-z+1/2 -x,-y+1/2,z x,y+1/2,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Y -2.7962 3.5667 17.7760 1.4029 10.2946 12.8006 5.7263 0.1256 3.2659 104.3540 1.9121 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C150 H122 O33 Y8 # Dc = 1.67 Fooo = 5704.00 Mu = 37.24 M = 1977.40 # Found Formula = C88 H155.20 O26 Y6.40 # Dc = 1.16 FOOO = 5704.00 Mu = 29.69 M = 1377.99 _chemical_formula_sum 'C110 H120 O33 Y8' _chemical_formula_moiety 'C110 H120 O33 Y8' _chemical_compound_source ? _chemical_formula_weight 2764.0 _cell_measurement_reflns_used 11557 _cell_measurement_theta_min 0 _cell_measurement_theta_max 28 _cell_measurement_temperature 293 _exptl_crystal_description cubic _exptl_crystal_colour colourless _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.52 _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 5704 _exptl_absorpt_coefficient_mu 2.969 # Sheldrick geometric approximatio 0.86 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.8595 _exptl_absorpt_correction_T_max 0.8750 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 30652 _reflns_number_total 14342 _diffrn_reflns_av_R_equivalents 0.191 # Number of reflections with Friedels Law is 14342 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 18694 _diffrn_reflns_theta_min 1.293 _diffrn_reflns_theta_max 27.865 _diffrn_measured_fraction_theta_max 0.764 _diffrn_reflns_theta_full 25.078 _diffrn_measured_fraction_theta_full 0.879 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _reflns_limit_h_min 0 _reflns_limit_h_max 23 _reflns_limit_k_min 0 _reflns_limit_k_max 33 _reflns_limit_l_min 0 _reflns_limit_l_max 37 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.48 _refine_diff_density_max 1.48 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 3856 _refine_ls_number_restraints 0 _refine_ls_number_parameters 439 _oxford_refine_ls_R_factor_ref 0.1360 _refine_ls_wR_factor_ref 0.1003 _refine_ls_goodness_of_fit_ref 1.1535 _refine_ls_shift/su_max 0.006718 # The values computed from all data _oxford_reflns_number_all 14289 _refine_ls_R_factor_all 0.3407 _refine_ls_wR_factor_all 0.1887 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3856 _refine_ls_R_factor_gt 0.1360 _refine_ls_wR_factor_gt 0.1003 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.65 0.457 1.34 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Y1 Y -0.02358(12) 0.18989(7) 0.08157(7) 0.0458 1.0000 Uani . . . . . . . Y2 Y 0.08245(11) 0.27971(7) 0.18251(7) 0.0456 1.0000 Uani . . . . . . . Y3 Y 0.08894(13) 0.14371(7) 0.17406(7) 0.0529 1.0000 Uani . . . . . . . Y4 Y 0.17758(12) 0.21966(8) 0.08953(7) 0.0517 1.0000 Uani . . . . . . . O11 O 0.0000 0.2500 0.1330(5) 0.0406 1.0000 Uani S T . . . . . O21 O -0.1363(7) 0.2053(4) 0.1119(4) 0.0454 1.0000 Uani . . . . . . . O22 O -0.0351(7) 0.2947(4) 0.2111(4) 0.0459 1.0000 Uani . . . . . . . O23 O 0.0722(8) 0.2383(4) 0.0514(4) 0.0477 1.0000 Uani . . . . . . . O24 O 0.1567(6) 0.2128(4) 0.1652(4) 0.0474 1.0000 Uani . . . . . . . O25 O 0.0932(8) 0.1565(4) 0.1008(4) 0.0452 1.0000 Uani . . . . . . . O26 O 0.0321(7) 0.3485(4) 0.1519(4) 0.0467 1.0000 Uani . . . . . . . O31 O -0.1502(9) 0.3712(6) 0.2349(5) 0.0726 1.0000 Uani . . . . . . . C32 C -0.1447(15) 0.4041(10) 0.2626(10) 0.0812 1.0000 Uani . . . . . . . C33 C -0.208(3) 0.4012(16) 0.2942(14) 0.148(7) 1.0000 Uiso . . . . . . . C34 C -0.274(2) 0.4008(14) 0.2778(13) 0.148(7) 1.0000 Uiso . . . . . . . C35 C -0.202(2) 0.3521(14) 0.3177(13) 0.148(7) 1.0000 Uiso . . . . . . . C36 C -0.215(2) 0.4383(14) 0.3261(13) 0.148(7) 1.0000 Uiso . . . . . . . C37 C -0.0954(15) 0.4381(8) 0.2640(8) 0.0665 1.0000 Uani . . . . . . . C38 C -0.0433(14) 0.4488(9) 0.2345(11) 0.0742 1.0000 Uani . . . . . . . C39 C 0.016(2) 0.4868(14) 0.2428(12) 0.133(6) 1.0000 Uiso . . . . . . . C40 C 0.090(2) 0.4655(13) 0.2336(11) 0.133(6) 1.0000 Uiso . . . . . . . C41 C 0.018(2) 0.5134(13) 0.2846(12) 0.133(6) 1.0000 Uiso . . . . . . . C42 C 0.002(2) 0.5212(13) 0.2126(12) 0.133(6) 1.0000 Uiso . . . . . . . O43 O -0.0386(10) 0.4234(6) 0.2004(7) 0.0880 1.0000 Uani . . . . . . . O44 O 0.0676(8) 0.3877(5) 0.0737(5) 0.0620 1.0000 Uani . . . . . . . C45 C 0.0878(17) 0.4133(8) 0.0417(13) 0.0920 1.0000 Uani . . . . . . . C46 C 0.116(3) 0.463(2) 0.0616(18) 0.210(11) 1.0000 Uiso . . . . . . . C47 C 0.041(3) 0.4879(19) 0.0802(17) 0.210(11) 1.0000 Uiso . . . . . . . C48 C 0.177(3) 0.4615(19) 0.0813(18) 0.210(11) 1.0000 Uiso . . . . . . . C49 C 0.110(3) 0.500(2) 0.0278(18) 0.210(11) 1.0000 Uiso . . . . . . . C50 C 0.085(2) 0.4000(10) 0.0016(10) 0.1023 1.0000 Uani . . . . . . . C51 C 0.0582(15) 0.3584(10) -0.0126(10) 0.0855 1.0000 Uani . . . . . . . C52 C 0.064(2) 0.3437(15) -0.0603(14) 0.141(7) 1.0000 Uiso . . . . . . . C53 C 0.110(2) 0.3798(13) -0.0930(12) 0.141(7) 1.0000 Uiso . . . . . . . C54 C 0.098(2) 0.2962(14) -0.0632(12) 0.141(7) 1.0000 Uiso . . . . . . . C55 C -0.013(2) 0.3402(13) -0.0781(12) 0.141(7) 1.0000 Uiso . . . . . . . O56 O 0.0327(9) 0.3263(5) 0.0085(5) 0.0625 1.0000 Uani . . . . . . . O57 O 0.2601(8) 0.2715(5) 0.0583(6) 0.0744 1.0000 Uani . . . . . . . C58 C 0.2952(13) 0.2690(9) 0.0251(8) 0.0632 1.0000 Uani . . . . . . . C59 C 0.341(3) 0.3145(19) 0.0157(18) 0.180(9) 1.0000 Uiso . . . . . . . C60 C 0.361(3) 0.3417(17) 0.0551(16) 0.180(9) 1.0000 Uiso . . . . . . . C61 C 0.410(3) 0.3069(17) -0.0069(16) 0.180(9) 1.0000 Uiso . . . . . . . C62 C 0.303(3) 0.3448(17) -0.0109(16) 0.180(9) 1.0000 Uiso . . . . . . . C63 C 0.3033(15) 0.2307(12) -0.0035(8) 0.0915 1.0000 Uani . . . . . . . C64 C 0.2591(18) 0.1852(9) 0.0048(9) 0.0718 1.0000 Uani . . . . . . . C65 C 0.275(2) 0.1447(15) -0.0295(14) 0.149(7) 1.0000 Uiso . . . . . . . C66 C 0.211(2) 0.1344(14) -0.0540(13) 0.149(7) 1.0000 Uiso . . . . . . . C67 C 0.345(2) 0.1538(14) -0.0572(13) 0.149(7) 1.0000 Uiso . . . . . . . C68 C 0.288(2) 0.0994(14) -0.0015(14) 0.149(7) 1.0000 Uiso . . . . . . . O69 O 0.2142(10) 0.1807(6) 0.0307(5) 0.0754 1.0000 Uani . . . . . . . O70 O 0.0990(10) 0.2918(6) 0.2548(6) 0.0765 1.0000 Uani . . . . . . . C71 C 0.1383(17) 0.3172(8) 0.2770(8) 0.0679 1.0000 Uani . . . . . . . C72 C 0.124(2) 0.3191(16) 0.3226(15) 0.152(7) 1.0000 Uiso . . . . . . . C73 C 0.120(2) 0.2765(15) 0.3429(13) 0.152(7) 1.0000 Uiso . . . . . . . C74 C 0.165(2) 0.3562(14) 0.3508(13) 0.152(7) 1.0000 Uiso . . . . . . . C75 C 0.044(2) 0.3326(15) 0.3270(13) 0.152(7) 1.0000 Uiso . . . . . . . C76 C 0.1997(13) 0.3431(8) 0.2640(8) 0.0635 1.0000 Uani . . . . . . . C77 C 0.2235(14) 0.3412(8) 0.2188(8) 0.0635 1.0000 Uani . . . . . . . C78 C 0.297(3) 0.367(2) 0.2056(18) 0.194(10) 1.0000 Uiso . . . . . . . C79 C 0.273(3) 0.4126(19) 0.1866(16) 0.194(10) 1.0000 Uiso . . . . . . . C80 C 0.342(3) 0.3296(18) 0.1788(17) 0.194(10) 1.0000 Uiso . . . . . . . C81 C 0.342(3) 0.3713(18) 0.2416(17) 0.194(10) 1.0000 Uiso . . . . . . . O82 O 0.1870(9) 0.3235(6) 0.1912(5) 0.0769 1.0000 Uani . . . . . . . O83 O 0.2724(8) 0.1775(5) 0.1197(5) 0.0643 1.0000 Uani . . . . . . . C84 C 0.3197(12) 0.1458(11) 0.1256(9) 0.0744 1.0000 Uani . . . . . . . C85 C 0.397(2) 0.1652(13) 0.1316(12) 0.1200 1.0000 Uiso . . . . . . . C86 C 0.4541(19) 0.1270(13) 0.1286(11) 0.1200 1.0000 Uiso . . . . . . . C87 C 0.4168(18) 0.1956(12) 0.0931(11) 0.1200 1.0000 Uiso . . . . . . . C88 C 0.3963(19) 0.2152(12) 0.1567(11) 0.1200 1.0000 Uiso . . . . . . . C89 C 0.3062(15) 0.0958(9) 0.1298(8) 0.0666 1.0000 Uani . . . . . . . C90 C 0.2377(17) 0.0769(8) 0.1365(8) 0.0609 1.0000 Uani . . . . . . . C91 C 0.227(3) 0.0215(17) 0.1318(16) 0.170(8) 1.0000 Uiso . . . . . . . C92 C 0.283(3) -0.0029(15) 0.1054(15) 0.170(8) 1.0000 Uiso . . . . . . . C93 C 0.156(3) 0.0099(15) 0.1077(14) 0.170(8) 1.0000 Uiso . . . . . . . C94 C 0.212(2) -0.0015(15) 0.1705(15) 0.170(8) 1.0000 Uiso . . . . . . . O95 O 0.1795(10) 0.0974(5) 0.1465(5) 0.0737 1.0000 Uani . . . . . . . H91 H -0.0374 0.2977 0.2440 0.0517 1.0000 Uiso . . . . . . . H71 H -0.1734 0.1784 0.1104 0.0561 1.0000 Uiso . . . . . . . H101 H 0.0776 0.2384 0.0191 0.0628 1.0000 Uiso . . . . . . . H81 H 0.1049 0.1264 0.0837 0.0575 1.0000 Uiso . . . . . . . H61 H 0.2043 0.2125 0.1815 0.0522 1.0000 Uiso . . . . . . . H111 H 0.0622 0.3783 0.1536 0.0524 1.0000 Uiso . . . . . . . H341 H -0.3226 0.4013 0.2914 0.1663 1.0000 Uiso . . . . . . . H342 H -0.2797 0.4078 0.2423 0.1663 1.0000 Uiso . . . . . . . H351 H -0.2439 0.3476 0.3383 0.1663 1.0000 Uiso . . . . . . . H352 H -0.1549 0.3502 0.3330 0.1663 1.0000 Uiso . . . . . . . H353 H -0.2045 0.3239 0.2963 0.1663 1.0000 Uiso . . . . . . . H361 H -0.2570 0.4350 0.3462 0.1663 1.0000 Uiso . . . . . . . H362 H -0.2188 0.4725 0.3125 0.1663 1.0000 Uiso . . . . . . . H363 H -0.1678 0.4402 0.3445 0.1663 1.0000 Uiso . . . . . . . H371 H -0.0988 0.4599 0.2911 0.0898 1.0000 Uiso . . . . . . . H401 H 0.1323 0.4870 0.2373 0.1590 1.0000 Uiso . . . . . . . H402 H 0.0990 0.4355 0.2541 0.1590 1.0000 Uiso . . . . . . . H403 H 0.0935 0.4499 0.2035 0.1590 1.0000 Uiso . . . . . . . H411 H 0.0589 0.5380 0.2871 0.1590 1.0000 Uiso . . . . . . . H412 H -0.0294 0.5301 0.2919 0.1590 1.0000 Uiso . . . . . . . H413 H 0.0272 0.4889 0.3096 0.1590 1.0000 Uiso . . . . . . . H421 H 0.0375 0.5512 0.2130 0.1590 1.0000 Uiso . . . . . . . H422 H -0.0496 0.5378 0.2156 0.1590 1.0000 Uiso . . . . . . . H423 H 0.0032 0.5102 0.1812 0.1590 1.0000 Uiso . . . . . . . H471 H 0.0525 0.5208 0.0930 0.2341 1.0000 Uiso . . . . . . . H472 H 0.0025 0.4928 0.0575 0.2341 1.0000 Uiso . . . . . . . H473 H 0.0200 0.4669 0.1033 0.2341 1.0000 Uiso . . . . . . . H481 H 0.2040 0.4915 0.0957 0.2341 1.0000 Uiso . . . . . . . H482 H 0.2084 0.4299 0.0857 0.2341 1.0000 Uiso . . . . . . . H491 H 0.1277 0.5335 0.0377 0.2341 1.0000 Uiso . . . . . . . H492 H 0.0590 0.5050 0.0155 0.2341 1.0000 Uiso . . . . . . . H493 H 0.1430 0.4919 0.0016 0.2341 1.0000 Uiso . . . . . . . H501 H 0.1028 0.4245 -0.0211 0.1101 1.0000 Uiso . . . . . . . H531 H 0.1147 0.3670 -0.1222 0.1652 1.0000 Uiso . . . . . . . H532 H 0.0940 0.4133 -0.0920 0.1652 1.0000 Uiso . . . . . . . H533 H 0.1665 0.3807 -0.0814 0.1652 1.0000 Uiso . . . . . . . H541 H 0.1059 0.2846 -0.0946 0.1652 1.0000 Uiso . . . . . . . H542 H 0.1509 0.2959 -0.0506 0.1652 1.0000 Uiso . . . . . . . H543 H 0.0706 0.2699 -0.0484 0.1652 1.0000 Uiso . . . . . . . H551 H -0.0181 0.3314 -0.1086 0.1652 1.0000 Uiso . . . . . . . H552 H -0.0427 0.3723 -0.0737 0.1652 1.0000 Uiso . . . . . . . H553 H -0.0445 0.3150 -0.0608 0.1652 1.0000 Uiso . . . . . . . H601 H 0.3894 0.3728 0.0480 0.2034 1.0000 Uiso . . . . . . . H602 H 0.3910 0.3224 0.0753 0.2034 1.0000 Uiso . . . . . . . H603 H 0.3147 0.3529 0.0708 0.2034 1.0000 Uiso . . . . . . . H611 H 0.4417 0.3364 -0.0125 0.2034 1.0000 Uiso . . . . . . . H612 H 0.4461 0.2829 0.0095 0.2034 1.0000 Uiso . . . . . . . H613 H 0.4040 0.2900 -0.0361 0.2034 1.0000 Uiso . . . . . . . H621 H 0.3244 0.3757 -0.0201 0.2034 1.0000 Uiso . . . . . . . H622 H 0.2495 0.3523 -0.0003 0.2034 1.0000 Uiso . . . . . . . H623 H 0.2900 0.3264 -0.0408 0.2034 1.0000 Uiso . . . . . . . H631 H 0.3374 0.2326 -0.0294 0.1037 1.0000 Uiso . . . . . . . H661 H 0.2192 0.1087 -0.0760 0.1747 1.0000 Uiso . . . . . . . H662 H 0.1930 0.1646 -0.0689 0.1747 1.0000 Uiso . . . . . . . H663 H 0.1700 0.1230 -0.0343 0.1747 1.0000 Uiso . . . . . . . H671 H 0.3522 0.1257 -0.0789 0.1747 1.0000 Uiso . . . . . . . H672 H 0.3905 0.1559 -0.0399 0.1747 1.0000 Uiso . . . . . . . H673 H 0.3394 0.1841 -0.0748 0.1747 1.0000 Uiso . . . . . . . H681 H 0.3001 0.0693 -0.0195 0.1747 1.0000 Uiso . . . . . . . H682 H 0.3303 0.1036 0.0192 0.1747 1.0000 Uiso . . . . . . . H683 H 0.2430 0.0911 0.0157 0.1747 1.0000 Uiso . . . . . . . H731 H 0.1133 0.2687 0.3741 0.1819 1.0000 Uiso . . . . . . . H732 H 0.1316 0.2442 0.3242 0.1819 1.0000 Uiso . . . . . . . H741 H 0.1497 0.3578 0.3820 0.1819 1.0000 Uiso . . . . . . . H742 H 0.1526 0.3924 0.3397 0.1819 1.0000 Uiso . . . . . . . H743 H 0.2187 0.3538 0.3489 0.1819 1.0000 Uiso . . . . . . . H751 H 0.0255 0.3374 0.3579 0.1819 1.0000 Uiso . . . . . . . H752 H 0.0333 0.3660 0.3125 0.1819 1.0000 Uiso . . . . . . . H753 H 0.0098 0.3090 0.3131 0.1819 1.0000 Uiso . . . . . . . H761 H 0.2262 0.3619 0.2885 0.0916 1.0000 Uiso . . . . . . . H791 H 0.3154 0.4325 0.1773 0.2374 1.0000 Uiso . . . . . . . H792 H 0.2451 0.4333 0.2097 0.2374 1.0000 Uiso . . . . . . . H793 H 0.2381 0.4077 0.1628 0.2374 1.0000 Uiso . . . . . . . H801 H 0.3887 0.3477 0.1717 0.2374 1.0000 Uiso . . . . . . . H802 H 0.3542 0.3026 0.1988 0.2374 1.0000 Uiso . . . . . . . H803 H 0.3144 0.3208 0.1549 0.2374 1.0000 Uiso . . . . . . . H811 H 0.3936 0.3895 0.2359 0.2374 1.0000 Uiso . . . . . . . H812 H 0.3222 0.3941 0.2671 0.2374 1.0000 Uiso . . . . . . . H813 H 0.3587 0.3411 0.2580 0.2374 1.0000 Uiso . . . . . . . H861 H 0.5058 0.1400 0.1441 0.2714 1.0000 Uiso . . . . . . . H862 H 0.4413 0.0939 0.1443 0.2714 1.0000 Uiso . . . . . . . H871 H 0.4689 0.2078 0.0955 0.2714 1.0000 Uiso . . . . . . . H872 H 0.3832 0.2248 0.0928 0.2714 1.0000 Uiso . . . . . . . H873 H 0.4114 0.1781 0.0653 0.2714 1.0000 Uiso . . . . . . . H881 H 0.4561 0.2223 0.1613 0.2714 1.0000 Uiso . . . . . . . H882 H 0.3824 0.2067 0.1875 0.2714 1.0000 Uiso . . . . . . . H883 H 0.3755 0.2386 0.1437 0.2714 1.0000 Uiso . . . . . . . H891 H 0.3530 0.0741 0.1305 0.0857 1.0000 Uiso . . . . . . . H921 H 0.2778 -0.0398 0.1014 0.1985 1.0000 Uiso . . . . . . . H922 H 0.3370 0.0016 0.1154 0.1985 1.0000 Uiso . . . . . . . H923 H 0.2846 0.0101 0.0737 0.1985 1.0000 Uiso . . . . . . . H931 H 0.1474 -0.0227 0.1010 0.1985 1.0000 Uiso . . . . . . . H932 H 0.1144 0.0282 0.1194 0.1985 1.0000 Uiso . . . . . . . H933 H 0.1640 0.0279 0.0759 0.1985 1.0000 Uiso . . . . . . . H941 H 0.2067 -0.0359 0.1721 0.1985 1.0000 Uiso . . . . . . . H942 H 0.2566 0.0068 0.1936 0.1985 1.0000 Uiso . . . . . . . H943 H 0.1687 0.0151 0.1866 0.1985 1.0000 Uiso . . . . . . . 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 Y1 0.0554(14) 0.0378(11) 0.0442(13) -0.0038(11) -0.0023(12) -0.0122(12) Y2 0.0453(12) 0.0431(13) 0.0484(14) -0.0056(12) -0.0045(12) -0.0073(12) Y3 0.0559(15) 0.0477(13) 0.0551(16) 0.0080(12) -0.0030(13) -0.0015(12) Y4 0.0534(13) 0.0484(13) 0.0534(16) -0.0060(13) 0.0083(12) -0.0054(12) O11 0.073(15) 0.028(10) 0.021(11) 0.0000 0.0000 -0.022(9) O21 0.031(8) 0.041(9) 0.065(10) 0.002(7) 0.001(7) -0.021(6) O22 0.054(9) 0.041(8) 0.043(9) -0.019(6) 0.006(7) 0.009(7) O23 0.069(11) 0.040(8) 0.034(8) -0.008(6) 0.007(8) -0.008(7) O24 0.038(7) 0.038(7) 0.067(10) -0.009(7) -0.025(7) 0.013(7) O25 0.056(9) 0.026(7) 0.054(9) -0.004(6) 0.005(8) -0.011(7) O26 0.046(9) 0.013(7) 0.082(11) -0.008(6) 0.008(8) -0.001(6) O31 0.100(14) 0.064(11) 0.053(11) -0.017(9) 0.016(10) 0.002(10) C32 0.07(2) 0.051(17) 0.12(3) 0.020(18) 0.070(19) 0.018(15) C37 0.07(2) 0.067(16) 0.058(18) -0.008(13) -0.020(15) -0.046(17) C38 0.056(19) 0.052(16) 0.12(3) 0.003(18) -0.021(18) 0.001(14) O43 0.084(14) 0.053(11) 0.127(17) -0.042(11) 0.015(12) -0.014(9) O44 0.084(12) 0.057(10) 0.045(10) 0.021(8) 0.009(9) -0.031(8) C45 0.10(2) 0.027(14) 0.15(3) -0.015(18) 0.00(3) -0.015(15) C50 0.19(3) 0.053(19) 0.06(2) 0.006(15) 0.09(2) -0.02(2) C51 0.10(2) 0.033(16) 0.12(3) 0.017(18) 0.014(19) -0.006(14) O56 0.092(12) 0.028(9) 0.068(11) 0.018(7) 0.006(10) -0.015(8) O57 0.062(11) 0.064(11) 0.097(14) 0.011(9) 0.041(10) -0.025(9) C58 0.055(15) 0.09(2) 0.047(16) 0.002(15) 0.037(13) -0.027(14) C63 0.10(2) 0.15(3) 0.029(16) -0.006(18) 0.014(15) 0.03(2) C64 0.11(2) 0.063(18) 0.047(18) -0.012(15) -0.010(17) -0.010(18) O69 0.087(13) 0.099(14) 0.040(11) -0.029(10) 0.041(10) -0.038(11) O70 0.083(13) 0.082(11) 0.064(12) -0.020(10) -0.008(10) -0.010(11) C71 0.13(2) 0.046(16) 0.028(15) 0.021(12) 0.005(16) 0.004(16) C76 0.063(4) 0.063(4) 0.063(4) 0.013(4) 0.013(4) 0.013(4) C77 0.063(4) 0.063(4) 0.063(4) 0.013(4) 0.013(4) 0.013(4) O82 0.069(11) 0.096(12) 0.066(11) 0.001(9) -0.030(9) -0.057(10) O83 0.034(9) 0.056(10) 0.103(14) 0.006(9) 0.015(9) 0.017(8) C84 0.022(14) 0.10(2) 0.10(2) -0.017(18) 0.013(14) 0.001(16) C89 0.07(2) 0.052(17) 0.074(19) -0.024(14) 0.008(16) 0.020(15) C90 0.08(2) 0.034(14) 0.066(18) 0.014(12) -0.016(16) 0.014(15) O95 0.076(12) 0.050(10) 0.094(14) 0.002(9) 0.012(10) 0.040(10) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.04364(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Y1 . O26 7_555 2.446(13) yes Y1 . O23 7_555 2.369(12) yes Y1 . O56 7_555 2.336(15) yes Y1 . O44 7_555 2.301(15) yes Y1 . O11 . 2.351(11) yes Y1 . O21 . 2.304(13) yes Y1 . O23 . 2.393(13) yes Y1 . O25 . 2.397(14) yes Y2 . O21 7_555 2.451(13) yes Y2 . O22 7_555 2.401(12) yes Y2 . O11 . 2.309(11) yes Y2 . O22 . 2.359(13) yes Y2 . O24 . 2.354(12) yes Y2 . O26 . 2.316(12) yes Y2 . O70 . 2.306(18) yes Y2 . O82 . 2.274(14) yes Y3 . O26 7_555 2.323(13) yes Y3 . O22 7_555 2.280(13) yes Y3 . O31 7_555 2.245(16) yes Y3 . O43 7_555 2.225(16) yes Y3 . O24 . 2.290(13) yes Y3 . O25 . 2.318(13) yes Y3 . O95 . 2.259(16) yes Y4 . O21 7_555 2.312(12) yes Y4 . O23 . 2.319(14) yes Y4 . O24 . 2.404(14) yes Y4 . O25 . 2.352(12) yes Y4 . O57 . 2.295(14) yes Y4 . O69 . 2.234(15) yes Y4 . O83 . 2.288(16) yes O21 . H71 . 1.007 no O22 . H91 . 1.033 no O23 . H101 . 1.015 no O24 . H61 . 1.007 no O25 . H81 . 1.012 no O26 . H111 . 0.993 no O31 . C32 . 1.26(3) yes C32 . C33 . 1.52(4) yes C32 . C37 . 1.30(3) yes C33 . C34 . 1.31(5) yes C33 . C35 . 1.55(5) yes C33 . C36 . 1.43(5) yes C34 . H341 . 0.989 no C34 . H342 . 1.132 no C35 . H351 . 1.012 no C35 . H352 . 0.981 no C35 . H353 . 1.027 no C36 . H361 . 0.996 no C36 . H362 . 1.040 no C36 . H363 . 1.036 no C37 . C38 . 1.36(3) yes C37 . H371 . 1.042 no C38 . C39 . 1.53(4) yes C38 . O43 . 1.28(3) yes C39 . C40 . 1.50(4) yes C39 . C41 . 1.50(4) yes C39 . C42 . 1.36(4) yes C40 . H401 . 0.987 no C40 . H402 . 1.062 no C40 . H403 . 1.037 no C41 . H411 . 1.017 no C41 . H412 . 1.001 no C41 . H413 . 1.050 no C42 . H421 . 1.052 no C42 . H422 . 1.051 no C42 . H423 . 1.029 no O44 . C45 . 1.28(3) yes C45 . C46 . 1.59(6) yes C45 . C50 . 1.31(4) yes C46 . C47 . 1.63(6) yes C46 . C48 . 1.27(6) yes C46 . C49 . 1.47(6) yes C47 . H471 . 1.013 no C47 . H472 . 1.014 no C47 . H473 . 1.004 no C48 . H481 . 1.068 no C48 . H482 . 1.057 no C49 . H491 . 1.029 no C49 . H492 . 1.014 no C49 . H493 . 1.043 no C50 . C51 . 1.33(4) yes C50 . H501 . 1.030 no C51 . C52 . 1.55(4) yes C51 . O56 . 1.20(3) yes C52 . C53 . 1.66(5) yes C52 . C54 . 1.45(5) yes C52 . C55 . 1.51(5) yes C53 . H531 . 0.982 no C53 . H532 . 0.973 no C53 . H533 . 1.089 no C54 . H541 . 1.042 no C54 . H542 . 1.039 no C54 . H543 . 0.998 no C55 . H551 . 0.989 no C55 . H552 . 1.052 no C55 . H553 . 1.054 no O57 . C58 . 1.22(2) yes C58 . C59 . 1.53(5) yes C58 . C63 . 1.39(3) yes C59 . C60 . 1.49(6) yes C59 . C61 . 1.47(5) yes C59 . C62 . 1.36(5) yes C60 . H601 . 1.027 no C60 . H602 . 0.994 no C60 . H603 . 1.023 no C61 . H611 . 1.012 no C61 . H612 . 1.062 no C61 . H613 . 1.033 no C62 . H621 . 0.980 no C62 . H622 . 1.055 no C62 . H623 . 1.090 no C63 . C64 . 1.52(4) yes C63 . H631 . 1.025 no C64 . C65 . 1.58(4) yes C64 . O69 . 1.16(3) yes C65 . C66 . 1.43(5) yes C65 . C67 . 1.55(5) yes C65 . C68 . 1.54(5) yes C66 . H661 . 1.002 no C66 . H662 . 1.010 no C66 . H663 . 1.022 no C67 . H671 . 1.037 no C67 . H672 . 0.994 no C67 . H673 . 1.007 no C68 . H681 . 1.028 no C68 . H682 . 1.014 no C68 . H683 . 1.009 no O70 . C71 . 1.22(3) yes C71 . C72 . 1.45(5) yes C71 . C76 . 1.39(3) yes C72 . C73 . 1.34(5) yes C72 . C74 . 1.54(5) yes C72 . C75 . 1.52(5) yes C73 . H731 . 1.006 no C73 . H732 . 1.090 no C74 . H741 . 1.016 no C74 . H742 . 1.079 no C74 . H743 . 0.989 no C75 . H751 . 1.034 no C75 . H752 . 1.045 no C75 . H753 . 1.002 no C76 . C77 . 1.48(3) yes C76 . H761 . 1.046 no C77 . C78 . 1.59(5) yes C77 . O82 . 1.19(3) yes C78 . C79 . 1.45(6) yes C78 . C80 . 1.57(6) yes C78 . C81 . 1.39(6) yes C79 . H791 . 0.995 no C79 . H792 . 1.050 no C79 . H793 . 0.988 no C80 . H801 . 1.012 no C80 . H802 . 0.996 no C80 . H803 . 0.936 no C81 . H811 . 1.077 no C81 . H812 . 1.080 no C81 . H813 . 1.024 no O83 . C84 . 1.24(3) yes C84 . C85 . 1.52(4) yes C84 . C89 . 1.41(3) yes C85 . C86 . 1.49(4) yes C85 . C87 . 1.51(4) yes C85 . C88 . 1.59(4) yes C86 . H861 . 1.119 no C86 . H862 . 1.064 no C87 . H871 . 1.011 no C87 . H872 . 1.011 no C87 . H873 . 1.000 no C88 . H881 . 1.117 no C88 . H882 . 1.023 no C88 . H883 . 0.854 no C89 . C90 . 1.37(3) yes C89 . H891 . 1.044 no C90 . C91 . 1.55(5) yes C90 . O95 . 1.24(3) yes C91 . C92 . 1.48(5) yes C91 . C93 . 1.53(5) yes C91 . C94 . 1.39(5) yes C92 . H921 . 1.032 no C92 . H922 . 1.037 no C92 . H923 . 1.054 no C93 . H931 . 0.938 no C93 . H932 . 0.980 no C93 . H933 . 1.121 no C94 . H941 . 0.956 no C94 . H942 . 1.105 no C94 . H943 . 1.048 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O26 7_555 Y1 . O23 7_555 134.2(4) yes O26 7_555 Y1 . O56 7_555 142.4(4) yes O23 7_555 Y1 . O56 7_555 75.2(5) yes O26 7_555 Y1 . O44 7_555 70.8(5) yes O23 7_555 Y1 . O44 7_555 127.3(5) yes O56 7_555 Y1 . O44 7_555 72.0(5) yes O26 7_555 Y1 . O11 . 72.7(4) yes O23 7_555 Y1 . O11 . 75.5(4) yes O56 7_555 Y1 . O11 . 144.9(5) yes O44 7_555 Y1 . O11 . 142.6(5) yes O26 7_555 Y1 . O21 . 69.7(4) yes O23 7_555 Y1 . O21 . 71.0(5) yes O56 7_555 Y1 . O21 . 112.0(5) yes O44 7_555 Y1 . O21 . 84.6(5) yes O11 . Y1 . O21 . 75.6(3) yes O26 7_555 Y1 . O23 . 130.0(4) yes O23 7_555 Y1 . O23 . 69.4(6) yes O56 7_555 Y1 . O23 . 76.9(5) yes O44 7_555 Y1 . O23 . 137.0(5) yes O11 . Y1 . O23 . 75.1(4) yes O26 7_555 Y1 . O25 . 70.4(4) yes O23 7_555 Y1 . O25 . 139.0(4) yes O56 7_555 Y1 . O25 . 103.6(5) yes O44 7_555 Y1 . O25 . 88.8(5) yes O11 . Y1 . O25 . 86.4(3) yes O21 . Y1 . O23 . 135.3(4) yes O21 . Y1 . O25 . 139.5(5) yes O23 . Y1 . O25 . 70.4(4) yes O21 7_555 Y2 . O22 7_555 128.6(4) yes O21 7_555 Y2 . O11 . 73.6(4) yes O22 7_555 Y2 . O11 . 73.2(4) yes O21 7_555 Y2 . O22 . 132.5(4) yes O22 7_555 Y2 . O22 . 71.5(5) yes O11 . Y2 . O22 . 74.0(4) yes O21 7_555 Y2 . O24 . 72.2(4) yes O22 7_555 Y2 . O24 . 67.7(5) yes O11 . Y2 . O24 . 86.7(3) yes O22 . Y2 . O24 . 138.4(4) yes O21 7_555 Y2 . O26 . 69.4(4) yes O22 7_555 Y2 . O26 . 135.4(4) yes O11 . Y2 . O26 . 75.9(3) yes O22 . Y2 . O26 . 69.6(4) yes O24 . Y2 . O26 . 141.0(5) yes O21 7_555 Y2 . O70 . 143.8(5) yes O22 7_555 Y2 . O70 . 78.8(5) yes O11 . Y2 . O70 . 142.6(5) yes O22 . Y2 . O70 . 73.8(5) yes O24 . Y2 . O70 . 105.3(5) yes O21 7_555 Y2 . O82 . 71.5(5) yes O22 7_555 Y2 . O82 . 135.4(5) yes O11 . Y2 . O82 . 144.6(5) yes O22 . Y2 . O82 . 128.5(5) yes O24 . Y2 . O82 . 87.9(5) yes O26 . Y2 . O70 . 109.8(5) yes O26 . Y2 . O82 . 86.9(5) yes O70 . Y2 . O82 . 72.3(6) yes O26 7_555 Y3 . O22 7_555 70.9(5) yes O26 7_555 Y3 . O31 7_555 138.0(6) yes O22 7_555 Y3 . O31 7_555 85.4(5) yes O26 7_555 Y3 . O43 7_555 78.3(5) yes O22 7_555 Y3 . O43 7_555 104.8(6) yes O31 7_555 Y3 . O43 7_555 74.8(6) yes O26 7_555 Y3 . O24 . 113.5(4) yes O22 7_555 Y3 . O24 . 70.9(5) yes O31 7_555 Y3 . O24 . 89.2(5) yes O43 7_555 Y3 . O24 . 163.9(6) yes O26 7_555 Y3 . O25 . 73.9(5) yes O22 7_555 Y3 . O25 . 113.7(4) yes O31 7_555 Y3 . O25 . 148.1(6) yes O43 7_555 Y3 . O25 . 120.5(6) yes O24 . Y3 . O25 . 74.6(4) yes O26 7_555 Y3 . O95 . 129.3(6) yes O22 7_555 Y3 . O95 . 158.5(6) yes O31 7_555 Y3 . O95 . 81.7(6) yes O43 7_555 Y3 . O95 . 88.4(6) yes O24 . Y3 . O95 . 91.8(5) yes O25 . Y3 . O95 . 71.6(5) yes O21 7_555 Y4 . O23 . 71.8(4) yes O21 7_555 Y4 . O24 . 73.8(4) yes O23 . Y4 . O24 . 113.1(4) yes O21 7_555 Y4 . O25 . 113.9(4) yes O23 . Y4 . O25 . 72.5(5) yes O24 . Y4 . O25 . 71.9(4) yes O21 7_555 Y4 . O57 . 77.5(5) yes O23 . Y4 . O57 . 100.7(5) yes O24 . Y4 . O57 . 124.9(5) yes O25 . Y4 . O57 . 162.8(5) yes O21 7_555 Y4 . O69 . 141.1(6) yes O23 . Y4 . O69 . 86.0(6) yes O24 . Y4 . O69 . 145.1(6) yes O25 . Y4 . O69 . 87.8(5) yes O57 . Y4 . O69 . 75.8(6) yes O21 7_555 Y4 . O83 . 125.2(5) yes O23 . Y4 . O83 . 162.0(5) yes O24 . Y4 . O83 . 71.0(5) yes O25 . Y4 . O83 . 93.2(5) yes O57 . Y4 . O83 . 89.8(6) yes O69 . Y4 . O83 . 82.4(6) yes Y1 . O11 . Y1 7_555 93.7(6) yes Y1 . O11 . Y2 . 145.97(7) yes Y1 7_555 O11 . Y2 . 95.09(7) yes Y1 . O11 . Y2 7_555 95.09(7) yes Y1 7_555 O11 . Y2 7_555 145.97(7) yes Y2 . O11 . Y2 7_555 95.8(6) yes Y2 7_555 O21 . Y4 7_555 104.6(5) yes Y2 7_555 O21 . Y1 . 92.6(4) yes Y4 7_555 O21 . Y1 . 109.4(5) yes Y2 7_555 O21 . H71 . 115.8 no Y4 7_555 O21 . H71 . 115.5 no Y1 . O21 . H71 . 116.4 no Y2 7_555 O22 . Y2 . 92.0(4) yes Y2 7_555 O22 . Y3 7_555 107.1(5) yes Y2 . O22 . Y3 7_555 109.2(5) yes Y2 7_555 O22 . H91 . 115.2 no Y2 . O22 . H91 . 115.4 no Y3 7_555 O22 . H91 . 115.3 no Y1 . O23 . Y1 7_555 92.1(5) yes Y1 . O23 . Y4 . 106.2(5) yes Y1 7_555 O23 . Y4 . 106.9(5) yes Y1 . O23 . H101 . 117.7 no Y1 7_555 O23 . H101 . 115.5 no Y4 . O23 . H101 . 115.6 no Y4 . O24 . Y2 . 104.8(5) yes Y4 . O24 . Y3 . 105.7(5) yes Y2 . O24 . Y3 . 108.4(5) yes Y4 . O24 . H61 . 111.3 no Y2 . O24 . H61 . 112.8 no Y3 . O24 . H61 . 113.3 no Y1 . O25 . Y4 . 105.0(4) yes Y1 . O25 . Y3 . 106.1(5) yes Y4 . O25 . Y3 . 106.5(5) yes Y1 . O25 . H81 . 111.7 no Y4 . O25 . H81 . 113.1 no Y3 . O25 . H81 . 113.9 no Y1 7_555 O26 . Y3 7_555 104.4(5) yes Y1 7_555 O26 . Y2 . 92.4(4) yes Y3 7_555 O26 . Y2 . 109.3(5) yes Y1 7_555 O26 . H111 . 116.2 no Y3 7_555 O26 . H111 . 115.7 no Y2 . O26 . H111 . 116.1 no Y3 7_555 O31 . C32 . 132.4(15) yes O31 . C32 . C33 . 110(3) yes O31 . C32 . C37 . 127(2) yes C33 . C32 . C37 . 123(3) yes C32 . C33 . C34 . 116(4) yes C32 . C33 . C35 . 107(3) yes C34 . C33 . C35 . 104(4) yes C32 . C33 . C36 . 119(4) yes C34 . C33 . C36 . 101(4) yes C35 . C33 . C36 . 108(4) yes C33 . C34 . H341 . 131.4 no C33 . C34 . H342 . 118.2 no H341 . C34 . H342 . 109.3 no C33 . C35 . H351 . 110.8 no C33 . C35 . H352 . 110.0 no H351 . C35 . H352 . 110.1 no C33 . C35 . H353 . 110.6 no H351 . C35 . H353 . 106.5 no H352 . C35 . H353 . 108.9 no C33 . C36 . H361 . 116.4 no C33 . C36 . H362 . 111.8 no H361 . C36 . H362 . 106.7 no C33 . C36 . H363 . 110.5 no H361 . C36 . H363 . 106.9 no H362 . C36 . H363 . 103.7 no C32 . C37 . C38 . 128(2) yes C32 . C37 . H371 . 113.8 no C38 . C37 . H371 . 118.0 no C37 . C38 . C39 . 122(3) yes C37 . C38 . O43 . 120(2) yes C39 . C38 . O43 . 118(3) yes C38 . C39 . C40 . 109(3) yes C38 . C39 . C41 . 120(3) yes C40 . C39 . C41 . 110(3) yes C38 . C39 . C42 . 103(3) yes C40 . C39 . C42 . 108(3) yes C41 . C39 . C42 . 106(3) yes C39 . C40 . H401 . 116.9 no C39 . C40 . H402 . 109.6 no H401 . C40 . H402 . 105.7 no C39 . C40 . H403 . 113.6 no H401 . C40 . H403 . 107.6 no H402 . C40 . H403 . 102.2 no C39 . C41 . H411 . 114.2 no C39 . C41 . H412 . 114.1 no H411 . C41 . H412 . 108.1 no C39 . C41 . H413 . 109.7 no H411 . C41 . H413 . 104.4 no H412 . C41 . H413 . 105.6 no C39 . C42 . H421 . 115.2 no C39 . C42 . H422 . 113.9 no H421 . C42 . H422 . 101.9 no C39 . C42 . H423 . 117.0 no H421 . C42 . H423 . 103.4 no H422 . C42 . H423 . 103.5 no C38 . O43 . Y3 7_555 137.6(18) yes Y1 7_555 O44 . C45 . 134.4(16) yes O44 . C45 . C46 . 105(3) yes O44 . C45 . C50 . 126(2) yes C46 . C45 . C50 . 129(4) yes C45 . C46 . C47 . 104(4) yes C45 . C46 . C48 . 116(6) yes C47 . C46 . C48 . 125(6) yes C45 . C46 . C49 . 107(5) yes C47 . C46 . C49 . 85(4) yes C48 . C46 . C49 . 116(6) yes C46 . C47 . H471 . 110.7 no C46 . C47 . H472 . 112.8 no H471 . C47 . H472 . 107.3 no C46 . C47 . H473 . 109.8 no H471 . C47 . H473 . 108.1 no H472 . C47 . H473 . 108.0 no C46 . C48 . H481 . 125.8 no C46 . C48 . H482 . 124.9 no H481 . C48 . H482 . 109.2 no C46 . C49 . H491 . 112.7 no C46 . C49 . H492 . 115.8 no H491 . C49 . H492 . 106.1 no C46 . C49 . H493 . 112.1 no H491 . C49 . H493 . 104.0 no H492 . C49 . H493 . 105.1 no C45 . C50 . C51 . 125(2) yes C45 . C50 . H501 . 117.7 no C51 . C50 . H501 . 116.9 no C50 . C51 . C52 . 122(3) yes C50 . C51 . O56 . 127(3) yes C52 . C51 . O56 . 111(3) yes C51 . C52 . C53 . 118(3) yes C51 . C52 . C54 . 109(3) yes C53 . C52 . C54 . 107(3) yes C51 . C52 . C55 . 108(3) yes C53 . C52 . C55 . 106(3) yes C54 . C52 . C55 . 108(3) yes C52 . C53 . H531 . 113.6 no C52 . C53 . H532 . 113.5 no H531 . C53 . H532 . 113.3 no C52 . C53 . H533 . 106.7 no H531 . C53 . H533 . 104.0 no H532 . C53 . H533 . 104.6 no C52 . C54 . H541 . 113.1 no C52 . C54 . H542 . 112.3 no H541 . C54 . H542 . 103.4 no C52 . C54 . H543 . 114.3 no H541 . C54 . H543 . 106.3 no H542 . C54 . H543 . 106.6 no C52 . C55 . H551 . 117.6 no C52 . C55 . H552 . 112.4 no H551 . C55 . H552 . 106.2 no C52 . C55 . H553 . 111.5 no H551 . C55 . H553 . 106.1 no H552 . C55 . H553 . 101.7 no Y1 7_555 O56 . C51 . 135.1(18) yes Y4 . O57 . C58 . 132.0(16) yes O57 . C58 . C59 . 113(3) yes O57 . C58 . C63 . 130(2) yes C59 . C58 . C63 . 116(3) yes C58 . C59 . C60 . 113(4) yes C58 . C59 . C61 . 116(4) yes C60 . C59 . C61 . 105(4) yes C58 . C59 . C62 . 110(4) yes C60 . C59 . C62 . 109(5) yes C61 . C59 . C62 . 103(5) yes C59 . C60 . H601 . 111.6 no C59 . C60 . H602 . 113.2 no H601 . C60 . H602 . 107.8 no C59 . C60 . H603 . 110.1 no H601 . C60 . H603 . 105.6 no H602 . C60 . H603 . 108.1 no C59 . C61 . H611 . 117.1 no C59 . C61 . H612 . 112.9 no H611 . C61 . H612 . 103.9 no C59 . C61 . H613 . 113.1 no H611 . C61 . H613 . 106.0 no H612 . C61 . H613 . 102.4 no C59 . C62 . H621 . 120.9 no C59 . C62 . H622 . 113.1 no H621 . C62 . H622 . 106.7 no C59 . C62 . H623 . 110.4 no H621 . C62 . H623 . 104.1 no H622 . C62 . H623 . 99.2 no C58 . C63 . C64 . 118(2) yes C58 . C63 . H631 . 122.3 no C64 . C63 . H631 . 120.0 no C63 . C64 . C65 . 112(3) yes C63 . C64 . O69 . 126(2) yes C65 . C64 . O69 . 122(3) yes C64 . C65 . C66 . 111(3) yes C64 . C65 . C67 . 115(3) yes C66 . C65 . C67 . 114(4) yes C64 . C65 . C68 . 102(3) yes C66 . C65 . C68 . 105(4) yes C67 . C65 . C68 . 109(3) yes C65 . C66 . H661 . 113.0 no C65 . C66 . H662 . 110.6 no H661 . C66 . H662 . 108.5 no C65 . C66 . H663 . 110.0 no H661 . C66 . H663 . 107.6 no H662 . C66 . H663 . 107.0 no C65 . C67 . H671 . 110.5 no C65 . C67 . H672 . 112.8 no H671 . C67 . H672 . 107.0 no C65 . C67 . H673 . 110.9 no H671 . C67 . H673 . 106.1 no H672 . C67 . H673 . 109.4 no C65 . C68 . H681 . 112.1 no C65 . C68 . H682 . 112.5 no H681 . C68 . H682 . 106.2 no C65 . C68 . H683 . 111.5 no H681 . C68 . H683 . 106.5 no H682 . C68 . H683 . 107.7 no C64 . O69 . Y4 . 137.3(17) yes Y2 . O70 . C71 . 135.9(17) yes O70 . C71 . C72 . 119(3) yes O70 . C71 . C76 . 127(2) yes C72 . C71 . C76 . 114(3) yes C71 . C72 . C73 . 117(4) yes C71 . C72 . C74 . 120(4) yes C73 . C72 . C74 . 110(4) yes C71 . C72 . C75 . 105(4) yes C73 . C72 . C75 . 96(4) yes C74 . C72 . C75 . 104(3) yes C72 . C73 . H731 . 131.1 no C72 . C73 . H732 . 116.9 no H731 . C73 . H732 . 111.4 no C72 . C74 . H741 . 117.0 no C72 . C74 . H742 . 109.6 no H741 . C74 . H742 . 102.4 no C72 . C74 . H743 . 113.4 no H741 . C74 . H743 . 109.1 no H742 . C74 . H743 . 104.2 no C72 . C75 . H751 . 115.5 no C72 . C75 . H752 . 110.9 no H751 . C75 . H752 . 103.5 no C72 . C75 . H753 . 113.6 no H751 . C75 . H753 . 106.6 no H752 . C75 . H753 . 105.8 no C71 . C76 . C77 . 120(2) yes C71 . C76 . H761 . 114.4 no C77 . C76 . H761 . 125.6 no C76 . C77 . C78 . 119(3) yes C76 . C77 . O82 . 123(2) yes C78 . C77 . O82 . 118(3) yes C77 . C78 . C79 . 104(4) yes C77 . C78 . C80 . 106(4) yes C79 . C78 . C80 . 121(5) yes C77 . C78 . C81 . 109(4) yes C79 . C78 . C81 . 116(5) yes C80 . C78 . C81 . 100(4) yes C78 . C79 . H791 . 110.7 no C78 . C79 . H792 . 109.5 no H791 . C79 . H792 . 106.0 no C78 . C79 . H793 . 112.9 no H791 . C79 . H793 . 110.9 no H792 . C79 . H793 . 106.5 no C78 . C80 . H801 . 103.0 no C78 . C80 . H802 . 106.1 no H801 . C80 . H802 . 108.8 no C78 . C80 . H803 . 108.7 no H801 . C80 . H803 . 113.9 no H802 . C80 . H803 . 115.4 no C78 . C81 . H811 . 114.2 no C78 . C81 . H812 . 116.2 no H811 . C81 . H812 . 98.4 no C78 . C81 . H813 . 120.9 no H811 . C81 . H813 . 102.0 no H812 . C81 . H813 . 101.8 no C77 . O82 . Y2 . 140.5(17) yes Y4 . O83 . C84 . 160.7(16) yes O83 . C84 . C85 . 114(3) yes O83 . C84 . C89 . 126(2) yes C85 . C84 . C89 . 120(3) yes C84 . C85 . C86 . 113(3) yes C84 . C85 . C87 . 109(3) yes C86 . C85 . C87 . 100(3) yes C84 . C85 . C88 . 111(3) yes C86 . C85 . C88 . 131(3) yes C87 . C85 . C88 . 85(2) yes C85 . C86 . H861 . 109.8 no C85 . C86 . H862 . 115.2 no H861 . C86 . H862 . 104.9 no C85 . C87 . H871 . 110.6 no C85 . C87 . H872 . 107.5 no H871 . C87 . H872 . 107.7 no C85 . C87 . H873 . 113.6 no H871 . C87 . H873 . 108.6 no H872 . C87 . H873 . 108.6 no C85 . C88 . H881 . 102.2 no C85 . C88 . H882 . 105.5 no H881 . C88 . H882 . 99.4 no C85 . C88 . H883 . 115.2 no H881 . C88 . H883 . 111.2 no H882 . C88 . H883 . 120.8 no C84 . C89 . C90 . 123(2) yes C84 . C89 . H891 . 115.0 no C90 . C89 . H891 . 121.5 no C89 . C90 . C91 . 119(3) yes C89 . C90 . O95 . 130(2) yes C91 . C90 . O95 . 111(3) yes C90 . C91 . C92 . 114(4) yes C90 . C91 . C93 . 111(4) yes C92 . C91 . C93 . 102(4) yes C90 . C91 . C94 . 113(4) yes C92 . C91 . C94 . 114(4) yes C93 . C91 . C94 . 100(4) yes C91 . C92 . H921 . 116.8 no C91 . C92 . H922 . 115.7 no H921 . C92 . H922 . 104.3 no C91 . C92 . H923 . 112.6 no H921 . C92 . H923 . 103.1 no H922 . C92 . H923 . 102.7 no C91 . C93 . H931 . 116.8 no C91 . C93 . H932 . 111.2 no H931 . C93 . H932 . 116.7 no C91 . C93 . H933 . 103.4 no H931 . C93 . H933 . 104.6 no H932 . C93 . H933 . 101.8 no C91 . C94 . H941 . 121.2 no C91 . C94 . H942 . 109.6 no H941 . C94 . H942 . 104.6 no C91 . C94 . H943 . 111.2 no H941 . C94 . H943 . 109.1 no H942 . C94 . H943 . 98.6 no C90 . O95 . Y3 . 167.9(17) yes # Attachment 'New-publication-Tb9.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 711971' _audit_creation_date 06-02-13 _audit_creation_method CRYSTALS_ver_12.82 #_oxford_structure_analysis_title 'import in P 4/n' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 19.0990(7) _cell_length_b 19.0990(7) _cell_length_c 15.5210(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5661.6(4) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 4/n ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -y+1/2,x,z y+1/2,-x,-z -x+1/2,-y+1/2,z x+1/2,y+1/2,-z y,-x+1/2,z -y,x+1/2,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Tb -0.1723 4.1537 25.8976 2.2426 18.2185 0.1961 14.3167 12.6648 2.9535 115.3620 3.5822 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C80 H121 O43 Tb9 # Dc = 1.88 Fooo = 2929.00 Mu = 56.17 M = 800.28 # Found Formula = C80 H122.25 O40.75 Tb8.25 # Dc = 1.88 FOOO = 2929.00 Mu = 56.17 M = 800.79 _chemical_formula_sum 'C80 H123 O43 Tb9' _chemical_formula_moiety 'C80 H123 O43 Tb9' _chemical_compound_source ? _chemical_formula_weight 3203.16 _cell_measurement_reflns_used 5768 _cell_measurement_theta_min 0 _cell_measurement_theta_max 28 _cell_measurement_temperature 290 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_max 0.10 _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2929 _exptl_absorpt_coefficient_mu 5.617 # Sheldrick geometric approximatio 0.60 0.89 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6032 _exptl_absorpt_correction_T_max 0.8937 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 290 _diffrn_reflns_number 11364 _reflns_number_total 6685 _diffrn_reflns_av_R_equivalents 0.036 # Number of reflections with Friedels Law is 6685 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6755 _diffrn_reflns_theta_min 1.691 _diffrn_reflns_theta_max 27.881 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.044 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 20 #_oxford_diffrn_Wilson_B_factor 0.00 #_oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.16 _refine_diff_density_max 1.48 _refine_ls_number_reflns 3372 _refine_ls_number_restraints 0 _refine_ls_number_parameters 300 #_refine_ls_R_factor_ref 0.0444 _refine_ls_wR_factor_ref 0.0523 _refine_ls_goodness_of_fit_ref 1.0698 #_reflns_number_all 6664 _refine_ls_R_factor_all 0.0998 _refine_ls_wR_factor_all 0.1087 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3372 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_gt 0.0523 _refine_ls_shift/su_max 0.000493 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.454 0.306 0.229 ; _publ_section_abstract # Text of the abstract ; ? ; _publ_section_comment # Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures ; ? ; _publ_section_exptl_refinement # Some potentially useful phrases are: ; Because the data were collected with molybdenum radiation, there were no measurable anomalous differences, as a consequence of which it was admissible to merge Friedel pairs of reflections. All hydrogen atoms were found in difference density syntheses. Hydrogen atoms were placed geometrically after each cycle. Hydrogen atoms were placed geometrically after each cycle, the preferred orientations of those groups whose conformations could not be assigned unambiguously having been previously identified by examination of a difference Fourier map. Hydrogen atoms were seen in a difference density synthesis. Those attached to carbon atoms were repositioned geometrically. Hydrogen were initially refined with soft restraints on the bonds to regularise their geometry (bond lengths to accepted values, angles either set by symmetry or to accepted values, and U[iso] dependent upon the adjacent bonded atom), after which they were refined with riding constraints only. donated by Bill Clegg: The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93-98, O---N in the range 0.86-0.89 and O---H = 0.82 \%A) and isotropic adps (U(H) in the range 1.2-1.5 times U~equiv~ of the adjacent atom), after which they were refined with riding constraints. . ; _publ_section_exptl_prep ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined data collection reference User defined data reduction User defined cell refinement Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Tb1 Tb 0.2500 0.2500 -0.13969(6) 0.0426 1.0000 Uani S T . . . . Tb2 Tb 0.35066(3) 0.33820(3) -0.31541(3) 0.0474 1.0000 Uani . . . . . . Tb3 Tb 0.38493(3) 0.24524(3) 0.03424(3) 0.0450 1.0000 Uani . . . . . . O1 O 0.2500 0.2500 0.0525(8) 0.0378 1.0000 Uani S T . . . . O2 O 0.2500 0.2500 -0.3322(8) 0.0539 1.0000 Uani S T . . . . O3 O 0.3253(3) 0.1701(4) -0.0573(4) 0.0439 1.0000 Uani . . . . . . O4 O 0.3580(3) 0.2442(4) -0.2225(4) 0.0443 1.0000 Uani . . . . . . O10 O 0.3739(4) 0.2436(4) -0.4137(4) 0.0512 1.0000 Uani . . . . . . C11 C 0.4222(8) 0.2382(7) -0.4757(7) 0.0632 1.0000 Uani . . . . . . C12 C 0.4831(7) 0.2727(8) -0.4782(7) 0.0732 1.0000 Uani . . . . . . C13 C 0.5069(8) 0.3134(7) -0.4116(8) 0.0701 1.0000 Uani . . . . . . O14 O 0.4702(4) 0.3339(5) -0.3475(6) 0.0718 1.0000 Uani . . . . . . C15 C 0.4009(8) 0.1853(7) -0.5459(8) 0.0764 1.0000 Uani . . . . . . C16 C 0.5841(8) 0.3362(11) -0.4095(10) 0.0991 1.0000 Uani . . . . . . O17 O 0.3787(5) 0.4491(4) -0.3577(5) 0.0699 1.0000 Uani . . . . . . C18 C 0.4179(8) 0.4977(8) -0.3270(9) 0.0765 1.0000 Uani . . . . . . C19 C 0.4447(7) 0.4975(7) -0.2464(8) 0.0654 1.0000 Uani . . . . . . C20 C 0.4327(6) 0.4491(6) -0.1818(7) 0.0555 1.0000 Uani . . . . . . O21 O 0.3988(4) 0.3930(4) -0.1935(4) 0.0570 1.0000 Uani . . . . . . C22 C 0.4326(11) 0.5559(9) -0.3916(12) 0.1104 1.0000 Uani . . . . . . C23 C 0.4579(7) 0.4618(7) -0.0914(8) 0.0690 1.0000 Uani . . . . . . O24 O 0.4578(4) 0.2441(4) -0.0873(4) 0.0543 1.0000 Uani . . . . . . C25 C 0.5225(6) 0.2574(6) -0.0994(7) 0.0543 1.0000 Uani . . . . . . C26 C 0.5648(5) 0.2854(6) -0.0359(8) 0.0604 1.0000 Uani . . . . . . C27 C 0.5451(7) 0.3114(7) 0.0430(8) 0.0640 1.0000 Uani . . . . . . O28 O 0.4810(4) 0.3147(4) 0.0684(5) 0.0661 1.0000 Uani . . . . . . C29 C 0.5513(6) 0.2405(8) -0.1873(8) 0.0673 1.0000 Uani . . . . . . C30 C 0.5990(7) 0.3420(9) 0.1025(10) 0.0904 1.0000 Uani . . . . . . O31 O 0.4731(4) 0.1699(5) 0.0832(5) 0.0678 1.0000 Uani . . . . . . C32 C 0.4855(7) 0.1423(7) 0.1566(9) 0.0673 1.0000 Uani . . . . . . C33 C 0.4326(7) 0.1214(7) 0.2139(7) 0.0614 1.0000 Uani . . . . . . C34 C 0.3635(8) 0.1268(6) 0.1992(6) 0.0631 1.0000 Uani . . . . . . O35 O 0.3348(4) 0.1590(4) 0.1332(4) 0.0512 1.0000 Uani . . . . . . C36 C 0.5625(8) 0.1315(9) 0.1801(10) 0.0872 1.0000 Uani . . . . . . C37 C 0.3113(7) 0.0971(8) 0.2606(8) 0.0762 1.0000 Uani . . . . . . O40 O 0.2500 0.7500 0.0000 0.1764 1.0000 Uani S T . . . . H371 H 0.2617 0.1055 0.2414 0.0747 1.0000 Uiso . . . . . . H372 H 0.3169 0.1198 0.3195 0.0747 1.0000 Uiso . . . . . . H373 H 0.3189 0.0458 0.2672 0.0747 1.0000 Uiso . . . . . . H361 H 0.5899 0.1495 0.1280 0.0832 1.0000 Uiso . . . . . . H362 H 0.5716 0.1583 0.2301 0.0832 1.0000 Uiso . . . . . . H363 H 0.5685 0.0812 0.1853 0.0832 1.0000 Uiso . . . . . . H331 H 0.4483 0.1034 0.2702 0.0534 1.0000 Uiso . . . . . . H291 H 0.5104 0.2205 -0.2228 0.0707 1.0000 Uiso . . . . . . H292 H 0.5651 0.2855 -0.2132 0.0707 1.0000 Uiso . . . . . . H293 H 0.5876 0.2075 -0.1812 0.0707 1.0000 Uiso . . . . . . H301 H 0.5735 0.3587 0.1590 0.0936 1.0000 Uiso . . . . . . H302 H 0.6193 0.3828 0.0754 0.0936 1.0000 Uiso . . . . . . H303 H 0.6315 0.3057 0.1180 0.0936 1.0000 Uiso . . . . . . H261 H 0.6150 0.2895 -0.0499 0.0622 1.0000 Uiso . . . . . . H151 H 0.3525 0.1642 -0.5308 0.0871 1.0000 Uiso . . . . . . H152 H 0.3968 0.2102 -0.6004 0.0871 1.0000 Uiso . . . . . . H153 H 0.4351 0.1476 -0.5468 0.0871 1.0000 Uiso . . . . . . H161 H 0.5892 0.3677 -0.3539 0.1028 1.0000 Uiso . . . . . . H162 H 0.5903 0.3667 -0.4590 0.1028 1.0000 Uiso . . . . . . H163 H 0.6112 0.2965 -0.4051 0.1028 1.0000 Uiso . . . . . . H121 H 0.5102 0.2698 -0.5293 0.0716 1.0000 Uiso . . . . . . H221 H 0.4071 0.5442 -0.4481 0.1278 1.0000 Uiso . . . . . . H222 H 0.4829 0.5565 -0.4022 0.1278 1.0000 Uiso . . . . . . H223 H 0.4142 0.5987 -0.3676 0.1278 1.0000 Uiso . . . . . . H231 H 0.4444 0.4214 -0.0530 0.0775 1.0000 Uiso . . . . . . H232 H 0.5099 0.4664 -0.0912 0.0775 1.0000 Uiso . . . . . . H233 H 0.4364 0.5054 -0.0683 0.0775 1.0000 Uiso . . . . . . H191 H 0.4772 0.5370 -0.2315 0.0662 1.0000 Uiso . . . . . . H3 H 0.2500 0.2500 -0.3908 0.0500 0.5000 Uiso . . . . . . H8 H 0.3914 0.2408 -0.1835 0.0500 1.0000 Uiso . . . . . . H12 H 0.2500 0.2500 0.1088 0.0500 0.5000 Uiso . . . . . . H99 H 0.2301 0.7220 -0.0271 0.0500 0.5000 Uiso . . . . . . H32 H 0.3581 0.1534 -0.1038 0.0527 1.0000 Uiso . . . . . . 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 0.0475(4) 0.0475(4) 0.0329(4) 0.0000 0.0000 0.0000 Tb2 0.0538(3) 0.0530(3) 0.0355(2) 0.0030(2) 0.0016(2) -0.0027(3) Tb3 0.0485(3) 0.0505(3) 0.0360(2) 0.00062(19) -0.0023(2) 0.0002(2) O1 0.029(4) 0.029(4) 0.055(7) 0.0000 0.0000 0.0000 O2 0.061(6) 0.061(6) 0.039(7) 0.0000 0.0000 0.0000 O3 0.043(4) 0.057(4) 0.032(3) -0.001(3) 0.000(3) -0.004(3) O4 0.046(4) 0.056(4) 0.031(3) 0.001(3) 0.002(3) 0.002(3) O10 0.053(4) 0.061(5) 0.040(3) 0.003(3) 0.010(3) 0.005(4) C11 0.085(9) 0.067(8) 0.038(5) 0.004(5) 0.007(5) 0.006(7) C12 0.067(8) 0.105(11) 0.048(6) 0.008(6) 0.016(6) 0.006(8) C13 0.089(10) 0.069(8) 0.052(7) 0.022(6) 0.005(6) 0.011(7) O14 0.049(5) 0.095(7) 0.071(5) 0.002(5) 0.005(4) -0.011(5) C15 0.111(11) 0.062(8) 0.056(7) -0.007(6) 0.018(7) -0.005(7) C16 0.063(9) 0.148(16) 0.087(10) 0.015(10) 0.023(7) -0.001(10) O17 0.075(6) 0.063(5) 0.072(5) 0.018(4) -0.021(4) -0.008(5) C18 0.071(9) 0.084(10) 0.075(8) 0.024(7) -0.005(7) -0.022(8) C19 0.069(8) 0.067(8) 0.060(6) 0.015(6) -0.004(6) -0.023(7) C20 0.051(6) 0.056(7) 0.059(6) -0.002(5) -0.002(5) -0.005(5) O21 0.068(5) 0.065(5) 0.038(4) -0.003(3) -0.001(3) -0.009(4) C22 0.134(16) 0.088(12) 0.109(12) 0.034(10) -0.032(11) -0.020(11) C23 0.075(9) 0.071(8) 0.061(7) -0.012(6) -0.008(6) -0.026(7) O24 0.056(5) 0.065(5) 0.042(4) 0.004(3) 0.000(3) -0.001(4) C25 0.042(6) 0.061(7) 0.060(6) 0.011(5) 0.004(5) -0.010(5) C26 0.028(5) 0.068(7) 0.085(8) 0.005(6) -0.003(5) -0.013(5) C27 0.064(8) 0.058(7) 0.070(7) -0.006(6) -0.007(6) -0.021(6) O28 0.060(5) 0.066(5) 0.072(5) -0.012(4) 0.000(4) -0.015(4) C29 0.051(7) 0.087(9) 0.064(7) 0.014(6) 0.012(6) 0.003(6) C30 0.056(8) 0.117(13) 0.097(10) -0.031(9) -0.007(7) -0.010(8) O31 0.057(5) 0.071(6) 0.075(5) 0.015(4) -0.001(4) 0.009(4) C32 0.066(8) 0.059(7) 0.078(8) 0.010(6) -0.015(6) 0.010(6) C33 0.069(8) 0.067(8) 0.048(6) 0.007(5) -0.008(5) 0.004(6) C34 0.096(10) 0.063(7) 0.031(5) -0.004(4) 0.001(5) 0.000(7) O35 0.056(4) 0.051(4) 0.046(4) 0.008(3) -0.005(3) 0.004(3) C36 0.071(9) 0.092(11) 0.099(11) 0.026(8) -0.012(8) 0.015(8) C37 0.064(8) 0.104(11) 0.061(7) 0.027(7) 0.002(6) -0.015(8) O40 0.152(19) 0.152(19) 0.23(4) 0.0000 0.0000 0.0000 _refine_ls_extinction_method None #_oxford_refine_ls_scale 0.05112(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Tb1 . O3 3_555 2.456(7) yes Tb1 . O3 5_555 2.456(7) yes Tb1 . O3 7_555 2.456(7) yes Tb1 . O4 3_555 2.433(6) yes Tb1 . O4 5_555 2.433(6) yes Tb1 . O4 7_555 2.433(6) yes Tb1 . O3 . 2.456(7) yes Tb1 . O4 . 2.433(6) yes Tb2 . O10 3_555 2.456(7) yes Tb2 . O4 3_555 2.346(7) yes Tb2 . O2 . 2.5694(14) yes Tb2 . O4 . 2.306(6) yes Tb2 . O10 . 2.407(7) yes Tb2 . O14 . 2.338(8) yes Tb2 . O17 . 2.281(8) yes Tb2 . O21 . 2.349(7) yes Tb3 . O35 3_555 2.447(7) yes Tb3 . O3 3_555 2.338(6) yes Tb3 . O1 . 2.5941(15) yes Tb3 . O3 . 2.318(6) yes Tb3 . O24 . 2.344(7) yes Tb3 . O28 . 2.325(8) yes Tb3 . O31 . 2.342(8) yes Tb3 . O35 . 2.447(7) yes O1 . H12 . 0.875 no O2 . H3 . 0.909 no O3 . H32 . 1.007 no O4 . H8 . 0.883 no O10 . C11 . 1.336(14) yes C11 . C12 . 1.338(19) yes C11 . C15 . 1.540(18) yes C12 . C13 . 1.370(19) yes C12 . H121 . 0.949 no C13 . O14 . 1.279(15) yes C13 . C16 . 1.54(2) yes C15 . H151 . 1.036 no C15 . H152 . 0.974 no C15 . H153 . 0.971 no C16 . H161 . 1.057 no C16 . H162 . 0.971 no C16 . H163 . 0.921 no O17 . C18 . 1.285(16) yes C18 . C19 . 1.352(17) yes C18 . C22 . 1.52(2) yes C19 . C20 . 1.384(16) yes C19 . H191 . 1.004 no C20 . O21 . 1.265(13) yes C20 . C23 . 1.503(16) yes C22 . H221 . 1.027 no C22 . H222 . 0.974 no C22 . H223 . 0.964 no C23 . H231 . 1.007 no C23 . H232 . 0.997 no C23 . H233 . 0.996 no O24 . C25 . 1.277(12) yes C25 . C26 . 1.382(16) yes C25 . C29 . 1.506(16) yes C26 . C27 . 1.373(17) yes C26 . H261 . 0.985 no C27 . O28 . 1.289(15) yes C27 . C30 . 1.502(17) yes C29 . H291 . 1.029 no C29 . H292 . 0.985 no C29 . H293 . 0.942 no C30 . H301 . 1.053 no C30 . H302 . 0.966 no C30 . H303 . 0.961 no O31 . C32 . 1.278(14) yes C32 . C33 . 1.405(18) yes C32 . C36 . 1.528(19) yes C33 . C34 . 1.343(18) yes C33 . H331 . 0.986 no C34 . O35 . 1.314(13) yes C34 . C37 . 1.491(17) yes C36 . H361 . 1.024 no C36 . H362 . 0.946 no C36 . H363 . 0.969 no C37 . H371 . 1.008 no C37 . H372 . 1.018 no C37 . H373 . 0.994 no O40 . H99 5_655 0.791 no O40 . H99 8_646 0.791 no O40 . H99 4_566 0.791 no O40 . H99 . 0.791 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 3_555 Tb1 . O3 5_555 74.27(13) yes O3 3_555 Tb1 . O3 7_555 117.3(3) yes O3 5_555 Tb1 . O3 7_555 74.27(13) yes O3 3_555 Tb1 . O4 3_555 75.5(2) yes O3 5_555 Tb1 . O4 3_555 77.0(2) yes O3 7_555 Tb1 . O4 3_555 143.1(2) yes O3 3_555 Tb1 . O4 5_555 140.8(2) yes O3 5_555 Tb1 . O4 5_555 75.5(2) yes O3 7_555 Tb1 . O4 5_555 77.0(2) yes O4 3_555 Tb1 . O4 5_555 73.79(14) yes O3 3_555 Tb1 . O4 7_555 143.1(2) yes O3 5_555 Tb1 . O4 7_555 140.8(2) yes O3 7_555 Tb1 . O4 7_555 75.5(2) yes O4 3_555 Tb1 . O4 7_555 116.2(3) yes O4 5_555 Tb1 . O4 7_555 73.78(14) yes O3 3_555 Tb1 . O3 . 74.27(13) yes O3 5_555 Tb1 . O3 . 117.3(3) yes O3 7_555 Tb1 . O3 . 74.27(13) yes O4 3_555 Tb1 . O3 . 140.8(2) yes O4 5_555 Tb1 . O3 . 143.1(2) yes O3 3_555 Tb1 . O4 . 77.0(2) yes O3 5_555 Tb1 . O4 . 143.1(2) yes O3 7_555 Tb1 . O4 . 140.8(2) yes O4 3_555 Tb1 . O4 . 73.79(14) yes O4 5_555 Tb1 . O4 . 116.2(3) yes O4 7_555 Tb1 . O3 . 77.0(2) yes O4 7_555 Tb1 . O4 . 73.78(14) yes O3 . Tb1 . O4 . 75.5(2) yes O10 3_555 Tb2 . O4 3_555 76.8(2) yes O10 3_555 Tb2 . O2 . 64.6(2) yes O4 3_555 Tb2 . O2 . 65.8(3) yes O10 3_555 Tb2 . O4 . 130.5(2) yes O4 3_555 Tb2 . O4 . 77.8(3) yes O2 . Tb2 . O4 . 66.4(3) yes O10 3_555 Tb2 . O10 . 87.1(3) yes O4 3_555 Tb2 . O10 . 130.8(2) yes O2 . Tb2 . O10 . 65.2(3) yes O4 . Tb2 . O10 . 78.5(2) yes O10 3_555 Tb2 . O14 . 126.3(3) yes O4 3_555 Tb2 . O14 . 153.0(3) yes O2 . Tb2 . O14 . 133.3(3) yes O4 . Tb2 . O14 . 92.7(3) yes O10 . Tb2 . O14 . 70.0(3) yes O10 3_555 Tb2 . O17 . 74.6(3) yes O4 3_555 Tb2 . O17 . 102.0(3) yes O2 . Tb2 . O17 . 139.0(3) yes O4 . Tb2 . O17 . 152.7(3) yes O10 . Tb2 . O17 . 118.1(3) yes O10 3_555 Tb2 . O21 . 131.5(3) yes O4 3_555 Tb2 . O21 . 74.6(2) yes O2 . Tb2 . O21 . 131.8(3) yes O4 . Tb2 . O21 . 79.6(3) yes O10 . Tb2 . O21 . 140.6(3) yes O14 . Tb2 . O17 . 75.0(3) yes O14 . Tb2 . O21 . 78.8(3) yes O17 . Tb2 . O21 . 74.1(3) yes O35 3_555 Tb3 . O3 3_555 76.7(2) yes O35 3_555 Tb3 . O1 . 64.3(2) yes O3 3_555 Tb3 . O1 . 66.2(3) yes O35 3_555 Tb3 . O3 . 130.5(2) yes O3 3_555 Tb3 . O3 . 79.1(3) yes O1 . Tb3 . O3 . 66.5(3) yes O35 3_555 Tb3 . O24 . 135.6(3) yes O3 3_555 Tb3 . O24 . 77.5(2) yes O1 . Tb3 . O24 . 132.7(3) yes O3 . Tb3 . O24 . 78.0(2) yes O35 3_555 Tb3 . O28 . 74.2(3) yes O3 3_555 Tb3 . O28 . 96.9(3) yes O1 . Tb3 . O28 . 137.6(3) yes O3 . Tb3 . O28 . 151.7(3) yes O24 . Tb3 . O28 . 73.8(3) yes O35 3_555 Tb3 . O31 . 118.2(3) yes O3 3_555 Tb3 . O31 . 157.3(3) yes O1 . Tb3 . O31 . 134.5(3) yes O3 . Tb3 . O31 . 99.9(3) yes O24 . Tb3 . O31 . 80.1(3) yes O35 3_555 Tb3 . O35 . 86.7(3) yes O3 3_555 Tb3 . O35 . 130.2(2) yes O1 . Tb3 . O35 . 64.3(2) yes O3 . Tb3 . O35 . 77.0(2) yes O24 . Tb3 . O35 . 137.0(3) yes O28 . Tb3 . O31 . 73.1(3) yes O28 . Tb3 . O35 . 123.3(3) yes O31 . Tb3 . O35 . 70.4(3) yes Tb3 5_555 O1 . Tb3 . 167.5(6) yes Tb3 5_555 O1 . Tb3 3_555 89.32(6) yes Tb3 . O1 . Tb3 3_555 89.32(6) yes Tb3 5_555 O1 . Tb3 7_555 89.32(6) yes Tb3 . O1 . Tb3 7_555 89.32(6) yes Tb3 3_555 O1 . Tb3 7_555 167.5(6) yes Tb3 5_555 O1 . H12 . 96.3 no Tb3 . O1 . H12 . 96.3 no Tb3 3_555 O1 . H12 . 96.3 no Tb3 7_555 O1 . H12 . 96.3 no Tb2 5_555 O2 . Tb2 . 168.3(6) yes Tb2 5_555 O2 . Tb2 3_555 89.41(6) yes Tb2 . O2 . Tb2 3_555 89.41(6) yes Tb2 5_555 O2 . Tb2 7_555 89.41(6) yes Tb2 . O2 . Tb2 7_555 89.41(6) yes Tb2 3_555 O2 . Tb2 7_555 168.3(6) yes Tb2 5_555 O2 . H3 . 95.8 no Tb2 . O2 . H3 . 95.8 no Tb2 3_555 O2 . H3 . 95.8 no Tb2 7_555 O2 . H3 . 95.8 no Tb1 . O3 . Tb3 7_555 102.3(2) yes Tb1 . O3 . Tb3 . 102.8(3) yes Tb3 7_555 O3 . Tb3 . 103.1(2) yes Tb1 . O3 . H32 . 100.8 no Tb3 7_555 O3 . H32 . 134.4 no Tb3 . O3 . H32 . 109.3 no Tb1 . O4 . Tb2 7_555 102.9(3) yes Tb1 . O4 . Tb2 . 104.1(3) yes Tb2 7_555 O4 . Tb2 . 102.0(2) yes Tb1 . O4 . H8 . 104.6 no Tb2 7_555 O4 . H8 . 118.8 no Tb2 . O4 . H8 . 122.1 no Tb2 7_555 O10 . Tb2 . 96.0(2) yes Tb2 7_555 O10 . C11 . 125.6(7) yes Tb2 . O10 . C11 . 129.9(7) yes O10 . C11 . C12 . 125.7(11) yes O10 . C11 . C15 . 112.2(11) yes C12 . C11 . C15 . 122.1(11) yes C11 . C12 . C13 . 123.1(11) yes C11 . C12 . H121 . 118.0 no C13 . C12 . H121 . 118.9 no C12 . C13 . O14 . 125.4(13) yes C12 . C13 . C16 . 119.7(13) yes O14 . C13 . C16 . 114.9(13) yes C13 . O14 . Tb2 . 135.4(9) yes C11 . C15 . H151 . 109.2 no C11 . C15 . H152 . 108.4 no H151 . C15 . H152 . 108.4 no C11 . C15 . H153 . 108.5 no H151 . C15 . H153 . 108.4 no H152 . C15 . H153 . 113.8 no C13 . C16 . H161 . 105.5 no C13 . C16 . H162 . 105.6 no H161 . C16 . H162 . 107.2 no C13 . C16 . H163 . 107.9 no H161 . C16 . H163 . 110.8 no H162 . C16 . H163 . 119.0 no Tb2 . O17 . C18 . 134.5(8) yes O17 . C18 . C19 . 124.2(12) yes O17 . C18 . C22 . 113.0(12) yes C19 . C18 . C22 . 122.8(13) yes C18 . C19 . C20 . 127.6(12) yes C18 . C19 . H191 . 116.5 no C20 . C19 . H191 . 115.9 no C19 . C20 . O21 . 123.1(10) yes C19 . C20 . C23 . 121.0(11) yes O21 . C20 . C23 . 115.8(10) yes Tb2 . O21 . C20 . 133.9(7) yes C18 . C22 . H221 . 108.4 no C18 . C22 . H222 . 107.5 no H221 . C22 . H222 . 109.0 no C18 . C22 . H223 . 107.4 no H221 . C22 . H223 . 110.0 no H222 . C22 . H223 . 114.5 no C20 . C23 . H231 . 110.2 no C20 . C23 . H232 . 109.6 no H231 . C23 . H232 . 108.8 no C20 . C23 . H233 . 109.8 no H231 . C23 . H233 . 108.8 no H232 . C23 . H233 . 109.7 no Tb3 . O24 . C25 . 133.7(7) yes O24 . C25 . C26 . 122.6(10) yes O24 . C25 . C29 . 116.3(10) yes C26 . C25 . C29 . 121.1(10) yes C25 . C26 . C27 . 128.0(10) yes C25 . C26 . H261 . 116.2 no C27 . C26 . H261 . 115.8 no C26 . C27 . O28 . 123.5(10) yes C26 . C27 . C30 . 120.1(12) yes O28 . C27 . C30 . 116.3(11) yes C27 . O28 . Tb3 . 130.7(7) yes C25 . C29 . H291 . 106.8 no C25 . C29 . H292 . 106.2 no H291 . C29 . H292 . 107.9 no C25 . C29 . H293 . 108.7 no H291 . C29 . H293 . 111.5 no H292 . C29 . H293 . 115.4 no C27 . C30 . H301 . 108.3 no C27 . C30 . H302 . 108.8 no H301 . C30 . H302 . 107.7 no C27 . C30 . H303 . 108.4 no H301 . C30 . H303 . 107.9 no H302 . C30 . H303 . 115.5 no Tb3 . O31 . C32 . 132.5(8) yes O31 . C32 . C33 . 123.3(11) yes O31 . C32 . C36 . 116.5(12) yes C33 . C32 . C36 . 120.2(11) yes C32 . C33 . C34 . 125.3(11) yes C32 . C33 . H331 . 116.1 no C34 . C33 . H331 . 118.6 no C33 . C34 . O35 . 125.3(11) yes C33 . C34 . C37 . 121.2(11) yes O35 . C34 . C37 . 113.5(12) yes Tb3 7_555 O35 . Tb3 . 96.3(2) yes Tb3 7_555 O35 . C34 . 128.3(7) yes Tb3 . O35 . C34 . 129.9(7) yes C32 . C36 . H361 . 104.9 no C32 . C36 . H362 . 107.4 no H361 . C36 . H362 . 111.9 no C32 . C36 . H363 . 105.6 no H361 . C36 . H363 . 109.7 no H362 . C36 . H363 . 116.6 no C34 . C37 . H371 . 112.2 no C34 . C37 . H372 . 110.0 no H371 . C37 . H372 . 107.2 no C34 . C37 . H373 . 110.1 no H371 . C37 . H373 . 108.9 no H372 . C37 . H373 . 108.2 no H99 5_655 O40 . H99 8_646 121.5 no H99 5_655 O40 . H99 4_566 121.5 no H99 8_646 O40 . H99 4_566 87.4 no H99 5_655 O40 . H99 . 87.4 no H99 8_646 O40 . H99 . 121.5 no H99 4_566 O40 . H99 . 121.5 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O4 . H8 . O24 . 171.4 0.883 1.959 2.834 yes O3 . H32 . O21 7_555 160.1 1.007 1.838 2.805 yes # Attachment 'Tb5-Revised.cif' data_II _database_code_depnum_ccdc_archive 'CCDC 711972' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 22.2773(6) _cell_length_b 17.4038(6) _cell_length_c 35.7676(9) _cell_angle_alpha 90 _cell_angle_beta 100.387(2) _cell_angle_gamma 90 _cell_volume 13640.2(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Tb -0.1723 4.1537 25.8976 2.2426 18.2185 0.1961 14.3167 12.6648 2.9535 115.3620 3.5822 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C150 H115 O25 Tb5 # Dc = 1.52 Fooo = 6160.00 Mu = 26.28 M = 3112.17 # Found Formula = C150 H115 O25 Tb5 # Dc = 1.52 FOOO = 6160.00 Mu = 26.28 M = 3112.17 _chemical_formula_sum 'C150 H115 O25 Tb5' _chemical_formula_moiety 'C150 H115 O25 Tb5' _chemical_compound_source ? _chemical_formula_weight 3112.17 _cell_measurement_reflns_used 19067 _cell_measurement_theta_min 0 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description cubic _exptl_crystal_colour colorless _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_max 0.11 _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 6160 _exptl_absorpt_coefficient_mu 2.628 # Sheldrick geometric approximatio 0.78 0.82 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7832 _exptl_absorpt_correction_T_max 0.8168 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 36082 _reflns_number_total 18911 _diffrn_reflns_av_R_equivalents 0.106 # Number of reflections with Friedels Law is 18911 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 18951 _diffrn_reflns_theta_min 1.305 _diffrn_reflns_theta_max 23.994 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.994 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _reflns_limit_h_min -24 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 39 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.91 _refine_diff_density_max 1.31 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>1.0\s(I) _refine_ls_number_reflns 9269 _refine_ls_number_restraints 0 _refine_ls_number_parameters 996 _oxford_refine_ls_R_factor_ref 0.0721 _refine_ls_wR_factor_ref 0.0749 _refine_ls_goodness_of_fit_ref 1.1676 _refine_ls_shift/su_max 0.000655 # The values computed from all data _oxford_reflns_number_all 18795 _refine_ls_R_factor_all 0.1621 _refine_ls_wR_factor_all 0.1802 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7505 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_gt 0.0597 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.392 0.287 0.271 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Tb1 Tb 0.24164(4) 0.89537(5) 0.17722(2) 0.0528 1.0000 Uani . . . . . . . Tb2 Tb 0.22986(4) 0.70104(5) 0.07124(2) 0.0557 1.0000 Uani . . . . . . . Tb3 Tb 0.29392(4) 0.89058(5) 0.08739(2) 0.0542 1.0000 Uani . . . . . . . Tb4 Tb 0.18300(4) 0.70401(5) 0.16186(2) 0.0552 1.0000 Uani . . . . . . . Tb5 Tb 0.35481(4) 0.73382(5) 0.16085(2) 0.0557 1.0000 Uani . . . . . . . O1 O 0.2161(4) 0.8060(6) 0.1192(3) 0.0621 1.0000 Uani . . . . . . . O11 O 0.2643(5) 0.6612(5) 0.1340(3) 0.0576 1.0000 Uani . . . . . . . O12 O 0.2711(4) 0.7685(5) 0.1921(3) 0.0563 1.0000 Uani . . . . . . . O13 O 0.3244(4) 0.7636(5) 0.0943(3) 0.0514 1.0000 Uani . . . . . . . O14 O 0.3306(5) 0.8698(5) 0.1517(3) 0.0596 1.0000 Uani . . . . . . . O21 O 0.2873(5) 0.7025(6) 0.0215(3) 0.0602 1.0000 Uani . . . . . . . C22 C 0.2818(7) 0.7411(12) -0.0089(5) 0.0685 1.0000 Uani . . . . . . . C23 C 0.2380(7) 0.8005(10) -0.0187(4) 0.0672 1.0000 Uani . . . . . . . C24 C 0.2074(7) 0.8386(10) 0.0052(5) 0.0639 1.0000 Uani . . . . . . . O25 O 0.2169(4) 0.8244(6) 0.0429(3) 0.0575 1.0000 Uani . . . . . . . C26 C 0.3252(7) 0.7235(10) -0.0367(5) 0.068(5) 1.0000 Uiso . . . . . . . C27 C 0.3524(9) 0.6523(11) -0.0334(5) 0.086(6) 1.0000 Uiso . . . . . . . C28 C 0.3964(11) 0.6388(14) -0.0572(7) 0.115(7) 1.0000 Uiso . . . . . . . C29 C 0.4111(10) 0.6963(15) -0.0781(6) 0.108(7) 1.0000 Uiso . . . . . . . C30 C 0.3874(10) 0.7622(13) -0.0799(6) 0.103(6) 1.0000 Uiso . . . . . . . C31 C 0.3430(9) 0.7789(11) -0.0573(5) 0.087(6) 1.0000 Uiso . . . . . . . C32 C 0.1646(7) 0.9001(9) -0.0078(4) 0.062(4) 1.0000 Uiso . . . . . . . C33 C 0.1582(8) 0.9323(11) -0.0438(5) 0.078(5) 1.0000 Uiso . . . . . . . C34 C 0.1181(9) 0.9955(11) -0.0545(5) 0.088(6) 1.0000 Uiso . . . . . . . C35 C 0.0811(8) 1.0220(11) -0.0307(5) 0.082(5) 1.0000 Uiso . . . . . . . C36 C 0.0860(8) 0.9890(10) 0.0037(5) 0.077(5) 1.0000 Uiso . . . . . . . C37 C 0.1262(8) 0.9270(10) 0.0152(5) 0.067(5) 1.0000 Uiso . . . . . . . O38 O 0.3694(5) 0.8722(6) 0.0521(4) 0.0716 1.0000 Uani . . . . . . . C39 C 0.3857(8) 0.9055(11) 0.0247(6) 0.0790 1.0000 Uani . . . . . . . C40 C 0.3584(9) 0.9679(11) 0.0046(5) 0.0828 1.0000 Uani . . . . . . . C41 C 0.3056(8) 1.0003(10) 0.0130(5) 0.0675 1.0000 Uani . . . . . . . O42 O 0.2781(5) 0.9782(6) 0.0387(3) 0.0683 1.0000 Uani . . . . . . . C43 C 0.4423(9) 0.8690(11) 0.0117(5) 0.085(5) 1.0000 Uiso . . . . . . . C44 C 0.4615(9) 0.7975(12) 0.0253(6) 0.096(6) 1.0000 Uiso . . . . . . . C45 C 0.5105(11) 0.7638(15) 0.0144(7) 0.118(7) 1.0000 Uiso . . . . . . . C46 C 0.5436(11) 0.8018(15) -0.0065(7) 0.125(8) 1.0000 Uiso . . . . . . . C47 C 0.5272(11) 0.8680(14) -0.0208(7) 0.114(7) 1.0000 Uiso . . . . . . . C48 C 0.4751(10) 0.9069(13) -0.0131(6) 0.106(7) 1.0000 Uiso . . . . . . . C49 C 0.2753(8) 1.0659(10) -0.0118(5) 0.073(5) 1.0000 Uiso . . . . . . . C50 C 0.2913(12) 1.0875(16) -0.0445(8) 0.138(9) 1.0000 Uiso . . . . . . . C51 C 0.2556(13) 1.1508(17) -0.0663(8) 0.138(9) 1.0000 Uiso . . . . . . . C52 C 0.2159(12) 1.1833(15) -0.0531(7) 0.123(8) 1.0000 Uiso . . . . . . . C53 C 0.1971(11) 1.1677(14) -0.0206(7) 0.118(7) 1.0000 Uiso . . . . . . . C54 C 0.2301(10) 1.1038(13) 0.0000(6) 0.103(7) 1.0000 Uiso . . . . . . . O55 O 0.2381(5) 0.5723(6) 0.0639(3) 0.0711 1.0000 Uani . . . . . . . C56 C 0.2234(9) 0.5259(10) 0.0369(6) 0.0809 1.0000 Uani . . . . . . . C57 C 0.1874(9) 0.5430(11) 0.0025(5) 0.0840 1.0000 Uani . . . . . . . C58 C 0.1549(8) 0.6156(11) -0.0043(5) 0.0677 1.0000 Uani . . . . . . . O59 O 0.1603(5) 0.6705(7) 0.0176(3) 0.0740 1.0000 Uani . . . . . . . C60 C 0.1102(8) 0.6211(10) -0.0420(5) 0.073(5) 1.0000 Uiso . . . . . . . C61 C 0.0887(9) 0.6951(12) -0.0519(6) 0.094(6) 1.0000 Uiso . . . . . . . C62 C 0.0493(11) 0.7065(14) -0.0874(7) 0.117(7) 1.0000 Uiso . . . . . . . C63 C 0.0301(11) 0.6450(15) -0.1104(7) 0.117(8) 1.0000 Uiso . . . . . . . C64 C 0.0517(10) 0.5763(13) -0.1004(6) 0.101(7) 1.0000 Uiso . . . . . . . C65 C 0.0909(9) 0.5627(11) -0.0683(6) 0.089(6) 1.0000 Uiso . . . . . . . C66 C 0.2499(9) 0.4438(11) 0.0430(6) 0.085(6) 1.0000 Uiso . . . . . . . C67 C 0.2603(9) 0.4166(12) 0.0768(6) 0.094(6) 1.0000 Uiso . . . . . . . C68 C 0.2788(12) 0.3385(16) 0.0841(8) 0.131(9) 1.0000 Uiso . . . . . . . C69 C 0.2902(13) 0.2968(18) 0.0552(10) 0.156(10) 1.0000 Uiso . . . . . . . C70 C 0.2869(12) 0.3237(17) 0.0211(9) 0.146(10) 1.0000 Uiso . . . . . . . C72 C 0.2619(11) 0.4010(15) 0.0121(7) 0.118(7) 1.0000 Uiso . . . . . . . O73 O 0.1360(5) 0.6801(6) 0.0976(3) 0.0618 1.0000 Uani . . . . . . . C74 C 0.0960(8) 0.6271(13) 0.0865(5) 0.0740 1.0000 Uani . . . . . . . C75 C 0.1012(8) 0.5514(11) 0.1026(6) 0.0865 1.0000 Uani . . . . . . . C76 C 0.1424(8) 0.5264(9) 0.1348(5) 0.0651 1.0000 Uani . . . . . . . O77 O 0.1777(5) 0.5711(6) 0.1556(3) 0.0703 1.0000 Uani . . . . . . . C78 C 0.0444(8) 0.6486(11) 0.0561(5) 0.079(5) 1.0000 Uiso . . . . . . . C79 C 0.0063(10) 0.5917(13) 0.0376(6) 0.104(7) 1.0000 Uiso . . . . . . . C80 C -0.0450(13) 0.6163(17) 0.0112(8) 0.141(9) 1.0000 Uiso . . . . . . . C82 C -0.0562(12) 0.6898(17) 0.0042(7) 0.130(8) 1.0000 Uiso . . . . . . . C83 C -0.0157(13) 0.7440(17) 0.0188(8) 0.138(9) 1.0000 Uiso . . . . . . . C84 C 0.0354(8) 0.7210(11) 0.0464(5) 0.081(5) 1.0000 Uiso . . . . . . . C85 C 0.1491(9) 0.4404(12) 0.1424(6) 0.090(6) 1.0000 Uiso . . . . . . . C86 C 0.1238(11) 0.3853(15) 0.1160(7) 0.117(7) 1.0000 Uiso . . . . . . . C87 C 0.1340(13) 0.3114(18) 0.1265(9) 0.147(10) 1.0000 Uiso . . . . . . . C88 C 0.1615(16) 0.289(2) 0.1583(11) 0.172(12) 1.0000 Uiso . . . . . . . C89 C 0.1929(19) 0.337(3) 0.1857(13) 0.230(17) 1.0000 Uiso . . . . . . . C90 C 0.1821(13) 0.4190(18) 0.1761(9) 0.150(10) 1.0000 Uiso . . . . . . . O91 O 0.1882(5) 0.6747(6) 0.2256(3) 0.0690 1.0000 Uani . . . . . . . C92 C 0.1511(9) 0.6399(9) 0.2440(5) 0.0670 1.0000 Uani . . . . . . . C93 C 0.0938(10) 0.6239(11) 0.2293(7) 0.0894 1.0000 Uani . . . . . . . C94 C 0.0611(8) 0.6370(11) 0.1934(6) 0.0701 1.0000 Uani . . . . . . . O95 O 0.0835(5) 0.6768(7) 0.1700(3) 0.0723 1.0000 Uani . . . . . . . C96 C -0.0012(9) 0.6125(11) 0.1815(5) 0.080(5) 1.0000 Uiso . . . . . . . C97 C -0.0341(10) 0.6375(11) 0.1492(6) 0.092(6) 1.0000 Uiso . . . . . . . C98 C -0.0972(14) 0.6114(17) 0.1358(8) 0.146(10) 1.0000 Uiso . . . . . . . C99 C -0.1219(12) 0.5677(16) 0.1588(8) 0.133(9) 1.0000 Uiso . . . . . . . C100 C -0.0911(17) 0.538(2) 0.1874(10) 0.179(12) 1.0000 Uiso . . . . . . . C101 C -0.0285(12) 0.5549(14) 0.2019(7) 0.119(8) 1.0000 Uiso . . . . . . . C102 C 0.1816(8) 0.6274(10) 0.2853(5) 0.074(5) 1.0000 Uiso . . . . . . . C103 C 0.2322(10) 0.6632(12) 0.3013(6) 0.099(6) 1.0000 Uiso . . . . . . . C104 C 0.2595(12) 0.6555(15) 0.3392(8) 0.128(8) 1.0000 Uiso . . . . . . . C105 C 0.2356(14) 0.5985(18) 0.3591(8) 0.148(10) 1.0000 Uiso . . . . . . . C106 C 0.1843(14) 0.5613(18) 0.3457(9) 0.154(10) 1.0000 Uiso . . . . . . . C107 C 0.1538(12) 0.5818(15) 0.3082(8) 0.129(8) 1.0000 Uiso . . . . . . . O108 O 0.3585(5) 0.6255(6) 0.2005(3) 0.0660 1.0000 Uani . . . . . . . C109 C 0.3592(8) 0.5545(10) 0.1936(5) 0.0692 1.0000 Uani . . . . . . . C110 C 0.3723(9) 0.5214(9) 0.1602(5) 0.0774 1.0000 Uani . . . . . . . C111 C 0.3959(9) 0.5637(12) 0.1316(5) 0.0770 1.0000 Uani . . . . . . . O112 O 0.4002(5) 0.6373(7) 0.1322(3) 0.0727 1.0000 Uani . . . . . . . C113 C 0.3454(8) 0.5008(11) 0.2237(5) 0.076(5) 1.0000 Uiso . . . . . . . C114 C 0.3087(10) 0.5238(13) 0.2465(7) 0.108(7) 1.0000 Uiso . . . . . . . C115 C 0.2919(12) 0.4748(17) 0.2747(8) 0.138(9) 1.0000 Uiso . . . . . . . C116 C 0.3158(13) 0.4046(17) 0.2764(8) 0.137(9) 1.0000 Uiso . . . . . . . C117 C 0.3517(12) 0.3785(15) 0.2525(8) 0.131(9) 1.0000 Uiso . . . . . . . C118 C 0.3699(10) 0.4276(13) 0.2273(6) 0.098(6) 1.0000 Uiso . . . . . . . C119 C 0.4130(9) 0.5199(13) 0.0993(6) 0.089(6) 1.0000 Uiso . . . . . . . C120 C 0.4196(9) 0.4466(13) 0.0969(6) 0.096(6) 1.0000 Uiso . . . . . . . C121 C 0.4350(9) 0.4071(13) 0.0649(6) 0.100(6) 1.0000 Uiso . . . . . . . C122 C 0.4461(11) 0.4506(16) 0.0364(7) 0.126(8) 1.0000 Uiso . . . . . . . C123 C 0.4434(14) 0.530(2) 0.0362(9) 0.164(11) 1.0000 Uiso . . . . . . . C124 C 0.4231(12) 0.5639(16) 0.0702(8) 0.134(9) 1.0000 Uiso . . . . . . . O125 O 0.4006(5) 0.7814(6) 0.2194(3) 0.0598 1.0000 Uani . . . . . . . C126 C 0.4356(7) 0.8397(9) 0.2297(4) 0.0536 1.0000 Uani . . . . . . . C127 C 0.4706(8) 0.8712(11) 0.2073(5) 0.0740 1.0000 Uani . . . . . . . C128 C 0.4776(8) 0.8508(10) 0.1714(6) 0.0648 1.0000 Uani . . . . . . . O129 O 0.4469(5) 0.7932(7) 0.1535(3) 0.0726 1.0000 Uani . . . . . . . C130 C 0.4335(8) 0.8670(10) 0.2702(5) 0.074(5) 1.0000 Uiso . . . . . . . C131 C 0.4664(8) 0.9315(11) 0.2846(5) 0.085(6) 1.0000 Uiso . . . . . . . C132 C 0.4607(10) 0.9574(12) 0.3213(6) 0.100(6) 1.0000 Uiso . . . . . . . C133 C 0.4232(10) 0.9214(12) 0.3394(6) 0.098(6) 1.0000 Uiso . . . . . . . C134 C 0.3911(10) 0.8536(13) 0.3265(6) 0.108(7) 1.0000 Uiso . . . . . . . C135 C 0.3972(9) 0.8290(11) 0.2902(5) 0.084(6) 1.0000 Uiso . . . . . . . C136 C 0.5147(9) 0.8936(12) 0.1498(6) 0.085(5) 1.0000 Uiso . . . . . . . C137 C 0.5236(16) 0.8780(19) 0.1163(10) 0.168(12) 1.0000 Uiso . . . . . . . C138 C 0.568(2) 0.907(3) 0.0978(13) 0.240(18) 1.0000 Uiso . . . . . . . C139 C 0.5866(14) 0.978(2) 0.1070(10) 0.162(11) 1.0000 Uiso . . . . . . . C140 C 0.5850(15) 1.0025(19) 0.1422(10) 0.168(11) 1.0000 Uiso . . . . . . . C141 C 0.5462(15) 0.958(2) 0.1607(9) 0.163(11) 1.0000 Uiso . . . . . . . O142 O 0.2292(6) 0.8728(6) 0.2399(3) 0.0683 1.0000 Uani . . . . . . . C143 C 0.1818(10) 0.8653(10) 0.2543(5) 0.0719 1.0000 Uani . . . . . . . C144 C 0.1230(9) 0.8604(11) 0.2350(5) 0.0739 1.0000 Uani . . . . . . . C145 C 0.1046(7) 0.8485(9) 0.1961(5) 0.0590 1.0000 Uani . . . . . . . O146 O 0.1450(4) 0.8344(6) 0.1738(3) 0.0570 1.0000 Uani . . . . . . . C147 C 0.1928(10) 0.8669(12) 0.2975(6) 0.096(6) 1.0000 Uiso . . . . . . . C148 C 0.2403(12) 0.9052(15) 0.3167(8) 0.128(8) 1.0000 Uiso . . . . . . . C149 C 0.2558(14) 0.9194(18) 0.3576(9) 0.159(11) 1.0000 Uiso . . . . . . . C150 C 0.2185(16) 0.872(2) 0.3716(9) 0.163(11) 1.0000 Uiso . . . . . . . C151 C 0.1734(15) 0.8284(18) 0.3597(9) 0.156(10) 1.0000 Uiso . . . . . . . C152 C 0.1539(11) 0.8283(14) 0.3152(7) 0.112(7) 1.0000 Uiso . . . . . . . C153 C 0.0394(8) 0.8537(10) 0.1780(5) 0.071(5) 1.0000 Uiso . . . . . . . C154 C 0.0242(9) 0.8345(11) 0.1399(5) 0.084(6) 1.0000 Uiso . . . . . . . C155 C -0.0376(9) 0.8352(12) 0.1207(6) 0.090(6) 1.0000 Uiso . . . . . . . C156 C -0.0804(12) 0.8635(14) 0.1427(8) 0.125(8) 1.0000 Uiso . . . . . . . C157 C -0.0646(13) 0.8864(15) 0.1768(8) 0.139(9) 1.0000 Uiso . . . . . . . C158 C -0.0038(12) 0.8775(14) 0.1964(7) 0.119(8) 1.0000 Uiso . . . . . . . O159 O 0.3416(5) 1.0065(7) 0.1127(3) 0.0675 1.0000 Uani . . . . . . . C160 C 0.3207(9) 1.0725(10) 0.1191(5) 0.0673 1.0000 Uani . . . . . . . C161 C 0.2581(9) 1.0861(9) 0.1127(5) 0.0679 1.0000 Uani . . . . . . . C162 C 0.2108(8) 1.0361(9) 0.1103(4) 0.0609 1.0000 Uani . . . . . . . O163 O 0.2209(5) 0.9607(6) 0.1151(3) 0.0603 1.0000 Uani . . . . . . . C164 C 0.3659(8) 1.1351(10) 0.1303(5) 0.064(4) 1.0000 Uiso . . . . . . . C165 C 0.4249(10) 1.1284(13) 0.1214(6) 0.103(7) 1.0000 Uiso . . . . . . . C166 C 0.4671(10) 1.1874(14) 0.1331(7) 0.115(7) 1.0000 Uiso . . . . . . . C167 C 0.4498(11) 1.2436(14) 0.1531(6) 0.110(7) 1.0000 Uiso . . . . . . . C168 C 0.3968(10) 1.2514(13) 0.1640(6) 0.102(6) 1.0000 Uiso . . . . . . . C169 C 0.3504(8) 1.1932(11) 0.1519(5) 0.086(5) 1.0000 Uiso . . . . . . . C170 C 0.1463(7) 1.0555(9) 0.1008(4) 0.054(4) 1.0000 Uiso . . . . . . . C171 C 0.1281(9) 1.1250(11) 0.0826(5) 0.087(6) 1.0000 Uiso . . . . . . . C172 C 0.0650(9) 1.1453(11) 0.0724(5) 0.086(6) 1.0000 Uiso . . . . . . . C173 C 0.0256(9) 1.0949(12) 0.0818(6) 0.092(6) 1.0000 Uiso . . . . . . . C174 C 0.0404(9) 1.0298(11) 0.1006(5) 0.083(5) 1.0000 Uiso . . . . . . . C175 C 0.1017(8) 1.0090(10) 0.1074(5) 0.067(5) 1.0000 Uiso . . . . . . . O176 O 0.1857(4) 1.0005(6) 0.1903(3) 0.061(3) 1.0000 Uiso . . . . . . . C177 C 0.1962(8) 1.0594(10) 0.2121(5) 0.070(5) 1.0000 Uiso . . . . . . . C178 C 0.2553(9) 1.0810(11) 0.2277(5) 0.083(6) 1.0000 Uiso . . . . . . . C179 C 0.3081(8) 1.0475(10) 0.2230(5) 0.066(5) 1.0000 Uiso . . . . . . . O180 O 0.3121(5) 0.9845(6) 0.2041(3) 0.071(3) 1.0000 Uiso . . . . . . . C182 C 0.1424(8) 1.1075(11) 0.2155(5) 0.077(5) 1.0000 Uiso . . . . . . . C183 C 0.0883(11) 1.0922(13) 0.1963(6) 0.108(7) 1.0000 Uiso . . . . . . . C184 C 0.0350(13) 1.1328(18) 0.1978(8) 0.144(9) 1.0000 Uiso . . . . . . . C185 C 0.0430(15) 1.1922(19) 0.2222(10) 0.158(11) 1.0000 Uiso . . . . . . . C186 C 0.0907(18) 1.205(2) 0.2477(10) 0.181(12) 1.0000 Uiso . . . . . . . C187 C 0.1474(14) 1.1658(18) 0.2466(8) 0.156(10) 1.0000 Uiso . . . . . . . C188 C 0.3710(9) 1.0824(11) 0.2371(6) 0.087(6) 1.0000 Uiso . . . . . . . C189 C 0.4179(10) 1.0708(12) 0.2214(6) 0.093(6) 1.0000 Uiso . . . . . . . C190 C 0.4762(11) 1.1054(15) 0.2356(7) 0.122(8) 1.0000 Uiso . . . . . . . C191 C 0.4775(13) 1.1515(16) 0.2639(9) 0.139(9) 1.0000 Uiso . . . . . . . C192 C 0.4343(15) 1.1676(18) 0.2821(9) 0.155(10) 1.0000 Uiso . . . . . . . C193 C 0.3750(12) 1.1317(15) 0.2700(7) 0.129(8) 1.0000 Uiso . . . . . . . H131 H 0.3478 0.7344 0.0861 0.0500 1.0000 Uiso . . . . . . . H111 H 0.2730 0.6157 0.1378 0.0500 1.0000 Uiso . . . . . . . H121 H 0.2745 0.7577 0.2147 0.0500 1.0000 Uiso . . . . . . . H141 H 0.3463 0.9031 0.1666 0.0500 1.0000 Uiso . . . . . . . H11 H 0.1863 0.8227 0.1045 0.0500 1.0000 Uiso . . . . . . . H231 H 0.2290 0.8162 -0.0451 0.0500 1.0000 Uiso . . . . . . . H271 H 0.3396 0.6139 -0.0169 0.0500 1.0000 Uiso . . . . . . . H281 H 0.4143 0.5875 -0.0580 0.0500 1.0000 Uiso . . . . . . . H291 H 0.4401 0.6869 -0.0940 0.0500 1.0000 Uiso . . . . . . . H301 H 0.4027 0.8047 -0.0949 0.0500 1.0000 Uiso . . . . . . . H311 H 0.3238 0.8308 -0.0587 0.0500 1.0000 Uiso . . . . . . . H401 H 0.3760 0.9898 -0.0156 0.0500 1.0000 Uiso . . . . . . . H441 H 0.4383 0.7683 0.0412 0.0500 1.0000 Uiso . . . . . . . H451 H 0.5248 0.7135 0.0247 0.0500 1.0000 Uiso . . . . . . . H461 H 0.5786 0.7779 -0.0140 0.0500 1.0000 Uiso . . . . . . . H471 H 0.5502 0.8937 -0.0386 0.0500 1.0000 Uiso . . . . . . . H481 H 0.4623 0.9579 -0.0229 0.0500 1.0000 Uiso . . . . . . . H571 H 0.1827 0.5041 -0.0177 0.0500 1.0000 Uiso . . . . . . . H611 H 0.1048 0.7391 -0.0356 0.0500 1.0000 Uiso . . . . . . . H621 H 0.0349 0.7588 -0.0941 0.0500 1.0000 Uiso . . . . . . . H631 H 0.0007 0.6562 -0.1343 0.0500 1.0000 Uiso . . . . . . . H641 H 0.0366 0.5315 -0.1169 0.0500 1.0000 Uiso . . . . . . . H651 H 0.1082 0.5112 -0.0618 0.0500 1.0000 Uiso . . . . . . . H671 H 0.2557 0.4487 0.0983 0.0500 1.0000 Uiso . . . . . . . H681 H 0.2849 0.3173 0.1097 0.0500 1.0000 Uiso . . . . . . . H691 H 0.3006 0.2435 0.0596 0.1500 1.0000 Uiso . . . . . . . H701 H 0.3009 0.2953 -0.0003 0.0500 1.0000 Uiso . . . . . . . H721 H 0.2532 0.4214 -0.0140 0.0500 1.0000 Uiso . . . . . . . H751 H 0.0716 0.5135 0.0895 0.0500 1.0000 Uiso . . . . . . . H791 H 0.0136 0.5374 0.0426 0.0500 1.0000 Uiso . . . . . . . H801 H -0.0735 0.5795 -0.0025 0.0500 1.0000 Uiso . . . . . . . H821 H -0.0925 0.7088 -0.0115 0.0500 1.0000 Uiso . . . . . . . H831 H -0.0186 0.7986 0.0098 0.0500 1.0000 Uiso . . . . . . . H841 H 0.0649 0.7615 0.0576 0.0500 1.0000 Uiso . . . . . . . H861 H 0.1024 0.4010 0.0913 0.0500 1.0000 Uiso . . . . . . . H871 H 0.1157 0.2712 0.1084 0.0500 1.0000 Uiso . . . . . . . H881 H 0.1643 0.2354 0.1648 0.1500 1.0000 Uiso . . . . . . . H891 H 0.2179 0.3211 0.2099 0.1500 1.0000 Uiso . . . . . . . H901 H 0.2013 0.4585 0.1938 0.0500 1.0000 Uiso . . . . . . . H931 H 0.0707 0.5983 0.2467 0.0500 1.0000 Uiso . . . . . . . H971 H -0.0146 0.6687 0.1328 0.0500 1.0000 Uiso . . . . . . . H981 H -0.1201 0.6359 0.1117 0.0500 1.0000 Uiso . . . . . . . H991 H -0.1641 0.5557 0.1501 0.0500 1.0000 Uiso . . . . . . . H1001 H -0.1087 0.4973 0.2013 0.150 1.0000 Uiso . . . . . . . H1011 H -0.0056 0.5309 0.2252 0.0500 1.0000 Uiso . . . . . . . H1031 H 0.2532 0.6985 0.2858 0.0500 1.0000 Uiso . . . . . . . H1041 H 0.2973 0.6827 0.3507 0.0500 1.0000 Uiso . . . . . . . H1051 H 0.2578 0.5919 0.3854 0.0500 1.0000 Uiso . . . . . . . H1061 H 0.1666 0.5261 0.3618 0.0500 1.0000 Uiso . . . . . . . H1071 H 0.1137 0.5617 0.2988 0.0500 1.0000 Uiso . . . . . . . H1101 H 0.3658 0.4675 0.1563 0.0500 1.0000 Uiso . . . . . . . H1141 H 0.2913 0.5740 0.2430 0.0500 1.0000 Uiso . . . . . . . H1151 H 0.2653 0.4928 0.2921 0.0500 1.0000 Uiso . . . . . . . H1161 H 0.3058 0.3723 0.2962 0.200 1.0000 Uiso . . . . . . . H1171 H 0.3667 0.3256 0.2547 0.0500 1.0000 Uiso . . . . . . . H1181 H 0.3964 0.4104 0.2107 0.0500 1.0000 Uiso . . . . . . . H1271 H 0.4956 0.9142 0.2179 0.0500 1.0000 Uiso . . . . . . . H1371 H 0.5074 0.8246 0.1080 0.1500 1.0000 Uiso . . . . . . . H1381 H 0.5729 0.8894 0.0735 0.1500 1.0000 Uiso . . . . . . . H1391 H 0.6127 1.0069 0.0926 0.1500 1.0000 Uiso . . . . . . . H1401 H 0.6048 1.0501 0.1519 0.1500 1.0000 Uiso . . . . . . . H1411 H 0.5418 0.9778 0.1863 0.1500 1.0000 Uiso . . . . . . . H1441 H 0.0898 0.8628 0.2492 0.0500 1.0000 Uiso . . . . . . . H1481 H 0.2650 0.9370 0.3005 0.0500 1.0000 Uiso . . . . . . . H1491 H 0.2895 0.9529 0.3704 0.1500 1.0000 Uiso . . . . . . . H1501 H 0.2347 0.8644 0.3953 0.1500 1.0000 Uiso . . . . . . . H1511 H 0.1388 0.7986 0.3774 0.1500 1.0000 Uiso . . . . . . . H1521 H 0.1191 0.7954 0.3019 0.0500 1.0000 Uiso . . . . . . . H1611 H 0.2470 1.1401 0.1109 0.0500 1.0000 Uiso . . . . . . . H1651 H 0.4338 1.0854 0.1054 0.0500 1.0000 Uiso . . . . . . . H1661 H 0.5084 1.1813 0.1273 0.0500 1.0000 Uiso . . . . . . . H1671 H 0.4790 1.2850 0.1594 0.0500 1.0000 Uiso . . . . . . . H1681 H 0.3873 1.2935 0.1801 0.0500 1.0000 Uiso . . . . . . . H1691 H 0.3099 1.1962 0.1596 0.0500 1.0000 Uiso . . . . . . . H1711 H 0.1586 1.1611 0.0763 0.0500 1.0000 Uiso . . . . . . . H1721 H 0.0534 1.1931 0.0595 0.0500 1.0000 Uiso . . . . . . . H1731 H -0.0180 1.1108 0.0755 0.0500 1.0000 Uiso . . . . . . . H1741 H 0.0097 0.9950 0.1075 0.0500 1.0000 Uiso . . . . . . . H1751 H 0.1134 0.9592 0.1193 0.0500 1.0000 Uiso . . . . . . . H1781 H 0.2586 1.1270 0.2437 0.0500 1.0000 Uiso . . . . . . . H1891 H 0.4137 1.0365 0.1995 0.0500 1.0000 Uiso . . . . . . . H1901 H 0.5108 1.0950 0.2220 0.0500 1.0000 Uiso . . . . . . . H1911 H 0.5171 1.1745 0.2719 0.0500 1.0000 Uiso . . . . . . . H1921 H 0.4415 1.2011 0.3049 0.1500 1.0000 Uiso . . . . . . . H1931 H 0.3400 1.1395 0.2831 0.0500 1.0000 Uiso . . . . . . . H491 H 0.2172 1.0902 0.0259 0.0500 1.0000 Uiso . . . . . . . H492 H 0.1615 1.1961 -0.0100 0.0500 1.0000 Uiso . . . . . . . H493 H 0.1949 1.2291 -0.0668 0.0500 1.0000 Uiso . . . . . . . H494 H 0.2657 1.1647 -0.0929 0.0500 1.0000 Uiso . . . . . . . H495 H 0.3281 1.0557 -0.0537 0.0500 1.0000 Uiso . . . . . . . H1191 H 0.4100 0.4134 0.1197 0.0500 1.0000 Uiso . . . . . . . H1192 H 0.4368 0.3485 0.0648 0.0500 1.0000 Uiso . . . . . . . H1193 H 0.4620 0.4220 0.0153 0.0500 1.0000 Uiso . . . . . . . H1194 H 0.4494 0.5624 0.0120 0.1500 1.0000 Uiso . . . . . . . H1195 H 0.4217 0.6247 0.0722 0.0500 1.0000 Uiso . . . . . . . H1531 H 0.0064 0.9001 0.2232 0.0500 1.0000 Uiso . . . . . . . H1532 H -0.0996 0.9020 0.1902 0.0500 1.0000 Uiso . . . . . . . H1533 H -0.1253 0.8680 0.1286 0.0500 1.0000 Uiso . . . . . . . H1534 H -0.0480 0.8165 0.0921 0.0500 1.0000 Uiso . . . . . . . H1535 H 0.0582 0.8158 0.1248 0.0500 1.0000 Uiso . . . . . . . H321 H 0.1834 0.9108 -0.0631 0.0500 1.0000 Uiso . . . . . . . H322 H 0.1186 1.0232 -0.0796 0.0500 1.0000 Uiso . . . . . . . H323 H 0.0489 1.0652 -0.0387 0.0500 1.0000 Uiso . . . . . . . H324 H 0.0593 1.0090 0.0226 0.0500 1.0000 Uiso . . . . . . . H325 H 0.1252 0.9009 0.0415 0.0500 1.0000 Uiso . . . . . . . H1301 H 0.3745 0.7785 0.2791 0.0500 1.0000 Uiso . . . . . . . H1302 H 0.3642 0.8256 0.3427 0.0500 1.0000 Uiso . . . . . . . H1303 H 0.4195 0.9455 0.3653 0.0500 1.0000 Uiso . . . . . . . H1304 H 0.4871 1.0023 0.3329 0.0500 1.0000 Uiso . . . . . . . H1305 H 0.4931 0.9626 0.2686 0.0500 1.0000 Uiso . . . . . . . H1821 H 0.1893 1.1706 0.2657 0.1500 1.0000 Uiso . . . . . . . H1822 H 0.0953 1.2563 0.2616 0.1500 1.0000 Uiso . . . . . . . H1823 H 0.0028 1.2159 0.2285 0.1500 1.0000 Uiso . . . . . . . H1824 H -0.0068 1.1246 0.1799 0.0500 1.0000 Uiso . . . . . . . H1825 H 0.0832 1.0471 0.1766 0.0500 1.0000 Uiso . . . . . . . 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 0.0529(5) 0.0466(5) 0.0579(5) -0.0030(4) 0.0070(4) 0.0001(4) Tb2 0.0637(6) 0.0486(5) 0.0530(5) -0.0030(4) 0.0062(4) 0.0002(4) Tb3 0.0588(6) 0.0455(5) 0.0580(5) 0.0011(4) 0.0094(4) 0.0025(4) Tb4 0.0594(5) 0.0487(5) 0.0569(5) 0.0003(4) 0.0087(4) -0.0052(4) Tb5 0.0567(5) 0.0499(5) 0.0587(5) 0.0012(4) 0.0051(4) 0.0059(4) O1 0.053(6) 0.061(7) 0.063(7) 0.013(6) -0.014(5) 0.003(6) O11 0.071(7) 0.042(6) 0.061(7) 0.005(5) 0.015(6) 0.012(5) O12 0.064(7) 0.048(6) 0.052(6) -0.009(5) -0.002(5) 0.005(5) O13 0.048(6) 0.035(5) 0.068(7) -0.015(5) 0.005(5) 0.013(5) O14 0.070(7) 0.043(6) 0.060(7) -0.012(5) -0.004(6) -0.005(5) O21 0.084(8) 0.048(6) 0.054(7) -0.001(6) 0.027(6) 0.011(6) C22 0.056(11) 0.100(15) 0.051(11) -0.018(11) 0.016(8) -0.013(11) C23 0.060(11) 0.082(12) 0.052(10) 0.000(10) -0.011(9) 0.026(10) C24 0.054(11) 0.063(12) 0.067(12) -0.001(10) -0.010(10) -0.007(9) O25 0.048(6) 0.068(7) 0.053(7) 0.002(5) -0.001(5) 0.011(5) O38 0.074(8) 0.064(8) 0.089(9) 0.009(7) 0.045(7) 0.014(6) C39 0.071(13) 0.079(14) 0.088(14) -0.001(12) 0.019(11) 0.000(11) C40 0.088(14) 0.073(13) 0.098(15) 0.035(11) 0.044(12) 0.006(11) C41 0.060(12) 0.063(12) 0.077(13) 0.000(10) 0.005(10) 0.002(10) O42 0.054(7) 0.077(8) 0.073(8) 0.009(7) 0.007(6) -0.007(6) O55 0.071(8) 0.063(8) 0.075(8) -0.013(7) 0.001(7) -0.001(6) C56 0.103(16) 0.055(12) 0.078(14) -0.016(11) -0.001(12) 0.017(11) C57 0.079(14) 0.085(14) 0.079(13) -0.037(11) -0.010(11) 0.003(11) C58 0.054(11) 0.075(13) 0.072(12) 0.009(11) 0.007(9) -0.003(10) O59 0.083(9) 0.071(8) 0.063(7) -0.028(7) -0.001(6) -0.006(6) O73 0.055(7) 0.064(8) 0.060(7) -0.004(6) -0.009(6) -0.011(6) C74 0.051(11) 0.112(17) 0.052(11) -0.010(11) -0.007(9) 0.017(11) C75 0.068(13) 0.058(12) 0.120(17) -0.005(12) -0.022(12) -0.024(10) C76 0.055(11) 0.042(10) 0.095(14) -0.003(10) 0.002(10) -0.013(9) O77 0.072(8) 0.061(8) 0.076(8) 0.008(6) 0.009(7) -0.018(6) O91 0.077(8) 0.069(8) 0.062(7) 0.012(6) 0.016(6) -0.004(6) C92 0.086(15) 0.056(11) 0.068(12) 0.003(9) 0.037(11) -0.009(10) C93 0.075(15) 0.083(15) 0.123(19) -0.009(13) 0.050(14) -0.038(12) C94 0.062(12) 0.079(13) 0.067(13) -0.015(11) 0.007(11) -0.017(10) O95 0.074(8) 0.081(9) 0.065(8) 0.001(7) 0.021(7) -0.014(6) O108 0.069(8) 0.066(8) 0.060(7) 0.001(6) 0.002(6) -0.002(6) C109 0.080(13) 0.040(11) 0.082(13) 0.003(10) 0.000(10) -0.011(9) C110 0.129(17) 0.054(11) 0.058(11) -0.007(10) 0.041(11) 0.021(11) C111 0.102(15) 0.070(14) 0.063(12) -0.002(11) 0.024(11) 0.027(12) O112 0.089(9) 0.071(9) 0.063(8) -0.006(6) 0.029(7) 0.029(7) O125 0.056(7) 0.056(7) 0.061(7) 0.002(5) -0.006(5) 0.005(6) C126 0.044(10) 0.048(10) 0.068(11) 0.002(9) 0.008(9) 0.006(8) C127 0.062(12) 0.111(16) 0.051(11) -0.004(10) 0.015(9) -0.044(11) C128 0.057(11) 0.056(11) 0.088(14) 0.013(10) 0.031(10) -0.012(9) O129 0.049(6) 0.091(9) 0.077(8) 0.009(7) 0.011(6) 0.003(7) O142 0.086(9) 0.063(8) 0.055(7) 0.002(6) 0.011(7) 0.014(6) C143 0.086(15) 0.075(13) 0.063(12) -0.001(10) 0.036(12) 0.021(11) C144 0.072(14) 0.084(13) 0.065(13) 0.016(10) 0.008(11) 0.008(10) C145 0.048(11) 0.057(11) 0.074(12) 0.004(9) 0.016(10) -0.002(8) O146 0.046(7) 0.055(7) 0.073(7) -0.004(6) 0.020(6) 0.005(5) O159 0.049(7) 0.074(8) 0.074(8) -0.003(6) -0.002(6) 0.002(6) C160 0.079(14) 0.048(11) 0.070(12) 0.017(9) 0.000(10) 0.007(10) C161 0.083(14) 0.046(11) 0.074(12) -0.004(9) 0.013(10) 0.000(10) C162 0.067(12) 0.044(10) 0.069(11) -0.004(8) 0.007(9) 0.009(10) O163 0.070(8) 0.043(6) 0.070(7) 0.004(6) 0.016(6) 0.009(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.01931(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Tb1 . O1 . 2.572(10) yes Tb1 . O12 . 2.337(10) yes Tb1 . O14 . 2.368(11) yes Tb1 . O142 . 2.343(11) yes Tb1 . O146 . 2.384(10) yes Tb1 . O163 . 2.465(10) yes Tb1 . O176 . 2.308(10) yes Tb1 . O180 . 2.292(11) yes Tb2 . O1 . 2.563(11) yes Tb2 . O11 . 2.342(10) yes Tb2 . O13 . 2.382(9) yes Tb2 . O21 . 2.373(10) yes Tb2 . O25 . 2.370(10) yes Tb2 . O55 . 2.267(11) yes Tb2 . O59 . 2.300(11) yes Tb2 . O73 . 2.470(11) yes Tb3 . O1 . 2.680(10) yes Tb3 . O13 . 2.312(9) yes Tb3 . O14 . 2.327(10) yes Tb3 . O25 . 2.412(10) yes Tb3 . O38 . 2.300(11) yes Tb3 . O42 . 2.294(12) yes Tb3 . O159 . 2.382(11) yes Tb3 . O163 . 2.386(10) yes Tb4 . O1 . 2.535(10) yes Tb4 . O11 . 2.341(10) yes Tb4 . O12 . 2.348(9) yes Tb4 . O73 . 2.384(10) yes Tb4 . O77 . 2.324(11) yes Tb4 . O91 . 2.319(11) yes Tb4 . O95 . 2.335(12) yes Tb4 . O146 . 2.485(10) yes Tb5 . O11 . 2.426(11) yes Tb5 . O12 . 2.418(10) yes Tb5 . O13 . 2.412(10) yes Tb5 . O14 . 2.436(10) yes Tb5 . O108 . 2.352(11) yes Tb5 . O112 . 2.295(11) yes Tb5 . O125 . 2.312(10) yes Tb5 . O129 . 2.353(11) yes O1 . H11 . 0.822 no O11 . H111 . 0.821 no O12 . H121 . 0.820 no O13 . H131 . 0.818 no O14 . H141 . 0.822 no O21 . C22 . 1.263(19) yes C22 . C23 . 1.42(2) yes C22 . C26 . 1.54(2) yes C23 . C24 . 1.36(2) yes C23 . H231 . 0.966 no C24 . O25 . 1.349(18) yes C24 . C32 . 1.45(2) yes C26 . C27 . 1.37(2) yes C26 . C31 . 1.32(2) yes C27 . C28 . 1.43(3) yes C27 . H271 . 0.968 no C28 . C29 . 1.32(3) yes C28 . H281 . 0.982 no C29 . C30 . 1.26(3) yes C29 . H291 . 0.949 no C30 . C31 . 1.42(3) yes C30 . H301 . 1.008 no C31 . H311 . 0.995 no C32 . C33 . 1.39(2) yes C32 . C37 . 1.37(2) yes C33 . C34 . 1.43(2) yes C33 . H321 . 1.035 no C34 . C35 . 1.37(2) yes C34 . H322 . 1.021 no C35 . C36 . 1.34(2) yes C35 . H323 . 1.043 no C36 . C37 . 1.41(2) yes C36 . H324 . 1.040 no C37 . H325 . 1.050 no O38 . C39 . 1.25(2) yes C39 . C40 . 1.38(2) yes C39 . C43 . 1.56(2) yes C40 . C41 . 1.39(2) yes C40 . H401 . 0.960 no C41 . O42 . 1.252(19) yes C41 . C49 . 1.53(2) yes C43 . C44 . 1.38(2) yes C43 . C48 . 1.41(3) yes C44 . C45 . 1.36(3) yes C44 . H441 . 0.977 no C45 . C46 . 1.32(3) yes C45 . H451 . 0.980 no C46 . C47 . 1.29(3) yes C46 . H461 . 0.963 no C47 . C48 . 1.41(3) yes C47 . H471 . 0.993 no C48 . H481 . 0.976 no C49 . C50 . 1.34(3) yes C49 . C54 . 1.33(2) yes C50 . C51 . 1.49(3) yes C50 . H495 . 1.089 no C51 . C52 . 1.22(3) yes C51 . H494 . 1.045 no C52 . C53 . 1.33(3) yes C52 . H493 . 1.005 no C53 . C54 . 1.46(3) yes C53 . H492 . 1.061 no C54 . H491 . 1.049 no O55 . C56 . 1.256(19) yes C56 . C57 . 1.37(2) yes C56 . C66 . 1.55(2) yes C57 . C58 . 1.46(2) yes C57 . H571 . 0.983 no C58 . O59 . 1.229(19) yes C58 . C60 . 1.53(2) yes C60 . C61 . 1.40(2) yes C60 . C65 . 1.40(2) yes C61 . C62 . 1.42(3) yes C61 . H611 . 0.989 no C62 . C63 . 1.37(3) yes C62 . H621 . 0.981 no C63 . C64 . 1.31(3) yes C63 . H631 . 0.998 no C64 . C65 . 1.33(2) yes C64 . H641 . 0.999 no C65 . H651 . 0.985 no C66 . C67 . 1.28(2) yes C66 . C72 . 1.40(3) yes C67 . C68 . 1.43(3) yes C67 . H671 . 0.971 no C68 . C69 . 1.32(3) yes C68 . H681 . 0.972 no C69 . C70 . 1.30(3) yes C69 . H691 . 0.962 no C70 . C72 . 1.47(3) yes C70 . H701 . 1.009 no C72 . H721 . 0.983 no O73 . C74 . 1.29(2) yes C74 . C75 . 1.44(3) yes C74 . C78 . 1.48(2) yes C75 . C76 . 1.41(2) yes C75 . H751 . 0.989 no C76 . O77 . 1.253(17) yes C76 . C85 . 1.52(2) yes C78 . C79 . 1.39(2) yes C78 . C84 . 1.31(2) yes C79 . C80 . 1.41(3) yes C79 . H791 . 0.971 no C80 . C82 . 1.32(3) yes C80 . H801 . 0.971 no C82 . C83 . 1.34(3) yes C82 . H821 . 0.955 no C83 . C84 . 1.42(3) yes C83 . H831 . 1.002 no C84 . H841 . 0.997 no C85 . C86 . 1.39(3) yes C85 . C90 . 1.34(3) yes C86 . C87 . 1.35(3) yes C86 . H861 . 0.966 no C87 . C88 . 1.25(4) yes C87 . H871 . 0.990 no C88 . C89 . 1.38(5) yes C88 . H881 . 0.956 no C89 . C90 . 1.47(5) yes C89 . H891 . 0.984 no C90 . H901 . 0.979 no O91 . C92 . 1.295(18) yes C92 . C93 . 1.32(2) yes C92 . C102 . 1.53(2) yes C93 . C94 . 1.38(3) yes C93 . H931 . 0.984 no C94 . O95 . 1.26(2) yes C94 . C96 . 1.44(2) yes C96 . C97 . 1.33(2) yes C96 . C101 . 1.44(3) yes C97 . C98 . 1.47(3) yes C97 . H971 . 0.960 no C98 . C99 . 1.31(3) yes C98 . H981 . 1.014 no C99 . C100 . 1.24(4) yes C99 . H991 . 0.959 no C100 . C101 . 1.43(4) yes C100 . H1001 . 0.981 no C101 . H1011 . 0.988 no C102 . C103 . 1.32(2) yes C102 . C107 . 1.36(3) yes C103 . C104 . 1.39(3) yes C103 . H1031 . 0.998 no C104 . C105 . 1.38(3) yes C104 . H1041 . 0.989 no C105 . C106 . 1.33(3) yes C105 . H1051 . 0.986 no C106 . C107 . 1.44(3) yes C106 . H1061 . 0.973 no C107 . H1071 . 0.960 no O108 . C109 . 1.262(18) yes C109 . C110 . 1.40(2) yes C109 . C113 . 1.50(2) yes C110 . C111 . 1.43(2) yes C110 . H1101 . 0.956 no C111 . O112 . 1.28(2) yes C111 . C119 . 1.49(2) yes C113 . C114 . 1.32(3) yes C113 . C118 . 1.38(2) yes C114 . C115 . 1.42(3) yes C114 . H1141 . 0.956 no C115 . C116 . 1.33(3) yes C115 . H1151 . 0.987 no C116 . C117 . 1.35(3) yes C116 . H1161 . 0.961 no C117 . C118 . 1.36(3) yes C117 . H1171 . 0.978 no C118 . H1181 . 0.956 no C119 . C120 . 1.29(3) yes C119 . C124 . 1.34(3) yes C120 . C121 . 1.43(3) yes C120 . H1191 . 1.054 no C121 . C122 . 1.33(3) yes C121 . H1192 . 1.020 no C122 . C123 . 1.39(3) yes C122 . H1193 . 1.021 no C123 . C124 . 1.49(4) yes C123 . H1194 . 1.059 no C124 . H1195 . 1.061 no O125 . C126 . 1.293(16) yes C126 . C127 . 1.33(2) yes C126 . C130 . 1.54(2) yes C127 . C128 . 1.37(2) yes C127 . H1271 . 0.968 no C128 . O129 . 1.315(19) yes C128 . C136 . 1.44(2) yes C130 . C131 . 1.39(2) yes C130 . C135 . 1.34(2) yes C131 . C132 . 1.42(2) yes C131 . H1305 . 1.047 no C132 . C133 . 1.31(3) yes C132 . H1304 . 1.019 no C133 . C134 . 1.41(3) yes C133 . H1303 . 1.033 no C134 . C135 . 1.40(3) yes C134 . H1302 . 1.028 no C135 . H1301 . 1.054 no C136 . C137 . 1.28(3) yes C136 . C141 . 1.34(3) yes C137 . C138 . 1.39(5) yes C137 . H1371 . 1.022 no C138 . C139 . 1.33(5) yes C138 . H1381 . 0.944 no C139 . C140 . 1.34(4) yes C139 . H1391 . 0.983 no C140 . C141 . 1.42(4) yes C140 . H1401 . 0.973 no C141 . H1411 . 1.003 no O142 . C143 . 1.263(19) yes C143 . C144 . 1.37(2) yes C143 . C147 . 1.52(3) yes C144 . C145 . 1.39(2) yes C144 . H1441 . 0.972 no C145 . O146 . 1.329(17) yes C145 . C153 . 1.48(2) yes C147 . C148 . 1.33(3) yes C147 . C152 . 1.34(3) yes C148 . C149 . 1.46(3) yes C148 . H1481 . 1.030 no C149 . C150 . 1.34(4) yes C149 . H1491 . 0.994 no C150 . C151 . 1.27(4) yes C150 . H1501 . 0.871 no C151 . C152 . 1.57(3) yes C151 . H1511 . 1.198 no C152 . H1521 . 1.010 no C153 . C154 . 1.39(2) yes C153 . C158 . 1.32(3) yes C154 . C155 . 1.42(2) yes C154 . H1535 . 1.057 no C155 . C156 . 1.43(3) yes C155 . H1534 . 1.062 no C156 . C157 . 1.27(3) yes C156 . H1533 . 1.039 no C157 . C158 . 1.42(3) yes C157 . H1532 . 1.024 no C158 . H1531 . 1.024 no O159 . C160 . 1.275(18) yes C160 . C161 . 1.39(2) yes C160 . C164 . 1.49(2) yes C161 . C162 . 1.36(2) yes C161 . H1611 . 0.971 no C162 . O163 . 1.338(17) yes C162 . C170 . 1.45(2) yes C164 . C165 . 1.41(2) yes C164 . C169 . 1.35(2) yes C165 . C166 . 1.40(3) yes C165 . H1651 . 0.986 no C166 . C167 . 1.31(3) yes C166 . H1661 . 0.984 no C167 . C168 . 1.32(3) yes C167 . H1671 . 0.971 no C168 . C169 . 1.46(3) yes C168 . H1681 . 0.980 no C169 . H1691 . 0.992 no C170 . C171 . 1.40(2) yes C170 . C175 . 1.33(2) yes C171 . C172 . 1.43(2) yes C171 . H1711 . 0.981 no C172 . C173 . 1.33(2) yes C172 . H1721 . 0.964 no C173 . C174 . 1.33(2) yes C173 . H1731 . 0.997 no C174 . C175 . 1.39(2) yes C174 . H1741 . 0.977 no C175 . H1751 . 0.980 no O176 . C177 . 1.283(18) yes C177 . C178 . 1.39(2) yes C177 . C182 . 1.49(2) yes C178 . C179 . 1.35(2) yes C178 . H1781 . 0.978 no C179 . O180 . 1.299(18) yes C179 . C188 . 1.53(2) yes C182 . C183 . 1.30(2) yes C182 . C187 . 1.49(3) yes C183 . C184 . 1.39(3) yes C183 . H1825 . 1.047 no C184 . C185 . 1.34(4) yes C184 . H1824 . 1.038 no C185 . C186 . 1.29(4) yes C185 . H1823 . 1.046 no C186 . C187 . 1.44(4) yes C186 . H1822 . 1.024 no C187 . H1821 . 1.056 no C188 . C189 . 1.29(2) yes C188 . C193 . 1.45(3) yes C189 . C190 . 1.44(3) yes C189 . H1891 . 0.976 no C190 . C191 . 1.29(3) yes C190 . H1901 . 1.002 no C191 . C192 . 1.29(3) yes C191 . H1911 . 0.964 no C192 . C193 . 1.45(3) yes C192 . H1921 . 0.990 no C193 . H1931 . 0.990 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Tb1 . O12 . 68.0(3) yes O1 . Tb1 . O14 . 69.8(3) yes O12 . Tb1 . O14 . 72.0(3) yes O1 . Tb1 . O142 . 128.6(4) yes O12 . Tb1 . O142 . 72.6(3) yes O14 . Tb1 . O142 . 126.1(4) yes O1 . Tb1 . O146 . 67.8(3) yes O12 . Tb1 . O146 . 78.7(3) yes O14 . Tb1 . O146 . 135.0(3) yes O142 . Tb1 . O146 . 73.3(4) yes O1 . Tb1 . O163 . 64.8(3) yes O12 . Tb1 . O163 . 129.8(3) yes O14 . Tb1 . O163 . 76.9(3) yes O142 . Tb1 . O163 . 154.9(4) yes O146 . Tb1 . O163 . 98.0(3) yes O1 . Tb1 . O176 . 126.4(3) yes O12 . Tb1 . O176 . 147.4(3) yes O14 . Tb1 . O176 . 138.3(3) yes O142 . Tb1 . O176 . 77.2(4) yes O146 . Tb1 . O176 . 81.3(3) yes O1 . Tb1 . O180 . 141.5(4) yes O12 . Tb1 . O180 . 113.7(4) yes O14 . Tb1 . O180 . 74.4(3) yes O142 . Tb1 . O180 . 84.4(4) yes O146 . Tb1 . O180 . 150.1(4) yes O163 . Tb1 . O176 . 78.3(3) yes O163 . Tb1 . O180 . 93.9(4) yes O176 . Tb1 . O180 . 74.5(4) yes O1 . Tb2 . O11 . 68.1(3) yes O1 . Tb2 . O13 . 69.4(3) yes O11 . Tb2 . O13 . 71.8(3) yes O1 . Tb2 . O21 . 129.9(3) yes O11 . Tb2 . O21 . 126.5(4) yes O13 . Tb2 . O21 . 72.0(3) yes O1 . Tb2 . O25 . 67.7(3) yes O11 . Tb2 . O25 . 132.2(3) yes O13 . Tb2 . O25 . 76.4(3) yes O21 . Tb2 . O25 . 73.1(3) yes O1 . Tb2 . O55 . 143.5(4) yes O11 . Tb2 . O55 . 78.4(4) yes O13 . Tb2 . O55 . 114.0(3) yes O21 . Tb2 . O55 . 81.8(4) yes O25 . Tb2 . O55 . 148.4(4) yes O1 . Tb2 . O59 . 125.4(4) yes O11 . Tb2 . O59 . 141.8(4) yes O13 . Tb2 . O59 . 144.6(4) yes O21 . Tb2 . O59 . 75.6(4) yes O25 . Tb2 . O59 . 80.8(4) yes O1 . Tb2 . O73 . 68.8(3) yes O11 . Tb2 . O73 . 75.2(4) yes O13 . Tb2 . O73 . 133.8(3) yes O21 . Tb2 . O73 . 153.6(4) yes O25 . Tb2 . O73 . 104.6(3) yes O55 . Tb2 . O59 . 74.4(4) yes O55 . Tb2 . O73 . 89.4(4) yes O59 . Tb2 . O73 . 78.1(4) yes O1 . Tb3 . O13 . 68.3(3) yes O1 . Tb3 . O14 . 68.5(3) yes O13 . Tb3 . O14 . 72.7(3) yes O1 . Tb3 . O25 . 65.2(3) yes O13 . Tb3 . O25 . 76.9(3) yes O14 . Tb3 . O25 . 131.3(4) yes O1 . Tb3 . O38 . 138.6(4) yes O13 . Tb3 . O38 . 72.3(4) yes O14 . Tb3 . O38 . 111.1(4) yes O25 . Tb3 . O38 . 94.2(4) yes O1 . Tb3 . O42 . 131.7(3) yes O13 . Tb3 . O42 . 135.9(4) yes O14 . Tb3 . O42 . 146.4(4) yes O25 . Tb3 . O42 . 79.7(4) yes O38 . Tb3 . O42 . 72.7(4) yes O1 . Tb3 . O159 . 125.6(3) yes O13 . Tb3 . O159 . 131.8(3) yes O14 . Tb3 . O159 . 72.7(3) yes O25 . Tb3 . O159 . 150.6(4) yes O38 . Tb3 . O159 . 90.4(4) yes O1 . Tb3 . O163 . 64.1(3) yes O13 . Tb3 . O163 . 130.8(3) yes O14 . Tb3 . O163 . 79.2(4) yes O25 . Tb3 . O163 . 93.5(3) yes O38 . Tb3 . O163 . 156.8(4) yes O42 . Tb3 . O159 . 73.9(4) yes O42 . Tb3 . O163 . 87.3(4) yes O159 . Tb3 . O163 . 72.5(4) yes O1 . Tb4 . O11 . 68.6(3) yes O1 . Tb4 . O12 . 68.4(3) yes O11 . Tb4 . O12 . 72.7(3) yes O1 . Tb4 . O73 . 70.6(3) yes O11 . Tb4 . O73 . 76.9(4) yes O12 . Tb4 . O73 . 135.4(4) yes O1 . Tb4 . O77 . 130.9(4) yes O11 . Tb4 . O77 . 70.9(4) yes O12 . Tb4 . O77 . 123.0(4) yes O73 . Tb4 . O77 . 74.2(4) yes O1 . Tb4 . O91 . 141.0(4) yes O11 . Tb4 . O91 . 116.3(4) yes O12 . Tb4 . O91 . 76.3(4) yes O73 . Tb4 . O91 . 147.6(4) yes O77 . Tb4 . O91 . 82.4(4) yes O1 . Tb4 . O95 . 127.1(4) yes O11 . Tb4 . O95 . 144.4(4) yes O12 . Tb4 . O95 . 140.6(4) yes O73 . Tb4 . O95 . 79.8(4) yes O77 . Tb4 . O95 . 77.1(4) yes O1 . Tb4 . O146 . 67.0(3) yes O11 . Tb4 . O146 . 132.6(3) yes O12 . Tb4 . O146 . 76.5(3) yes O73 . Tb4 . O146 . 102.8(4) yes O77 . Tb4 . O146 . 155.7(4) yes O91 . Tb4 . O95 . 73.3(4) yes O91 . Tb4 . O146 . 89.4(4) yes O95 . Tb4 . O146 . 78.7(4) yes O11 . Tb5 . O12 . 70.0(3) yes O11 . Tb5 . O13 . 69.8(3) yes O12 . Tb5 . O13 . 107.5(3) yes O11 . Tb5 . O14 . 107.7(3) yes O12 . Tb5 . O14 . 69.4(3) yes O13 . Tb5 . O14 . 69.1(3) yes O11 . Tb5 . O108 . 76.0(3) yes O12 . Tb5 . O108 . 82.4(4) yes O13 . Tb5 . O108 . 137.8(3) yes O14 . Tb5 . O108 . 147.4(4) yes O11 . Tb5 . O112 . 81.0(4) yes O12 . Tb5 . O112 . 145.9(4) yes O13 . Tb5 . O112 . 77.6(3) yes O14 . Tb5 . O112 . 139.1(4) yes O108 . Tb5 . O112 . 73.3(4) yes O11 . Tb5 . O125 . 138.1(4) yes O12 . Tb5 . O125 . 75.1(3) yes O13 . Tb5 . O125 . 144.8(3) yes O14 . Tb5 . O125 . 79.9(3) yes O108 . Tb5 . O125 . 77.2(3) yes O11 . Tb5 . O129 . 149.7(4) yes O12 . Tb5 . O129 . 134.7(4) yes O13 . Tb5 . O129 . 83.7(3) yes O14 . Tb5 . O129 . 74.6(4) yes O108 . Tb5 . O129 . 118.9(4) yes O112 . Tb5 . O125 . 120.6(4) yes O112 . Tb5 . O129 . 78.9(4) yes O125 . Tb5 . O129 . 72.2(4) yes Tb1 . O1 . Tb2 . 159.3(4) yes Tb1 . O1 . Tb3 . 86.8(3) yes Tb2 . O1 . Tb3 . 86.7(3) yes Tb1 . O1 . Tb4 . 89.1(3) yes Tb2 . O1 . Tb4 . 89.2(3) yes Tb3 . O1 . Tb4 . 157.1(4) yes Tb1 . O1 . H11 . 109.7 no Tb2 . O1 . H11 . 90.2 no Tb3 . O1 . H11 . 92.5 no Tb4 . O1 . H11 . 110.0 no Tb5 . O11 . Tb2 . 109.3(4) yes Tb5 . O11 . Tb4 . 108.5(4) yes Tb2 . O11 . Tb4 . 99.7(4) yes Tb5 . O11 . H111 . 106.4 no Tb2 . O11 . H111 . 118.1 no Tb4 . O11 . H111 . 114.5 no Tb5 . O12 . Tb4 . 108.5(4) yes Tb5 . O12 . Tb1 . 109.8(4) yes Tb4 . O12 . Tb1 . 99.8(3) yes Tb5 . O12 . H121 . 117.1 no Tb4 . O12 . H121 . 105.4 no Tb1 . O12 . H121 . 114.4 no Tb5 . O13 . Tb2 . 108.4(4) yes Tb5 . O13 . Tb3 . 109.6(3) yes Tb2 . O13 . Tb3 . 100.1(3) yes Tb5 . O13 . H131 . 97.8 no Tb2 . O13 . H131 . 99.9 no Tb3 . O13 . H131 . 138.6 no Tb5 . O14 . Tb1 . 108.2(4) yes Tb5 . O14 . Tb3 . 108.3(4) yes Tb1 . O14 . Tb3 . 100.5(4) yes Tb5 . O14 . H141 . 122.6 no Tb1 . O14 . H141 . 84.6 no Tb3 . O14 . H141 . 124.4 no Tb2 . O21 . C22 . 131.9(10) yes O21 . C22 . C23 . 123.8(14) yes O21 . C22 . C26 . 118.3(16) yes C23 . C22 . C26 . 117.9(16) yes C22 . C23 . C24 . 126.7(15) yes C22 . C23 . H231 . 117.4 no C24 . C23 . H231 . 115.9 no C23 . C24 . O25 . 122.3(14) yes C23 . C24 . C32 . 122.2(16) yes O25 . C24 . C32 . 115.5(16) yes C24 . O25 . Tb3 . 122.5(9) yes C24 . O25 . Tb2 . 125.3(9) yes Tb3 . O25 . Tb2 . 97.6(3) yes C22 . C26 . C27 . 116.3(17) yes C22 . C26 . C31 . 120.2(17) yes C27 . C26 . C31 . 122.4(18) yes C26 . C27 . C28 . 115.9(19) yes C26 . C27 . H271 . 120.0 no C28 . C27 . H271 . 124.0 no C27 . C28 . C29 . 119(2) yes C27 . C28 . H281 . 119.5 no C29 . C28 . H281 . 121.9 no C28 . C29 . C30 . 125(2) yes C28 . C29 . H291 . 118.2 no C30 . C29 . H291 . 116.6 no C29 . C30 . C31 . 119(2) yes C29 . C30 . H301 . 121.3 no C31 . C30 . H301 . 119.4 no C30 . C31 . C26 . 118.7(19) yes C30 . C31 . H311 . 119.7 no C26 . C31 . H311 . 121.5 no C24 . C32 . C33 . 123.1(16) yes C24 . C32 . C37 . 120.2(15) yes C33 . C32 . C37 . 116.6(16) yes C32 . C33 . C34 . 120.9(17) yes C32 . C33 . H321 . 119.7 no C34 . C33 . H321 . 119.4 no C33 . C34 . C35 . 121.0(18) yes C33 . C34 . H322 . 119.5 no C35 . C34 . H322 . 119.5 no C34 . C35 . C36 . 117.7(18) yes C34 . C35 . H323 . 122.4 no C36 . C35 . H323 . 119.8 no C35 . C36 . C37 . 122.5(17) yes C35 . C36 . H324 . 119.4 no C37 . C36 . H324 . 118.1 no C36 . C37 . C32 . 121.0(16) yes C36 . C37 . H325 . 118.5 no C32 . C37 . H325 . 120.5 no Tb3 . O38 . C39 . 135.3(12) yes O38 . C39 . C40 . 127.7(18) yes O38 . C39 . C43 . 114.3(17) yes C40 . C39 . C43 . 118.0(18) yes C39 . C40 . C41 . 121.2(17) yes C39 . C40 . H401 . 120.2 no C41 . C40 . H401 . 118.6 no C40 . C41 . O42 . 125.5(16) yes C40 . C41 . C49 . 118.8(18) yes O42 . C41 . C49 . 115.6(16) yes C41 . O42 . Tb3 . 137.1(11) yes C39 . C43 . C44 . 118.7(19) yes C39 . C43 . C48 . 122.4(19) yes C44 . C43 . C48 . 118.9(20) yes C43 . C44 . C45 . 120(2) yes C43 . C44 . H441 . 120.9 no C45 . C44 . H441 . 118.7 no C44 . C45 . C46 . 120(2) yes C44 . C45 . H451 . 120.1 no C46 . C45 . H451 . 119.0 no C45 . C46 . C47 . 122(3) yes C45 . C46 . H461 . 120.2 no C47 . C46 . H461 . 117.8 no C46 . C47 . C48 . 123(2) yes C46 . C47 . H471 . 120.8 no C48 . C47 . H471 . 116.6 no C47 . C48 . C43 . 116(2) yes C47 . C48 . H481 . 124.2 no C43 . C48 . H481 . 120.0 no C41 . C49 . C50 . 124(2) yes C41 . C49 . C54 . 117.9(18) yes C50 . C49 . C54 . 118(2) yes C49 . C50 . C51 . 118(2) yes C49 . C50 . H495 . 117.2 no C51 . C50 . H495 . 125.1 no C50 . C51 . C52 . 120(3) yes C50 . C51 . H494 . 117.8 no C52 . C51 . H494 . 122.5 no C51 . C52 . C53 . 128(3) yes C51 . C52 . H493 . 119.1 no C53 . C52 . H493 . 113.2 no C52 . C53 . C54 . 113(2) yes C52 . C53 . H492 . 126.1 no C54 . C53 . H492 . 121.2 no C53 . C54 . C49 . 124(2) yes C53 . C54 . H491 . 115.1 no C49 . C54 . H491 . 120.7 no Tb2 . O55 . C56 . 135.2(11) yes O55 . C56 . C57 . 125.3(16) yes O55 . C56 . C66 . 116.5(17) yes C57 . C56 . C66 . 118.2(17) yes C56 . C57 . C58 . 122.0(16) yes C56 . C57 . H571 . 118.5 no C58 . C57 . H571 . 119.4 no C57 . C58 . O59 . 125.5(16) yes C57 . C58 . C60 . 115.4(17) yes O59 . C58 . C60 . 119.2(16) yes C58 . O59 . Tb2 . 133.3(11) yes C58 . C60 . C61 . 114.9(16) yes C58 . C60 . C65 . 128.3(17) yes C61 . C60 . C65 . 116.7(17) yes C60 . C61 . C62 . 118.9(19) yes C60 . C61 . H611 . 119.5 no C62 . C61 . H611 . 121.3 no C61 . C62 . C63 . 120(2) yes C61 . C62 . H621 . 118.1 no C63 . C62 . H621 . 121.6 no C62 . C63 . C64 . 119(2) yes C62 . C63 . H631 . 116.6 no C64 . C63 . H631 . 124.2 no C63 . C64 . C65 . 123(2) yes C63 . C64 . H641 . 118.7 no C65 . C64 . H641 . 118.0 no C60 . C65 . C64 . 121.6(19) yes C60 . C65 . H651 . 116.3 no C64 . C65 . H651 . 122.2 no C56 . C66 . C67 . 118.2(19) yes C56 . C66 . C72 . 120.2(19) yes C67 . C66 . C72 . 122(2) yes C66 . C67 . C68 . 121(2) yes C66 . C67 . H671 . 120.6 no C68 . C67 . H671 . 118.1 no C67 . C68 . C69 . 118(3) yes C67 . C68 . H681 . 121.2 no C69 . C68 . H681 . 120.9 no C68 . C69 . C70 . 123(3) yes C68 . C69 . H691 . 118.4 no C70 . C69 . H691 . 118.2 no C69 . C70 . C72 . 120(3) yes C69 . C70 . H701 . 124.5 no C72 . C70 . H701 . 116.0 no C70 . C72 . C66 . 116(2) yes C70 . C72 . H721 . 122.7 no C66 . C72 . H721 . 121.6 no Tb2 . O73 . Tb4 . 95.0(4) yes Tb2 . O73 . C74 . 124.9(10) yes Tb4 . O73 . C74 . 125.3(11) yes O73 . C74 . C75 . 122.0(14) yes O73 . C74 . C78 . 116.5(18) yes C75 . C74 . C78 . 121.5(18) yes C74 . C75 . C76 . 127.3(15) yes C74 . C75 . H751 . 115.1 no C76 . C75 . H751 . 117.6 no C75 . C76 . O77 . 122.8(15) yes C75 . C76 . C85 . 118.6(16) yes O77 . C76 . C85 . 118.2(17) yes C76 . O77 . Tb4 . 133.8(11) yes C74 . C78 . C79 . 119.8(19) yes C74 . C78 . C84 . 119.9(19) yes C79 . C78 . C84 . 120.4(19) yes C78 . C79 . C80 . 117(2) yes C78 . C79 . H791 . 122.6 no C80 . C79 . H791 . 120.4 no C79 . C80 . C82 . 122(3) yes C79 . C80 . H801 . 121.1 no C82 . C80 . H801 . 117.3 no C80 . C82 . C83 . 121(3) yes C80 . C82 . H821 . 123.8 no C83 . C82 . H821 . 115.0 no C82 . C83 . C84 . 118(3) yes C82 . C83 . H831 . 122.7 no C84 . C83 . H831 . 119.2 no C83 . C84 . C78 . 121.2(20) yes C83 . C84 . H841 . 117.8 no C78 . C84 . H841 . 121.0 no C76 . C85 . C86 . 122.7(20) yes C76 . C85 . C90 . 117(2) yes C86 . C85 . C90 . 120(2) yes C85 . C86 . C87 . 116(2) yes C85 . C86 . H861 . 119.9 no C87 . C86 . H861 . 123.7 no C86 . C87 . C88 . 126(3) yes C86 . C87 . H871 . 117.6 no C88 . C87 . H871 . 116.5 no C87 . C88 . C89 . 123(4) yes C87 . C88 . H881 . 121.6 no C89 . C88 . H881 . 114.8 no C88 . C89 . C90 . 113(4) yes C88 . C89 . H891 . 125.7 no C90 . C89 . H891 . 121.6 no C89 . C90 . C85 . 121(3) yes C89 . C90 . H901 . 119.5 no C85 . C90 . H901 . 119.2 no Tb4 . O91 . C92 . 132.8(11) yes O91 . C92 . C93 . 123.8(17) yes O91 . C92 . C102 . 110.2(16) yes C93 . C92 . C102 . 125.8(18) yes C92 . C93 . C94 . 130.4(18) yes C92 . C93 . H931 . 114.9 no C94 . C93 . H931 . 114.8 no C93 . C94 . O95 . 120.4(16) yes C93 . C94 . C96 . 123.0(19) yes O95 . C94 . C96 . 116.3(18) yes C94 . O95 . Tb4 . 134.0(12) yes C94 . C96 . C97 . 120.8(19) yes C94 . C96 . C101 . 122.0(19) yes C97 . C96 . C101 . 116.9(20) yes C96 . C97 . C98 . 122(2) yes C96 . C97 . H971 . 118.5 no C98 . C97 . H971 . 119.2 no C97 . C98 . C99 . 117(3) yes C97 . C98 . H981 . 116.8 no C99 . C98 . H981 . 125.0 no C98 . C99 . C100 . 122(3) yes C98 . C99 . H991 . 114.9 no C100 . C99 . H991 . 122.7 no C99 . C100 . C101 . 125(3) yes C99 . C100 . H1001 . 120.5 no C101 . C100 . H1001 . 114.8 no C96 . C101 . C100 . 116(2) yes C96 . C101 . H1011 . 121.4 no C100 . C101 . H1011 . 122.6 no C92 . C102 . C103 . 123.1(18) yes C92 . C102 . C107 . 119.5(19) yes C103 . C102 . C107 . 117.3(20) yes C102 . C103 . C104 . 124(2) yes C102 . C103 . H1031 . 119.9 no C104 . C103 . H1031 . 115.7 no C103 . C104 . C105 . 116(2) yes C103 . C104 . H1041 . 123.4 no C105 . C104 . H1041 . 120.5 no C104 . C105 . C106 . 123(3) yes C104 . C105 . H1051 . 113.7 no C106 . C105 . H1051 . 122.7 no C105 . C106 . C107 . 117(3) yes C105 . C106 . H1061 . 120.5 no C107 . C106 . H1061 . 122.3 no C106 . C107 . C102 . 121(2) yes C106 . C107 . H1071 . 119.4 no C102 . C107 . H1071 . 119.6 no Tb5 . O108 . C109 . 131.8(11) yes O108 . C109 . C110 . 125.6(16) yes O108 . C109 . C113 . 117.2(17) yes C110 . C109 . C113 . 117.2(16) yes C109 . C110 . C111 . 123.7(16) yes C109 . C110 . H1101 . 118.4 no C111 . C110 . H1101 . 117.9 no C110 . C111 . O112 . 122.4(16) yes C110 . C111 . C119 . 117.9(18) yes O112 . C111 . C119 . 119.7(18) yes C111 . O112 . Tb5 . 134.4(12) yes C109 . C113 . C114 . 119.1(19) yes C109 . C113 . C118 . 120.8(18) yes C114 . C113 . C118 . 120.0(20) yes C113 . C114 . C115 . 122(2) yes C113 . C114 . H1141 . 118.7 no C115 . C114 . H1141 . 119.2 no C114 . C115 . C116 . 115(3) yes C114 . C115 . H1151 . 121.7 no C116 . C115 . H1151 . 122.8 no C115 . C116 . C117 . 124(3) yes C115 . C116 . H1161 . 115.4 no C117 . C116 . H1161 . 120.7 no C116 . C117 . C118 . 119(3) yes C116 . C117 . H1171 . 120.1 no C118 . C117 . H1171 . 120.3 no C113 . C118 . C117 . 119(2) yes C113 . C118 . H1181 . 120.5 no C117 . C118 . H1181 . 120.4 no C111 . C119 . C120 . 127(2) yes C111 . C119 . C124 . 114(2) yes C120 . C119 . C124 . 118(2) yes C119 . C120 . C121 . 125(2) yes C119 . C120 . H1191 . 116.8 no C121 . C120 . H1191 . 117.9 no C120 . C121 . C122 . 116(2) yes C120 . C121 . H1192 . 120.0 no C122 . C121 . H1192 . 123.7 no C121 . C122 . C123 . 124(3) yes C121 . C122 . H1193 . 115.4 no C123 . C122 . H1193 . 120.1 no C122 . C123 . C124 . 114(3) yes C122 . C123 . H1194 . 121.5 no C124 . C123 . H1194 . 123.9 no C123 . C124 . C119 . 122(3) yes C123 . C124 . H1195 . 117.6 no C119 . C124 . H1195 . 120.4 no Tb5 . O125 . C126 . 133.1(10) yes O125 . C126 . C127 . 122.8(15) yes O125 . C126 . C130 . 112.9(14) yes C127 . C126 . C130 . 124.2(16) yes C126 . C127 . C128 . 129.5(16) yes C126 . C127 . H1271 . 116.3 no C128 . C127 . H1271 . 114.2 no C127 . C128 . O129 . 121.2(14) yes C127 . C128 . C136 . 123.1(18) yes O129 . C128 . C136 . 115.5(17) yes C128 . O129 . Tb5 . 131.9(10) yes C126 . C130 . C131 . 119.7(17) yes C126 . C130 . C135 . 118.3(17) yes C131 . C130 . C135 . 121.9(18) yes C130 . C131 . C132 . 118.1(18) yes C130 . C131 . H1305 . 122.0 no C132 . C131 . H1305 . 119.8 no C131 . C132 . C133 . 119(2) yes C131 . C132 . H1304 . 118.6 no C133 . C132 . H1304 . 122.8 no C132 . C133 . C134 . 125(2) yes C132 . C133 . H1303 . 114.2 no C134 . C133 . H1303 . 121.0 no C133 . C134 . C135 . 116(2) yes C133 . C134 . H1302 . 121.6 no C135 . C134 . H1302 . 122.8 no C134 . C135 . C130 . 120.8(19) yes C134 . C135 . H1301 . 119.0 no C130 . C135 . H1301 . 120.2 no C128 . C136 . C137 . 127(3) yes C128 . C136 . C141 . 127(2) yes C137 . C136 . C141 . 107(3) yes C136 . C137 . C138 . 128(4) yes C136 . C137 . H1371 . 111.1 no C138 . C137 . H1371 . 115.8 no C137 . C138 . C139 . 116(4) yes C137 . C138 . H1381 . 122.1 no C139 . C138 . H1381 . 116.7 no C138 . C139 . C140 . 118(4) yes C138 . C139 . H1391 . 122.2 no C140 . C139 . H1391 . 116.6 no C139 . C140 . C141 . 113(3) yes C139 . C140 . H1401 . 121.4 no C141 . C140 . H1401 . 125.5 no C140 . C141 . C136 . 131(3) yes C140 . C141 . H1411 . 113.6 no C136 . C141 . H1411 . 115.3 no Tb1 . O142 . C143 . 131.3(11) yes O142 . C143 . C144 . 126.5(16) yes O142 . C143 . C147 . 114.7(18) yes C144 . C143 . C147 . 118.6(18) yes C143 . C144 . C145 . 126.6(17) yes C143 . C144 . H1441 . 118.7 no C145 . C144 . H1441 . 114.6 no C144 . C145 . O146 . 121.3(15) yes C144 . C145 . C153 . 121.0(16) yes O146 . C145 . C153 . 117.7(15) yes Tb4 . O146 . C145 . 124.1(9) yes Tb4 . O146 . Tb1 . 94.7(3) yes C145 . O146 . Tb1 . 126.1(9) yes C143 . C147 . C148 . 120(2) yes C143 . C147 . C152 . 118(2) yes C148 . C147 . C152 . 122(2) yes C147 . C148 . C149 . 129(3) yes C147 . C148 . H1481 . 115.5 no C149 . C148 . H1481 . 114.8 no C148 . C149 . C150 . 103(3) yes C148 . C149 . H1491 . 125.6 no C150 . C149 . H1491 . 131.5 no C149 . C150 . C151 . 139(4) yes C149 . C150 . H1501 . 106.2 no C151 . C150 . H1501 . 114.0 no C150 . C151 . C152 . 113(3) yes C150 . C151 . H1511 . 128.7 no C152 . C151 . H1511 . 116.6 no C151 . C152 . C147 . 113(2) yes C151 . C152 . H1521 . 121.7 no C147 . C152 . H1521 . 124.5 no C145 . C153 . C154 . 117.3(17) yes C145 . C153 . C158 . 123.0(18) yes C154 . C153 . C158 . 119.7(19) yes C153 . C154 . C155 . 120.8(18) yes C153 . C154 . H1535 . 120.5 no C155 . C154 . H1535 . 118.5 no C154 . C155 . C156 . 115.0(19) yes C154 . C155 . H1534 . 118.9 no C156 . C155 . H1534 . 126.0 no C155 . C156 . C157 . 123(3) yes C155 . C156 . H1533 . 116.0 no C157 . C156 . H1533 . 121.2 no C156 . C157 . C158 . 121(3) yes C156 . C157 . H1532 . 115.5 no C158 . C157 . H1532 . 122.5 no C157 . C158 . C153 . 120(2) yes C157 . C158 . H1531 . 116.9 no C153 . C158 . H1531 . 121.9 no Tb3 . O159 . C160 . 132.7(11) yes O159 . C160 . C161 . 120.7(15) yes O159 . C160 . C164 . 117.2(16) yes C161 . C160 . C164 . 121.9(16) yes C160 . C161 . C162 . 130.1(15) yes C160 . C161 . H1611 . 114.2 no C162 . C161 . H1611 . 115.6 no C161 . C162 . O163 . 120.7(15) yes C161 . C162 . C170 . 126.1(15) yes O163 . C162 . C170 . 113.2(14) yes Tb1 . O163 . C162 . 124.7(9) yes Tb1 . O163 . Tb3 . 96.2(3) yes C162 . O163 . Tb3 . 124.0(10) yes C160 . C164 . C165 . 119.4(17) yes C160 . C164 . C169 . 118.0(17) yes C165 . C164 . C169 . 122.3(18) yes C164 . C165 . C166 . 118(2) yes C164 . C165 . H1651 . 119.2 no C166 . C165 . H1651 . 122.3 no C165 . C166 . C167 . 117(2) yes C165 . C166 . H1661 . 117.4 no C167 . C166 . H1661 . 125.0 no C166 . C167 . C168 . 127(2) yes C166 . C167 . H1671 . 115.6 no C168 . C167 . H1671 . 116.9 no C167 . C168 . C169 . 118(2) yes C167 . C168 . H1681 . 123.6 no C169 . C168 . H1681 . 118.6 no C168 . C169 . C164 . 116.6(18) yes C168 . C169 . H1691 . 120.8 no C164 . C169 . H1691 . 122.5 no C162 . C170 . C171 . 119.9(15) yes C162 . C170 . C175 . 123.7(15) yes C171 . C170 . C175 . 116.4(16) yes C170 . C171 . C172 . 121.3(17) yes C170 . C171 . H1711 . 120.4 no C172 . C171 . H1711 . 118.3 no C171 . C172 . C173 . 116.0(18) yes C171 . C172 . H1721 . 120.0 no C173 . C172 . H1721 . 124.0 no C172 . C173 . C174 . 125.2(20) yes C172 . C173 . H1731 . 115.0 no C174 . C173 . H1731 . 119.6 no C173 . C174 . C175 . 117.2(18) yes C173 . C174 . H1741 . 122.4 no C175 . C174 . H1741 . 120.2 no C174 . C175 . C170 . 123.4(17) yes C174 . C175 . H1751 . 118.8 no C170 . C175 . H1751 . 117.7 no Tb1 . O176 . C177 . 135.3(10) yes O176 . C177 . C178 . 121.2(16) yes O176 . C177 . C182 . 116.1(15) yes C178 . C177 . C182 . 122.3(17) yes C177 . C178 . C179 . 128.1(18) yes C177 . C178 . H1781 . 115.1 no C179 . C178 . H1781 . 116.8 no C178 . C179 . O180 . 125.0(16) yes C178 . C179 . C188 . 123.7(17) yes O180 . C179 . C188 . 111.2(15) yes C179 . O180 . Tb1 . 133.0(10) yes C177 . C182 . C183 . 121.6(19) yes C177 . C182 . C187 . 119.4(19) yes C183 . C182 . C187 . 118(2) yes C182 . C183 . C184 . 126(2) yes C182 . C183 . H1825 . 119.1 no C184 . C183 . H1825 . 114.5 no C183 . C184 . C185 . 114(3) yes C183 . C184 . H1824 . 125.8 no C185 . C184 . H1824 . 120.2 no C184 . C185 . C186 . 126(3) yes C184 . C185 . H1823 . 115.2 no C186 . C185 . H1823 . 114.2 no C185 . C186 . C187 . 121(3) yes C185 . C186 . H1822 . 119.2 no C187 . C186 . H1822 . 114.4 no C182 . C187 . C186 . 113(3) yes C182 . C187 . H1821 . 118.3 no C186 . C187 . H1821 . 128.4 no C179 . C188 . C189 . 124.2(19) yes C179 . C188 . C193 . 115.0(19) yes C189 . C188 . C193 . 121(2) yes C188 . C189 . C190 . 122(2) yes C188 . C189 . H1891 . 118.6 no C190 . C189 . H1891 . 119.2 no C189 . C190 . C191 . 115(2) yes C189 . C190 . H1901 . 118.6 no C191 . C190 . H1901 . 125.9 no C190 . C191 . C192 . 128(3) yes C190 . C191 . H1911 . 112.3 no C192 . C191 . H1911 . 119.3 no C191 . C192 . C193 . 118(3) yes C191 . C192 . H1921 . 121.2 no C193 . C192 . H1921 . 120.2 no C192 . C193 . C188 . 115(2) yes C192 . C193 . H1931 . 123.3 no C188 . C193 . H1931 . 122.0 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O14 . H141 . O180 . 135 0.82 2.18 2.82(3) yes C151 . H1511 . C62 4_565 156 1.20 2.55 3.67(3) yes C191 . H1911 . O125 3_655 158 0.96 2.59 3.50(3) yes # Attachment 'publication-Eu5.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 730241' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 22.0525(7) _cell_length_b 17.3193(7) _cell_length_c 35.4127(13) _cell_angle_alpha 90 _cell_angle_beta 101.051(2) _cell_angle_gamma 90 _cell_volume 13274.5(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Eu -0.1578 3.6682 24.6274 2.3879 19.0886 0.1942 13.7603 13.7546 2.9227 123.1740 2.5745 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C75 H55 Eu5 O10 # Dc = 1.88 Fooo = 6120.00 Mu = 47.14 M = 3752.11 # Found Formula = C75 H57.50 Eu2.50 O12.50 # Dc = 1.54 FOOO = 6120.00 Mu = 23.99 M = 3077.35 _chemical_formula_sum 'C150 H115 Eu5 O25' _chemical_formula_moiety 'C150 H115 Eu5 O25' _chemical_compound_source ? _chemical_formula_weight 3077.3 _cell_measurement_reflns_used 14358 _cell_measurement_theta_min 0 _cell_measurement_theta_max 24 _cell_measurement_temperature 293 _exptl_crystal_description cubic _exptl_crystal_colour colourless _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_max 0.03 _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 6120 _exptl_absorpt_coefficient_mu 2.399 # Sheldrick geometric approximatio 0.93 0.94 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9328 _exptl_absorpt_correction_T_max 0.9373 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 32579 _reflns_number_total 20307 _diffrn_reflns_av_R_equivalents 0.051 # Number of reflections with Friedels Law is 20307 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 21068 _diffrn_reflns_theta_min 0.941 _diffrn_reflns_theta_max 24.093 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 18.070 _diffrn_measured_fraction_theta_full 0.978 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _reflns_limit_h_min -25 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 40 #_oxford_diffrn_Wilson_B_factor 0.00 #_oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.49 _refine_diff_density_max 1.28 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement #_oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 10326 _refine_ls_number_restraints 0 _refine_ls_number_parameters 1621 #_oxford_refine_ls_R_factor_ref 0.0544 _refine_ls_wR_factor_ref 0.0569 _refine_ls_goodness_of_fit_ref 1.0834 _refine_ls_shift/su_max 0.000740 # The values computed from all data #_oxford_reflns_number_all 20183 _refine_ls_R_factor_all 0.1112 _refine_ls_wR_factor_all 0.1141 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 11062 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_gt 0.0592 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.305 0.204 0.131 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Eu1 Eu 0.23992(3) 0.90080(4) 0.17632(2) 0.0424 1.0000 Uani . . . . . . . Eu2 Eu 0.22652(3) 0.70259(4) 0.06932(2) 0.0436 1.0000 Uani . . . . . . . Eu3 Eu 0.29439(3) 0.89543(3) 0.08521(2) 0.0432 1.0000 Uani . . . . . . . Eu4 Eu 0.18108(3) 0.70579(4) 0.16194(2) 0.0434 1.0000 Uani . . . . . . . Eu5 Eu 0.35620(3) 0.73798(3) 0.16104(2) 0.0444 1.0000 Uani . . . . . . . O1 O 0.2128(3) 0.8084(4) 0.1184(2) 0.0415 1.0000 Uani . . . . . . . O11 O 0.2649(4) 0.6624(4) 0.1331(3) 0.0440 1.0000 Uani . . . . . . . O12 O 0.2697(4) 0.7709(4) 0.1926(3) 0.0444 1.0000 Uani . . . . . . . O13 O 0.3229(4) 0.7654(5) 0.0933(3) 0.0508 1.0000 Uani . . . . . . . O14 O 0.3297(3) 0.8764(4) 0.1513(2) 0.0386 1.0000 Uani . . . . . . . O21 O 0.2855(4) 0.7035(4) 0.0196(3) 0.0464 1.0000 Uani . . . . . . . C22 C 0.2816(6) 0.7416(8) -0.0108(4) 0.0513 1.0000 Uani . . . . . . . C23 C 0.2372(6) 0.8024(8) -0.0225(4) 0.0509 1.0000 Uani . . . . . . . C24 C 0.2057(6) 0.8421(7) 0.0011(4) 0.0473 1.0000 Uani . . . . . . . O25 O 0.2151(4) 0.8269(4) 0.0395(3) 0.0453 1.0000 Uani . . . . . . . C26 C 0.3266(6) 0.7257(8) -0.0356(4) 0.0498 1.0000 Uani . . . . . . . C27 C 0.3547(7) 0.6541(8) -0.0331(5) 0.0588 1.0000 Uani . . . . . . . C28 C 0.4014(7) 0.6403(9) -0.0532(4) 0.0656 1.0000 Uani . . . . . . . C29 C 0.4228(7) 0.6973(11) -0.0749(5) 0.0737 1.0000 Uani . . . . . . . C30 C 0.3935(7) 0.7683(9) -0.0785(5) 0.0631 1.0000 Uani . . . . . . . C31 C 0.3462(6) 0.7828(8) -0.0580(4) 0.0554 1.0000 Uani . . . . . . . C32 C 0.1626(6) 0.9052(7) -0.0121(4) 0.0460 1.0000 Uani . . . . . . . C33 C 0.1594(6) 0.9411(8) -0.0463(4) 0.0500 1.0000 Uani . . . . . . . C34 C 0.1206(6) 1.0041(8) -0.0573(4) 0.0556 1.0000 Uani . . . . . . . C35 C 0.0830(6) 1.0304(8) -0.0327(5) 0.0561 1.0000 Uani . . . . . . . C36 C 0.0847(6) 0.9953(8) 0.0021(4) 0.0553 1.0000 Uani . . . . . . . C37 C 0.1235(6) 0.9324(8) 0.0126(4) 0.0545 1.0000 Uani . . . . . . . O38 O 0.3724(4) 0.8749(5) 0.0499(3) 0.0496 1.0000 Uani . . . . . . . C39 C 0.3901(6) 0.9054(8) 0.0216(4) 0.0523 1.0000 Uani . . . . . . . C40 C 0.3618(6) 0.9676(8) 0.0007(5) 0.0580 1.0000 Uani . . . . . . . C41 C 0.3076(7) 1.0023(8) 0.0066(4) 0.0543 1.0000 Uani . . . . . . . O42 O 0.2794(4) 0.9815(5) 0.0342(3) 0.0512 1.0000 Uani . . . . . . . C43 C 0.4475(7) 0.8687(8) 0.0109(5) 0.0597 1.0000 Uani . . . . . . . C44 C 0.4668(6) 0.7991(9) 0.0253(5) 0.0665 1.0000 Uani . . . . . . . C45 C 0.5181(8) 0.7625(10) 0.0183(5) 0.0770 1.0000 Uani . . . . . . . C46 C 0.5520(8) 0.7980(13) -0.0053(7) 0.0921 1.0000 Uani . . . . . . . C47 C 0.5347(8) 0.8682(13) -0.0200(5) 0.0814 1.0000 Uani . . . . . . . C48 C 0.4806(7) 0.9070(9) -0.0132(5) 0.0638 1.0000 Uani . . . . . . . C49 C 0.2772(6) 1.0668(7) -0.0177(4) 0.0525 1.0000 Uani . . . . . . . C50 C 0.2889(8) 1.0822(10) -0.0548(6) 0.0832 1.0000 Uani . . . . . . . C51 C 0.2573(10) 1.1421(11) -0.0753(6) 0.0871 1.0000 Uani . . . . . . . C52 C 0.2169(9) 1.1861(10) -0.0619(6) 0.0839 1.0000 Uani . . . . . . . C53 C 0.2037(7) 1.1718(9) -0.0269(6) 0.0769 1.0000 Uani . . . . . . . C54 C 0.2337(7) 1.1122(8) -0.0049(5) 0.0617 1.0000 Uani . . . . . . . O55 O 0.2335(4) 0.5717(5) 0.0612(3) 0.0522 1.0000 Uani . . . . . . . C56 C 0.2190(7) 0.5260(7) 0.0318(4) 0.0564 1.0000 Uani . . . . . . . C57 C 0.1826(7) 0.5480(7) -0.0035(4) 0.0514 1.0000 Uani . . . . . . . C58 C 0.1489(6) 0.6169(7) -0.0108(4) 0.0519 1.0000 Uani . . . . . . . O59 O 0.1537(4) 0.6727(4) 0.0130(3) 0.0466 1.0000 Uani . . . . . . . C60 C 0.1058(6) 0.6281(8) -0.0486(4) 0.0509 1.0000 Uani . . . . . . . C61 C 0.0851(7) 0.7013(9) -0.0591(5) 0.0659 1.0000 Uani . . . . . . . C62 C 0.0484(7) 0.7136(10) -0.0949(5) 0.0754 1.0000 Uani . . . . . . . C63 C 0.0287(7) 0.6538(9) -0.1199(5) 0.0622 1.0000 Uani . . . . . . . C64 C 0.0476(7) 0.5801(8) -0.1084(4) 0.0645 1.0000 Uani . . . . . . . C65 C 0.0868(6) 0.5665(8) -0.0738(4) 0.0558 1.0000 Uani . . . . . . . C66 C 0.2446(6) 0.4461(7) 0.0366(5) 0.0527 1.0000 Uani . . . . . . . C67 C 0.2533(7) 0.4127(8) 0.0723(5) 0.0638 1.0000 Uani . . . . . . . C68 C 0.2729(8) 0.3364(9) 0.0789(5) 0.0720 1.0000 Uani . . . . . . . C69 C 0.2878(8) 0.2954(10) 0.0485(7) 0.0885 1.0000 Uani . . . . . . . C70 C 0.2817(8) 0.3291(10) 0.0124(6) 0.0805 1.0000 Uani . . . . . . . C72 C 0.2599(7) 0.4031(8) 0.0066(5) 0.0658 1.0000 Uani . . . . . . . O73 O 0.1322(3) 0.6783(4) 0.0960(3) 0.0411 1.0000 Uani . . . . . . . C74 C 0.0934(6) 0.6219(7) 0.0858(4) 0.0507 1.0000 Uani . . . . . . . C75 C 0.0976(6) 0.5479(8) 0.1008(5) 0.0623 1.0000 Uani . . . . . . . C76 C 0.1443(6) 0.5246(7) 0.1341(4) 0.0466 1.0000 Uani . . . . . . . O77 O 0.1773(4) 0.5708(5) 0.1557(3) 0.0471 1.0000 Uani . . . . . . . C78 C 0.0385(6) 0.6419(8) 0.0553(5) 0.0594 1.0000 Uani . . . . . . . C79 C -0.0002(7) 0.5859(8) 0.0354(5) 0.0732 1.0000 Uani . . . . . . . C80 C -0.0522(8) 0.6069(11) 0.0073(5) 0.0807 1.0000 Uani . . . . . . . C82 C -0.0653(7) 0.6829(11) 0.0000(5) 0.0751 1.0000 Uani . . . . . . . C83 C -0.0281(9) 0.7379(10) 0.0196(5) 0.0861 1.0000 Uani . . . . . . . C84 C 0.0256(8) 0.7184(8) 0.0477(5) 0.0701 1.0000 Uani . . . . . . . C85 C 0.1522(6) 0.4404(7) 0.1423(5) 0.0561 1.0000 Uani . . . . . . . C86 C 0.1215(6) 0.3824(7) 0.1205(5) 0.0664 1.0000 Uani . . . . . . . C87 C 0.1328(7) 0.3057(8) 0.1304(6) 0.0867 1.0000 Uani . . . . . . . C88 C 0.1760(9) 0.2844(8) 0.1612(6) 0.0869 1.0000 Uani . . . . . . . C89 C 0.2077(9) 0.3411(10) 0.1831(6) 0.0965 1.0000 Uani . . . . . . . C90 C 0.1957(9) 0.4188(8) 0.1745(6) 0.0855 1.0000 Uani . . . . . . . O91 O 0.1856(4) 0.6781(5) 0.2266(3) 0.0525 1.0000 Uani . . . . . . . C92 C 0.1523(7) 0.6447(7) 0.2460(4) 0.0561 1.0000 Uani . . . . . . . C93 C 0.0885(7) 0.6254(8) 0.2311(5) 0.0612 1.0000 Uani . . . . . . . C94 C 0.0571(6) 0.6405(8) 0.1939(5) 0.0524 1.0000 Uani . . . . . . . O95 O 0.0808(4) 0.6772(5) 0.1688(3) 0.0517 1.0000 Uani . . . . . . . C96 C -0.0092(7) 0.6155(8) 0.1802(5) 0.0611 1.0000 Uani . . . . . . . C97 C -0.0402(6) 0.6357(8) 0.1437(5) 0.0582 1.0000 Uani . . . . . . . C98 C -0.1007(8) 0.6153(9) 0.1304(6) 0.0811 1.0000 Uani . . . . . . . C99 C -0.1300(8) 0.5712(10) 0.1545(7) 0.0877 1.0000 Uani . . . . . . . C100 C -0.1003(10) 0.5497(13) 0.1901(6) 0.0979 1.0000 Uani . . . . . . . C101 C -0.0404(8) 0.5707(11) 0.2037(6) 0.0860 1.0000 Uani . . . . . . . C102 C 0.1784(7) 0.6296(8) 0.2873(5) 0.0602 1.0000 Uani . . . . . . . C103 C 0.2326(8) 0.6677(9) 0.3037(5) 0.0659 1.0000 Uani . . . . . . . C104 C 0.2592(8) 0.6542(10) 0.3428(5) 0.0744 1.0000 Uani . . . . . . . C105 C 0.2365(9) 0.5989(13) 0.3629(6) 0.0906 1.0000 Uani . . . . . . . C106 C 0.1840(9) 0.5604(12) 0.3465(5) 0.0840 1.0000 Uani . . . . . . . C107 C 0.1542(7) 0.5734(10) 0.3085(5) 0.0734 1.0000 Uani . . . . . . . O108 O 0.3618(4) 0.6297(5) 0.2029(2) 0.0481 1.0000 Uani . . . . . . . C109 C 0.3638(6) 0.5576(7) 0.1962(4) 0.0509 1.0000 Uani . . . . . . . C110 C 0.3753(7) 0.5248(8) 0.1621(5) 0.0598 1.0000 Uani . . . . . . . C111 C 0.3969(6) 0.5649(8) 0.1329(4) 0.0496 1.0000 Uani . . . . . . . O112 O 0.4037(4) 0.6382(5) 0.1328(3) 0.0552 1.0000 Uani . . . . . . . C113 C 0.3497(7) 0.5049(8) 0.2273(4) 0.0586 1.0000 Uani . . . . . . . C114 C 0.3121(8) 0.5313(9) 0.2512(5) 0.0732 1.0000 Uani . . . . . . . C115 C 0.2956(8) 0.4825(11) 0.2801(5) 0.0802 1.0000 Uani . . . . . . . C116 C 0.3219(9) 0.4099(10) 0.2837(6) 0.0870 1.0000 Uani . . . . . . . C117 C 0.3616(7) 0.3841(9) 0.2608(5) 0.0664 1.0000 Uani . . . . . . . C118 C 0.3746(7) 0.4309(8) 0.2324(4) 0.0554 1.0000 Uani . . . . . . . C119 C 0.4127(6) 0.5226(8) 0.0995(4) 0.0577 1.0000 Uani . . . . . . . C120 C 0.4115(6) 0.4441(8) 0.0959(5) 0.0617 1.0000 Uani . . . . . . . C121 C 0.4260(8) 0.4044(9) 0.0655(5) 0.0706 1.0000 Uani . . . . . . . C122 C 0.4430(9) 0.4461(11) 0.0364(5) 0.0818 1.0000 Uani . . . . . . . C123 C 0.4455(9) 0.5252(12) 0.0385(6) 0.0973 1.0000 Uani . . . . . . . C124 C 0.4309(9) 0.5640(9) 0.0705(5) 0.0794 1.0000 Uani . . . . . . . O125 O 0.4011(4) 0.7872(5) 0.2217(3) 0.0514 1.0000 Uani . . . . . . . C126 C 0.4336(6) 0.8474(7) 0.2325(4) 0.0488 1.0000 Uani . . . . . . . C127 C 0.4690(6) 0.8861(7) 0.2087(4) 0.0474 1.0000 Uani . . . . . . . C128 C 0.4749(5) 0.8617(7) 0.1714(4) 0.0438 1.0000 Uani . . . . . . . O129 O 0.4503(3) 0.8016(5) 0.1548(3) 0.0459 1.0000 Uani . . . . . . . C130 C 0.4341(6) 0.8744(7) 0.2719(4) 0.0463 1.0000 Uani . . . . . . . C131 C 0.4620(6) 0.9406(8) 0.2879(4) 0.0528 1.0000 Uani . . . . . . . C132 C 0.4594(7) 0.9655(8) 0.3241(5) 0.0602 1.0000 Uani . . . . . . . C133 C 0.4265(7) 0.9218(10) 0.3461(4) 0.0603 1.0000 Uani . . . . . . . C134 C 0.3961(7) 0.8539(9) 0.3310(5) 0.0670 1.0000 Uani . . . . . . . C135 C 0.4010(7) 0.8311(9) 0.2943(4) 0.0598 1.0000 Uani . . . . . . . C136 C 0.5150(6) 0.9086(8) 0.1501(4) 0.0515 1.0000 Uani . . . . . . . C137 C 0.5274(9) 0.8799(12) 0.1174(6) 0.1015 1.0000 Uani . . . . . . . C138 C 0.5648(10) 0.9234(13) 0.0967(5) 0.1072 1.0000 Uani . . . . . . . C139 C 0.5869(8) 0.9945(11) 0.1083(5) 0.0841 1.0000 Uani . . . . . . . C140 C 0.5748(9) 1.0206(9) 0.1414(6) 0.0834 1.0000 Uani . . . . . . . C141 C 0.5382(9) 0.9804(9) 0.1620(6) 0.0828 1.0000 Uani . . . . . . . O142 O 0.2319(4) 0.8809(5) 0.2412(3) 0.0508 1.0000 Uani . . . . . . . C143 C 0.1872(6) 0.8756(8) 0.2582(4) 0.0526 1.0000 Uani . . . . . . . C144 C 0.1241(6) 0.8663(8) 0.2381(4) 0.0480 1.0000 Uani . . . . . . . C145 C 0.1039(6) 0.8515(7) 0.1995(4) 0.0473 1.0000 Uani . . . . . . . O146 O 0.1427(4) 0.8370(5) 0.1760(3) 0.0477 1.0000 Uani . . . . . . . C147 C 0.2014(7) 0.8799(9) 0.3014(4) 0.0583 1.0000 Uani . . . . . . . C148 C 0.2514(8) 0.9206(11) 0.3191(5) 0.0781 1.0000 Uani . . . . . . . C149 C 0.2656(8) 0.9287(14) 0.3574(6) 0.0968 1.0000 Uani . . . . . . . C150 C 0.2309(11) 0.8878(18) 0.3795(6) 0.1148 1.0000 Uani . . . . . . . C151 C 0.1815(11) 0.8445(14) 0.3638(6) 0.1024 1.0000 Uani . . . . . . . C152 C 0.1655(8) 0.8389(11) 0.3222(5) 0.0832 1.0000 Uani . . . . . . . C153 C 0.0385(6) 0.8547(7) 0.1812(5) 0.0522 1.0000 Uani . . . . . . . C154 C 0.0185(6) 0.8335(8) 0.1433(5) 0.0558 1.0000 Uani . . . . . . . C155 C -0.0431(8) 0.8375(8) 0.1259(5) 0.0676 1.0000 Uani . . . . . . . C156 C -0.0863(8) 0.8605(10) 0.1472(6) 0.0755 1.0000 Uani . . . . . . . C157 C -0.0698(8) 0.8828(11) 0.1849(6) 0.0873 1.0000 Uani . . . . . . . C158 C -0.0053(7) 0.8800(10) 0.2022(5) 0.0728 1.0000 Uani . . . . . . . O159 O 0.3414(4) 1.0134(5) 0.1118(3) 0.0521 1.0000 Uani . . . . . . . C160 C 0.3190(6) 1.0778(7) 0.1166(4) 0.0484 1.0000 Uani . . . . . . . C161 C 0.2521(6) 1.0932(6) 0.1100(4) 0.0433 1.0000 Uani . . . . . . . C162 C 0.2083(5) 1.0393(7) 0.1066(4) 0.0416 1.0000 Uani . . . . . . . O163 O 0.2198(4) 0.9644(5) 0.1125(3) 0.0496 1.0000 Uani . . . . . . . C164 C 0.3609(6) 1.1430(7) 0.1300(4) 0.0504 1.0000 Uani . . . . . . . C165 C 0.4221(7) 1.1411(8) 0.1242(5) 0.0615 1.0000 Uani . . . . . . . C166 C 0.4628(7) 1.2002(10) 0.1363(5) 0.0704 1.0000 Uani . . . . . . . C167 C 0.4442(8) 1.2604(9) 0.1581(5) 0.0730 1.0000 Uani . . . . . . . C168 C 0.3840(8) 1.2621(9) 0.1649(5) 0.0758 1.0000 Uani . . . . . . . C169 C 0.3435(7) 1.2046(8) 0.1510(4) 0.0570 1.0000 Uani . . . . . . . C170 C 0.1422(6) 1.0607(7) 0.0967(4) 0.0477 1.0000 Uani . . . . . . . C171 C 0.1210(7) 1.1303(8) 0.0781(5) 0.0612 1.0000 Uani . . . . . . . C172 C 0.0595(7) 1.1479(7) 0.0699(5) 0.0696 1.0000 Uani . . . . . . . C173 C 0.0164(6) 1.0966(8) 0.0781(4) 0.0529 1.0000 Uani . . . . . . . C174 C 0.0353(6) 1.0282(7) 0.0967(4) 0.0520 1.0000 Uani . . . . . . . C175 C 0.0973(5) 1.0099(7) 0.1050(4) 0.0463 1.0000 Uani . . . . . . . O176 O 0.1792(4) 1.0050(4) 0.1886(2) 0.0465 1.0000 Uani . . . . . . . C177 C 0.1896(6) 1.0662(7) 0.2095(4) 0.0465 1.0000 Uani . . . . . . . C178 C 0.2475(7) 1.0921(7) 0.2271(4) 0.0551 1.0000 Uani . . . . . . . C179 C 0.3021(7) 1.0574(8) 0.2227(4) 0.0544 1.0000 Uani . . . . . . . O180 O 0.3077(4) 0.9962(5) 0.2028(3) 0.0494 1.0000 Uani . . . . . . . C182 C 0.1318(7) 1.1114(8) 0.2116(5) 0.0591 1.0000 Uani . . . . . . . C183 C 0.0757(7) 1.0900(10) 0.1928(5) 0.0715 1.0000 Uani . . . . . . . C184 C 0.0236(8) 1.1325(13) 0.1925(6) 0.0910 1.0000 Uani . . . . . . . C185 C 0.0255(11) 1.1958(13) 0.2148(8) 0.1108 1.0000 Uani . . . . . . . C186 C 0.0788(13) 1.2193(11) 0.2354(11) 0.1546 1.0000 Uani . . . . . . . C187 C 0.1338(9) 1.1776(11) 0.2351(7) 0.1042 1.0000 Uani . . . . . . . C188 C 0.3639(7) 1.0949(7) 0.2410(5) 0.0586 1.0000 Uani . . . . . . . C189 C 0.4141(7) 1.0861(7) 0.2230(5) 0.0639 1.0000 Uani . . . . . . . C190 C 0.4704(9) 1.1210(10) 0.2378(6) 0.0868 1.0000 Uani . . . . . . . C191 C 0.4758(9) 1.1645(10) 0.2702(8) 0.0960 1.0000 Uani . . . . . . . C192 C 0.4277(10) 1.1732(9) 0.2887(5) 0.0821 1.0000 Uani . . . . . . . C193 C 0.3706(8) 1.1394(8) 0.2749(5) 0.0754 1.0000 Uani . . . . . . . H231 H 0.2278 0.8169 -0.0507 0.0623 1.0000 Uiso . . . . . . . H271 H 0.3407 0.6116 -0.0169 0.0692 1.0000 Uiso . . . . . . . H281 H 0.4208 0.5869 -0.0526 0.0805 1.0000 Uiso . . . . . . . H291 H 0.4595 0.6867 -0.0874 0.0861 1.0000 Uiso . . . . . . . H301 H 0.4074 0.8099 -0.0958 0.0804 1.0000 Uiso . . . . . . . H311 H 0.3257 0.8363 -0.0599 0.0686 1.0000 Uiso . . . . . . . H331 H 0.1865 0.9210 -0.0645 0.0613 1.0000 Uiso . . . . . . . H341 H 0.1193 1.0315 -0.0832 0.0655 1.0000 Uiso . . . . . . . H351 H 0.0547 1.0754 -0.0406 0.0622 1.0000 Uiso . . . . . . . H361 H 0.0572 1.0159 0.0198 0.0655 1.0000 Uiso . . . . . . . H371 H 0.1245 0.9045 0.0381 0.0643 1.0000 Uiso . . . . . . . H401 H 0.3817 0.9882 -0.0211 0.0730 1.0000 Uiso . . . . . . . H441 H 0.4393 0.7711 0.0413 0.0810 1.0000 Uiso . . . . . . . H451 H 0.5316 0.7103 0.0309 0.0957 1.0000 Uiso . . . . . . . H461 H 0.5884 0.7728 -0.0136 0.1042 1.0000 Uiso . . . . . . . H471 H 0.5610 0.8945 -0.0371 0.0976 1.0000 Uiso . . . . . . . H481 H 0.4677 0.9587 -0.0251 0.0804 1.0000 Uiso . . . . . . . H501 H 0.3197 1.0505 -0.0659 0.0965 1.0000 Uiso . . . . . . . H511 H 0.2643 1.1522 -0.1025 0.1044 1.0000 Uiso . . . . . . . H521 H 0.1971 1.2304 -0.0780 0.0920 1.0000 Uiso . . . . . . . H531 H 0.1720 1.2044 -0.0171 0.0864 1.0000 Uiso . . . . . . . H541 H 0.2238 1.1009 0.0217 0.0752 1.0000 Uiso . . . . . . . H571 H 0.1798 0.5106 -0.0260 0.0611 1.0000 Uiso . . . . . . . H611 H 0.0967 0.7468 -0.0406 0.0805 1.0000 Uiso . . . . . . . H621 H 0.0353 0.7681 -0.1036 0.0855 1.0000 Uiso . . . . . . . H631 H 0.0006 0.6642 -0.1466 0.0779 1.0000 Uiso . . . . . . . H641 H 0.0321 0.5350 -0.1263 0.0762 1.0000 Uiso . . . . . . . H651 H 0.1023 0.5119 -0.0663 0.0666 1.0000 Uiso . . . . . . . H671 H 0.2451 0.4454 0.0949 0.0734 1.0000 Uiso . . . . . . . H681 H 0.2755 0.3112 0.1053 0.0832 1.0000 Uiso . . . . . . . H691 H 0.3033 0.2400 0.0526 0.1025 1.0000 Uiso . . . . . . . H701 H 0.2935 0.2993 -0.0106 0.0982 1.0000 Uiso . . . . . . . H721 H 0.2536 0.4271 -0.0205 0.0822 1.0000 Uiso . . . . . . . H751 H 0.0661 0.5079 0.0890 0.0704 1.0000 Uiso . . . . . . . H791 H 0.0092 0.5290 0.0411 0.0878 1.0000 Uiso . . . . . . . H801 H -0.0785 0.5653 -0.0076 0.0963 1.0000 Uiso . . . . . . . H821 H -0.1027 0.7004 -0.0204 0.0874 1.0000 Uiso . . . . . . . H831 H -0.0390 0.7935 0.0145 0.0979 1.0000 Uiso . . . . . . . H841 H 0.0541 0.7605 0.0605 0.0858 1.0000 Uiso . . . . . . . H861 H 0.0878 0.3963 0.0978 0.0824 1.0000 Uiso . . . . . . . H871 H 0.1101 0.2646 0.1127 0.0976 1.0000 Uiso . . . . . . . H881 H 0.1843 0.2278 0.1679 0.1010 1.0000 Uiso . . . . . . . H891 H 0.2423 0.3270 0.2061 0.1092 1.0000 Uiso . . . . . . . H901 H 0.2186 0.4602 0.1915 0.0965 1.0000 Uiso . . . . . . . H931 H 0.0636 0.5993 0.2491 0.0774 1.0000 Uiso . . . . . . . H971 H -0.0159 0.6675 0.1271 0.0670 1.0000 Uiso . . . . . . . H981 H -0.1229 0.6305 0.1028 0.0980 1.0000 Uiso . . . . . . . H991 H -0.1755 0.5571 0.1453 0.1092 1.0000 Uiso . . . . . . . H1001 H -0.1223 0.5146 0.2067 0.1109 1.0000 Uiso . . . . . . . H1011 H -0.0171 0.5561 0.2306 0.0995 1.0000 Uiso . . . . . . . H1031 H 0.2526 0.7045 0.2871 0.0755 1.0000 Uiso . . . . . . . H1041 H 0.2951 0.6881 0.3562 0.0892 1.0000 Uiso . . . . . . . H1051 H 0.2589 0.5860 0.3905 0.1091 1.0000 Uiso . . . . . . . H1061 H 0.1655 0.5209 0.3631 0.0985 1.0000 Uiso . . . . . . . H1071 H 0.1157 0.5439 0.2965 0.0933 1.0000 Uiso . . . . . . . H1101 H 0.3687 0.4675 0.1586 0.0710 1.0000 Uiso . . . . . . . H1141 H 0.2973 0.5868 0.2493 0.0858 1.0000 Uiso . . . . . . . H1151 H 0.2641 0.5000 0.2962 0.0963 1.0000 Uiso . . . . . . . H1161 H 0.3111 0.3740 0.3043 0.0974 1.0000 Uiso . . . . . . . H1171 H 0.3811 0.3307 0.2651 0.0772 1.0000 Uiso . . . . . . . H1181 H 0.4025 0.4124 0.2146 0.0633 1.0000 Uiso . . . . . . . H1201 H 0.3991 0.4134 0.1178 0.0735 1.0000 Uiso . . . . . . . H1211 H 0.4243 0.3453 0.0648 0.0821 1.0000 Uiso . . . . . . . H1221 H 0.4520 0.4173 0.0130 0.0997 1.0000 Uiso . . . . . . . H1231 H 0.4589 0.5570 0.0168 0.1108 1.0000 Uiso . . . . . . . H1241 H 0.4345 0.6225 0.0723 0.0913 1.0000 Uiso . . . . . . . H1271 H 0.4917 0.9348 0.2195 0.0560 1.0000 Uiso . . . . . . . H1311 H 0.4856 0.9727 0.2714 0.0639 1.0000 Uiso . . . . . . . H1321 H 0.4816 1.0145 0.3343 0.0714 1.0000 Uiso . . . . . . . H1331 H 0.4257 0.9386 0.3736 0.0694 1.0000 Uiso . . . . . . . H1341 H 0.3690 0.8238 0.3465 0.0837 1.0000 Uiso . . . . . . . H1351 H 0.3793 0.7815 0.2835 0.0758 1.0000 Uiso . . . . . . . H1371 H 0.5134 0.8256 0.1078 0.1270 1.0000 Uiso . . . . . . . H1381 H 0.5772 0.8995 0.0728 0.1272 1.0000 Uiso . . . . . . . H1391 H 0.6094 1.0279 0.0922 0.1088 1.0000 Uiso . . . . . . . H1401 H 0.5932 1.0715 0.1512 0.0967 1.0000 Uiso . . . . . . . H1411 H 0.5279 1.0042 0.1867 0.1031 1.0000 Uiso . . . . . . . H1441 H 0.0902 0.8703 0.2538 0.0583 1.0000 Uiso . . . . . . . H1481 H 0.2782 0.9477 0.3017 0.0963 1.0000 Uiso . . . . . . . H1491 H 0.3012 0.9652 0.3701 0.1130 1.0000 Uiso . . . . . . . H1501 H 0.2431 0.8896 0.4088 0.1307 1.0000 Uiso . . . . . . . H1511 H 0.1562 0.8172 0.3813 0.1231 1.0000 Uiso . . . . . . . H1521 H 0.1295 0.8055 0.3092 0.1064 1.0000 Uiso . . . . . . . H1541 H 0.0505 0.8131 0.1285 0.0654 1.0000 Uiso . . . . . . . H1551 H -0.0564 0.8225 0.0972 0.0832 1.0000 Uiso . . . . . . . H1561 H -0.1316 0.8616 0.1339 0.0900 1.0000 Uiso . . . . . . . H1571 H -0.1025 0.8984 0.2003 0.1105 1.0000 Uiso . . . . . . . H1581 H 0.0093 0.8985 0.2298 0.0862 1.0000 Uiso . . . . . . . H1611 H 0.2387 1.1487 0.1077 0.0483 1.0000 Uiso . . . . . . . H1651 H 0.4361 1.0950 0.1101 0.0754 1.0000 Uiso . . . . . . . H1661 H 0.5054 1.2012 0.1295 0.0866 1.0000 Uiso . . . . . . . H1671 H 0.4742 1.3024 0.1692 0.0860 1.0000 Uiso . . . . . . . H1681 H 0.3700 1.3070 0.1804 0.0849 1.0000 Uiso . . . . . . . H1691 H 0.2997 1.2058 0.1564 0.0674 1.0000 Uiso . . . . . . . H1711 H 0.1525 1.1673 0.0705 0.0751 1.0000 Uiso . . . . . . . H1721 H 0.0458 1.1994 0.0576 0.0774 1.0000 Uiso . . . . . . . H1731 H -0.0290 1.1099 0.0707 0.0608 1.0000 Uiso . . . . . . . H1741 H 0.0037 0.9919 0.1046 0.0653 1.0000 Uiso . . . . . . . H1751 H 0.1105 0.9584 0.1172 0.0583 1.0000 Uiso . . . . . . . H1781 H 0.2502 1.1399 0.2441 0.0650 1.0000 Uiso . . . . . . . H1891 H 0.4102 1.0535 0.1984 0.0721 1.0000 Uiso . . . . . . . H1901 H 0.5081 1.1159 0.2242 0.0976 1.0000 Uiso . . . . . . . H1911 H 0.5165 1.1905 0.2816 0.1011 1.0000 Uiso . . . . . . . H1921 H 0.4322 1.2060 0.3134 0.0923 1.0000 Uiso . . . . . . . H1931 H 0.3331 1.1461 0.2882 0.0871 1.0000 Uiso . . . . . . . H1821 H 0.0722 1.0400 0.1778 0.0874 1.0000 Uiso . . . . . . . H1822 H -0.0161 1.1161 0.1759 0.1105 1.0000 Uiso . . . . . . . H1823 H -0.0141 1.2240 0.2158 0.1325 1.0000 Uiso . . . . . . . H1824 H 0.0790 1.2670 0.2512 0.1886 1.0000 Uiso . . . . . . . H1825 H 0.1732 1.1953 0.2517 0.1270 1.0000 Uiso . . . . . . . H131 H 0.3556 0.7512 0.0779 0.0592 1.0000 Uiso . . . . . . . H111 H 0.2717 0.6051 0.1354 0.0518 1.0000 Uiso . . . . . . . H121 H 0.2796 0.7618 0.2214 0.0531 1.0000 Uiso . . . . . . . H141 H 0.3650 0.9118 0.1625 0.0458 1.0000 Uiso . . . . . . . H11 H 0.1706 0.8285 0.1059 0.0479 1.0000 Uiso . . . . . . . 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 0.0343(4) 0.0322(3) 0.0582(5) -0.0024(3) 0.0022(3) -0.0013(3) Eu2 0.0419(4) 0.0310(3) 0.0550(5) -0.0012(3) 0.0020(3) -0.0010(3) Eu3 0.0379(4) 0.0308(3) 0.0584(5) 0.0002(3) 0.0030(3) 0.0012(3) Eu4 0.0385(4) 0.0318(3) 0.0574(5) -0.0005(3) 0.0027(3) -0.0035(3) Eu5 0.0377(4) 0.0323(3) 0.0598(4) 0.0007(3) 0.0007(3) 0.0018(3) O1 0.037(5) 0.033(4) 0.051(5) -0.002(4) 0.002(4) -0.004(4) O11 0.041(5) 0.030(4) 0.061(6) 0.003(4) 0.009(4) 0.000(4) O12 0.040(5) 0.033(4) 0.062(6) -0.005(4) 0.017(4) -0.009(4) O13 0.048(5) 0.041(5) 0.062(6) -0.001(4) 0.005(5) 0.000(4) O14 0.033(4) 0.026(4) 0.056(6) -0.001(4) 0.004(4) -0.003(3) O21 0.050(5) 0.029(4) 0.058(6) 0.000(4) 0.003(5) 0.000(4) C22 0.032(7) 0.051(8) 0.069(10) -0.005(8) 0.003(7) -0.011(6) C23 0.033(7) 0.056(8) 0.060(9) -0.002(7) 0.001(7) -0.003(6) C24 0.040(8) 0.035(7) 0.064(10) -0.011(7) 0.004(7) -0.009(6) O25 0.045(5) 0.037(5) 0.056(6) -0.006(4) 0.014(5) 0.000(4) C26 0.045(8) 0.059(9) 0.047(8) -0.011(7) 0.014(7) -0.008(6) C27 0.053(9) 0.049(8) 0.072(11) -0.018(7) 0.004(8) -0.001(7) C28 0.071(11) 0.073(10) 0.055(10) -0.001(8) 0.018(9) 0.027(9) C29 0.058(10) 0.108(14) 0.059(10) -0.014(10) 0.022(8) 0.010(10) C30 0.050(9) 0.072(10) 0.071(10) -0.006(8) 0.020(8) 0.001(8) C31 0.042(8) 0.064(9) 0.061(9) 0.001(7) 0.012(7) 0.009(7) C32 0.038(7) 0.042(7) 0.055(9) -0.004(7) 0.002(7) -0.013(6) C33 0.036(7) 0.056(8) 0.057(10) 0.001(7) 0.005(7) -0.002(6) C34 0.030(7) 0.058(8) 0.072(10) 0.015(8) -0.008(7) -0.008(6) C35 0.029(8) 0.046(8) 0.082(12) -0.013(8) -0.017(8) 0.006(6) C36 0.044(8) 0.054(8) 0.060(10) -0.010(7) -0.011(7) 0.008(7) C37 0.043(8) 0.050(8) 0.067(10) 0.003(7) 0.001(7) 0.002(6) O38 0.049(6) 0.049(5) 0.055(6) 0.001(5) 0.017(5) 0.002(4) C39 0.050(8) 0.046(8) 0.055(9) -0.017(7) -0.005(7) 0.005(7) C40 0.044(8) 0.051(8) 0.077(11) 0.002(8) 0.008(8) 0.006(7) C41 0.052(9) 0.048(8) 0.060(10) 0.009(7) 0.002(8) -0.007(7) O42 0.042(5) 0.052(5) 0.059(6) -0.006(5) 0.009(5) 0.007(4) C43 0.060(10) 0.050(8) 0.069(10) -0.005(7) 0.012(8) -0.010(7) C44 0.047(9) 0.061(9) 0.093(12) -0.020(9) 0.019(8) 0.000(7) C45 0.070(11) 0.074(11) 0.092(13) -0.003(10) 0.027(10) 0.016(9) C46 0.048(10) 0.105(15) 0.123(17) -0.037(14) 0.016(11) 0.014(10) C47 0.066(12) 0.115(15) 0.063(11) -0.028(11) 0.011(9) -0.028(11) C48 0.048(9) 0.076(10) 0.071(11) -0.016(9) 0.019(8) -0.015(8) C49 0.044(8) 0.038(7) 0.067(10) 0.011(7) -0.009(7) -0.004(6) C50 0.084(13) 0.072(11) 0.086(14) 0.018(10) 0.000(11) -0.005(9) C51 0.102(15) 0.076(12) 0.081(13) 0.026(10) 0.015(12) -0.007(11) C52 0.085(13) 0.055(10) 0.099(15) 0.028(10) -0.013(12) -0.005(9) C53 0.059(10) 0.050(9) 0.112(15) 0.005(10) -0.009(11) 0.004(8) C54 0.048(9) 0.049(8) 0.075(11) 0.009(8) -0.021(8) -0.004(7) O55 0.054(6) 0.034(5) 0.062(6) 0.000(4) -0.006(5) -0.005(4) C56 0.067(10) 0.031(7) 0.070(11) -0.003(7) 0.010(8) -0.007(6) C57 0.065(9) 0.041(7) 0.047(9) 0.001(6) 0.008(7) 0.005(7) C58 0.027(7) 0.041(8) 0.079(11) -0.005(7) -0.010(7) -0.014(5) O59 0.044(5) 0.035(5) 0.056(6) -0.010(4) -0.003(4) -0.007(4) C60 0.039(8) 0.048(8) 0.063(10) -0.001(7) 0.005(7) 0.003(6) C61 0.063(10) 0.060(9) 0.074(11) -0.002(8) 0.013(9) 0.010(8) C62 0.067(11) 0.076(11) 0.075(12) -0.008(9) -0.010(9) 0.020(9) C63 0.048(9) 0.067(10) 0.068(11) -0.005(8) 0.002(8) 0.006(7) C64 0.071(10) 0.058(9) 0.057(10) -0.009(7) -0.009(8) -0.010(8) C65 0.053(9) 0.049(8) 0.060(10) -0.001(7) 0.000(8) -0.016(7) C66 0.039(8) 0.038(7) 0.072(11) -0.003(7) -0.010(7) 0.001(6) C67 0.065(10) 0.043(8) 0.080(12) -0.008(8) 0.006(9) -0.016(7) C68 0.082(12) 0.058(10) 0.076(12) 0.009(9) 0.013(10) -0.006(8) C69 0.073(12) 0.050(9) 0.129(18) -0.022(11) -0.014(12) 0.007(9) C70 0.073(12) 0.058(10) 0.109(16) -0.015(10) 0.012(11) 0.004(9) C72 0.055(9) 0.049(8) 0.088(12) -0.012(8) -0.001(8) 0.002(7) O73 0.022(4) 0.038(5) 0.062(6) -0.003(4) 0.006(4) -0.005(3) C74 0.054(9) 0.044(8) 0.053(9) -0.006(7) 0.007(7) -0.006(6) C75 0.042(8) 0.042(8) 0.091(12) -0.015(8) -0.018(8) -0.012(6) C76 0.036(7) 0.033(7) 0.066(10) -0.010(6) -0.003(7) -0.002(6) O77 0.042(5) 0.038(5) 0.060(6) 0.003(4) 0.005(5) -0.003(4) C78 0.044(9) 0.063(9) 0.072(11) 0.000(8) 0.013(8) -0.006(7) C79 0.064(10) 0.049(9) 0.102(13) 0.011(8) 0.005(10) -0.020(8) C80 0.069(11) 0.089(13) 0.075(12) 0.011(10) -0.012(10) -0.028(10) C82 0.061(10) 0.086(13) 0.072(11) -0.004(10) -0.004(9) 0.006(9) C83 0.108(14) 0.066(10) 0.074(12) -0.012(9) -0.010(11) 0.036(10) C84 0.078(11) 0.050(9) 0.077(11) 0.002(8) 0.001(9) 0.018(8) C85 0.041(8) 0.037(7) 0.088(12) 0.001(7) 0.007(8) -0.004(6) C86 0.041(8) 0.037(8) 0.116(14) -0.006(8) 0.001(9) -0.002(6) C87 0.057(10) 0.040(8) 0.153(18) -0.019(10) -0.007(11) -0.003(8) C88 0.088(13) 0.034(8) 0.133(17) 0.010(9) 0.006(13) -0.004(8) C89 0.105(15) 0.053(10) 0.111(16) 0.022(10) -0.031(12) 0.004(10) C90 0.105(14) 0.032(8) 0.107(15) 0.002(8) -0.010(12) -0.008(8) O91 0.051(6) 0.047(5) 0.058(6) 0.011(5) 0.007(5) -0.007(4) C92 0.074(11) 0.037(7) 0.056(9) 0.004(7) 0.008(8) 0.002(7) C93 0.050(9) 0.064(9) 0.071(11) -0.011(8) 0.013(8) -0.021(7) C94 0.041(8) 0.046(8) 0.072(11) -0.017(7) 0.012(8) -0.013(6) O95 0.034(5) 0.047(5) 0.075(7) 0.009(5) 0.012(5) 0.005(4) C96 0.047(9) 0.051(8) 0.085(12) -0.019(8) 0.011(8) -0.014(7) C97 0.041(8) 0.044(8) 0.080(11) -0.007(7) -0.011(8) 0.002(6) C98 0.061(11) 0.052(9) 0.118(15) -0.009(10) -0.014(11) 0.002(8) C99 0.060(11) 0.058(10) 0.15(2) -0.031(12) 0.037(13) -0.030(8) C100 0.089(15) 0.132(18) 0.078(14) -0.006(13) 0.028(12) -0.043(13) C101 0.057(11) 0.097(13) 0.100(15) -0.005(11) 0.006(10) -0.038(10) C102 0.060(10) 0.053(8) 0.069(11) 0.001(8) 0.016(8) 0.005(7) C103 0.081(12) 0.057(9) 0.059(11) -0.009(8) 0.012(9) -0.004(8) C104 0.082(12) 0.070(11) 0.069(12) -0.014(9) 0.006(10) -0.008(9) C105 0.085(14) 0.109(15) 0.082(14) 0.016(12) 0.025(11) 0.010(12) C106 0.082(13) 0.110(15) 0.059(12) 0.014(10) 0.010(10) -0.012(11) C107 0.059(10) 0.095(12) 0.067(11) 0.018(9) 0.014(9) -0.010(9) O108 0.053(6) 0.035(5) 0.051(6) 0.004(4) -0.003(5) 0.010(4) C109 0.041(8) 0.036(7) 0.072(10) 0.011(7) 0.000(7) 0.010(6) C110 0.060(10) 0.043(8) 0.075(11) -0.007(8) 0.009(9) 0.005(7) C111 0.034(7) 0.052(9) 0.057(9) -0.005(7) -0.003(7) 0.011(6) O112 0.055(6) 0.037(5) 0.073(7) 0.012(5) 0.012(5) 0.014(4) C113 0.065(10) 0.043(8) 0.067(10) -0.003(7) 0.012(8) -0.002(7) C114 0.084(12) 0.049(9) 0.086(13) 0.007(9) 0.015(10) 0.013(8) C115 0.086(13) 0.086(12) 0.076(12) 0.011(10) 0.035(10) 0.018(10) C116 0.091(13) 0.067(11) 0.101(15) 0.033(10) 0.016(12) 0.010(10) C117 0.054(10) 0.058(9) 0.079(12) 0.013(9) -0.006(9) 0.014(7) C118 0.057(9) 0.044(7) 0.059(9) 0.013(7) -0.005(7) 0.009(7) C119 0.049(9) 0.055(9) 0.070(11) 0.001(8) 0.013(8) 0.015(7) C120 0.045(9) 0.057(9) 0.082(12) -0.010(8) 0.010(8) 0.010(7) C121 0.071(11) 0.057(9) 0.077(12) -0.018(9) -0.001(9) 0.017(8) C122 0.093(14) 0.089(13) 0.060(11) -0.009(10) 0.004(10) 0.042(11) C123 0.114(16) 0.113(16) 0.079(14) 0.035(12) 0.053(12) 0.052(13) C124 0.106(14) 0.061(10) 0.084(13) 0.023(9) 0.051(11) 0.034(9) O125 0.051(5) 0.045(5) 0.055(6) -0.007(4) 0.002(5) -0.013(4) C126 0.029(7) 0.039(7) 0.071(10) 0.000(7) -0.008(7) 0.007(6) C127 0.031(7) 0.046(7) 0.055(9) 0.005(7) -0.017(7) 0.000(6) C128 0.028(7) 0.047(8) 0.056(9) 0.009(7) 0.006(6) 0.014(6) O129 0.028(4) 0.045(5) 0.060(6) 0.001(5) -0.004(4) 0.002(4) C130 0.044(8) 0.038(7) 0.055(9) 0.001(6) 0.005(7) -0.002(6) C131 0.038(8) 0.059(9) 0.054(10) 0.009(7) -0.008(7) 0.004(6) C132 0.062(10) 0.054(8) 0.060(10) -0.004(8) -0.001(8) 0.011(7) C133 0.045(8) 0.090(11) 0.045(9) 0.002(8) 0.004(7) 0.009(8) C134 0.057(10) 0.073(11) 0.076(12) -0.006(9) 0.024(9) -0.009(8) C135 0.053(9) 0.065(9) 0.060(10) 0.008(8) 0.007(8) 0.013(7) C136 0.031(7) 0.060(9) 0.058(9) 0.010(7) -0.007(7) 0.010(6) C137 0.107(15) 0.127(17) 0.080(13) -0.037(12) 0.043(12) -0.066(13) C138 0.130(17) 0.132(17) 0.072(13) -0.045(12) 0.049(12) -0.084(14) C139 0.085(13) 0.106(14) 0.070(12) -0.012(11) 0.038(10) -0.020(11) C140 0.090(13) 0.058(10) 0.106(15) 0.007(10) 0.027(12) -0.024(9) C141 0.100(13) 0.045(9) 0.115(15) -0.002(9) 0.050(12) -0.002(9) O142 0.041(5) 0.054(5) 0.061(6) 0.000(5) 0.018(5) 0.000(4) C143 0.034(8) 0.053(8) 0.070(10) 0.015(7) 0.008(7) 0.009(6) C144 0.036(8) 0.058(8) 0.052(9) 0.003(7) 0.013(7) 0.002(6) C145 0.034(8) 0.040(7) 0.064(10) -0.009(7) 0.003(7) -0.006(6) O146 0.036(5) 0.043(5) 0.062(6) -0.002(4) 0.001(5) 0.001(4) C147 0.062(10) 0.070(10) 0.042(9) -0.001(7) 0.008(8) 0.026(8) C148 0.057(11) 0.107(14) 0.066(12) -0.014(10) 0.000(9) 0.026(10) C149 0.052(11) 0.18(2) 0.059(12) -0.027(13) 0.002(10) 0.021(12) C150 0.065(13) 0.21(3) 0.068(14) 0.005(16) 0.004(12) 0.071(16) C151 0.091(16) 0.145(19) 0.082(15) 0.034(14) 0.041(13) 0.042(14) C152 0.085(13) 0.103(13) 0.066(12) 0.035(10) 0.025(10) 0.040(11) C153 0.031(7) 0.031(7) 0.087(11) -0.006(7) -0.008(8) 0.000(5) C154 0.033(8) 0.054(8) 0.075(11) -0.008(8) -0.005(8) -0.008(6) C155 0.068(11) 0.046(8) 0.082(12) 0.013(8) -0.001(10) 0.002(7) C156 0.059(11) 0.067(10) 0.098(15) -0.002(10) 0.008(10) 0.002(8) C157 0.057(11) 0.097(14) 0.115(17) 0.002(12) 0.034(11) 0.015(9) C158 0.034(9) 0.095(12) 0.088(13) 0.005(10) 0.007(8) -0.002(8) O159 0.047(5) 0.040(5) 0.068(6) 0.007(4) 0.005(5) 0.000(4) C160 0.051(8) 0.030(7) 0.055(9) 0.017(6) -0.011(7) 0.007(6) C161 0.045(7) 0.027(6) 0.054(8) 0.003(6) -0.001(6) 0.008(6) C162 0.028(7) 0.036(7) 0.056(9) -0.006(6) -0.006(6) 0.006(5) O163 0.034(5) 0.035(5) 0.078(7) 0.003(4) 0.006(5) 0.002(4) C164 0.057(9) 0.034(7) 0.054(9) 0.010(6) -0.005(7) 0.001(6) C165 0.053(9) 0.044(8) 0.089(12) 0.002(8) 0.019(9) -0.005(7) C166 0.059(10) 0.074(10) 0.079(11) -0.005(9) 0.013(9) -0.022(8) C167 0.070(11) 0.046(8) 0.090(12) -0.002(8) -0.015(9) -0.004(8) C168 0.064(10) 0.048(8) 0.109(14) -0.005(9) 0.000(10) -0.007(8) C169 0.064(9) 0.040(7) 0.059(9) 0.000(7) -0.010(7) -0.009(7) C170 0.053(8) 0.037(7) 0.050(9) -0.012(6) 0.003(7) 0.009(6) C171 0.050(9) 0.049(8) 0.077(11) 0.006(8) -0.005(8) 0.004(7) C172 0.050(9) 0.034(7) 0.108(14) 0.000(8) -0.025(9) 0.013(7) C173 0.031(7) 0.050(8) 0.071(10) -0.017(7) -0.006(7) 0.008(6) C174 0.045(8) 0.040(7) 0.072(10) -0.005(7) 0.014(7) -0.004(6) C175 0.027(7) 0.036(7) 0.073(10) -0.012(7) 0.004(7) 0.000(5) O176 0.048(5) 0.033(5) 0.057(6) -0.004(4) 0.006(5) 0.000(4) C177 0.046(8) 0.037(7) 0.054(9) 0.004(6) 0.006(7) -0.001(6) C178 0.056(9) 0.040(7) 0.066(10) -0.004(7) 0.003(8) 0.003(7) C179 0.054(9) 0.050(8) 0.055(9) -0.002(7) 0.000(7) -0.022(7) O180 0.051(6) 0.033(5) 0.061(6) -0.003(4) 0.004(5) -0.008(4) C182 0.053(9) 0.044(8) 0.086(11) 0.000(8) 0.028(8) 0.010(7) C183 0.039(9) 0.100(13) 0.074(11) 0.004(10) 0.009(8) 0.022(9) C184 0.062(12) 0.131(17) 0.082(13) 0.027(12) 0.018(10) 0.052(12) C185 0.090(16) 0.073(13) 0.19(2) 0.021(15) 0.066(17) 0.023(12) C186 0.122(19) 0.053(12) 0.33(4) -0.041(17) 0.14(3) -0.002(12) C187 0.079(13) 0.078(12) 0.16(2) -0.040(13) 0.046(14) -0.008(10) C188 0.049(9) 0.035(7) 0.080(11) 0.003(7) -0.016(8) 0.001(6) C189 0.049(9) 0.041(8) 0.088(12) 0.017(7) -0.022(9) -0.010(7) C190 0.087(14) 0.051(10) 0.105(15) 0.023(10) -0.023(12) -0.020(9) C191 0.062(12) 0.054(10) 0.15(2) 0.032(12) -0.023(14) -0.016(9) C192 0.095(14) 0.051(9) 0.082(13) -0.017(9) -0.030(12) -0.015(9) C193 0.088(12) 0.042(8) 0.083(12) -0.003(8) -0.016(10) 0.002(8) _refine_ls_extinction_method None #_oxford_refine_ls_scale 0.02229(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Eu1 . O1 . 2.580(8) yes Eu1 . O12 . 2.384(8) yes Eu1 . O14 . 2.357(8) yes Eu1 . O142 . 2.364(9) yes Eu1 . O146 . 2.410(8) yes Eu1 . O163 . 2.478(9) yes Eu1 . O176 . 2.337(8) yes Eu1 . O180 . 2.304(8) yes Eu2 . O1 . 2.583(8) yes Eu2 . O11 . 2.361(9) yes Eu2 . O13 . 2.395(8) yes Eu2 . O21 . 2.382(9) yes Eu2 . O25 . 2.391(8) yes Eu2 . O55 . 2.294(8) yes Eu2 . O59 . 2.365(8) yes Eu2 . O73 . 2.480(8) yes Eu3 . O1 . 2.774(8) yes Eu3 . O13 . 2.341(8) yes Eu3 . O14 . 2.343(8) yes Eu3 . O25 . 2.451(8) yes Eu3 . O38 . 2.340(9) yes Eu3 . O42 . 2.318(10) yes Eu3 . O159 . 2.401(9) yes Eu3 . O163 . 2.381(9) yes Eu4 . O1 . 2.538(8) yes Eu4 . O11 . 2.397(8) yes Eu4 . O12 . 2.337(8) yes Eu4 . O73 . 2.425(8) yes Eu4 . O77 . 2.348(8) yes Eu4 . O91 . 2.323(9) yes Eu4 . O95 . 2.325(8) yes Eu4 . O146 . 2.508(8) yes Eu5 . O11 . 2.446(8) yes Eu5 . O12 . 2.456(8) yes Eu5 . O13 . 2.418(9) yes Eu5 . O14 . 2.476(7) yes Eu5 . O108 . 2.378(8) yes Eu5 . O112 . 2.343(9) yes Eu5 . O125 . 2.344(9) yes Eu5 . O129 . 2.397(8) yes O1 . H11 . 1.012 no O11 . H111 . 1.005 no O12 . H121 . 1.011 no O13 . H131 . 1.012 no O14 . H141 . 1.010 no O21 . C22 . 1.251(16) yes C22 . C23 . 1.444(18) yes C22 . C26 . 1.470(18) yes C23 . C24 . 1.369(18) yes C23 . H231 . 1.011 no C24 . O25 . 1.361(16) yes C24 . C32 . 1.465(18) yes C26 . C27 . 1.381(18) yes C26 . C31 . 1.387(19) yes C27 . C28 . 1.38(2) yes C27 . H271 . 1.017 no C28 . C29 . 1.39(2) yes C28 . H281 . 1.017 no C29 . C30 . 1.38(2) yes C29 . H291 . 1.010 no C30 . C31 . 1.404(19) yes C30 . H301 . 1.030 no C31 . H311 . 1.027 no C32 . C33 . 1.351(18) yes C32 . C37 . 1.421(19) yes C33 . C34 . 1.395(18) yes C33 . H331 . 1.019 no C34 . C35 . 1.39(2) yes C34 . H341 . 1.030 no C35 . C36 . 1.37(2) yes C35 . H351 . 1.004 no C36 . C37 . 1.390(18) yes C36 . H361 . 1.017 no C37 . H371 . 1.023 no O38 . C39 . 1.258(16) yes C39 . C40 . 1.387(19) yes C39 . C43 . 1.53(2) yes C40 . C41 . 1.390(19) yes C40 . H401 . 1.021 no C41 . O42 . 1.304(16) yes C41 . C49 . 1.490(18) yes C43 . C44 . 1.35(2) yes C43 . C48 . 1.39(2) yes C44 . C45 . 1.36(2) yes C44 . H441 . 1.027 no C45 . C46 . 1.37(3) yes C45 . H451 . 1.027 no C46 . C47 . 1.35(3) yes C46 . H461 . 1.007 no C47 . C48 . 1.43(2) yes C47 . H471 . 1.023 no C48 . H481 . 1.007 no C49 . C50 . 1.41(2) yes C49 . C54 . 1.38(2) yes C50 . C51 . 1.38(2) yes C50 . H501 . 1.011 no C51 . C52 . 1.33(3) yes C51 . H511 . 1.019 no C52 . C53 . 1.35(3) yes C52 . H521 . 1.004 no C53 . C54 . 1.38(2) yes C53 . H531 . 1.009 no C54 . H541 . 1.025 no O55 . C56 . 1.298(16) yes C56 . C57 . 1.403(19) yes C56 . C66 . 1.492(18) yes C57 . C58 . 1.404(18) yes C57 . H571 . 1.020 no C58 . O59 . 1.274(15) yes C58 . C60 . 1.496(19) yes C60 . C61 . 1.376(19) yes C60 . C65 . 1.402(18) yes C61 . C62 . 1.38(2) yes C61 . H611 . 1.024 no C62 . C63 . 1.38(2) yes C62 . H621 . 1.018 no C63 . C64 . 1.38(2) yes C63 . H631 . 1.041 no C64 . C65 . 1.378(19) yes C64 . H641 . 1.024 no C65 . H651 . 1.024 no C66 . C67 . 1.37(2) yes C66 . C72 . 1.39(2) yes C67 . C68 . 1.39(2) yes C67 . H671 . 1.023 no C68 . C69 . 1.38(2) yes C68 . H681 . 1.025 no C69 . C70 . 1.39(3) yes C69 . H691 . 1.021 no C70 . C72 . 1.37(2) yes C70 . H701 . 1.037 no C72 . H721 . 1.030 no O73 . C74 . 1.302(14) yes C74 . C75 . 1.385(19) yes C74 . C78 . 1.50(2) yes C75 . C76 . 1.465(19) yes C75 . H751 . 1.012 no C76 . O77 . 1.242(14) yes C76 . C85 . 1.491(17) yes C78 . C79 . 1.39(2) yes C78 . C84 . 1.370(19) yes C79 . C80 . 1.41(2) yes C79 . H791 . 1.019 no C80 . C82 . 1.36(2) yes C80 . H801 . 1.008 no C82 . C83 . 1.36(2) yes C82 . H821 . 1.033 no C83 . C84 . 1.43(2) yes C83 . H831 . 1.000 no C84 . H841 . 1.013 no C85 . C86 . 1.366(19) yes C85 . C90 . 1.39(2) yes C86 . C87 . 1.38(2) yes C86 . H861 . 1.013 no C87 . C88 . 1.36(2) yes C87 . H871 . 1.015 no C88 . C89 . 1.36(2) yes C88 . H881 . 1.017 no C89 . C90 . 1.39(2) yes C89 . H891 . 1.032 no C90 . H901 . 1.008 no O91 . C92 . 1.240(16) yes C92 . C93 . 1.45(2) yes C92 . C102 . 1.49(2) yes C93 . C94 . 1.39(2) yes C93 . H931 . 1.023 no C94 . O95 . 1.281(16) yes C94 . C96 . 1.512(18) yes C96 . C97 . 1.39(2) yes C96 . C101 . 1.41(2) yes C97 . C98 . 1.37(2) yes C97 . H971 . 1.029 no C98 . C99 . 1.39(3) yes C98 . H981 . 1.038 no C99 . C100 . 1.36(3) yes C99 . H991 . 1.023 no C100 . C101 . 1.37(2) yes C100 . H1001 . 1.030 no C101 . H1011 . 1.023 no C102 . C103 . 1.39(2) yes C102 . C107 . 1.40(2) yes C103 . C104 . 1.41(2) yes C103 . H1031 . 1.024 no C104 . C105 . 1.35(2) yes C104 . H1041 . 1.026 no C105 . C106 . 1.37(2) yes C105 . H1051 . 1.031 no C106 . C107 . 1.40(2) yes C106 . H1061 . 1.036 no C107 . H1071 . 1.013 no O108 . C109 . 1.273(14) yes C109 . C110 . 1.40(2) yes C109 . C113 . 1.508(19) yes C110 . C111 . 1.40(2) yes C110 . H1101 . 1.006 no C111 . O112 . 1.279(15) yes C111 . C119 . 1.488(19) yes C113 . C114 . 1.37(2) yes C113 . C118 . 1.393(18) yes C114 . C115 . 1.43(2) yes C114 . H1141 . 1.013 no C115 . C116 . 1.38(2) yes C115 . H1151 . 1.024 no C116 . C117 . 1.37(2) yes C116 . H1161 . 1.023 no C117 . C118 . 1.37(2) yes C117 . H1171 . 1.017 no C118 . H1181 . 1.015 no C119 . C120 . 1.365(19) yes C119 . C124 . 1.37(2) yes C120 . C121 . 1.36(2) yes C120 . H1201 . 1.022 no C121 . C122 . 1.37(2) yes C121 . H1211 . 1.023 no C122 . C123 . 1.37(3) yes C122 . H1221 . 1.021 no C123 . C124 . 1.41(2) yes C123 . H1231 . 1.032 no C124 . H1241 . 1.018 no O125 . C126 . 1.283(14) yes C126 . C127 . 1.421(19) yes C126 . C130 . 1.469(19) yes C127 . C128 . 1.417(18) yes C127 . H1271 . 1.018 no C128 . O129 . 1.265(15) yes C128 . C136 . 1.505(18) yes C130 . C131 . 1.371(18) yes C130 . C135 . 1.395(19) yes C131 . C132 . 1.363(19) yes C131 . H1311 . 1.020 no C132 . C133 . 1.39(2) yes C132 . H1321 . 1.013 no C133 . C134 . 1.41(2) yes C133 . H1331 . 1.019 no C134 . C135 . 1.38(2) yes C134 . H1341 . 1.027 no C135 . H1351 . 1.021 no C136 . C137 . 1.34(2) yes C136 . C141 . 1.38(2) yes C137 . C138 . 1.42(2) yes C137 . H1371 . 1.027 no C138 . C139 . 1.36(2) yes C138 . H1381 . 1.026 no C139 . C140 . 1.33(2) yes C139 . H1391 . 1.006 no C140 . C141 . 1.37(2) yes C140 . H1401 . 1.004 no C141 . H1411 . 1.030 no O142 . C143 . 1.251(15) yes C143 . C144 . 1.446(18) yes C143 . C147 . 1.50(2) yes C144 . C145 . 1.377(18) yes C144 . H1441 . 1.017 no C145 . O146 . 1.329(15) yes C145 . C153 . 1.465(17) yes C147 . C148 . 1.36(2) yes C147 . C152 . 1.38(2) yes C148 . C149 . 1.34(2) yes C148 . H1481 . 1.044 no C149 . C150 . 1.39(3) yes C149 . H1491 . 1.040 no C150 . C151 . 1.35(3) yes C150 . H1501 . 1.019 no C151 . C152 . 1.45(3) yes C151 . H1511 . 1.027 no C152 . H1521 . 1.019 no C153 . C154 . 1.38(2) yes C153 . C158 . 1.40(2) yes C154 . C155 . 1.381(19) yes C154 . H1541 . 1.022 no C155 . C156 . 1.38(2) yes C155 . H1551 . 1.035 no C156 . C157 . 1.37(3) yes C156 . H1561 . 1.019 no C157 . C158 . 1.44(2) yes C157 . H1571 . 1.022 no C158 . H1581 . 1.021 no O159 . C160 . 1.244(14) yes C160 . C161 . 1.474(18) yes C160 . C164 . 1.478(17) yes C161 . C162 . 1.332(16) yes C161 . H1611 . 1.003 no C162 . O163 . 1.330(14) yes C162 . C170 . 1.480(17) yes C164 . C165 . 1.405(19) yes C164 . C169 . 1.397(19) yes C165 . C166 . 1.374(19) yes C165 . H1651 . 1.021 no C166 . C167 . 1.40(2) yes C166 . H1661 . 1.012 no C167 . C168 . 1.40(2) yes C167 . H1671 . 1.011 no C168 . C169 . 1.366(19) yes C168 . H1681 . 1.031 no C169 . H1691 . 1.019 no C170 . C171 . 1.409(18) yes C170 . C175 . 1.396(18) yes C171 . C172 . 1.365(19) yes C171 . H1711 . 1.020 no C172 . C173 . 1.37(2) yes C172 . H1721 . 1.014 no C173 . C174 . 1.381(18) yes C173 . H1731 . 1.012 no C174 . C175 . 1.381(17) yes C174 . H1741 . 1.016 no C175 . H1751 . 1.009 no O176 . C177 . 1.290(15) yes C177 . C178 . 1.385(18) yes C177 . C182 . 1.509(18) yes C178 . C179 . 1.381(19) yes C178 . H1781 . 1.019 no C179 . O180 . 1.291(16) yes C179 . C188 . 1.536(18) yes C182 . C183 . 1.34(2) yes C182 . C187 . 1.41(2) yes C183 . C184 . 1.36(2) yes C183 . H1821 . 1.011 no C184 . C185 . 1.35(3) yes C184 . H1822 . 0.997 no C185 . C186 . 1.32(3) yes C185 . H1823 . 1.007 no C186 . C187 . 1.41(3) yes C186 . H1824 . 0.998 no C187 . H1825 . 0.999 no C188 . C189 . 1.39(2) yes C188 . C193 . 1.41(2) yes C189 . C190 . 1.39(2) yes C189 . H1891 . 1.029 no C190 . C191 . 1.36(3) yes C190 . H1901 . 1.041 no C191 . C192 . 1.36(3) yes C191 . H1911 . 1.016 no C192 . C193 . 1.39(2) yes C192 . H1921 . 1.032 no C193 . H1931 . 1.034 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Eu1 . O12 . 67.6(3) yes O1 . Eu1 . O14 . 70.9(3) yes O12 . Eu1 . O14 . 73.1(3) yes O1 . Eu1 . O142 . 129.3(3) yes O12 . Eu1 . O142 . 72.3(3) yes O14 . Eu1 . O142 . 124.4(3) yes O1 . Eu1 . O146 . 69.0(3) yes O12 . Eu1 . O146 . 76.8(3) yes O14 . Eu1 . O146 . 136.6(3) yes O142 . Eu1 . O146 . 72.9(3) yes O1 . Eu1 . O163 . 64.9(3) yes O12 . Eu1 . O163 . 129.3(3) yes O14 . Eu1 . O163 . 75.7(3) yes O142 . Eu1 . O163 . 156.7(3) yes O146 . Eu1 . O163 . 101.3(3) yes O1 . Eu1 . O176 . 124.9(3) yes O12 . Eu1 . O176 . 145.6(3) yes O14 . Eu1 . O176 . 139.5(3) yes O142 . Eu1 . O176 . 77.3(3) yes O146 . Eu1 . O176 . 79.3(3) yes O1 . Eu1 . O180 . 143.3(3) yes O12 . Eu1 . O180 . 116.8(3) yes O14 . Eu1 . O180 . 75.8(3) yes O142 . Eu1 . O180 . 82.7(3) yes O146 . Eu1 . O180 . 146.9(3) yes O163 . Eu1 . O176 . 79.5(3) yes O163 . Eu1 . O180 . 92.3(3) yes O176 . Eu1 . O180 . 73.8(3) yes O1 . Eu2 . O11 . 68.4(3) yes O1 . Eu2 . O13 . 69.5(3) yes O11 . Eu2 . O13 . 70.4(3) yes O1 . Eu2 . O21 . 130.1(3) yes O11 . Eu2 . O21 . 124.3(3) yes O13 . Eu2 . O21 . 71.7(3) yes O1 . Eu2 . O25 . 69.0(3) yes O11 . Eu2 . O25 . 132.6(3) yes O13 . Eu2 . O25 . 76.1(3) yes O21 . Eu2 . O25 . 72.2(3) yes O1 . Eu2 . O55 . 143.6(3) yes O11 . Eu2 . O55 . 79.0(3) yes O13 . Eu2 . O55 . 114.7(3) yes O21 . Eu2 . O55 . 81.6(3) yes O25 . Eu2 . O55 . 147.0(3) yes O1 . Eu2 . O59 . 125.1(3) yes O11 . Eu2 . O59 . 143.4(3) yes O13 . Eu2 . O59 . 144.3(3) yes O21 . Eu2 . O59 . 75.9(3) yes O25 . Eu2 . O59 . 80.1(3) yes O1 . Eu2 . O73 . 69.5(3) yes O11 . Eu2 . O73 . 76.0(3) yes O13 . Eu2 . O73 . 134.0(3) yes O21 . Eu2 . O73 . 154.1(3) yes O25 . Eu2 . O73 . 107.2(3) yes O55 . Eu2 . O59 . 74.2(3) yes O55 . Eu2 . O73 . 87.8(3) yes O59 . Eu2 . O73 . 78.5(3) yes O1 . Eu3 . O13 . 66.9(3) yes O1 . Eu3 . O14 . 67.6(2) yes O13 . Eu3 . O14 . 73.3(3) yes O1 . Eu3 . O25 . 65.0(3) yes O13 . Eu3 . O25 . 75.9(3) yes O14 . Eu3 . O25 . 130.6(3) yes O1 . Eu3 . O38 . 138.3(3) yes O13 . Eu3 . O38 . 73.2(3) yes O14 . Eu3 . O38 . 112.0(3) yes O25 . Eu3 . O38 . 94.4(3) yes O1 . Eu3 . O42 . 132.2(3) yes O13 . Eu3 . O42 . 135.2(3) yes O14 . Eu3 . O42 . 147.1(3) yes O25 . Eu3 . O42 . 79.6(3) yes O38 . Eu3 . O42 . 72.0(3) yes O1 . Eu3 . O159 . 124.2(3) yes O13 . Eu3 . O159 . 133.2(3) yes O14 . Eu3 . O159 . 72.0(3) yes O25 . Eu3 . O159 . 150.6(3) yes O38 . Eu3 . O159 . 91.9(3) yes O1 . Eu3 . O163 . 63.1(3) yes O13 . Eu3 . O163 . 128.6(3) yes O14 . Eu3 . O163 . 77.8(3) yes O25 . Eu3 . O163 . 92.9(3) yes O38 . Eu3 . O163 . 158.2(3) yes O42 . Eu3 . O159 . 75.2(3) yes O42 . Eu3 . O163 . 89.2(3) yes O159 . Eu3 . O163 . 72.2(3) yes O1 . Eu4 . O11 . 68.7(3) yes O1 . Eu4 . O12 . 69.0(3) yes O11 . Eu4 . O12 . 72.8(3) yes O1 . Eu4 . O73 . 71.0(3) yes O11 . Eu4 . O73 . 76.4(3) yes O12 . Eu4 . O73 . 136.1(3) yes O1 . Eu4 . O77 . 130.5(3) yes O11 . Eu4 . O77 . 70.3(3) yes O12 . Eu4 . O77 . 122.4(3) yes O73 . Eu4 . O77 . 73.3(3) yes O1 . Eu4 . O91 . 141.2(3) yes O11 . Eu4 . O91 . 117.6(3) yes O12 . Eu4 . O91 . 76.6(3) yes O73 . Eu4 . O91 . 146.7(3) yes O77 . Eu4 . O91 . 83.2(3) yes O1 . Eu4 . O95 . 126.3(3) yes O11 . Eu4 . O95 . 143.5(3) yes O12 . Eu4 . O95 . 141.5(3) yes O73 . Eu4 . O95 . 78.6(3) yes O77 . Eu4 . O95 . 77.3(3) yes O1 . Eu4 . O146 . 68.2(3) yes O11 . Eu4 . O146 . 133.3(3) yes O12 . Eu4 . O146 . 75.8(3) yes O73 . Eu4 . O146 . 105.3(3) yes O77 . Eu4 . O146 . 156.0(3) yes O91 . Eu4 . O95 . 73.4(3) yes O91 . Eu4 . O146 . 86.8(3) yes O95 . Eu4 . O146 . 79.0(3) yes O11 . Eu5 . O12 . 70.0(3) yes O11 . Eu5 . O13 . 68.6(3) yes O12 . Eu5 . O13 . 107.0(3) yes O11 . Eu5 . O14 . 107.9(2) yes O12 . Eu5 . O14 . 69.9(3) yes O13 . Eu5 . O14 . 69.7(3) yes O11 . Eu5 . O108 . 76.7(3) yes O12 . Eu5 . O108 . 81.5(3) yes O13 . Eu5 . O108 . 137.9(3) yes O14 . Eu5 . O108 . 146.4(3) yes O11 . Eu5 . O112 . 80.4(3) yes O12 . Eu5 . O112 . 144.7(3) yes O13 . Eu5 . O112 . 78.2(3) yes O14 . Eu5 . O112 . 140.1(3) yes O108 . Eu5 . O112 . 73.2(3) yes O11 . Eu5 . O125 . 137.3(3) yes O12 . Eu5 . O125 . 74.1(3) yes O13 . Eu5 . O125 . 146.3(3) yes O14 . Eu5 . O125 . 79.8(3) yes O108 . Eu5 . O125 . 75.8(3) yes O11 . Eu5 . O129 . 150.3(3) yes O12 . Eu5 . O129 . 134.2(3) yes O13 . Eu5 . O129 . 85.5(3) yes O14 . Eu5 . O129 . 74.2(3) yes O108 . Eu5 . O129 . 118.6(3) yes O112 . Eu5 . O125 . 121.0(3) yes O112 . Eu5 . O129 . 80.4(3) yes O125 . Eu5 . O129 . 72.4(3) yes Eu3 . O1 . Eu2 . 86.1(2) yes Eu3 . O1 . Eu1 . 86.0(2) yes Eu2 . O1 . Eu1 . 159.3(3) yes Eu3 . O1 . Eu4 . 156.1(3) yes Eu2 . O1 . Eu4 . 89.6(2) yes Eu1 . O1 . Eu4 . 90.0(3) yes Eu3 . O1 . H11 . 104.1 no Eu2 . O1 . H11 . 99.6 no Eu1 . O1 . H11 . 100.8 no Eu4 . O1 . H11 . 99.8 no Eu5 . O11 . Eu4 . 107.6(3) yes Eu5 . O11 . Eu2 . 110.2(3) yes Eu4 . O11 . Eu2 . 98.7(3) yes Eu5 . O11 . H111 . 113.5 no Eu4 . O11 . H111 . 113.1 no Eu2 . O11 . H111 . 112.8 no Eu5 . O12 . Eu1 . 108.1(3) yes Eu5 . O12 . Eu4 . 109.2(3) yes Eu1 . O12 . Eu4 . 100.1(3) yes Eu5 . O12 . H121 . 112.7 no Eu1 . O12 . H121 . 112.8 no Eu4 . O12 . H121 . 113.1 no Eu5 . O13 . Eu2 . 110.0(3) yes Eu5 . O13 . Eu3 . 109.5(3) yes Eu2 . O13 . Eu3 . 101.2(3) yes Eu5 . O13 . H131 . 111.9 no Eu2 . O13 . H131 . 111.9 no Eu3 . O13 . H131 . 111.8 no Eu5 . O14 . Eu1 . 108.3(3) yes Eu5 . O14 . Eu3 . 107.5(3) yes Eu1 . O14 . Eu3 . 102.0(3) yes Eu5 . O14 . H141 . 112.9 no Eu1 . O14 . H141 . 112.5 no Eu3 . O14 . H141 . 113.0 no Eu2 . O21 . C22 . 133.0(8) yes O21 . C22 . C23 . 124.2(13) yes O21 . C22 . C26 . 118.1(12) yes C23 . C22 . C26 . 117.6(13) yes C22 . C23 . C24 . 126.0(13) yes C22 . C23 . H231 . 117.5 no C24 . C23 . H231 . 116.5 no C23 . C24 . O25 . 120.9(12) yes C23 . C24 . C32 . 123.6(14) yes O25 . C24 . C32 . 115.4(12) yes C24 . O25 . Eu3 . 121.2(7) yes C24 . O25 . Eu2 . 126.8(7) yes Eu3 . O25 . Eu2 . 98.2(3) yes C22 . C26 . C27 . 118.4(13) yes C22 . C26 . C31 . 121.9(13) yes C27 . C26 . C31 . 119.3(13) yes C26 . C27 . C28 . 119.6(14) yes C26 . C27 . H271 . 120.3 no C28 . C27 . H271 . 120.1 no C27 . C28 . C29 . 121.9(14) yes C27 . C28 . H281 . 120.0 no C29 . C28 . H281 . 118.1 no C28 . C29 . C30 . 118.7(14) yes C28 . C29 . H291 . 120.0 no C30 . C29 . H291 . 121.3 no C29 . C30 . C31 . 119.4(14) yes C29 . C30 . H301 . 119.3 no C31 . C30 . H301 . 121.3 no C30 . C31 . C26 . 120.9(13) yes C30 . C31 . H311 . 119.2 no C26 . C31 . H311 . 119.9 no C24 . C32 . C33 . 123.3(13) yes C24 . C32 . C37 . 118.9(13) yes C33 . C32 . C37 . 117.8(13) yes C32 . C33 . C34 . 122.1(14) yes C32 . C33 . H331 . 118.2 no C34 . C33 . H331 . 119.6 no C33 . C34 . C35 . 119.5(13) yes C33 . C34 . H341 . 121.3 no C35 . C34 . H341 . 119.2 no C34 . C35 . C36 . 120.0(12) yes C34 . C35 . H351 . 119.6 no C36 . C35 . H351 . 120.3 no C35 . C36 . C37 . 119.8(14) yes C35 . C36 . H361 . 118.8 no C37 . C36 . H361 . 121.4 no C32 . C37 . C36 . 120.8(14) yes C32 . C37 . H371 . 118.4 no C36 . C37 . H371 . 120.8 no Eu3 . O38 . C39 . 137.2(8) yes O38 . C39 . C40 . 125.1(13) yes O38 . C39 . C43 . 114.9(12) yes C40 . C39 . C43 . 120.0(14) yes C39 . C40 . C41 . 124.6(14) yes C39 . C40 . H401 . 117.4 no C41 . C40 . H401 . 118.0 no C40 . C41 . O42 . 122.8(13) yes C40 . C41 . C49 . 122.7(14) yes O42 . C41 . C49 . 114.5(13) yes C41 . O42 . Eu3 . 138.0(8) yes C39 . C43 . C44 . 119.7(14) yes C39 . C43 . C48 . 120.7(14) yes C44 . C43 . C48 . 119.6(15) yes C43 . C44 . C45 . 124.1(16) yes C43 . C44 . H441 . 117.1 no C45 . C44 . H441 . 118.7 no C44 . C45 . C46 . 118.2(17) yes C44 . C45 . H451 . 120.8 no C46 . C45 . H451 . 120.9 no C45 . C46 . C47 . 119.5(16) yes C45 . C46 . H461 . 122.9 no C47 . C46 . H461 . 117.5 no C46 . C47 . C48 . 122.9(17) yes C46 . C47 . H471 . 118.6 no C48 . C47 . H471 . 118.5 no C47 . C48 . C43 . 115.5(16) yes C47 . C48 . H481 . 121.8 no C43 . C48 . H481 . 122.7 no C41 . C49 . C50 . 122.6(14) yes C41 . C49 . C54 . 119.9(14) yes C50 . C49 . C54 . 117.5(13) yes C49 . C50 . C51 . 118.0(18) yes C49 . C50 . H501 . 121.1 no C51 . C50 . H501 . 120.9 no C50 . C51 . C52 . 123.3(19) yes C50 . C51 . H511 . 118.3 no C52 . C51 . H511 . 118.3 no C51 . C52 . C53 . 120.1(16) yes C51 . C52 . H521 . 118.9 no C53 . C52 . H521 . 121.0 no C52 . C53 . C54 . 119.4(17) yes C52 . C53 . H531 . 119.7 no C54 . C53 . H531 . 120.9 no C49 . C54 . C53 . 121.7(16) yes C49 . C54 . H541 . 118.5 no C53 . C54 . H541 . 119.8 no Eu2 . O55 . C56 . 133.8(8) yes O55 . C56 . C57 . 124.0(12) yes O55 . C56 . C66 . 116.4(13) yes C57 . C56 . C66 . 119.5(13) yes C56 . C57 . C58 . 126.0(13) yes C56 . C57 . H571 . 117.6 no C58 . C57 . H571 . 116.4 no C57 . C58 . O59 . 123.2(12) yes C57 . C58 . C60 . 119.8(12) yes O59 . C58 . C60 . 117.0(11) yes C58 . O59 . Eu2 . 133.0(8) yes C58 . C60 . C61 . 118.8(13) yes C58 . C60 . C65 . 122.1(12) yes C61 . C60 . C65 . 119.0(13) yes C60 . C61 . C62 . 119.7(14) yes C60 . C61 . H611 . 120.4 no C62 . C61 . H611 . 119.9 no C61 . C62 . C63 . 122.1(15) yes C61 . C62 . H621 . 120.1 no C63 . C62 . H621 . 117.8 no C62 . C63 . C64 . 117.7(14) yes C62 . C63 . H631 . 120.8 no C64 . C63 . H631 . 121.5 no C63 . C64 . C65 . 121.6(13) yes C63 . C64 . H641 . 118.5 no C65 . C64 . H641 . 119.9 no C60 . C65 . C64 . 119.8(13) yes C60 . C65 . H651 . 119.5 no C64 . C65 . H651 . 120.7 no C56 . C66 . C67 . 118.6(14) yes C56 . C66 . C72 . 123.5(14) yes C67 . C66 . C72 . 117.9(13) yes C66 . C67 . C68 . 122.5(15) yes C66 . C67 . H671 . 118.2 no C68 . C67 . H671 . 119.4 no C67 . C68 . C69 . 118.0(16) yes C67 . C68 . H681 . 121.2 no C69 . C68 . H681 . 120.8 no C68 . C69 . C70 . 120.5(16) yes C68 . C69 . H691 . 119.6 no C70 . C69 . H691 . 119.9 no C69 . C70 . C72 . 119.9(17) yes C69 . C70 . H701 . 121.3 no C72 . C70 . H701 . 118.8 no C66 . C72 . C70 . 121.1(16) yes C66 . C72 . H721 . 119.1 no C70 . C72 . H721 . 119.8 no Eu2 . O73 . Eu4 . 94.8(2) yes Eu2 . O73 . C74 . 125.1(8) yes Eu4 . O73 . C74 . 124.1(8) yes O73 . C74 . C75 . 126.6(12) yes O73 . C74 . C78 . 115.0(11) yes C75 . C74 . C78 . 118.4(12) yes C74 . C75 . C76 . 123.3(11) yes C74 . C75 . H751 . 119.0 no C76 . C75 . H751 . 117.7 no C75 . C76 . O77 . 123.8(11) yes C75 . C76 . C85 . 117.7(11) yes O77 . C76 . C85 . 118.5(12) yes C76 . O77 . Eu4 . 134.9(8) yes C74 . C78 . C79 . 122.4(13) yes C74 . C78 . C84 . 118.2(13) yes C79 . C78 . C84 . 119.3(15) yes C78 . C79 . C80 . 120.9(14) yes C78 . C79 . H791 . 119.5 no C80 . C79 . H791 . 119.6 no C79 . C80 . C82 . 119.8(15) yes C79 . C80 . H801 . 119.5 no C82 . C80 . H801 . 120.7 no C80 . C82 . C83 . 119.7(15) yes C80 . C82 . H821 . 121.9 no C83 . C82 . H821 . 118.4 no C82 . C83 . C84 . 121.9(15) yes C82 . C83 . H831 . 118.8 no C84 . C83 . H831 . 119.3 no C83 . C84 . C78 . 118.5(15) yes C83 . C84 . H841 . 120.1 no C78 . C84 . H841 . 121.4 no C76 . C85 . C86 . 125.6(14) yes C76 . C85 . C90 . 117.4(12) yes C86 . C85 . C90 . 117.1(13) yes C85 . C86 . C87 . 121.1(15) yes C85 . C86 . H861 . 119.0 no C87 . C86 . H861 . 119.8 no C86 . C87 . C88 . 122.0(15) yes C86 . C87 . H871 . 118.3 no C88 . C87 . H871 . 119.6 no C87 . C88 . C89 . 117.9(14) yes C87 . C88 . H881 . 121.2 no C89 . C88 . H881 . 120.9 no C88 . C89 . C90 . 121.2(16) yes C88 . C89 . H891 . 120.0 no C90 . C89 . H891 . 118.8 no C89 . C90 . C85 . 120.7(15) yes C89 . C90 . H901 . 120.3 no C85 . C90 . H901 . 119.0 no Eu4 . O91 . C92 . 136.4(9) yes O91 . C92 . C93 . 122.9(13) yes O91 . C92 . C102 . 117.9(13) yes C93 . C92 . C102 . 119.0(14) yes C92 . C93 . C94 . 125.2(13) yes C92 . C93 . H931 . 118.4 no C94 . C93 . H931 . 116.4 no C93 . C94 . O95 . 123.7(12) yes C93 . C94 . C96 . 121.6(14) yes O95 . C94 . C96 . 114.6(14) yes C94 . O95 . Eu4 . 134.4(8) yes C94 . C96 . C97 . 120.1(14) yes C94 . C96 . C101 . 121.3(15) yes C97 . C96 . C101 . 118.6(13) yes C96 . C97 . C98 . 122.0(16) yes C96 . C97 . H971 . 116.7 no C98 . C97 . H971 . 121.4 no C97 . C98 . C99 . 117.7(17) yes C97 . C98 . H981 . 120.7 no C99 . C98 . H981 . 121.5 no C98 . C99 . C100 . 121.4(16) yes C98 . C99 . H991 . 118.6 no C100 . C99 . H991 . 119.9 no C99 . C100 . C101 . 121.2(18) yes C99 . C100 . H1001 . 119.9 no C101 . C100 . H1001 . 118.8 no C96 . C101 . C100 . 119.0(18) yes C96 . C101 . H1011 . 118.0 no C100 . C101 . H1011 . 123.0 no C92 . C102 . C103 . 117.9(14) yes C92 . C102 . C107 . 122.4(14) yes C103 . C102 . C107 . 119.3(15) yes C102 . C103 . C104 . 119.6(15) yes C102 . C103 . H1031 . 118.9 no C104 . C103 . H1031 . 121.5 no C103 . C104 . C105 . 120.5(16) yes C103 . C104 . H1041 . 119.7 no C105 . C104 . H1041 . 119.7 no C104 . C105 . C106 . 119.6(18) yes C104 . C105 . H1051 . 119.7 no C106 . C105 . H1051 . 120.7 no C105 . C106 . C107 . 122.3(17) yes C105 . C106 . H1061 . 118.4 no C107 . C106 . H1061 . 119.3 no C102 . C107 . C106 . 118.3(15) yes C102 . C107 . H1071 . 120.1 no C106 . C107 . H1071 . 121.7 no Eu5 . O108 . C109 . 131.2(9) yes O108 . C109 . C110 . 125.1(13) yes O108 . C109 . C113 . 116.1(13) yes C110 . C109 . C113 . 118.8(12) yes C109 . C110 . C111 . 125.3(13) yes C109 . C110 . H1101 . 117.4 no C111 . C110 . H1101 . 117.2 no C110 . C111 . O112 . 123.5(13) yes C110 . C111 . C119 . 120.4(13) yes O112 . C111 . C119 . 116.1(13) yes C111 . O112 . Eu5 . 131.9(9) yes C109 . C113 . C114 . 118.8(13) yes C109 . C113 . C118 . 121.3(14) yes C114 . C113 . C118 . 120.0(14) yes C113 . C114 . C115 . 120.7(14) yes C113 . C114 . H1141 . 120.1 no C115 . C114 . H1141 . 119.1 no C114 . C115 . C116 . 116.4(16) yes C114 . C115 . H1151 . 121.1 no C116 . C115 . H1151 . 122.4 no C115 . C116 . C117 . 123.1(16) yes C115 . C116 . H1161 . 117.9 no C117 . C116 . H1161 . 119.0 no C116 . C117 . C118 . 119.2(14) yes C116 . C117 . H1171 . 120.5 no C118 . C117 . H1171 . 120.3 no C113 . C118 . C117 . 120.5(15) yes C113 . C118 . H1181 . 118.8 no C117 . C118 . H1181 . 120.7 no C111 . C119 . C120 . 124.3(15) yes C111 . C119 . C124 . 118.9(14) yes C120 . C119 . C124 . 116.8(15) yes C119 . C120 . C121 . 125.1(16) yes C119 . C120 . H1201 . 116.7 no C121 . C120 . H1201 . 118.3 no C120 . C121 . C122 . 117.7(15) yes C120 . C121 . H1211 . 120.8 no C122 . C121 . H1211 . 121.5 no C121 . C122 . C123 . 120.1(16) yes C121 . C122 . H1221 . 118.6 no C123 . C122 . H1221 . 121.2 no C122 . C123 . C124 . 120.3(17) yes C122 . C123 . H1231 . 120.5 no C124 . C123 . H1231 . 119.2 no C123 . C124 . C119 . 120.0(16) yes C123 . C124 . H1241 . 119.7 no C119 . C124 . H1241 . 120.3 no Eu5 . O125 . C126 . 133.1(9) yes O125 . C126 . C127 . 123.0(13) yes O125 . C126 . C130 . 116.4(13) yes C127 . C126 . C130 . 120.5(11) yes C126 . C127 . C128 . 124.9(12) yes C126 . C127 . H1271 . 117.1 no C128 . C127 . H1271 . 118.0 no C127 . C128 . O129 . 124.8(12) yes C127 . C128 . C136 . 118.3(12) yes O129 . C128 . C136 . 116.8(12) yes C128 . O129 . Eu5 . 129.5(8) yes C126 . C130 . C131 . 125.4(13) yes C126 . C130 . C135 . 117.4(12) yes C131 . C130 . C135 . 117.2(14) yes C130 . C131 . C132 . 123.8(14) yes C130 . C131 . H1311 . 117.2 no C132 . C131 . H1311 . 119.0 no C131 . C132 . C133 . 118.5(14) yes C131 . C132 . H1321 . 119.8 no C133 . C132 . H1321 . 121.7 no C132 . C133 . C134 . 120.2(14) yes C132 . C133 . H1331 . 119.3 no C134 . C133 . H1331 . 120.5 no C133 . C134 . C135 . 118.7(14) yes C133 . C134 . H1341 . 120.3 no C135 . C134 . H1341 . 121.0 no C130 . C135 . C134 . 121.6(14) yes C130 . C135 . H1351 . 119.8 no C134 . C135 . H1351 . 118.5 no C128 . C136 . C137 . 118.1(14) yes C128 . C136 . C141 . 123.6(14) yes C137 . C136 . C141 . 118.3(15) yes C136 . C137 . C138 . 119.1(16) yes C136 . C137 . H1371 . 121.9 no C138 . C137 . H1371 . 118.8 no C137 . C138 . C139 . 122.3(17) yes C137 . C138 . H1381 . 119.0 no C139 . C138 . H1381 . 118.7 no C138 . C139 . C140 . 117.0(16) yes C138 . C139 . H1391 . 122.5 no C140 . C139 . H1391 . 120.4 no C139 . C140 . C141 . 122.1(16) yes C139 . C140 . H1401 . 117.8 no C141 . C140 . H1401 . 120.1 no C136 . C141 . C140 . 121.2(17) yes C136 . C141 . H1411 . 119.2 no C140 . C141 . H1411 . 119.6 no Eu1 . O142 . C143 . 133.6(9) yes O142 . C143 . C144 . 122.9(13) yes O142 . C143 . C147 . 117.2(12) yes C144 . C143 . C147 . 119.9(13) yes C143 . C144 . C145 . 127.4(13) yes C143 . C144 . H1441 . 117.5 no C145 . C144 . H1441 . 115.1 no C144 . C145 . O146 . 122.1(11) yes C144 . C145 . C153 . 122.5(13) yes O146 . C145 . C153 . 115.3(12) yes C145 . O146 . Eu4 . 125.3(7) yes C145 . O146 . Eu1 . 126.2(7) yes Eu4 . O146 . Eu1 . 94.7(3) yes C143 . C147 . C148 . 119.2(15) yes C143 . C147 . C152 . 119.4(15) yes C148 . C147 . C152 . 121.2(16) yes C147 . C148 . C149 . 122.3(19) yes C147 . C148 . H1481 . 117.6 no C149 . C148 . H1481 . 120.1 no C148 . C149 . C150 . 118.0(20) yes C148 . C149 . H1491 . 120.7 no C150 . C149 . H1491 . 121.3 no C149 . C150 . C151 . 122.5(19) yes C149 . C150 . H1501 . 119.3 no C151 . C150 . H1501 . 118.1 no C150 . C151 . C152 . 118.4(20) yes C150 . C151 . H1511 . 119.5 no C152 . C151 . H1511 . 122.0 no C151 . C152 . C147 . 117.2(19) yes C151 . C152 . H1521 . 120.9 no C147 . C152 . H1521 . 121.9 no C145 . C153 . C154 . 121.7(13) yes C145 . C153 . C158 . 119.8(14) yes C154 . C153 . C158 . 118.5(12) yes C153 . C154 . C155 . 121.7(14) yes C153 . C154 . H1541 . 118.0 no C155 . C154 . H1541 . 120.3 no C154 . C155 . C156 . 119.5(16) yes C154 . C155 . H1551 . 119.8 no C156 . C155 . H1551 . 120.7 no C155 . C156 . C157 . 122.0(16) yes C155 . C156 . H1561 . 118.2 no C157 . C156 . H1561 . 119.8 no C156 . C157 . C158 . 117.5(16) yes C156 . C157 . H1571 . 120.8 no C158 . C157 . H1571 . 121.6 no C157 . C158 . C153 . 120.7(16) yes C157 . C158 . H1581 . 120.1 no C153 . C158 . H1581 . 119.1 no Eu3 . O159 . C160 . 131.5(8) yes O159 . C160 . C161 . 123.5(11) yes O159 . C160 . C164 . 119.2(12) yes C161 . C160 . C164 . 117.2(11) yes C160 . C161 . C162 . 125.0(10) yes C160 . C161 . H1611 . 117.2 no C162 . C161 . H1611 . 117.8 no C161 . C162 . O163 . 123.8(10) yes C161 . C162 . C170 . 120.7(11) yes O163 . C162 . C170 . 115.5(10) yes C162 . O163 . Eu1 . 124.8(8) yes C162 . O163 . Eu3 . 123.5(8) yes Eu1 . O163 . Eu3 . 97.5(3) yes C160 . C164 . C165 . 119.7(13) yes C160 . C164 . C169 . 122.4(13) yes C165 . C164 . C169 . 117.7(12) yes C164 . C165 . C166 . 121.8(14) yes C164 . C165 . H1651 . 118.6 no C166 . C165 . H1651 . 119.6 no C165 . C166 . C167 . 118.8(14) yes C165 . C166 . H1661 . 121.3 no C167 . C166 . H1661 . 119.9 no C166 . C167 . C168 . 120.0(14) yes C166 . C167 . H1671 . 120.7 no C168 . C167 . H1671 . 119.3 no C167 . C168 . C169 . 120.0(15) yes C167 . C168 . H1681 . 120.0 no C169 . C168 . H1681 . 119.9 no C164 . C169 . C168 . 121.5(15) yes C164 . C169 . H1691 . 118.8 no C168 . C169 . H1691 . 119.7 no C162 . C170 . C171 . 123.3(13) yes C162 . C170 . C175 . 119.9(11) yes C171 . C170 . C175 . 116.8(12) yes C170 . C171 . C172 . 121.2(14) yes C170 . C171 . H1711 . 118.7 no C172 . C171 . H1711 . 120.1 no C171 . C172 . C173 . 120.7(12) yes C171 . C172 . H1721 . 119.5 no C173 . C172 . H1721 . 119.8 no C172 . C173 . C174 . 119.8(12) yes C172 . C173 . H1731 . 119.4 no C174 . C173 . H1731 . 120.7 no C173 . C174 . C175 . 119.6(12) yes C173 . C174 . H1741 . 120.2 no C175 . C174 . H1741 . 120.2 no C170 . C175 . C174 . 121.6(12) yes C170 . C175 . H1751 . 119.3 no C174 . C175 . H1751 . 119.0 no Eu1 . O176 . C177 . 134.2(8) yes O176 . C177 . C178 . 124.9(12) yes O176 . C177 . C182 . 113.4(11) yes C178 . C177 . C182 . 121.7(12) yes C177 . C178 . C179 . 123.9(13) yes C177 . C178 . H1781 . 118.2 no C179 . C178 . H1781 . 117.8 no C178 . C179 . O180 . 126.5(12) yes C178 . C179 . C188 . 119.4(13) yes O180 . C179 . C188 . 114.0(13) yes C179 . O180 . Eu1 . 133.5(8) yes C177 . C182 . C183 . 122.6(13) yes C177 . C182 . C187 . 121.2(15) yes C183 . C182 . C187 . 116.1(14) yes C182 . C183 . C184 . 123.4(18) yes C182 . C183 . H1821 . 118.0 no C184 . C183 . H1821 . 118.6 no C183 . C184 . C185 . 120.3(20) yes C183 . C184 . H1822 . 119.7 no C185 . C184 . H1822 . 120.0 no C184 . C185 . C186 . 119.8(19) yes C184 . C185 . H1823 . 119.0 no C186 . C185 . H1823 . 121.1 no C185 . C186 . C187 . 121(2) yes C185 . C186 . H1824 . 118.1 no C187 . C186 . H1824 . 121.2 no C186 . C187 . C182 . 119.3(20) yes C186 . C187 . H1825 . 119.3 no C182 . C187 . H1825 . 121.4 no C179 . C188 . C189 . 118.9(14) yes C179 . C188 . C193 . 121.9(15) yes C189 . C188 . C193 . 119.3(14) yes C188 . C189 . C190 . 120.9(17) yes C188 . C189 . H1891 . 120.4 no C190 . C189 . H1891 . 118.8 no C189 . C190 . C191 . 119(2) yes C189 . C190 . H1901 . 121.5 no C191 . C190 . H1901 . 119.4 no C190 . C191 . C192 . 121.3(17) yes C190 . C191 . H1911 . 120.7 no C192 . C191 . H1911 . 118.0 no C191 . C192 . C193 . 121.5(17) yes C191 . C192 . H1921 . 120.9 no C193 . C192 . H1921 . 117.7 no C188 . C193 . C192 . 117.9(17) yes C188 . C193 . H1931 . 119.2 no C192 . C193 . H1931 . 122.9 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C191 . H1911 . O125 3_655 151 1.02 2.49 3.42(2) yes O14 . H141 . C127 . 132 1.01 2.59 3.35(2) yes