# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? #looking for refcif _publ_contact_author_name 'Euan K.Brechin ' _publ_requested_coeditor_name A.Prescimone@ed.ac.uk _publ_contact_author_email ebrechin@staffmail.ed.ac.uk _publ_author_name 'Euan K.Brechin' # Attachment '- complex1.cif' data_eb0067 _database_code_depnum_ccdc_archive 'CCDC 810533' #TrackingRef '- complex1.cif' _audit_creation_date 11-03-09 _audit_creation_method CRYSTALS_ver_14.05 _oxford_structure_analysis_title eb0067 _chemical_name_systematic ? _chemical_melting_point ? _chemical_compound_source 'Guillaume Rigaux' _exptl_crystal_recrystallization_method ; diffusion of hexane into MeOH solution ; _publ_section_exptl_refinement ; The H atoms were all positioned geometrically. U~iso~(H) (in the range 1.2 times U~eq~ of the parent atom), the positions were refined with riding constraints. One of the Ethyl groups on the Sao ligands is disordered over two orientations. One non-fully occupied MeCN molecule per cluster is present in the crystal lattice: this molecule had to be refined isotropically and its C-C and C-N bonds restrained to chemically sensible values. see the bottom part of the file for the full list of the applied restraints. #-------------------------------------------------------------- CHECKCIF OUTPUT: #-------------------------------------------------------------- 301_ALERT_3_B Note: Main Residue Disorder ................... 1.00 Perc. 302_ALERT_4_B Note: Anion/Solvent Disorder ................... 70.00 Perc. 202_ALERT_3_G Isotropic non-H Atoms in Anion/Solvent ......... 3 One of the Ethyl groups on the Sao ligands is disordered over two orientations. One non-fully occupied MeCN molecule per cluster is present in the crystal lattice: this molecule had to be refined isotropically and its C-C and C-N bonds restrained to chemically sensible values. 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 321 911_ALERT_3_G Missing # FCF Refl Between THmin & STh/L= 0.600 3 Completeness meets IUCr limits. Some data were collected above the planned upper resolution limit, these have been included in the refinement. 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C17 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C18 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C57 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C58 H-atoms have been geometrically placed 795_ALERT_4_B C-Atom in CIF Coordinate List out of Sequence .. C250 413_ALERT_2_C Short Inter XH3 .. XHn H183 .. H301 .. 1.98 Ang. 410_ALERT_2_G Short Intra H...H Contact H311 .. H2411 .. 1.98 Ang. 042_ALERT_1_G Calc. and Reported MoietyFormula Strings Differ ? 060_ALERT_4_G Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.11 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 57 790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 2 C2 H3 N 796_ALERT_4_G O-Atom in CIF Coordinate List out of Sequence .. O11 797_ALERT_4_G N-Atom in CIF Coordinate List out of Sequence .. N10 142_ALERT_4_G su on b - Axis Small or Missing (x 100000) ..... 13 Ang. 342_ALERT_3_G Low Bond Precision on C-C Bonds (x 1000) Ang .. 11 Noted, no action taken 213_ALERT_2_G Atom C43 has ADP max/min Ratio ..... 3.30 prolat 241_ALERT_2_G Check High Ueq as Compared to Neighbors for C43 High thermal motion in C-atom in peripheral ring of a large cluster is not unusual. 213_ALERT_2_G Atom C250 has ADP max/min Ratio ..... 3.50 oblate This atom is on the disordered tail of a ligand in large metal cluster. Having increased displacement is not unexpected and it is likely such motion might be confined to a particular direction given the overall shape of the molecule. Regardless this is not a significantly distorted ADP. ; #end of refcif _cell_length_a 26.3789(3) _cell_length_b 14.04530(13) _cell_length_c 25.8211(3) _cell_angle_alpha 90 _cell_angle_beta 117.7884(14) _cell_angle_gamma 90 _cell_volume 8463.43(19) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' 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 0.0181 0.0091 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' Gd -8.8380 11.9157 25.0709 2.2534 19.0798 0.1820 13.8518 12.9331 3.5454 101.3980 2.4196 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mn -0.5299 2.8052 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0492 0.0322 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 = C73.25 H94 Gd2 Mn6 N6.50 O27 # Dc = 1.68 Fooo = 4317.60 Mu = 176.56 M = 2141.65 # Found Formula = C73.40 H98.10 Gd2 Mn6 N6.70 O27 # Dc = 1.69 FOOO = 4317.60 Mu = 176.59 M = 2150.39 _chemical_formula_sum 'C73.40 H98.10 Gd2 Mn6 N6.70 O27' _chemical_formula_moiety '[Gd2Mn6O3(OMe)4(Et-sao)6(acac)2(MeOH)4].0.7MeCN' _chemical_formula_weight 2150.39 _cell_measurement_reflns_used 27749 _cell_measurement_theta_min 2 _cell_measurement_theta_max 73 _cell_measurement_temperature 100 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_max 0.170 _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 4317.600 _exptl_absorpt_coefficient_mu 17.659 # Sheldrick geometric approximatio 0.29 0.41 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2905 _exptl_absorpt_correction_T_max 0.4136 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_device Serial _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'Shelxs Sheldrick' _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 100 _diffrn_reflns_number 83524 _reflns_number_total 16710 _diffrn_reflns_av_R_equivalents 0.092 # Number of reflections without Friedels Law is 16710 # Number of reflections with Friedels Law is 16710 # Theoretical number of reflections is about 17018 _diffrn_reflns_theta_min 1.893 _diffrn_reflns_theta_max 73.368 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 70.434 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _reflns_limit_h_min -32 _reflns_limit_h_max 28 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _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 -1.47 _refine_diff_density_max 1.56 # 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>-10.0\s(I) _refine_ls_number_reflns 16707 _refine_ls_number_restraints 3 _refine_ls_number_parameters 1039 _oxford_refine_ls_R_factor_ref 0.0752 _refine_ls_wR_factor_ref 0.0774 _refine_ls_goodness_of_fit_ref 1.1801 _refine_ls_shift/su_max 0.0072174 _refine_ls_shift/su_mean 1.7566460 # The values computed from all data _oxford_reflns_number_all 16707 _refine_ls_R_factor_all 0.0752 _refine_ls_wR_factor_all 0.0774 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 11881 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_gt 0.0705 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # 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: 585. 577. 198. ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference User-defined data collection reference User defined data reduction User defined cell refinement 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Mn1 Mn 0.29788(4) 0.37830(7) 0.12158(4) 0.0178 1.0000 Uani . . . . . . . Mn2 Mn 0.35980(4) 0.51377(7) 0.07472(4) 0.0167 1.0000 Uani . . . . . . . Mn3 Mn 0.19662(4) 0.45227(7) 0.13809(4) 0.0187 1.0000 Uani . . . . . . . Mn4 Mn 0.30488(4) 0.69239(7) 0.00421(4) 0.0187 1.0000 Uani . . . . . . . Mn5 Mn 0.13005(4) 0.63355(7) 0.07140(4) 0.0173 1.0000 Uani . . . . . . . Mn6 Mn 0.18265(4) 0.78598(7) 0.02586(4) 0.0188 1.0000 Uani . . . . . . . Gd1 Gd 0.203278(15) 0.52249(3) 0.003758(15) 0.0131 1.0000 Uani . . . . . . . Gd2 Gd 0.286872(15) 0.63758(3) 0.137918(15) 0.0128 1.0000 Uani . . . . . . . O13 O 0.24703(16) 0.4812(3) 0.10627(15) 0.0211 1.0000 Uani . . . . . . . O24 O 0.29669(17) 0.5986(3) 0.05313(17) 0.0223 1.0000 Uani . . . . . . . O56 O 0.19110(16) 0.6583(3) 0.05343(17) 0.0230 1.0000 Uani . . . . . . . O11 O 0.35287(19) 0.2870(3) 0.13537(18) 0.0329 1.0000 Uani . . . . . . . C11 C 0.3799(3) 0.2264(5) 0.1785(3) 0.0308 1.0000 Uani . . . . . . . C21 C 0.3741(3) 0.2220(5) 0.2305(3) 0.0283 1.0000 Uani . . . . . . . C31 C 0.4051(3) 0.1526(5) 0.2724(3) 0.0338 1.0000 Uani . . . . . . . C41 C 0.4415(3) 0.0907(5) 0.2651(3) 0.0352 1.0000 Uani . . . . . . . C51 C 0.4477(3) 0.0938(5) 0.2143(3) 0.0361 1.0000 Uani . . . . . . . C61 C 0.4176(3) 0.1621(4) 0.1725(3) 0.0287 1.0000 Uani . . . . . . . C211 C 0.3364(3) 0.2880(5) 0.2406(3) 0.0298 1.0000 Uani . . . . . . . N221 N 0.3075(2) 0.3557(4) 0.2035(2) 0.0268 1.0000 Uani . . . . . . . O231 O 0.27521(19) 0.4144(3) 0.21830(18) 0.0291 1.0000 Uani . . . . . . . C241 C 0.3320(4) 0.2837(6) 0.2973(3) 0.0512 1.0000 Uani D . . . . . . C251 C 0.3760(6) 0.3346(9) 0.3445(4) 0.0624 0.7000 Uani . . . . 2 . . C250 C 0.2896(12) 0.2263(19) 0.2982(12) 0.0595 0.3000 Uani D . . . 1 . . C12 C 0.4408(3) 0.3833(5) 0.0694(3) 0.0278 1.0000 Uani . . . . . . . O12 O 0.42697(19) 0.4441(3) 0.09943(18) 0.0322 1.0000 Uani . . . . . . . C22 C 0.4186(3) 0.3889(5) 0.0073(3) 0.0293 1.0000 Uani . . . . . . . C32 C 0.4371(3) 0.3211(5) -0.0195(3) 0.0375 1.0000 Uani . . . . . . . C42 C 0.4758(3) 0.2504(5) 0.0111(3) 0.0430 1.0000 Uani . . . . . . . C52 C 0.4971(3) 0.2460(5) 0.0718(3) 0.0387 1.0000 Uani . . . . . . . C62 C 0.4798(3) 0.3103(5) 0.0995(3) 0.0335 1.0000 Uani . . . . . . . C212 C 0.3816(3) 0.4669(5) -0.0267(3) 0.0266 1.0000 Uani . . . . . . . N222 N 0.3574(2) 0.5216(4) -0.0038(2) 0.0243 1.0000 Uani . . . . . . . O232 O 0.32847(19) 0.5997(3) -0.03553(18) 0.0311 1.0000 Uani . . . . . . . C242 C 0.3724(3) 0.4881(5) -0.0875(3) 0.0318 1.0000 Uani . . . . . . . C252 C 0.4246(3) 0.5345(7) -0.0871(3) 0.0531 1.0000 Uani . . . . . . . O237 O 0.1440(2) 0.4330(3) 0.1662(2) 0.0334 1.0000 Uani . . . . . . . C13 C 0.1324(3) 0.3519(5) 0.1853(3) 0.0308 1.0000 Uani . . . . . . . C23 C 0.1381(3) 0.2607(5) 0.1672(3) 0.0328 1.0000 Uani . . . . . . . C33 C 0.1201(4) 0.1828(6) 0.1886(4) 0.0543 1.0000 Uani . . . . . . . C43 C 0.0984(4) 0.1956(7) 0.2278(4) 0.0686 1.0000 Uani . . . . . . . C53 C 0.0950(3) 0.2856(6) 0.2469(4) 0.0495 1.0000 Uani . . . . . . . C63 C 0.1105(3) 0.3640(6) 0.2260(3) 0.0378 1.0000 Uani . . . . . . . C213 C 0.1659(3) 0.2424(5) 0.1293(3) 0.0294 1.0000 Uani . . . . . . . N223 N 0.1911(2) 0.3115(4) 0.1174(2) 0.0257 1.0000 Uani . . . . . . . O233 O 0.22057(18) 0.2885(3) 0.08676(18) 0.0274 1.0000 Uani . . . . . . . C243 C 0.1684(3) 0.1452(5) 0.1093(3) 0.0442 1.0000 Uani . . . . . . . C253 C 0.2213(4) 0.0917(6) 0.1529(4) 0.0550 1.0000 Uani . . . . . . . O14 O 0.3138(2) 0.7836(3) -0.04418(19) 0.0346 1.0000 Uani . . . . . . . C14 C 0.3505(3) 0.8543(5) -0.0236(3) 0.0321 1.0000 Uani . . . . . . . C24 C 0.3588(3) 0.9076(5) 0.0261(3) 0.0320 1.0000 Uani . . . . . . . C34 C 0.3994(3) 0.9814(6) 0.0445(3) 0.0424 1.0000 Uani . . . . . . . C44 C 0.4294(3) 1.0045(6) 0.0151(4) 0.0558 1.0000 Uani . . . . . . . C54 C 0.4200(4) 0.9528(6) -0.0345(4) 0.0515 1.0000 Uani . . . . . . . C64 C 0.3811(3) 0.8786(5) -0.0539(3) 0.0376 1.0000 Uani . . . . . . . C214 C 0.3248(3) 0.8887(5) 0.0567(3) 0.0278 1.0000 Uani . . . . . . . N224 N 0.3033(2) 0.8049(4) 0.0531(2) 0.0280 1.0000 Uani . . . . . . . O234 O 0.27147(17) 0.7875(3) 0.08115(17) 0.0252 1.0000 Uani . . . . . . . C244 C 0.3149(3) 0.9671(5) 0.0908(3) 0.0342 1.0000 Uani . . . . . . . C254 C 0.2862(3) 1.0563(5) 0.0538(3) 0.0405 1.0000 Uani . . . . . . . C15 C 0.0539(3) 0.6493(5) 0.1223(3) 0.0271 1.0000 Uani . . . . . . . O15 O 0.06585(18) 0.6121(3) 0.08243(18) 0.0280 1.0000 Uani . . . . . . . C25 C 0.0697(3) 0.7421(5) 0.1445(3) 0.0279 1.0000 Uani . . . . . . . C35 C 0.0531(3) 0.7739(5) 0.1854(3) 0.0294 1.0000 Uani . . . . . . . C45 C 0.0218(3) 0.7182(5) 0.2037(3) 0.0330 1.0000 Uani . . . . . . . C55 C 0.0056(3) 0.6275(5) 0.1810(3) 0.0339 1.0000 Uani . . . . . . . C65 C 0.0215(3) 0.5936(5) 0.1408(3) 0.0322 1.0000 Uani . . . . . . . C215 C 0.1014(3) 0.8044(5) 0.1245(3) 0.0300 1.0000 Uani . . . . . . . N225 N 0.1294(2) 0.7683(4) 0.0978(2) 0.0263 1.0000 Uani . . . . . . . O235 O 0.15481(19) 0.8323(3) 0.07916(19) 0.0323 1.0000 Uani . . . . . . . C245 C 0.1006(3) 0.9109(5) 0.1301(3) 0.0416 1.0000 Uani . . . . . . . C255 C 0.0515(4) 0.9521(5) 0.0738(4) 0.0608 1.0000 Uani . . . . . . . C16 C 0.1373(3) 0.9384(5) -0.0546(3) 0.0327 1.0000 Uani . . . . . . . O16 O 0.17498(19) 0.9122(3) -0.00016(19) 0.0333 1.0000 Uani . . . . . . . C26 C 0.1289(3) 0.8841(5) -0.1038(3) 0.0326 1.0000 Uani . . . . . . . C36 C 0.0908(3) 0.9189(6) -0.1596(3) 0.0455 1.0000 Uani . . . . . . . C46 C 0.0611(3) 1.0034(5) -0.1662(3) 0.0488 1.0000 Uani . . . . . . . C56 C 0.0714(4) 1.0567(6) -0.1182(4) 0.0539 1.0000 Uani . . . . . . . C66 C 0.1088(3) 1.0246(6) -0.0629(3) 0.0430 1.0000 Uani . . . . . . . C216 C 0.1619(3) 0.7967(5) -0.0987(3) 0.0314 1.0000 Uani . . . . . . . N226 N 0.1832(2) 0.7510(4) -0.0494(2) 0.0283 1.0000 Uani . . . . . . . O236 O 0.21516(18) 0.6711(3) -0.04332(18) 0.0275 1.0000 Uani . . . . . . . C246 C 0.1715(3) 0.7628(5) -0.1481(3) 0.0402 1.0000 Uani . . . . . . . C256 C 0.2049(4) 0.8336(7) -0.1651(4) 0.0687 1.0000 Uani . . . . . . . C17 C 0.2955(3) 0.8943(6) 0.2572(3) 0.0499 1.0000 Uani . . . . . . . O27 O 0.28351(19) 0.7613(3) 0.19669(19) 0.0289 1.0000 Uani . . . . . . . C27 C 0.3167(3) 0.8299(5) 0.2246(3) 0.0318 1.0000 Uani . . . . . . . C37 C 0.3721(3) 0.8429(5) 0.2306(3) 0.0364 1.0000 Uani . . . . . . . C47 C 0.3987(3) 0.7897(5) 0.2050(3) 0.0297 1.0000 Uani . . . . . . . O47 O 0.37735(17) 0.7150(3) 0.17364(18) 0.0243 1.0000 Uani . . . . . . . C57 C 0.4565(3) 0.8199(5) 0.2124(3) 0.0418 1.0000 Uani . . . . . . . C18 C 0.2086(3) 0.4689(7) -0.1713(3) 0.0530 1.0000 Uani . . . . . . . O28 O 0.20936(18) 0.4772(3) -0.07986(16) 0.0288 1.0000 Uani . . . . . . . C28 C 0.1807(3) 0.4911(5) -0.1338(3) 0.0379 1.0000 Uani . . . . . . . C38 C 0.1246(3) 0.5325(5) -0.1599(3) 0.0357 1.0000 Uani . . . . . . . C48 C 0.0958(3) 0.5685(5) -0.1315(3) 0.0302 1.0000 Uani . . . . . . . O48 O 0.11225(17) 0.5633(3) -0.07609(17) 0.0266 1.0000 Uani . . . . . . . C58 C 0.0406(3) 0.6239(6) -0.1661(3) 0.0419 1.0000 Uani . . . . . . . O19 O 0.29052(17) 0.4049(3) 0.04412(18) 0.0233 1.0000 Uani . . . . . . . C29 C 0.2934(3) 0.3253(5) 0.0106(3) 0.0290 1.0000 Uani . . . . . . . O10 O 0.36054(16) 0.5082(3) 0.14996(16) 0.0233 1.0000 Uani . . . . . . . C20 C 0.4138(3) 0.4932(5) 0.2025(3) 0.0287 1.0000 Uani . . . . . . . O238 O 0.40421(18) 0.6658(3) 0.08803(18) 0.0305 1.0000 Uani . . . . . . . C257 C 0.4555(3) 0.6867(6) 0.0842(3) 0.0410 1.0000 Uani . . . . . . . O239 O 0.13121(16) 0.5047(3) 0.04487(16) 0.0231 1.0000 Uani . . . . . . . C258 C 0.0778(3) 0.4535(5) 0.0171(3) 0.0335 1.0000 Uani . . . . . . . O240 O 0.20210(18) 0.5887(3) 0.15646(16) 0.0242 1.0000 Uani . . . . . . . C259 C 0.2000(3) 0.6154(5) 0.2091(2) 0.0314 1.0000 Uani . . . . . . . O241 O 0.07825(19) 0.6970(4) -0.02303(18) 0.0355 1.0000 Uani . . . . . . . C260 C 0.0212(3) 0.7331(6) -0.0489(3) 0.0542 1.0000 Uani . . . . . . . O242 O 0.16648(17) 0.3631(3) -0.01523(17) 0.0257 1.0000 Uani . . . . . . . C261 C 0.1365(3) 0.3026(6) -0.0649(3) 0.0460 1.0000 Uani . . . . . . . O243 O 0.32743(18) 0.5754(3) 0.23603(16) 0.0288 1.0000 Uani . . . . . . . C262 C 0.3594(3) 0.6099(6) 0.2936(3) 0.0494 1.0000 Uani . . . . . . . N10 N 0.2383(8) 1.0731(13) -0.1187(8) 0.137(6) 0.7000 Uiso D . . . 2 . . C263 C 0.2487(9) 1.1532(15) -0.1184(9) 0.118(7) 0.7000 Uiso D . . . 2 . . C30 C 0.2700(6) 1.2365(11) -0.1170(7) 0.087(5) 0.7000 Uiso D . . . 2 . . H311 H 0.4008 0.1485 0.3069 0.0407 1.0000 Uiso R . . . . . . H411 H 0.4627 0.0455 0.2948 0.0422 1.0000 Uiso R . . . . . . H511 H 0.4720 0.0499 0.2085 0.0432 1.0000 Uiso R . . . . . . H611 H 0.4227 0.1658 0.1385 0.0344 1.0000 Uiso R . . . . . . H2511 H 0.3708 0.3286 0.3783 0.0765 0.7000 Uiso R . . . 2 . . H2512 H 0.4124 0.3097 0.3524 0.0765 0.7000 Uiso R . . . 2 . . H2513 H 0.3741 0.3999 0.3341 0.0765 0.7000 Uiso R . . . 2 . . H2501 H 0.2931 0.2316 0.3364 0.0725 0.3000 Uiso R . . . 1 . . H2502 H 0.2945 0.1617 0.2906 0.0725 0.3000 Uiso R . . . 1 . . H2503 H 0.2526 0.2474 0.2703 0.0725 0.3000 Uiso R . . . 1 . . H321 H 0.4223 0.3237 -0.0608 0.0446 1.0000 Uiso R . . . . . . H421 H 0.4877 0.2057 -0.0086 0.0513 1.0000 Uiso R . . . . . . H521 H 0.5239 0.1979 0.0937 0.0462 1.0000 Uiso R . . . . . . H621 H 0.4945 0.3056 0.1407 0.0395 1.0000 Uiso R . . . . . . H2421 H 0.3407 0.5300 -0.1060 0.0380 1.0000 Uiso R . . . . . . H2422 H 0.3644 0.4302 -0.1088 0.0380 1.0000 Uiso R . . . . . . H2521 H 0.4172 0.5466 -0.1262 0.0626 1.0000 Uiso R . . . . . . H2522 H 0.4328 0.5927 -0.0660 0.0626 1.0000 Uiso R . . . . . . H2523 H 0.4566 0.4928 -0.0689 0.0626 1.0000 Uiso R . . . . . . H331 H 0.1226 0.1205 0.1757 0.0650 1.0000 Uiso R . . . . . . H431 H 0.0858 0.1422 0.2414 0.0828 1.0000 Uiso R . . . . . . H531 H 0.0818 0.2935 0.2752 0.0592 1.0000 Uiso R . . . . . . H631 H 0.1068 0.4260 0.2386 0.0455 1.0000 Uiso R . . . . . . H2431 H 0.1693 0.1489 0.0730 0.0528 1.0000 Uiso R . . . . . . H2432 H 0.1352 0.1113 0.1041 0.0528 1.0000 Uiso R . . . . . . H2531 H 0.2215 0.0295 0.1385 0.0652 1.0000 Uiso R . . . . . . H2532 H 0.2548 0.1249 0.1582 0.0652 1.0000 Uiso R . . . . . . H2533 H 0.2207 0.0873 0.1893 0.0652 1.0000 Uiso R . . . . . . H341 H 0.4059 1.0169 0.0784 0.0502 1.0000 Uiso R . . . . . . H441 H 0.4565 1.0550 0.0286 0.0666 1.0000 Uiso R . . . . . . H541 H 0.4404 0.9688 -0.0554 0.0613 1.0000 Uiso R . . . . . . H641 H 0.3750 0.8439 -0.0879 0.0449 1.0000 Uiso R . . . . . . H2441 H 0.3508 0.9852 0.1221 0.0406 1.0000 Uiso R . . . . . . H2442 H 0.2909 0.9432 0.1062 0.0406 1.0000 Uiso R . . . . . . H2541 H 0.2811 1.1030 0.0776 0.0491 1.0000 Uiso R . . . . . . H2542 H 0.3099 1.0814 0.0384 0.0491 1.0000 Uiso R . . . . . . H2543 H 0.2500 1.0394 0.0225 0.0491 1.0000 Uiso R . . . . . . H351 H 0.0637 0.8362 0.2011 0.0355 1.0000 Uiso R . . . . . . H451 H 0.0113 0.7417 0.2319 0.0394 1.0000 Uiso R . . . . . . H551 H -0.0166 0.5889 0.1931 0.0406 1.0000 Uiso R . . . . . . H651 H 0.0104 0.5312 0.1254 0.0389 1.0000 Uiso R . . . . . . H2451 H 0.1361 0.9366 0.1355 0.0499 1.0000 Uiso R . . . . . . H2452 H 0.0948 0.9269 0.1627 0.0499 1.0000 Uiso R . . . . . . H2551 H 0.0508 1.0194 0.0772 0.0731 1.0000 Uiso R . . . . . . H2552 H 0.0573 0.9361 0.0413 0.0731 1.0000 Uiso R . . . . . . H2553 H 0.0160 0.9264 0.0684 0.0731 1.0000 Uiso R . . . . . . H361 H 0.0852 0.8838 -0.1934 0.0546 1.0000 Uiso R . . . . . . H461 H 0.0336 1.0240 -0.2040 0.0584 1.0000 Uiso R . . . . . . H561 H 0.0527 1.1163 -0.1227 0.0637 1.0000 Uiso R . . . . . . H661 H 0.1153 1.0623 -0.0298 0.0511 1.0000 Uiso R . . . . . . H2461 H 0.1354 0.7520 -0.1811 0.0485 1.0000 Uiso R . . . . . . H2462 H 0.1924 0.7048 -0.1368 0.0485 1.0000 Uiso R . . . . . . H2561 H 0.2098 0.8084 -0.1966 0.0813 1.0000 Uiso R . . . . . . H2562 H 0.1843 0.8919 -0.1769 0.0813 1.0000 Uiso R . . . . . . H2563 H 0.2413 0.8447 -0.1325 0.0813 1.0000 Uiso R . . . . . . H171 H 0.3230 0.9427 0.2766 0.0592 1.0000 Uiso R . . . . . . H172 H 0.2603 0.9226 0.2301 0.0592 1.0000 Uiso R . . . . . . H173 H 0.2897 0.8584 0.2851 0.0592 1.0000 Uiso R . . . . . . H371 H 0.3937 0.8942 0.2548 0.0433 1.0000 Uiso R . . . . . . H571 H 0.4689 0.7764 0.1924 0.0498 1.0000 Uiso R . . . . . . H572 H 0.4537 0.8819 0.1966 0.0498 1.0000 Uiso R . . . . . . H573 H 0.4834 0.8205 0.2528 0.0498 1.0000 Uiso R . . . . . . H181 H 0.1825 0.4824 -0.2110 0.0632 1.0000 Uiso R . . . . . . H182 H 0.2420 0.5068 -0.1593 0.0632 1.0000 Uiso R . . . . . . H183 H 0.2188 0.4034 -0.1675 0.0632 1.0000 Uiso R . . . . . . H381 H 0.1053 0.5354 -0.2014 0.0428 1.0000 Uiso R . . . . . . H581 H 0.0258 0.6440 -0.1407 0.0492 1.0000 Uiso R . . . . . . H582 H 0.0482 0.6780 -0.1835 0.0492 1.0000 Uiso R . . . . . . H583 H 0.0133 0.5843 -0.1959 0.0492 1.0000 Uiso R . . . . . . H301 H 0.2424 1.2837 -0.1218 0.1085 0.7000 Uiso R . . . 2 . . H302 H 0.2802 1.2420 -0.1477 0.1085 0.7000 Uiso R . . . 2 . . H303 H 0.3031 1.2452 -0.0804 0.1085 0.7000 Uiso R . . . 2 . . H2601 H 0.0105 0.7543 -0.0875 0.0643 1.0000 Uiso R . . . . . . H2602 H 0.0195 0.7849 -0.0261 0.0643 1.0000 Uiso R . . . . . . H2603 H -0.0043 0.6844 -0.0500 0.0643 1.0000 Uiso R . . . . . . H2611 H 0.1301 0.2425 -0.0521 0.0541 1.0000 Uiso R . . . . . . H2612 H 0.1589 0.2943 -0.0847 0.0541 1.0000 Uiso R . . . . . . H2613 H 0.1008 0.3307 -0.0907 0.0541 1.0000 Uiso R . . . . . . H2621 H 0.3666 0.5595 0.3207 0.0584 1.0000 Uiso R . . . . . . H2622 H 0.3948 0.6346 0.2982 0.0584 1.0000 Uiso R . . . . . . H2623 H 0.3387 0.6590 0.3007 0.0584 1.0000 Uiso R . . . . . . H2571 H 0.4879 0.6716 0.1203 0.0485 1.0000 Uiso R . . . . . . H2572 H 0.4562 0.7524 0.0760 0.0485 1.0000 Uiso R . . . . . . H2573 H 0.4563 0.6498 0.0537 0.0485 1.0000 Uiso R . . . . . . H2581 H 0.0591 0.4574 0.0408 0.0397 1.0000 Uiso R . . . . . . H2582 H 0.0540 0.4805 -0.0202 0.0397 1.0000 Uiso R . . . . . . H2583 H 0.0852 0.3886 0.0126 0.0397 1.0000 Uiso R . . . . . . H2591 H 0.2031 0.6826 0.2135 0.0375 1.0000 Uiso R . . . . . . H2592 H 0.2307 0.5861 0.2419 0.0375 1.0000 Uiso R . . . . . . H2593 H 0.1646 0.5950 0.2066 0.0375 1.0000 Uiso R . . . . . . H201 H 0.4070 0.4922 0.2355 0.0343 1.0000 Uiso R . . . . . . H202 H 0.4396 0.5434 0.2067 0.0343 1.0000 Uiso R . . . . . . H203 H 0.4301 0.4342 0.1998 0.0343 1.0000 Uiso R . . . . . . H291 H 0.2893 0.3470 -0.0259 0.0351 1.0000 Uiso R . . . . . . H292 H 0.3293 0.2943 0.0316 0.0351 1.0000 Uiso R . . . . . . H293 H 0.2634 0.2817 0.0042 0.0351 1.0000 Uiso R . . . . . . H2411 H 0.3680 0.2613 0.3266 0.0666 0.3000 Uiso R . . . 1 . . H2412 H 0.3261 0.3470 0.3063 0.0666 0.3000 Uiso R . . . 1 . . H2413 H 0.3343 0.2188 0.3085 0.0666 0.7000 Uiso R . . . 2 . . H2414 H 0.2959 0.3080 0.2896 0.0666 0.7000 Uiso . . . . 2 . . H2410 H 0.0889 0.6551 -0.0396 0.0423 1.0000 Uiso R . . . . . . H2430 H 0.3102 0.5223 0.2302 0.0341 1.0000 Uiso R . . . . . . H2420 H 0.1845 0.3384 0.0186 0.0310 1.0000 Uiso R . . . . . . H2380 H 0.3958 0.6812 0.1149 0.0366 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0202(5) 0.0190(5) 0.0150(4) 0.0032(4) 0.0089(4) 0.0008(4) Mn2 0.0187(5) 0.0189(5) 0.0148(5) 0.0011(4) 0.0097(4) 0.0008(4) Mn3 0.0224(5) 0.0189(5) 0.0185(5) 0.0027(4) 0.0128(4) -0.0007(4) Mn4 0.0227(5) 0.0186(5) 0.0172(5) 0.0003(4) 0.0112(4) -0.0029(4) Mn5 0.0181(5) 0.0179(5) 0.0184(5) 0.0005(4) 0.0106(4) -0.0011(4) Mn6 0.0195(5) 0.0200(5) 0.0170(5) 0.0035(4) 0.0085(4) 0.0001(4) Gd1 0.01537(18) 0.01395(19) 0.00993(17) -0.00013(15) 0.00589(14) -0.00205(16) Gd2 0.01443(18) 0.01495(19) 0.00965(16) -0.00056(15) 0.00619(14) -0.00175(16) O13 0.025(2) 0.027(2) 0.0144(19) -0.0057(18) 0.0116(17) -0.0102(19) O24 0.025(2) 0.029(2) 0.019(2) 0.0023(18) 0.0150(19) -0.0068(19) O56 0.020(2) 0.019(2) 0.029(2) -0.0097(18) 0.0107(18) 0.0017(18) O11 0.040(3) 0.037(3) 0.026(2) 0.009(2) 0.019(2) 0.002(2) C11 0.029(4) 0.025(4) 0.034(4) 0.004(3) 0.010(3) -0.005(3) C21 0.031(4) 0.023(4) 0.032(4) 0.005(3) 0.016(3) 0.002(3) C31 0.037(4) 0.031(4) 0.029(3) 0.006(3) 0.011(3) -0.005(3) C41 0.033(4) 0.030(4) 0.034(4) 0.004(3) 0.009(3) 0.004(3) C51 0.031(4) 0.032(4) 0.037(4) -0.001(3) 0.010(3) 0.007(3) C61 0.024(3) 0.024(4) 0.030(3) -0.001(3) 0.006(3) 0.001(3) C211 0.032(4) 0.033(4) 0.024(3) 0.012(3) 0.013(3) 0.011(3) N221 0.031(3) 0.033(3) 0.025(3) 0.001(3) 0.020(2) 0.001(3) O231 0.034(3) 0.032(3) 0.025(2) 0.005(2) 0.016(2) 0.006(2) C241 0.063(6) 0.058(6) 0.041(4) 0.027(4) 0.031(4) 0.033(5) C251 0.099(10) 0.059(9) 0.023(6) 0.007(6) 0.023(6) 0.015(8) C250 0.09(2) 0.044(17) 0.07(2) 0.024(15) 0.063(19) -0.003(16) C12 0.028(3) 0.029(4) 0.033(3) 0.003(3) 0.020(3) -0.001(3) O12 0.036(3) 0.042(3) 0.024(2) 0.000(2) 0.018(2) 0.002(2) C22 0.036(4) 0.025(4) 0.034(4) -0.005(3) 0.022(3) -0.002(3) C32 0.046(4) 0.034(4) 0.038(4) -0.005(3) 0.024(4) -0.001(4) C42 0.059(5) 0.036(4) 0.051(5) -0.007(4) 0.040(4) 0.001(4) C52 0.046(4) 0.037(4) 0.046(4) 0.008(4) 0.032(4) 0.007(4) C62 0.032(4) 0.037(4) 0.033(4) 0.002(3) 0.017(3) 0.000(3) C212 0.034(4) 0.027(4) 0.022(3) -0.006(3) 0.015(3) -0.009(3) N222 0.033(3) 0.018(3) 0.022(3) 0.001(2) 0.014(2) 0.000(2) O232 0.035(3) 0.035(3) 0.027(2) 0.002(2) 0.017(2) 0.004(2) C242 0.035(4) 0.041(4) 0.024(3) -0.004(3) 0.018(3) -0.001(3) C252 0.048(5) 0.081(7) 0.031(4) 0.004(4) 0.020(4) -0.015(5) O237 0.035(3) 0.035(3) 0.038(3) 0.000(2) 0.023(2) 0.000(2) C13 0.018(3) 0.044(4) 0.029(3) 0.013(3) 0.011(3) -0.001(3) C23 0.030(4) 0.033(4) 0.041(4) 0.007(3) 0.022(3) -0.001(3) C33 0.065(6) 0.032(5) 0.087(7) 0.022(4) 0.053(5) 0.007(4) C43 0.070(6) 0.055(6) 0.119(8) 0.047(6) 0.076(6) 0.016(5) C53 0.045(5) 0.058(6) 0.064(5) 0.036(5) 0.042(4) 0.027(4) C63 0.030(4) 0.049(5) 0.043(4) 0.013(4) 0.024(3) 0.009(4) C213 0.030(4) 0.023(4) 0.036(4) 0.004(3) 0.017(3) -0.001(3) N223 0.031(3) 0.026(3) 0.022(3) 0.005(2) 0.014(2) 0.003(2) O233 0.031(2) 0.024(2) 0.031(2) 0.001(2) 0.017(2) -0.005(2) C243 0.056(5) 0.026(4) 0.064(5) 0.001(4) 0.039(4) -0.009(4) C253 0.074(6) 0.036(5) 0.081(6) 0.010(4) 0.058(6) 0.006(4) O14 0.043(3) 0.033(3) 0.029(2) 0.003(2) 0.019(2) -0.006(2) C14 0.038(4) 0.027(4) 0.030(3) 0.006(3) 0.016(3) 0.007(3) C24 0.036(4) 0.026(4) 0.039(4) 0.000(3) 0.022(3) -0.008(3) C34 0.045(4) 0.035(4) 0.054(5) -0.009(4) 0.029(4) -0.008(4) C44 0.055(5) 0.049(5) 0.081(6) -0.014(5) 0.046(5) -0.028(4) C54 0.060(5) 0.051(5) 0.063(5) 0.002(4) 0.045(5) -0.005(4) C64 0.049(4) 0.029(4) 0.048(4) 0.004(3) 0.034(4) -0.001(3) C214 0.027(3) 0.023(4) 0.033(4) 0.002(3) 0.014(3) -0.006(3) N224 0.028(3) 0.032(3) 0.026(3) 0.006(2) 0.015(2) -0.001(3) O234 0.026(2) 0.025(2) 0.024(2) 0.0101(19) 0.0113(19) -0.0025(19) C244 0.037(4) 0.027(4) 0.039(4) -0.004(3) 0.018(3) -0.006(3) C254 0.044(4) 0.035(4) 0.047(5) -0.008(4) 0.025(4) -0.006(4) C15 0.025(3) 0.029(4) 0.025(3) 0.001(3) 0.009(3) 0.000(3) O15 0.028(2) 0.030(3) 0.033(2) -0.003(2) 0.020(2) -0.001(2) C25 0.024(3) 0.032(4) 0.026(3) 0.004(3) 0.011(3) 0.007(3) C35 0.030(4) 0.026(4) 0.034(4) -0.001(3) 0.016(3) 0.001(3) C45 0.035(4) 0.040(4) 0.030(4) -0.005(3) 0.020(3) 0.004(3) C55 0.034(4) 0.038(4) 0.033(4) 0.006(3) 0.019(3) -0.001(3) C65 0.033(4) 0.035(4) 0.034(4) -0.005(3) 0.020(3) -0.009(3) C215 0.030(4) 0.030(4) 0.029(4) 0.000(3) 0.014(3) 0.003(3) N225 0.025(3) 0.022(3) 0.031(3) 0.003(2) 0.012(2) -0.003(2) O235 0.039(3) 0.032(3) 0.035(3) -0.004(2) 0.026(2) -0.007(2) C245 0.055(5) 0.033(4) 0.052(5) -0.003(4) 0.038(4) -0.007(4) C255 0.062(6) 0.025(4) 0.106(8) 0.007(5) 0.049(6) 0.003(4) C16 0.034(4) 0.028(4) 0.036(4) 0.005(3) 0.017(3) 0.004(3) O16 0.034(3) 0.036(3) 0.025(2) -0.001(2) 0.010(2) 0.002(2) C26 0.044(4) 0.026(4) 0.027(3) 0.005(3) 0.016(3) 0.003(3) C36 0.049(5) 0.044(5) 0.032(4) 0.006(4) 0.009(4) 0.002(4) C46 0.052(5) 0.035(5) 0.037(4) 0.008(3) 0.001(4) 0.008(4) C56 0.059(6) 0.033(5) 0.058(5) 0.006(4) 0.017(5) 0.012(4) C66 0.045(4) 0.040(4) 0.033(4) 0.003(4) 0.010(3) 0.004(4) C216 0.033(4) 0.034(4) 0.021(3) 0.005(3) 0.008(3) -0.002(3) N226 0.031(3) 0.023(3) 0.026(3) -0.004(2) 0.009(2) -0.007(2) O236 0.028(2) 0.022(2) 0.028(2) 0.0031(19) 0.0097(19) -0.002(2) C246 0.053(5) 0.039(4) 0.026(4) 0.004(3) 0.017(4) 0.009(4) C256 0.074(7) 0.097(8) 0.047(5) 0.018(5) 0.039(5) 0.003(6) C17 0.051(5) 0.047(5) 0.048(5) -0.020(4) 0.019(4) 0.004(4) O27 0.044(3) 0.019(2) 0.030(2) -0.012(2) 0.023(2) -0.002(2) C27 0.048(4) 0.023(4) 0.024(3) 0.005(3) 0.017(3) 0.007(3) C37 0.044(4) 0.029(4) 0.027(4) -0.010(3) 0.009(3) -0.005(3) C47 0.027(4) 0.031(4) 0.020(3) -0.002(3) 0.002(3) -0.004(3) O47 0.018(2) 0.021(2) 0.029(2) -0.0032(19) 0.0071(19) -0.0036(18) C57 0.027(4) 0.040(5) 0.046(4) -0.007(4) 0.006(3) -0.010(3) C18 0.046(5) 0.092(7) 0.024(4) 0.001(4) 0.019(4) -0.003(5) O28 0.038(3) 0.035(3) 0.016(2) -0.001(2) 0.0154(19) -0.004(2) C28 0.046(4) 0.041(5) 0.033(4) -0.012(3) 0.023(3) -0.010(4) C38 0.037(4) 0.044(5) 0.015(3) 0.005(3) 0.002(3) -0.004(4) C48 0.029(4) 0.028(4) 0.024(3) 0.001(3) 0.004(3) -0.008(3) O48 0.022(2) 0.032(3) 0.019(2) 0.0023(19) 0.0037(18) -0.0011(19) C58 0.039(4) 0.047(5) 0.028(4) 0.006(4) 0.006(3) -0.001(4) O19 0.025(2) 0.022(2) 0.024(2) -0.0053(19) 0.0119(19) -0.0054(19) C29 0.028(4) 0.025(4) 0.036(4) -0.004(3) 0.017(3) 0.000(3) O10 0.026(2) 0.027(2) 0.016(2) -0.0020(18) 0.0096(17) -0.0055(19) C20 0.026(3) 0.031(4) 0.025(3) 0.000(3) 0.009(3) -0.002(3) O238 0.028(2) 0.037(3) 0.032(2) -0.010(2) 0.018(2) -0.006(2) C257 0.035(4) 0.052(5) 0.036(4) 0.001(4) 0.017(3) -0.005(4) O239 0.020(2) 0.025(2) 0.019(2) 0.0022(18) 0.0054(17) -0.0071(18) C258 0.032(4) 0.034(4) 0.032(4) -0.006(3) 0.012(3) 0.000(3) O240 0.031(2) 0.029(2) 0.014(2) 0.0014(18) 0.0121(19) 0.002(2) C259 0.036(4) 0.041(4) 0.018(3) 0.003(3) 0.013(3) 0.003(3) O241 0.035(3) 0.048(3) 0.022(2) 0.002(2) 0.012(2) 0.009(2) C260 0.043(5) 0.068(6) 0.047(5) 0.002(4) 0.017(4) 0.010(5) O242 0.032(2) 0.022(2) 0.023(2) -0.0025(19) 0.0129(19) -0.007(2) C261 0.047(5) 0.050(5) 0.031(4) -0.008(4) 0.009(4) -0.011(4) O243 0.033(3) 0.037(3) 0.012(2) 0.0005(19) 0.0071(19) 0.002(2) C262 0.060(5) 0.046(5) 0.025(4) -0.003(3) 0.005(4) 0.000(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.0309(11) 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 Mn1 . Mn3 . 3.0754(13) yes Mn1 . O13 . 1.884(4) yes Mn1 . O11 . 1.842(5) yes Mn1 . N221 . 2.034(5) yes Mn1 . O233 . 2.202(4) yes Mn1 . O19 . 1.953(4) yes Mn1 . O10 . 2.338(4) yes Mn2 . O24 . 1.907(4) yes Mn2 . O12 . 1.858(5) yes Mn2 . N222 . 2.002(5) yes Mn2 . O19 . 2.226(4) yes Mn2 . O10 . 1.935(4) yes Mn2 . O238 . 2.382(4) yes Mn3 . O13 . 1.904(4) yes Mn3 . O231 . 2.206(4) yes Mn3 . O237 . 1.861(4) yes Mn3 . N223 . 2.035(5) yes Mn3 . O239 . 2.333(4) yes Mn3 . O240 . 1.963(4) yes Mn4 . O24 . 1.906(4) yes Mn4 . O232 . 1.931(4) yes Mn4 . O14 . 1.880(4) yes Mn4 . N224 . 2.034(6) yes Mn4 . O236 . 2.119(4) yes Mn4 . O238 . 2.530(4) yes Mn5 . O56 . 1.904(4) yes Mn5 . O15 . 1.868(4) yes Mn5 . N225 . 2.014(5) yes Mn5 . O239 . 1.940(4) yes Mn5 . O240 . 2.223(4) yes Mn5 . O241 . 2.345(4) yes Mn6 . O56 . 1.903(4) yes Mn6 . O234 . 2.100(4) yes Mn6 . O235 . 1.949(4) yes Mn6 . O16 . 1.874(5) yes Mn6 . N226 . 2.010(5) yes Gd1 . O13 . 2.414(4) yes Gd1 . O24 . 2.431(4) yes Gd1 . O56 . 2.403(4) yes Gd1 . O236 . 2.508(4) yes Gd1 . O28 . 2.327(4) yes Gd1 . O48 . 2.393(4) yes Gd1 . O19 . 2.622(4) yes Gd1 . O239 . 2.585(4) yes Gd1 . O242 . 2.398(4) yes Gd2 . O13 . 2.408(4) yes Gd2 . O24 . 2.385(4) yes Gd2 . O56 . 2.467(4) yes Gd2 . O234 . 2.488(4) yes Gd2 . O27 . 2.336(4) yes Gd2 . O47 . 2.383(4) yes Gd2 . O10 . 2.572(4) yes Gd2 . O240 . 2.588(4) yes Gd2 . O243 . 2.408(4) yes O11 . C11 . 1.316(7) yes C11 . C21 . 1.423(9) yes C11 . C61 . 1.403(9) yes C21 . C31 . 1.402(9) yes C21 . C211 . 1.468(9) yes C31 . C41 . 1.373(9) yes C31 . H311 . 0.950 no C41 . C51 . 1.397(9) yes C41 . H411 . 0.950 no C51 . C61 . 1.384(9) yes C51 . H511 . 0.950 no C61 . H611 . 0.950 no C211 . N221 . 1.313(8) yes C211 . C241 . 1.524(9) yes N221 . O231 . 1.362(6) yes C241 . C250 . 1.39(2) yes C241 . H2411 . 0.950 no C241 . H2412 . 0.950 no C251 . H2511 . 0.950 no C251 . H2512 . 0.950 no C251 . H2513 . 0.950 no C250 . H2501 . 0.950 no C250 . H2502 . 0.950 no C250 . H2503 . 0.950 no C12 . O12 . 1.315(7) yes C12 . C22 . 1.428(8) yes C12 . C62 . 1.403(9) yes C22 . C32 . 1.392(9) yes C22 . C212 . 1.459(9) yes C32 . C42 . 1.379(10) yes C32 . H321 . 0.950 no C42 . C52 . 1.397(10) yes C42 . H421 . 0.950 no C52 . C62 . 1.357(9) yes C52 . H521 . 0.950 no C62 . H621 . 0.950 no C212 . N222 . 1.302(8) yes C212 . C242 . 1.503(8) yes N222 . O232 . 1.369(6) yes C242 . C252 . 1.520(9) yes C242 . H2421 . 0.950 no C242 . H2422 . 0.950 no C252 . H2521 . 0.950 no C252 . H2522 . 0.950 no C252 . H2523 . 0.950 no O237 . C13 . 1.333(8) yes C13 . C23 . 1.396(10) yes C13 . C63 . 1.425(9) yes C23 . C33 . 1.404(9) yes C23 . C213 . 1.493(9) yes C33 . C43 . 1.388(11) yes C33 . H331 . 0.950 no C43 . C53 . 1.375(12) yes C43 . H431 . 0.950 no C53 . C63 . 1.371(10) yes C53 . H531 . 0.950 no C63 . H631 . 0.950 no C213 . N223 . 1.291(8) yes C213 . C243 . 1.473(9) yes N223 . O233 . 1.382(6) yes C243 . C253 . 1.521(10) yes C243 . H2431 . 0.950 no C243 . H2432 . 0.950 no C253 . H2531 . 0.950 no C253 . H2532 . 0.950 no C253 . H2533 . 0.950 no O14 . C14 . 1.313(8) yes C14 . C24 . 1.413(9) yes C14 . C64 . 1.401(9) yes C24 . C34 . 1.404(9) yes C24 . C214 . 1.471(9) yes C34 . C44 . 1.368(9) yes C34 . H341 . 0.950 no C44 . C54 . 1.390(11) yes C44 . H441 . 0.950 no C54 . C64 . 1.382(10) yes C54 . H541 . 0.950 no C64 . H641 . 0.950 no C214 . N224 . 1.290(8) yes C214 . C244 . 1.506(9) yes N224 . O234 . 1.364(6) yes C244 . C254 . 1.544(9) yes C244 . H2441 . 0.950 no C244 . H2442 . 0.950 no C254 . H2541 . 0.950 no C254 . H2542 . 0.950 no C254 . H2543 . 0.950 no C15 . O15 . 1.316(7) yes C15 . C25 . 1.406(9) yes C15 . C65 . 1.397(9) yes C25 . C35 . 1.394(8) yes C25 . C215 . 1.459(9) yes C35 . C45 . 1.372(9) yes C35 . H351 . 0.950 no C45 . C55 . 1.384(9) yes C45 . H451 . 0.950 no C55 . C65 . 1.374(9) yes C55 . H551 . 0.950 no C65 . H651 . 0.950 no C215 . N225 . 1.325(8) yes C215 . C245 . 1.503(9) yes N225 . O235 . 1.339(6) yes C245 . C255 . 1.538(10) yes C245 . H2451 . 0.950 no C245 . H2452 . 0.950 no C255 . H2551 . 0.950 no C255 . H2552 . 0.950 no C255 . H2553 . 0.950 no C16 . O16 . 1.341(8) yes C16 . C26 . 1.408(9) yes C16 . C66 . 1.388(10) yes C26 . C36 . 1.404(9) yes C26 . C216 . 1.475(9) yes C36 . C46 . 1.390(10) yes C36 . H361 . 0.950 no C46 . C56 . 1.363(10) yes C46 . H461 . 0.950 no C56 . C66 . 1.379(10) yes C56 . H561 . 0.950 no C66 . H661 . 0.950 no C216 . N226 . 1.297(8) yes C216 . C246 . 1.491(9) yes N226 . O236 . 1.368(6) yes C246 . C256 . 1.521(10) yes C246 . H2461 . 0.950 no C246 . H2462 . 0.950 no C256 . H2561 . 0.950 no C256 . H2562 . 0.950 no C256 . H2563 . 0.950 no C17 . C27 . 1.510(9) yes C17 . H171 . 0.950 no C17 . H172 . 0.950 no C17 . H173 . 0.950 no O27 . C27 . 1.275(8) yes C27 . C37 . 1.408(10) yes C37 . C47 . 1.384(9) yes C37 . H371 . 0.950 no C47 . O47 . 1.284(7) yes C47 . C57 . 1.509(9) yes C57 . H571 . 0.950 no C57 . H572 . 0.950 no C57 . H573 . 0.950 no C18 . C28 . 1.497(9) yes C18 . H181 . 0.950 no C18 . H182 . 0.950 no C18 . H183 . 0.950 no O28 . C28 . 1.252(7) yes C28 . C38 . 1.432(9) yes C38 . C48 . 1.376(9) yes C38 . H381 . 0.950 no C48 . O48 . 1.289(7) yes C48 . C58 . 1.520(9) yes C58 . H581 . 0.950 no C58 . H582 . 0.950 no C58 . H583 . 0.950 no O19 . C29 . 1.437(7) yes C29 . H291 . 0.950 no C29 . H292 . 0.950 no C29 . H293 . 0.950 no O10 . C20 . 1.443(6) yes C20 . H201 . 0.950 no C20 . H202 . 0.950 no C20 . H203 . 0.950 no O238 . C257 . 1.432(7) yes O238 . H2380 . 0.850 no C257 . H2571 . 0.950 no C257 . H2572 . 0.950 no C257 . H2573 . 0.950 no O239 . C258 . 1.440(7) yes C258 . H2581 . 0.950 no C258 . H2582 . 0.950 no C258 . H2583 . 0.950 no O240 . C259 . 1.436(7) yes C259 . H2591 . 0.950 no C259 . H2592 . 0.950 no C259 . H2593 . 0.950 no O241 . C260 . 1.424(8) yes O241 . H2410 . 0.850 no C260 . H2601 . 0.950 no C260 . H2602 . 0.950 no C260 . H2603 . 0.950 no O242 . C261 . 1.431(7) yes O242 . H2420 . 0.850 no C261 . H2611 . 0.950 no C261 . H2612 . 0.950 no C261 . H2613 . 0.950 no O243 . C262 . 1.410(7) yes O243 . H2430 . 0.850 no C262 . H2621 . 0.950 no C262 . H2622 . 0.950 no C262 . H2623 . 0.950 no N10 . C263 . 1.157(18) yes C263 . C30 . 1.291(18) yes C30 . H301 . 0.950 no C30 . H302 . 0.950 no C30 . H303 . 0.950 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 Mn3 . Mn1 . O13 . 35.95(11) yes Mn3 . Mn1 . O11 . 149.87(14) yes O13 . Mn1 . O11 . 173.69(19) yes Mn3 . Mn1 . N221 . 66.67(15) yes O13 . Mn1 . N221 . 93.97(19) yes O11 . Mn1 . N221 . 89.1(2) yes Mn3 . Mn1 . O233 . 63.32(12) yes O13 . Mn1 . O233 . 85.42(17) yes O11 . Mn1 . O233 . 100.15(19) yes N221 . Mn1 . O233 . 88.73(19) yes Mn3 . Mn1 . O19 . 113.53(13) yes O13 . Mn1 . O19 . 85.26(17) yes O11 . Mn1 . O19 . 91.41(18) yes N221 . Mn1 . O19 . 177.6(2) yes O233 . Mn1 . O19 . 93.48(16) yes Mn3 . Mn1 . O10 . 103.05(11) yes O13 . Mn1 . O10 . 78.32(16) yes O11 . Mn1 . O10 . 96.00(18) yes N221 . Mn1 . O10 . 93.93(18) yes O233 . Mn1 . O10 . 163.67(16) yes O19 . Mn1 . O10 . 83.68(15) yes O24 . Mn2 . O12 . 173.0(2) yes O24 . Mn2 . N222 . 93.37(19) yes O12 . Mn2 . N222 . 87.21(19) yes O24 . Mn2 . O19 . 82.23(16) yes O12 . Mn2 . O19 . 104.69(19) yes N222 . Mn2 . O19 . 92.61(18) yes O24 . Mn2 . O10 . 85.27(17) yes O12 . Mn2 . O10 . 94.14(18) yes N222 . Mn2 . O10 . 178.6(2) yes O19 . Mn2 . O10 . 87.18(16) yes O24 . Mn2 . O238 . 77.64(16) yes O12 . Mn2 . O238 . 95.55(18) yes N222 . Mn2 . O238 . 82.98(18) yes O19 . Mn2 . O238 . 159.07(16) yes O10 . Mn2 . O238 . 96.75(16) yes Mn1 . Mn3 . O13 . 35.50(13) yes Mn1 . Mn3 . O231 . 63.38(11) yes O13 . Mn3 . O231 . 85.23(16) yes Mn1 . Mn3 . O237 . 149.18(15) yes O13 . Mn3 . O237 . 175.3(2) yes O231 . Mn3 . O237 . 98.30(18) yes Mn1 . Mn3 . N223 . 66.20(15) yes O13 . Mn3 . N223 . 94.19(19) yes O231 . Mn3 . N223 . 86.18(18) yes O237 . Mn3 . N223 . 89.2(2) yes Mn1 . Mn3 . O239 . 103.65(10) yes O13 . Mn3 . O239 . 79.45(15) yes O231 . Mn3 . O239 . 164.62(15) yes O237 . Mn3 . O239 . 96.93(18) yes N223 . Mn3 . O239 . 96.19(17) yes Mn1 . Mn3 . O240 . 113.10(13) yes O13 . Mn3 . O240 . 84.76(18) yes O231 . Mn3 . O240 . 94.44(17) yes O237 . Mn3 . O240 . 91.82(19) yes N223 . Mn3 . O240 . 178.73(18) yes O239 . Mn3 . O240 . 82.92(15) yes O24 . Mn4 . O232 . 92.89(18) yes O24 . Mn4 . O14 . 179.1(2) yes O232 . Mn4 . O14 . 86.26(19) yes O24 . Mn4 . N224 . 94.85(19) yes O232 . Mn4 . N224 . 163.3(2) yes O14 . Mn4 . N224 . 85.9(2) yes O24 . Mn4 . O236 . 81.10(17) yes O232 . Mn4 . O236 . 98.45(18) yes O14 . Mn4 . O236 . 99.41(18) yes N224 . Mn4 . O236 . 97.38(19) yes O24 . Mn4 . O238 . 73.93(16) yes O232 . Mn4 . O238 . 83.87(16) yes O14 . Mn4 . O238 . 105.57(18) yes N224 . Mn4 . O238 . 84.07(18) yes O236 . Mn4 . O238 . 155.02(15) yes O56 . Mn5 . O15 . 175.10(18) yes O56 . Mn5 . N225 . 93.02(19) yes O15 . Mn5 . N225 . 87.0(2) yes O56 . Mn5 . O239 . 85.99(16) yes O15 . Mn5 . O239 . 93.91(17) yes N225 . Mn5 . O239 . 178.86(19) yes O56 . Mn5 . O240 . 82.07(16) yes O15 . Mn5 . O240 . 102.82(17) yes N225 . Mn5 . O240 . 94.00(18) yes O239 . Mn5 . O240 . 86.42(15) yes O56 . Mn5 . O241 . 79.99(17) yes O15 . Mn5 . O241 . 95.14(17) yes N225 . Mn5 . O241 . 84.40(19) yes O239 . Mn5 . O241 . 94.87(16) yes O240 . Mn5 . O241 . 161.87(16) yes O56 . Mn6 . O234 . 81.72(16) yes O56 . Mn6 . O235 . 93.85(18) yes O234 . Mn6 . O235 . 100.65(18) yes O56 . Mn6 . O16 . 179.17(18) yes O234 . Mn6 . O16 . 97.71(18) yes O235 . Mn6 . O16 . 85.65(19) yes O56 . Mn6 . N226 . 94.5(2) yes O234 . Mn6 . N226 . 98.69(19) yes O235 . Mn6 . N226 . 159.8(2) yes O16 . Mn6 . N226 . 86.2(2) yes O13 . Gd1 . O24 . 71.40(13) yes O13 . Gd1 . O56 . 73.75(14) yes O24 . Gd1 . O56 . 74.10(13) yes O13 . Gd1 . O236 . 128.88(13) yes O24 . Gd1 . O236 . 64.09(13) yes O56 . Gd1 . O236 . 71.07(14) yes O13 . Gd1 . O28 . 138.34(15) yes O24 . Gd1 . O28 . 96.63(14) yes O56 . Gd1 . O28 . 142.82(15) yes O236 . Gd1 . O28 . 72.53(15) yes O13 . Gd1 . O48 . 140.98(13) yes O24 . Gd1 . O48 . 135.32(14) yes O56 . Gd1 . O48 . 86.53(14) yes O236 . Gd1 . O48 . 71.64(14) yes O28 . Gd1 . O48 . 75.03(15) yes O13 . Gd1 . O19 . 61.99(13) yes O24 . Gd1 . O19 . 65.23(13) yes O56 . Gd1 . O19 . 126.80(13) yes O236 . Gd1 . O19 . 115.60(13) yes O28 . Gd1 . O19 . 76.65(14) yes O13 . Gd1 . O239 . 66.03(12) yes O24 . Gd1 . O239 . 125.92(12) yes O56 . Gd1 . O239 . 63.29(13) yes O236 . Gd1 . O239 . 124.14(14) yes O28 . Gd1 . O239 . 137.43(14) yes O13 . Gd1 . O242 . 86.61(14) yes O24 . Gd1 . O242 . 137.08(14) yes O56 . Gd1 . O242 . 135.10(14) yes O236 . Gd1 . O242 . 143.92(13) yes O28 . Gd1 . O242 . 75.60(15) yes O48 . Gd1 . O19 . 146.66(14) yes O48 . Gd1 . O239 . 75.07(13) yes O19 . Gd1 . O239 . 116.95(12) yes O48 . Gd1 . O242 . 84.23(14) yes O19 . Gd1 . O242 . 71.94(13) yes O239 . Gd1 . O242 . 71.87(13) yes O13 . Gd2 . O24 . 72.30(13) yes O13 . Gd2 . O56 . 72.71(13) yes O24 . Gd2 . O56 . 73.75(13) yes O13 . Gd2 . O234 . 130.28(13) yes O24 . Gd2 . O234 . 73.23(14) yes O56 . Gd2 . O234 . 63.92(13) yes O13 . Gd2 . O27 . 139.15(14) yes O24 . Gd2 . O27 . 145.14(15) yes O56 . Gd2 . O27 . 98.81(14) yes O234 . Gd2 . O27 . 73.03(14) yes O13 . Gd2 . O47 . 138.39(14) yes O24 . Gd2 . O47 . 86.69(14) yes O56 . Gd2 . O47 . 135.76(14) yes O234 . Gd2 . O47 . 72.60(14) yes O27 . Gd2 . O47 . 75.15(15) yes O13 . Gd2 . O10 . 65.28(13) yes O24 . Gd2 . O10 . 63.21(13) yes O56 . Gd2 . O10 . 126.51(12) yes O234 . Gd2 . O10 . 125.17(13) yes O27 . Gd2 . O10 . 134.65(14) yes O13 . Gd2 . O240 . 62.78(13) yes O24 . Gd2 . O240 . 125.57(13) yes O56 . Gd2 . O240 . 65.05(13) yes O234 . Gd2 . O240 . 114.55(13) yes O27 . Gd2 . O240 . 77.25(14) yes O13 . Gd2 . O243 . 86.30(14) yes O24 . Gd2 . O243 . 134.20(14) yes O56 . Gd2 . O243 . 137.96(14) yes O234 . Gd2 . O243 . 142.87(14) yes O27 . Gd2 . O243 . 73.69(15) yes O47 . Gd2 . O10 . 73.23(14) yes O47 . Gd2 . O240 . 147.71(13) yes O10 . Gd2 . O240 . 117.35(13) yes O47 . Gd2 . O243 . 83.38(15) yes O10 . Gd2 . O243 . 71.11(13) yes O240 . Gd2 . O243 . 72.99(13) yes Gd1 . O13 . Gd2 . 93.59(14) yes Gd1 . O13 . Mn3 . 116.82(18) yes Gd2 . O13 . Mn3 . 109.28(17) yes Gd1 . O13 . Mn1 . 110.12(17) yes Gd2 . O13 . Mn1 . 118.24(18) yes Mn3 . O13 . Mn1 . 108.6(2) yes Gd1 . O24 . Gd2 . 93.73(13) yes Gd1 . O24 . Mn2 . 114.34(19) yes Gd2 . O24 . Mn2 . 109.20(17) yes Gd1 . O24 . Mn4 . 110.89(18) yes Gd2 . O24 . Mn4 . 122.9(2) yes Mn2 . O24 . Mn4 . 105.80(18) yes Gd2 . O56 . Gd1 . 92.38(13) yes Gd2 . O56 . Mn5 . 113.36(18) yes Gd1 . O56 . Mn5 . 108.88(18) yes Gd2 . O56 . Mn6 . 109.58(17) yes Gd1 . O56 . Mn6 . 124.75(19) yes Mn5 . O56 . Mn6 . 107.36(19) yes Mn1 . O11 . C11 . 133.0(4) yes O11 . C11 . C21 . 124.8(6) yes O11 . C11 . C61 . 117.1(6) yes C21 . C11 . C61 . 118.0(6) yes C11 . C21 . C31 . 118.6(6) yes C11 . C21 . C211 . 121.4(6) yes C31 . C21 . C211 . 120.1(6) yes C21 . C31 . C41 . 121.9(6) yes C21 . C31 . H311 . 119.1 no C41 . C31 . H311 . 119.0 no C31 . C41 . C51 . 120.3(6) yes C31 . C41 . H411 . 119.9 no C51 . C41 . H411 . 119.7 no C41 . C51 . C61 . 118.6(7) yes C41 . C51 . H511 . 120.8 no C61 . C51 . H511 . 120.7 no C11 . C61 . C51 . 122.6(7) yes C11 . C61 . H611 . 118.6 no C51 . C61 . H611 . 118.8 no C21 . C211 . N221 . 122.6(6) yes C21 . C211 . C241 . 120.5(6) yes N221 . C211 . C241 . 116.9(6) yes Mn1 . N221 . C211 . 128.3(4) yes Mn1 . N221 . O231 . 114.0(4) yes C211 . N221 . O231 . 117.4(5) yes Mn3 . O231 . N221 . 108.6(3) yes C211 . C241 . C250 . 117.5(14) yes C211 . C241 . H2411 . 106.5 no C250 . C241 . H2411 . 108.0 no C211 . C241 . H2412 . 107.0 no C250 . C241 . H2412 . 108.3 no H2411 . C241 . H2412 . 109.5 no C241 . C251 . H2511 . 109.4 no C241 . C251 . H2512 . 109.8 no H2511 . C251 . H2512 . 109.5 no C241 . C251 . H2513 . 109.2 no H2511 . C251 . H2513 . 109.5 no H2512 . C251 . H2513 . 109.5 no C241 . C250 . H2501 . 106.3 no C241 . C250 . H2502 . 111.2 no H2501 . C250 . H2502 . 109.5 no C241 . C250 . H2503 . 110.8 no H2501 . C250 . H2503 . 109.5 no H2502 . C250 . H2503 . 109.5 no O12 . C12 . C22 . 123.0(6) yes O12 . C12 . C62 . 118.8(6) yes C22 . C12 . C62 . 118.2(6) yes C12 . O12 . Mn2 . 128.5(4) yes C12 . C22 . C32 . 117.8(6) yes C12 . C22 . C212 . 121.7(6) yes C32 . C22 . C212 . 120.4(6) yes C22 . C32 . C42 . 123.0(7) yes C22 . C32 . H321 . 118.6 no C42 . C32 . H321 . 118.5 no C32 . C42 . C52 . 118.5(7) yes C32 . C42 . H421 . 120.8 no C52 . C42 . H421 . 120.7 no C42 . C52 . C62 . 120.2(7) yes C42 . C52 . H521 . 119.9 no C62 . C52 . H521 . 119.9 no C12 . C62 . C52 . 122.3(7) yes C12 . C62 . H621 . 118.8 no C52 . C62 . H621 . 118.9 no C22 . C212 . N222 . 120.2(5) yes C22 . C212 . C242 . 120.9(6) yes N222 . C212 . C242 . 118.9(6) yes Mn2 . N222 . C212 . 129.5(4) yes Mn2 . N222 . O232 . 113.3(4) yes C212 . N222 . O232 . 117.1(5) yes N222 . O232 . Mn4 . 116.7(3) yes C212 . C242 . C252 . 112.0(5) yes C212 . C242 . H2421 . 108.9 no C252 . C242 . H2421 . 108.7 no C212 . C242 . H2422 . 108.8 no C252 . C242 . H2422 . 109.0 no H2421 . C242 . H2422 . 109.5 no C242 . C252 . H2521 . 109.4 no C242 . C252 . H2522 . 109.7 no H2521 . C252 . H2522 . 109.5 no C242 . C252 . H2523 . 109.3 no H2521 . C252 . H2523 . 109.5 no H2522 . C252 . H2523 . 109.5 no Mn3 . O237 . C13 . 127.6(4) yes O237 . C13 . C23 . 125.5(6) yes O237 . C13 . C63 . 114.4(7) yes C23 . C13 . C63 . 120.0(7) yes C13 . C23 . C33 . 118.3(6) yes C13 . C23 . C213 . 122.7(6) yes C33 . C23 . C213 . 118.9(7) yes C23 . C33 . C43 . 121.1(8) yes C23 . C33 . H331 . 119.3 no C43 . C33 . H331 . 119.5 no C33 . C43 . C53 . 119.9(7) yes C33 . C43 . H431 . 120.0 no C53 . C43 . H431 . 120.1 no C43 . C53 . C63 . 121.0(7) yes C43 . C53 . H531 . 119.5 no C63 . C53 . H531 . 119.5 no C13 . C63 . C53 . 119.5(8) yes C13 . C63 . H631 . 120.2 no C53 . C63 . H631 . 120.3 no C23 . C213 . N223 . 119.4(6) yes C23 . C213 . C243 . 120.4(6) yes N223 . C213 . C243 . 120.0(6) yes Mn3 . N223 . C213 . 130.5(5) yes Mn3 . N223 . O233 . 112.7(4) yes C213 . N223 . O233 . 116.8(5) yes Mn1 . O233 . N223 . 107.1(3) yes C213 . C243 . C253 . 111.9(7) yes C213 . C243 . H2431 . 108.8 no C253 . C243 . H2431 . 108.8 no C213 . C243 . H2432 . 108.9 no C253 . C243 . H2432 . 108.9 no H2431 . C243 . H2432 . 109.5 no C243 . C253 . H2531 . 109.5 no C243 . C253 . H2532 . 109.5 no H2531 . C253 . H2532 . 109.5 no C243 . C253 . H2533 . 109.4 no H2531 . C253 . H2533 . 109.5 no H2532 . C253 . H2533 . 109.5 no Mn4 . O14 . C14 . 123.0(4) yes O14 . C14 . C24 . 122.7(6) yes O14 . C14 . C64 . 117.8(6) yes C24 . C14 . C64 . 119.5(7) yes C14 . C24 . C34 . 118.0(6) yes C14 . C24 . C214 . 121.2(6) yes C34 . C24 . C214 . 120.7(6) yes C24 . C34 . C44 . 122.3(7) yes C24 . C34 . H341 . 118.8 no C44 . C34 . H341 . 119.0 no C34 . C44 . C54 . 119.1(7) yes C34 . C44 . H441 . 120.3 no C54 . C44 . H441 . 120.6 no C44 . C54 . C64 . 120.7(7) yes C44 . C54 . H541 . 119.6 no C64 . C54 . H541 . 119.7 no C14 . C64 . C54 . 120.4(7) yes C14 . C64 . H641 . 119.8 no C54 . C64 . H641 . 119.9 no C24 . C214 . N224 . 118.8(6) yes C24 . C214 . C244 . 119.8(6) yes N224 . C214 . C244 . 121.4(6) yes Mn4 . N224 . C214 . 128.3(4) yes Mn4 . N224 . O234 . 112.7(4) yes C214 . N224 . O234 . 118.8(5) yes Mn6 . O234 . Gd2 . 102.49(16) yes Mn6 . O234 . N224 . 114.1(3) yes Gd2 . O234 . N224 . 119.5(3) yes C214 . C244 . C254 . 113.5(5) yes C214 . C244 . H2441 . 108.5 no C254 . C244 . H2441 . 108.4 no C214 . C244 . H2442 . 108.4 no C254 . C244 . H2442 . 108.5 no H2441 . C244 . H2442 . 109.5 no C244 . C254 . H2541 . 109.6 no C244 . C254 . H2542 . 109.5 no H2541 . C254 . H2542 . 109.5 no C244 . C254 . H2543 . 109.4 no H2541 . C254 . H2543 . 109.5 no H2542 . C254 . H2543 . 109.5 no O15 . C15 . C25 . 123.6(6) yes O15 . C15 . C65 . 116.9(6) yes C25 . C15 . C65 . 119.5(6) yes C15 . O15 . Mn5 . 128.3(4) yes C15 . C25 . C35 . 117.9(6) yes C15 . C25 . C215 . 121.5(6) yes C35 . C25 . C215 . 120.6(6) yes C25 . C35 . C45 . 122.1(6) yes C25 . C35 . H351 . 119.0 no C45 . C35 . H351 . 119.0 no C35 . C45 . C55 . 119.7(6) yes C35 . C45 . H451 . 120.2 no C55 . C45 . H451 . 120.1 no C45 . C55 . C65 . 119.8(6) yes C45 . C55 . H551 . 120.1 no C65 . C55 . H551 . 120.1 no C15 . C65 . C55 . 121.0(7) yes C15 . C65 . H651 . 119.5 no C55 . C65 . H651 . 119.4 no C25 . C215 . N225 . 120.2(6) yes C25 . C215 . C245 . 121.9(6) yes N225 . C215 . C245 . 117.8(6) yes Mn5 . N225 . C215 . 129.2(5) yes Mn5 . N225 . O235 . 115.1(4) yes C215 . N225 . O235 . 115.1(5) yes N225 . O235 . Mn6 . 116.6(4) yes C215 . C245 . C255 . 109.1(6) yes C215 . C245 . H2451 . 109.6 no C255 . C245 . H2451 . 109.5 no C215 . C245 . H2452 . 109.6 no C255 . C245 . H2452 . 109.5 no H2451 . C245 . H2452 . 109.5 no C245 . C255 . H2551 . 109.4 no C245 . C255 . H2552 . 109.5 no H2551 . C255 . H2552 . 109.5 no C245 . C255 . H2553 . 109.5 no H2551 . C255 . H2553 . 109.5 no H2552 . C255 . H2553 . 109.5 no O16 . C16 . C26 . 121.7(6) yes O16 . C16 . C66 . 118.9(6) yes C26 . C16 . C66 . 119.2(6) yes C16 . O16 . Mn6 . 122.6(4) yes C16 . C26 . C36 . 118.3(6) yes C16 . C26 . C216 . 122.1(6) yes C36 . C26 . C216 . 119.5(6) yes C26 . C36 . C46 . 121.0(7) yes C26 . C36 . H361 . 119.5 no C46 . C36 . H361 . 119.5 no C36 . C46 . C56 . 119.7(7) yes C36 . C46 . H461 . 120.2 no C56 . C46 . H461 . 120.1 no C46 . C56 . C66 . 120.4(8) yes C46 . C56 . H561 . 119.9 no C66 . C56 . H561 . 119.7 no C16 . C66 . C56 . 121.2(7) yes C16 . C66 . H661 . 119.3 no C56 . C66 . H661 . 119.4 no C26 . C216 . N226 . 117.9(6) yes C26 . C216 . C246 . 121.1(6) yes N226 . C216 . C246 . 120.9(6) yes Mn6 . N226 . C216 . 129.2(5) yes Mn6 . N226 . O236 . 111.9(4) yes C216 . N226 . O236 . 118.7(5) yes Mn4 . O236 . Gd1 . 101.24(16) yes Mn4 . O236 . N226 . 114.4(3) yes Gd1 . O236 . N226 . 121.9(3) yes C216 . C246 . C256 . 113.0(7) yes C216 . C246 . H2461 . 108.6 no C256 . C246 . H2461 . 108.7 no C216 . C246 . H2462 . 108.4 no C256 . C246 . H2462 . 108.7 no H2461 . C246 . H2462 . 109.5 no C246 . C256 . H2561 . 109.4 no C246 . C256 . H2562 . 109.5 no H2561 . C256 . H2562 . 109.5 no C246 . C256 . H2563 . 109.5 no H2561 . C256 . H2563 . 109.5 no H2562 . C256 . H2563 . 109.5 no C27 . C17 . H171 . 109.4 no C27 . C17 . H172 . 109.2 no H171 . C17 . H172 . 109.5 no C27 . C17 . H173 . 109.7 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no Gd2 . O27 . C27 . 134.8(4) yes C17 . C27 . O27 . 115.6(6) yes C17 . C27 . C37 . 119.8(6) yes O27 . C27 . C37 . 124.4(6) yes C27 . C37 . C47 . 127.4(6) yes C27 . C37 . H371 . 116.3 no C47 . C37 . H371 . 116.2 no C37 . C47 . O47 . 124.9(6) yes C37 . C47 . C57 . 119.7(6) yes O47 . C47 . C57 . 115.4(6) yes C47 . O47 . Gd2 . 133.0(4) yes C47 . C57 . H571 . 109.5 no C47 . C57 . H572 . 109.4 no H571 . C57 . H572 . 109.5 no C47 . C57 . H573 . 109.5 no H571 . C57 . H573 . 109.5 no H572 . C57 . H573 . 109.5 no C28 . C18 . H181 . 109.3 no C28 . C18 . H182 . 109.5 no H181 . C18 . H182 . 109.5 no C28 . C18 . H183 . 109.6 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no Gd1 . O28 . C28 . 136.2(5) yes C18 . C28 . O28 . 117.6(6) yes C18 . C28 . C38 . 119.4(6) yes O28 . C28 . C38 . 122.9(6) yes C28 . C38 . C48 . 127.2(6) yes C28 . C38 . H381 . 116.3 no C48 . C38 . H381 . 116.5 no C38 . C48 . O48 . 125.9(6) yes C38 . C48 . C58 . 119.4(6) yes O48 . C48 . C58 . 114.7(6) yes C48 . O48 . Gd1 . 130.8(4) yes C48 . C58 . H581 . 109.5 no C48 . C58 . H582 . 109.4 no H581 . C58 . H582 . 109.5 no C48 . C58 . H583 . 109.5 no H581 . C58 . H583 . 109.5 no H582 . C58 . H583 . 109.5 no Mn2 . O19 . Gd1 . 97.57(15) yes Mn2 . O19 . Mn1 . 95.44(17) yes Gd1 . O19 . Mn1 . 100.22(16) yes Mn2 . O19 . C29 . 118.9(3) yes Gd1 . O19 . C29 . 122.3(4) yes Mn1 . O19 . C29 . 117.3(4) yes O19 . C29 . H291 . 109.5 no O19 . C29 . H292 . 109.4 no H291 . C29 . H292 . 109.5 no O19 . C29 . H293 . 109.5 no H291 . C29 . H293 . 109.5 no H292 . C29 . H293 . 109.5 no Gd2 . O10 . Mn1 . 97.45(14) yes Gd2 . O10 . Mn2 . 101.33(16) yes Mn1 . O10 . Mn2 . 92.42(15) yes Gd2 . O10 . C20 . 124.5(3) yes Mn1 . O10 . C20 . 114.7(4) yes Mn2 . O10 . C20 . 119.9(3) yes O10 . C20 . H201 . 109.6 no O10 . C20 . H202 . 109.3 no H201 . C20 . H202 . 109.5 no O10 . C20 . H203 . 109.5 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no Mn2 . O238 . Mn4 . 76.43(12) yes Mn2 . O238 . C257 . 126.2(4) yes Mn4 . O238 . C257 . 123.1(4) yes Mn2 . O238 . H2380 . 92.8 no Mn4 . O238 . H2380 . 95.8 no C257 . O238 . H2380 . 128.3 no O238 . C257 . H2571 . 109.5 no O238 . C257 . H2572 . 109.5 no H2571 . C257 . H2572 . 109.5 no O238 . C257 . H2573 . 109.4 no H2571 . C257 . H2573 . 109.5 no H2572 . C257 . H2573 . 109.5 no Gd1 . O239 . Mn3 . 97.03(13) yes Gd1 . O239 . Mn5 . 100.99(16) yes Mn3 . O239 . Mn5 . 93.21(15) yes Gd1 . O239 . C258 . 125.4(3) yes Mn3 . O239 . C258 . 115.9(3) yes Mn5 . O239 . C258 . 118.0(4) yes O239 . C258 . H2581 . 109.4 no O239 . C258 . H2582 . 109.6 no H2581 . C258 . H2582 . 109.5 no O239 . C258 . H2583 . 109.4 no H2581 . C258 . H2583 . 109.5 no H2582 . C258 . H2583 . 109.5 no Mn5 . O240 . Gd2 . 99.00(14) yes Mn5 . O240 . Mn3 . 96.03(17) yes Gd2 . O240 . Mn3 . 100.77(16) yes Mn5 . O240 . C259 . 118.0(4) yes Gd2 . O240 . C259 . 121.6(4) yes Mn3 . O240 . C259 . 116.9(4) yes O240 . C259 . H2591 . 109.5 no O240 . C259 . H2592 . 109.7 no H2591 . C259 . H2592 . 109.5 no O240 . C259 . H2593 . 109.2 no H2591 . C259 . H2593 . 109.5 no H2592 . C259 . H2593 . 109.5 no Mn5 . O241 . C260 . 126.7(4) yes Mn5 . O241 . H2410 . 95.2 no C260 . O241 . H2410 . 122.4 no O241 . C260 . H2601 . 109.6 no O241 . C260 . H2602 . 109.1 no H2601 . C260 . H2602 . 109.5 no O241 . C260 . H2603 . 109.7 no H2601 . C260 . H2603 . 109.5 no H2602 . C260 . H2603 . 109.5 no Gd1 . O242 . C261 . 137.7(4) yes Gd1 . O242 . H2420 . 101.1 no C261 . O242 . H2420 . 119.3 no O242 . C261 . H2611 . 109.3 no O242 . C261 . H2612 . 109.5 no H2611 . C261 . H2612 . 109.5 no O242 . C261 . H2613 . 109.6 no H2611 . C261 . H2613 . 109.5 no H2612 . C261 . H2613 . 109.5 no Gd2 . O243 . C262 . 137.6(4) yes Gd2 . O243 . H2430 . 101.1 no C262 . O243 . H2430 . 119.8 no O243 . C262 . H2621 . 109.6 no O243 . C262 . H2622 . 109.1 no H2621 . C262 . H2622 . 109.5 no O243 . C262 . H2623 . 109.8 no H2621 . C262 . H2623 . 109.5 no H2622 . C262 . H2623 . 109.5 no N10 . C263 . C30 . 169(3) yes C263 . C30 . H301 . 109.4 no C263 . C30 . H302 . 109.7 no H301 . C30 . H302 . 109.5 no C263 . C30 . H303 . 109.3 no H301 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no # Attachment '- complex2.cif' data_eb0224 _database_code_depnum_ccdc_archive 'CCDC 810534' #TrackingRef '- complex2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Ross Inglis' _exptl_crystal_recrystallization_method 'diffusion of hexane into MeOH/MeCN solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H91 La2 Mn6 N6 O27, C6 H14' _chemical_formula_sum 'C78 H105 La2 Mn6 N6 O27' _chemical_formula_weight 2166.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, y, -z+1/2' '-x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z+1/2' '-x+1/2, -y+1/2, z+1/2' _cell_length_a 15.3154(6) _cell_length_b 22.8884(6) _cell_length_c 25.7786(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9036.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9882 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 26.4405 _exptl_crystal_description cuboid _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4380 _exptl_absorpt_coefficient_mu 1.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6042 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II CCD on D8' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 66786 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.46 _reflns_number_total 9309 _reflns_number_gt 8961 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'Shelxs Sheldrick' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. list of restraints applied: SIMU 0.02 O1A C1A SIMU 0.02 C1A C2A SIMU 0.02 C2A C3A SIMU 0.02 C3A C4A SIMU 0.02 C4A C5A SIMU 0.02 C5A C6A SIMU 0.02 C1A C6A SIMU 0.02 C2A C21A SIMU 0.02 C21A N22A SIMU 0.02 N22A O23A SIMU 0.02 C21A C24A SIMU 0.02 C24A C25A SIMU 0.02 O1A' C1A' SIMU 0.02 C1A' C2A SIMU 0.02 C2A C3A' SIMU 0.02 C3A' C4A' SIMU 0.02 C4A' C5A' SIMU 0.02 C5A' C6A' SIMU 0.02 C6A' C1A' SIMU 0.02 O1B C1B SIMU 0.02 C1B C2B SIMU 0.02 C2B C3B SIMU 0.02 C3B C4B SIMU 0.02 C4B C5B SIMU 0.02 C5B C6B SIMU 0.02 C1B C6B SIMU 0.02 C2B C21B SIMU 0.02 C21B N22B SIMU 0.02 N22B O23B SIMU 0.02 C21B C24B SIMU 0.02 C24B C25B SIMU 0.02 C2B C3B' SIMU 0.02 C3B' C4B' SIMU 0.02 C4B' C5B SIMU 0.02 C21B C24' SIMU 0.02 C24' C25' SIMU 0.02 O1C C1C SIMU 0.02 C1C C2C SIMU 0.02 C2C C3C SIMU 0.02 C3C C4C SIMU 0.02 C4C C5C SIMU 0.02 C5C C6C SIMU 0.02 C1C C6C SIMU 0.02 C2C C21C SIMU 0.02 C21C N22C SIMU 0.02 N22C O23C SIMU 0.02 C21C C24C SIMU 0.02 C24C C25C SIMU 0.02 C1C C2C' SIMU 0.02 C2C' C3C' SIMU 0.02 C3C' C4C' SIMU 0.02 C4C' C5C' SIMU 0.02 C5C' C6C SIMU 0.02 C2C' C21" SIMU 0.02 C21" C24" SIMU 0.02 C24" C25" SIMU 0.02 C1D C2D SIMU 0.02 C2D C3D SIMU 0.02 C2D O2D SIMU 0.02 C3D C4D SIMU 0.02 C4D C5D SIMU 0.02 C4D O4D SIMU 0.02 C1D' C2D' SIMU 0.02 C2D' C3D' SIMU 0.02 C2D' O2D' SIMU 0.02 C3D' C4D' SIMU 0.02 C4D' C5D' SIMU 0.02 C4D' O4D' SIMU 0.02 O1G C2G SIMU 0.02 O1G C2G' DELU 0.01 O1A C1A DELU 0.01 C1A C2A DELU 0.01 C2A C3A DELU 0.01 C3A C4A DELU 0.01 C4A C5A DELU 0.01 C5A C6A DELU 0.01 C1A C6A DELU 0.01 C2A C21A DELU 0.01 C21A N22A DELU 0.01 N22A O23A DELU 0.01 C21A C24A DELU 0.01 C24A C25A DELU 0.01 O1A' C1A' DELU 0.01 C1A' C2A DELU 0.01 C2A C3A' DELU 0.01 C3A' C4A' DELU 0.01 C4A' C5A' DELU 0.01 C5A' C6A' DELU 0.01 C6A' C1A' DELU 0.01 O1B C1B DELU 0.01 C1B C2B DELU 0.01 C2B C3B DELU 0.01 C3B C4B DELU 0.01 C4B C5B DELU 0.01 C5B C6B DELU 0.01 C1B C6B DELU 0.01 C2B C21B DELU 0.01 C21B N22B DELU 0.01 N22B O23B DELU 0.01 C21B C24B DELU 0.01 C24B C25B DELU 0.01 C2B C3B' DELU 0.01 C3B' C4B' DELU 0.01 C4B' C5B DELU 0.01 C21B C24' DELU 0.01 C24' C25' DELU 0.01 O1C C1C DELU 0.01 C1C C2C DELU 0.01 C2C C3C DELU 0.01 C3C C4C DELU 0.01 C4C C5C DELU 0.01 C5C C6C DELU 0.01 C1C C6C DELU 0.01 C2C C21C DELU 0.01 C21C N22C DELU 0.01 N22C O23C DELU 0.01 C21C C24C DELU 0.01 C24C C25C DELU 0.01 C1C C2C' DELU 0.01 C2C' C3C' DELU 0.01 C3C' C4C' DELU 0.01 C4C' C5C' DELU 0.01 C5C' C6C DELU 0.01 C2C' C21" DELU 0.01 C21" C24" DELU 0.01 C24" C25" DELU 0.01 C1D C2D DELU 0.01 C2D C3D DELU 0.01 C2D O2D DELU 0.01 C3D C4D DELU 0.01 C4D C5D DELU 0.01 C4D O4D DELU 0.01 C1D' C2D' DELU 0.01 C2D' C3D' DELU 0.01 C2D' O2D' DELU 0.01 C3D' C4D' DELU 0.01 C4D' C5D' DELU 0.01 C4D' O4D' DELU 0.01 O1G C2G DELU 0.01 O1G C2G' DFIX 1.54 C1S C2S DFIX 1.54 C2S C3S DFIX 1.54 C3S C4S DFIX 1.54 C4S C5S DFIX 1.54 C5S C6S DFIX 2.51 C1S C3S DFIX 2.51 C2S C4S DFIX 2.51 C3S C5S DFIX 2.51 C4S C6S DELU 0.01 C1S C2S DELU 0.01 C2S C3S DELU 0.01 C3S C4S DELU 0.01 C4S C5S DELU 0.01 C5S C6S ISOR 0.01 O1A ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+9.3551P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(16) _refine_ls_number_reflns 9309 _refine_ls_number_parameters 766 _refine_ls_number_restraints 505 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0578 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La -0.109964(10) 0.134655(7) 0.719045(6) 0.01659(4) Uani 1 1 d . . . Mn1 Mn 0.08010(3) 0.14038(2) 0.637866(16) 0.01860(9) Uani 1 1 d . . . Mn3 Mn -0.06539(3) 0.018803(19) 0.813679(18) 0.02018(10) Uani 1 1 d . . . Mn4 Mn -0.05433(3) 0.256803(19) 0.800354(18) 0.01960(10) Uani 1 1 d . . . O13 O -0.04016(13) 0.09909(8) 0.80326(7) 0.0163(4) Uani 1 1 d . . . O14 O 0.0000 0.20952(12) 0.7500 0.0162(6) Uani 1 2 d S . . C2A C -0.0529(3) -0.08395(15) 0.63514(14) 0.0339(8) Uani 1 1 d U . . C1A C 0.0494(14) -0.0850(16) 0.6406(10) 0.027(4) Uani 0.40 1 d PU A 1 O1A O 0.0969(18) -0.0556(13) 0.6749(10) 0.030(4) Uani 0.40 1 d PU . 1 C3A C -0.0868(18) -0.1201(14) 0.6019(13) 0.047(5) Uani 0.40 1 d PU A 1 H3A H -0.1486 -0.1240 0.6022 0.056 Uiso 0.40 1 calc PR A 1 C4A C -0.0414(15) -0.1541(11) 0.5655(10) 0.055(5) Uani 0.40 1 d PU A 1 H4A H -0.0701 -0.1780 0.5407 0.066 Uiso 0.40 1 calc PR A 1 C5A C 0.0491(13) -0.1500(12) 0.5688(8) 0.058(5) Uani 0.40 1 d PU A 1 H5A H 0.0829 -0.1706 0.5438 0.069 Uiso 0.40 1 calc PR A 1 C6A C 0.0904(19) -0.1199(16) 0.6037(10) 0.041(5) Uani 0.40 1 d PU A 1 H6A H 0.1523 -0.1218 0.6040 0.049 Uiso 0.40 1 calc PR A 1 O1A' O 0.0838(10) -0.0608(8) 0.6648(6) 0.022(2) Uani 0.60 1 d PU . 2 C1A' C 0.0330(10) -0.0876(10) 0.6307(7) 0.027(3) Uani 0.60 1 d PU A 2 C3A' C -0.1070(10) -0.1122(8) 0.5948(8) 0.036(3) Uani 0.60 1 d PU A 2 H3A' H -0.1687 -0.1077 0.5952 0.043 Uiso 0.60 1 calc PR A 2 C4A' C -0.0681(7) -0.1446(7) 0.5573(6) 0.041(3) Uani 0.60 1 d PU A 2 H4A' H -0.1029 -0.1642 0.5322 0.050 Uiso 0.60 1 calc PR A 2 C5A' C 0.0230(7) -0.1495(5) 0.5553(4) 0.032(2) Uani 0.60 1 d PU A 2 H5A' H 0.0497 -0.1723 0.5289 0.038 Uiso 0.60 1 calc PR A 2 C6A' C 0.0738(11) -0.1215(9) 0.5911(6) 0.032(3) Uani 0.60 1 d PU A 2 H6A' H 0.1356 -0.1246 0.5897 0.039 Uiso 0.60 1 calc PR A 2 C21A C -0.0991(2) -0.05074(13) 0.67512(12) 0.0284(7) Uani 1 1 d U A . N22A N -0.05838(17) -0.00791(11) 0.69764(10) 0.0235(6) Uani 1 1 d U . . O23A O -0.10330(14) 0.02319(8) 0.73484(7) 0.0220(4) Uani 1 1 d U A . C24A C -0.1905(2) -0.06772(16) 0.69037(16) 0.0388(9) Uani 1 1 d U . . H24A H -0.2277 -0.0693 0.6590 0.047 Uiso 1 1 calc R A . H24B H -0.2149 -0.0377 0.7139 0.047 Uiso 1 1 calc R . . C25A C -0.1918(3) -0.12695(16) 0.71734(19) 0.0559(12) Uani 1 1 d U A . H25A H -0.2520 -0.1370 0.7266 0.084 Uiso 1 1 calc R . . H25B H -0.1560 -0.1252 0.7488 0.084 Uiso 1 1 calc R . . H25C H -0.1682 -0.1568 0.6939 0.084 Uiso 1 1 calc R . . C1B C 0.1890(2) 0.17902(14) 0.55229(12) 0.0262(7) Uani 1 1 d U B . O1B O 0.11327(16) 0.17792(10) 0.57689(8) 0.0280(5) Uani 1 1 d U . . C2B C 0.2558(2) 0.13778(17) 0.55928(13) 0.0338(7) Uani 1 1 d U . . C3B C 0.3191(16) 0.1373(13) 0.5173(8) 0.033(4) Uani 0.30 1 d PU B 1 H3B H 0.3557 0.1040 0.5144 0.040 Uiso 0.30 1 calc PR B 1 C4B C 0.330(2) 0.1790(13) 0.4834(10) 0.037(5) Uani 0.30 1 d PU B 1 H4B H 0.3735 0.1762 0.4574 0.045 Uiso 0.30 1 calc PR B 1 C3B' C 0.3355(8) 0.1450(6) 0.5327(3) 0.042(2) Uani 0.70 1 d PU B 2 H3B' H 0.3831 0.1195 0.5396 0.051 Uiso 0.70 1 calc PR B 2 C4B' C 0.3447(9) 0.1903(6) 0.4958(4) 0.047(3) Uani 0.70 1 d PU B 2 H4B' H 0.3981 0.1951 0.4775 0.056 Uiso 0.70 1 calc PR B 2 C5B C 0.2754(3) 0.22760(18) 0.48637(15) 0.0446(10) Uani 1 1 d U . . H5B H 0.2896 0.2624 0.4682 0.054 Uiso 0.30 1 calc PR B 1 H5B' H 0.2792 0.2557 0.4594 0.054 Uiso 0.70 1 d PR B 2 C6B C 0.2013(2) 0.22452(16) 0.51581(13) 0.0327(8) Uani 1 1 d U B . H6B H 0.1573 0.2534 0.5117 0.039 Uiso 1 1 calc R . . C21B C 0.2475(2) 0.08920(15) 0.59624(15) 0.0355(8) Uani 1 1 d U B . N22B N 0.18227(18) 0.08707(11) 0.62852(11) 0.0260(6) Uani 1 1 d U . . O23B O 0.17966(17) 0.03914(10) 0.66028(11) 0.0404(7) Uani 1 1 d U . . C24B C 0.3252(9) 0.0470(7) 0.6060(5) 0.024(2) Uani 0.40 1 d PU B 1 H24C H 0.3013 0.0103 0.6206 0.029 Uiso 0.40 1 calc PR B 1 H24D H 0.3514 0.0372 0.5720 0.029 Uiso 0.40 1 calc PR B 1 C25B C 0.3976(6) 0.0675(4) 0.6413(3) 0.0309(18) Uani 0.40 1 d PU B 1 H25D H 0.4417 0.0366 0.6445 0.046 Uiso 0.40 1 calc PR B 1 H25E H 0.3736 0.0764 0.6756 0.046 Uiso 0.40 1 calc PR B 1 H25F H 0.4245 0.1026 0.6267 0.046 Uiso 0.40 1 calc PR B 1 C24' C 0.3048(8) 0.0369(5) 0.5888(4) 0.048(3) Uani 0.60 1 d PU B 2 H24E H 0.3095 0.0158 0.6222 0.058 Uiso 0.60 1 calc PR B 2 H24F H 0.3641 0.0503 0.5791 0.058 Uiso 0.60 1 calc PR B 2 C25' C 0.2711(7) -0.0068(4) 0.5461(3) 0.085(3) Uani 0.60 1 d PU B 2 H25G H 0.3123 -0.0393 0.5427 0.127 Uiso 0.60 1 calc PR B 2 H25H H 0.2663 0.0137 0.5128 0.127 Uiso 0.60 1 calc PR B 2 H25I H 0.2137 -0.0219 0.5562 0.127 Uiso 0.60 1 calc PR B 2 C1C C 0.0840(2) 0.34469(14) 0.62006(14) 0.0323(8) Uani 1 1 d U . . O1C O 0.10891(17) 0.29910(10) 0.64757(9) 0.0342(5) Uani 1 1 d U . . C2C C -0.0055(11) 0.3726(11) 0.6248(9) 0.033(3) Uani 0.45 1 d PU C 1 C3C C -0.0258(12) 0.4175(8) 0.5897(7) 0.057(4) Uani 0.45 1 d PU C 1 H3C H -0.0783 0.4391 0.5939 0.068 Uiso 0.45 1 calc PR C 1 C4C C 0.0290(12) 0.4303(7) 0.5496(7) 0.065(4) Uani 0.45 1 d PU C 1 H4C H 0.0121 0.4594 0.5253 0.078 Uiso 0.45 1 calc PR C 1 C5C C 0.1091(18) 0.4022(12) 0.5430(10) 0.057(5) Uani 0.45 1 d PU C 1 H5C H 0.1434 0.4102 0.5131 0.069 Uiso 0.45 1 calc PR C 1 C2C' C 0.0166(9) 0.3781(9) 0.6327(8) 0.035(3) Uani 0.55 1 d PU C 2 C3C' C 0.0001(8) 0.4298(6) 0.6024(6) 0.044(3) Uani 0.55 1 d PU C 2 H3C' H -0.0501 0.4527 0.6098 0.053 Uiso 0.55 1 calc PR C 2 C4C' C 0.0540(8) 0.4464(5) 0.5639(5) 0.046(3) Uani 0.55 1 d PU C 2 H4C' H 0.0419 0.4804 0.5440 0.055 Uiso 0.55 1 calc PR C 2 C5C' C 0.1272(11) 0.4131(9) 0.5538(7) 0.044(3) Uani 0.55 1 d PU C 2 H5C' H 0.1687 0.4255 0.5288 0.053 Uiso 0.55 1 calc PR C 2 C6C C 0.1394(2) 0.36196(18) 0.58030(14) 0.0392(8) Uani 1 1 d U C . H6C H 0.1971 0.3468 0.5782 0.047 Uiso 0.45 1 calc PR D 1 H6C' H 0.1868 0.3374 0.5708 0.047 Uiso 0.55 1 d PR D 2 N22C N -0.04585(19) 0.31429(11) 0.69812(10) 0.0272(6) Uani 1 1 d U . . O23C O -0.10873(16) 0.30429(9) 0.73532(8) 0.0282(5) Uani 1 1 d U . . C21C C -0.0692(9) 0.3547(8) 0.6643(6) 0.028(3) Uani 0.45 1 d PU C 1 C24C C -0.1466(8) 0.3905(5) 0.6724(4) 0.031(2) Uani 0.45 1 d PU C 1 H24G H -0.1948 0.3648 0.6839 0.037 Uiso 0.45 1 calc PR C 1 H24H H -0.1638 0.4076 0.6386 0.037 Uiso 0.45 1 calc PR C 1 C25C C -0.1369(6) 0.4401(4) 0.7116(3) 0.040(2) Uani 0.45 1 d PU C 1 H25J H -0.1926 0.4609 0.7148 0.060 Uiso 0.45 1 calc PR C 1 H25K H -0.0917 0.4673 0.6997 0.060 Uiso 0.45 1 calc PR C 1 H25L H -0.1204 0.4239 0.7454 0.060 Uiso 0.45 1 calc PR C 1 C21" C -0.0463(8) 0.3649(6) 0.6740(6) 0.031(3) Uani 0.55 1 d PU C 2 C24" C -0.1196(6) 0.4084(4) 0.6894(4) 0.043(2) Uani 0.55 1 d PU C 2 H24I H -0.1326 0.4048 0.7269 0.052 Uiso 0.55 1 calc PR C 2 H24J H -0.1006 0.4490 0.6824 0.052 Uiso 0.55 1 calc PR C 2 C25" C -0.1992(7) 0.3945(4) 0.6583(4) 0.054(2) Uani 0.55 1 d PU C 2 H25M H -0.2462 0.4217 0.6675 0.081 Uiso 0.55 1 calc PR C 2 H25N H -0.2178 0.3544 0.6657 0.081 Uiso 0.55 1 calc PR C 2 H25O H -0.1858 0.3983 0.6213 0.081 Uiso 0.55 1 calc PR C 2 C1D C -0.2307(7) 0.0394(6) 0.5685(5) 0.050(3) Uani 0.50 1 d PU E 1 H1D1 H -0.1734 0.0482 0.5536 0.074 Uiso 0.50 1 calc PR E 1 H1D2 H -0.2765 0.0562 0.5465 0.074 Uiso 0.50 1 calc PR E 1 H1D3 H -0.2384 -0.0031 0.5705 0.074 Uiso 0.50 1 calc PR E 1 C2D C -0.2367(11) 0.0656(8) 0.6230(5) 0.036(3) Uani 0.50 1 d PU E 1 C3D C -0.3071(11) 0.0600(8) 0.6512(6) 0.042(3) Uani 0.50 1 d PU E 1 H3D H -0.3558 0.0418 0.6351 0.051 Uiso 0.50 1 calc PR E 1 C4D C -0.3183(11) 0.0783(9) 0.7031(5) 0.037(3) Uani 0.50 1 d PU E 1 C5D C -0.4050(10) 0.0633(9) 0.7307(5) 0.084(5) Uani 0.50 1 d PU E 1 H5D1 H -0.4035 0.0783 0.7663 0.125 Uiso 0.50 1 calc PR E 1 H5D2 H -0.4128 0.0208 0.7314 0.125 Uiso 0.50 1 calc PR E 1 H5D3 H -0.4537 0.0813 0.7119 0.125 Uiso 0.50 1 calc PR E 1 O2D O -0.1571(19) 0.0889(14) 0.6387(9) 0.030(3) Uani 0.50 1 d PU E 1 O4D O -0.2633(18) 0.1054(12) 0.7297(6) 0.033(3) Uani 0.50 1 d PU E 1 C1D' C -0.1957(7) 0.0382(7) 0.5567(5) 0.056(3) Uani 0.50 1 d PU E 2 H1D4 H -0.1352 0.0447 0.5458 0.084 Uiso 0.50 1 calc PR E 2 H1D5 H -0.2354 0.0570 0.5320 0.084 Uiso 0.50 1 calc PR E 2 H1D6 H -0.2076 -0.0038 0.5578 0.084 Uiso 0.50 1 calc PR E 2 C2D' C -0.2095(8) 0.0643(8) 0.6105(5) 0.030(3) Uani 0.50 1 d PU E 2 C3D' C -0.2919(12) 0.0594(9) 0.6318(5) 0.042(3) Uani 0.50 1 d PU E 2 C4D' C -0.3131(10) 0.0758(8) 0.6825(6) 0.037(3) Uani 0.50 1 d PU E 2 C5D' C -0.4027(9) 0.0609(7) 0.7037(5) 0.064(3) Uani 0.50 1 d PU E 2 H5D4 H -0.4076 0.0752 0.7394 0.096 Uiso 0.50 1 calc PR E 2 H5D5 H -0.4108 0.0184 0.7032 0.096 Uiso 0.50 1 calc PR E 2 H5D6 H -0.4475 0.0795 0.6822 0.096 Uiso 0.50 1 calc PR E 2 O2D' O -0.146(2) 0.0890(14) 0.6284(9) 0.035(4) Uani 0.50 1 d PU E 2 O4D' O -0.2635(18) 0.1030(13) 0.7144(6) 0.033(3) Uani 0.50 1 d PU E 2 O1E O -0.20019(15) 0.22319(10) 0.69119(9) 0.0312(5) Uani 1 1 d . E . C2E C -0.2831(3) 0.2344(2) 0.66817(19) 0.0532(11) Uani 1 1 d . . . H2E1 H -0.2914 0.2766 0.6645 0.080 Uiso 1 1 calc R E . H2E2 H -0.3293 0.2183 0.6903 0.080 Uiso 1 1 calc R . . H2E3 H -0.2857 0.2159 0.6339 0.080 Uiso 1 1 calc R . . O1F O -0.14619(13) 0.19678(9) 0.80292(8) 0.0192(4) Uani 1 1 d . . . C2F C -0.2351(2) 0.21419(15) 0.81453(14) 0.0279(7) Uani 1 1 d . . . H2F1 H -0.2730 0.1797 0.8143 0.042 Uiso 1 1 calc R E . H2F2 H -0.2553 0.2421 0.7883 0.042 Uiso 1 1 calc R . . H2F3 H -0.2370 0.2326 0.8488 0.042 Uiso 1 1 calc R . . O1G O 0.0066(2) 0.06155(11) 0.60107(9) 0.0391(7) Uani 1 1 d U . . C2G C 0.0354(8) 0.0354(7) 0.5515(6) 0.062(4) Uani 0.67 1 d PU B 1 H2G1 H -0.0032 0.0028 0.5424 0.093 Uiso 0.67 1 calc PR B 1 H2G2 H 0.0954 0.0211 0.5550 0.093 Uiso 0.67 1 calc PR B 1 H2G3 H 0.0330 0.0650 0.5240 0.093 Uiso 0.67 1 calc PR B 1 C2G' C 0.0062(13) 0.0452(9) 0.5475(10) 0.028(4) Uani 0.33 1 d PU B 2 H2G4 H -0.0294 0.0100 0.5429 0.042 Uiso 0.33 1 calc PR B 2 H2G5 H 0.0662 0.0372 0.5362 0.042 Uiso 0.33 1 calc PR B 2 H2G6 H -0.0182 0.0771 0.5267 0.042 Uiso 0.33 1 calc PR B 2 O1H O -0.02127(14) 0.18965(9) 0.64529(8) 0.0216(5) Uani 1 1 d . . . C2H C -0.0611(2) 0.21404(16) 0.60007(12) 0.0321(8) Uani 1 1 d . . . H2H1 H -0.1113 0.2379 0.6103 0.048 Uiso 1 1 calc R E . H2H2 H -0.0806 0.1825 0.5772 0.048 Uiso 1 1 calc R . . H2H3 H -0.0185 0.2385 0.5817 0.048 Uiso 1 1 calc R . . C1S C 0.5281(10) 0.1848(6) 0.5881(5) 0.108(5) Uiso 0.50 1 d PDU F -1 H1S1 H 0.5151 0.1972 0.5525 0.161 Uiso 0.50 1 calc PR F -1 H1S2 H 0.5158 0.1430 0.5917 0.161 Uiso 0.50 1 calc PR F -1 H1S3 H 0.5898 0.1921 0.5957 0.161 Uiso 0.50 1 calc PR F -1 C2S C 0.4663(14) 0.2223(9) 0.6292(6) 0.160(8) Uiso 0.50 1 d PDU F -1 H2S1 H 0.4698 0.2639 0.6190 0.192 Uiso 0.50 1 calc PR F -1 H2S2 H 0.4051 0.2098 0.6236 0.192 Uiso 0.50 1 calc PR F -1 C3S C 0.4826(15) 0.2195(9) 0.6845(5) 0.139(7) Uiso 0.50 1 d PDU F -1 H3S1 H 0.5375 0.1966 0.6854 0.167 Uiso 0.50 1 calc PR F -1 H3S2 H 0.4370 0.1915 0.6956 0.167 Uiso 0.50 1 calc PR F -1 C4S C 0.493(2) 0.2574(7) 0.7341(6) 0.178(9) Uiso 0.50 1 d PDU F -1 H4S1 H 0.5367 0.2883 0.7284 0.214 Uiso 0.50 1 calc PR F -1 H4S2 H 0.4363 0.2763 0.7427 0.214 Uiso 0.50 1 calc PR F -1 C5S C 0.5214(13) 0.2171(7) 0.7785(5) 0.124(6) Uiso 0.50 1 d PDU F -1 H5S1 H 0.5764 0.1976 0.7682 0.149 Uiso 0.50 1 calc PR F -1 H5S2 H 0.4766 0.1863 0.7830 0.149 Uiso 0.50 1 calc PR F -1 C6S C 0.5365(14) 0.2485(8) 0.8332(6) 0.145(7) Uiso 0.50 1 d PDU F -1 H6S1 H 0.5468 0.2189 0.8600 0.218 Uiso 0.50 1 calc PR F -1 H6S2 H 0.4846 0.2714 0.8423 0.218 Uiso 0.50 1 calc PR F -1 H6S3 H 0.5872 0.2744 0.8309 0.218 Uiso 0.50 1 calc PR F -1 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 La1 0.01511(7) 0.01902(8) 0.01563(7) -0.00117(7) -0.00012(6) 0.00043(7) Mn1 0.0228(2) 0.0195(2) 0.01354(19) 0.00318(18) 0.00473(16) 0.00199(18) Mn3 0.0246(2) 0.0160(2) 0.0200(2) 0.00042(18) 0.00783(19) -0.00146(18) Mn4 0.0218(2) 0.0157(2) 0.0213(2) -0.00331(17) 0.00633(18) -0.00088(18) O13 0.0200(10) 0.0157(10) 0.0132(9) -0.0002(8) 0.0025(8) -0.0022(8) O14 0.0175(14) 0.0151(14) 0.0162(14) 0.000 0.0023(11) 0.000 C2A 0.044(2) 0.0272(17) 0.0307(18) -0.0094(15) 0.0132(16) -0.0075(15) C1A 0.033(7) 0.021(7) 0.027(10) -0.012(7) 0.011(6) -0.008(6) O1A 0.035(7) 0.025(6) 0.028(7) -0.016(5) -0.006(5) -0.001(5) C3A 0.051(12) 0.046(9) 0.044(9) -0.011(6) 0.005(8) -0.002(8) C4A 0.059(11) 0.051(9) 0.055(9) -0.036(7) -0.003(9) -0.006(8) C5A 0.052(10) 0.074(9) 0.047(11) -0.026(8) -0.001(7) -0.001(8) C6A 0.048(10) 0.046(8) 0.029(10) -0.019(7) 0.009(7) -0.005(7) O1A' 0.024(4) 0.013(3) 0.028(6) -0.015(4) -0.001(4) -0.001(3) C1A' 0.044(6) 0.015(4) 0.022(5) -0.011(4) -0.001(4) -0.009(4) C3A' 0.032(6) 0.037(6) 0.037(6) -0.019(5) 0.002(4) -0.005(4) C4A' 0.038(5) 0.044(6) 0.042(5) -0.021(4) 0.001(4) -0.007(5) C5A' 0.039(6) 0.036(4) 0.021(4) -0.023(3) 0.006(4) -0.010(4) C6A' 0.038(6) 0.029(4) 0.031(8) -0.025(5) 0.010(5) -0.010(4) C21A 0.0362(19) 0.0209(15) 0.0279(16) -0.0061(12) 0.0044(15) -0.0067(14) N22A 0.0327(15) 0.0181(12) 0.0197(13) -0.0041(10) 0.0072(11) 0.0014(11) O23A 0.0245(11) 0.0196(10) 0.0217(10) -0.0071(8) 0.0061(9) -0.0002(9) C24A 0.0314(18) 0.0359(19) 0.049(2) -0.0229(17) 0.0074(17) -0.0055(15) C25A 0.057(2) 0.035(2) 0.076(3) -0.018(2) 0.034(2) -0.0192(19) C1B 0.0317(17) 0.0304(17) 0.0164(15) 0.0013(13) 0.0054(13) -0.0055(14) O1B 0.0310(11) 0.0339(12) 0.0193(10) 0.0092(9) 0.0073(10) 0.0053(11) C2B 0.0403(18) 0.0345(18) 0.0266(16) 0.0055(16) 0.0163(14) 0.0028(17) C3B 0.037(9) 0.042(8) 0.021(9) 0.004(7) 0.014(7) 0.008(8) C4B 0.052(11) 0.037(9) 0.022(9) -0.005(6) 0.019(8) -0.007(7) C3B' 0.043(4) 0.055(5) 0.029(5) 0.015(4) 0.011(4) 0.002(4) C4B' 0.044(4) 0.054(7) 0.042(6) 0.016(5) 0.015(4) -0.014(4) C5B 0.044(2) 0.052(2) 0.038(2) 0.0216(19) 0.0066(18) -0.0121(18) C6B 0.0370(19) 0.037(2) 0.0239(17) 0.0107(14) 0.0002(14) -0.0042(15) C21B 0.041(2) 0.0262(17) 0.039(2) 0.0053(15) 0.0183(16) 0.0056(15) N22B 0.0286(14) 0.0217(13) 0.0277(14) 0.0088(11) 0.0142(12) 0.0042(11) O23B 0.0377(14) 0.0274(13) 0.0562(17) 0.0261(12) 0.0283(13) 0.0123(11) C24B 0.021(5) 0.022(5) 0.029(7) 0.002(5) 0.013(4) 0.001(4) C25B 0.030(4) 0.029(4) 0.035(4) 0.011(3) -0.009(4) 0.003(4) C24' 0.054(7) 0.044(6) 0.047(6) 0.018(4) 0.030(5) 0.023(5) C25' 0.122(8) 0.072(6) 0.061(5) -0.007(4) 0.017(5) 0.054(6) C1C 0.044(2) 0.0214(16) 0.0313(18) 0.0061(13) 0.0101(15) -0.0002(14) O1C 0.0364(12) 0.0260(11) 0.0401(13) 0.0145(10) 0.0183(12) 0.0023(11) C2C 0.037(7) 0.026(6) 0.035(7) 0.012(5) 0.008(6) 0.012(6) C3C 0.076(10) 0.050(8) 0.045(8) 0.034(6) 0.012(7) 0.011(7) C4C 0.083(10) 0.059(10) 0.053(9) 0.037(7) 0.015(7) 0.004(7) C5C 0.077(10) 0.060(11) 0.036(8) 0.026(7) 0.014(7) -0.004(7) C2C' 0.031(6) 0.032(5) 0.041(6) 0.019(4) 0.005(5) 0.000(4) C3C' 0.040(6) 0.039(6) 0.053(7) 0.020(5) 0.008(4) 0.016(4) C4C' 0.053(6) 0.037(5) 0.048(6) 0.025(4) 0.010(4) 0.001(4) C5C' 0.050(7) 0.043(6) 0.041(8) 0.019(5) 0.021(5) -0.004(5) C6C 0.046(2) 0.0319(19) 0.0392(19) 0.0117(17) 0.0123(16) -0.0045(18) N22C 0.0305(14) 0.0221(13) 0.0290(14) 0.0069(11) 0.0124(12) 0.0051(11) O23C 0.0281(11) 0.0261(11) 0.0305(12) 0.0064(9) 0.0087(11) 0.0062(11) C21C 0.027(6) 0.027(7) 0.032(6) 0.011(4) 0.010(5) 0.007(5) C24C 0.031(6) 0.025(5) 0.037(6) 0.011(4) 0.001(4) 0.011(4) C25C 0.051(5) 0.021(4) 0.047(5) 0.001(4) 0.025(4) 0.017(4) C21" 0.024(5) 0.021(5) 0.049(6) 0.003(4) 0.007(4) 0.005(4) C24" 0.040(5) 0.031(5) 0.060(6) 0.015(4) 0.006(4) 0.007(4) C25" 0.054(5) 0.043(5) 0.064(6) 0.014(4) 0.018(4) 0.012(4) C1D 0.037(7) 0.073(7) 0.039(6) -0.011(5) -0.009(5) 0.001(6) C2D 0.041(8) 0.040(5) 0.028(6) -0.010(5) -0.011(6) 0.004(7) C3D 0.031(7) 0.055(6) 0.041(8) -0.015(8) -0.009(6) -0.009(5) C4D 0.023(5) 0.043(5) 0.045(7) -0.005(7) -0.008(6) -0.009(4) C5D 0.042(7) 0.134(12) 0.075(9) -0.024(10) 0.013(8) -0.047(7) O2D 0.044(6) 0.038(5) 0.008(7) 0.006(5) -0.006(5) -0.005(4) O4D 0.023(4) 0.035(4) 0.041(8) -0.003(7) -0.002(7) -0.005(3) C1D' 0.033(6) 0.102(9) 0.032(6) -0.040(5) -0.005(5) -0.018(6) C2D' 0.027(6) 0.035(5) 0.027(6) -0.011(4) -0.006(4) 0.003(5) C3D' 0.022(6) 0.065(6) 0.038(7) -0.007(7) -0.002(6) -0.010(5) C4D' 0.024(5) 0.038(5) 0.050(9) -0.006(8) -0.003(7) -0.006(4) C5D' 0.028(5) 0.091(8) 0.073(8) -0.007(8) 0.011(7) -0.014(5) O2D' 0.051(8) 0.041(5) 0.014(8) -0.007(6) -0.007(6) -0.014(5) O4D' 0.022(4) 0.041(5) 0.035(8) -0.005(6) -0.003(6) 0.000(3) O1E 0.0255(12) 0.0375(13) 0.0306(13) 0.0059(10) 0.0000(10) 0.0094(10) C2E 0.041(2) 0.052(3) 0.066(3) 0.005(2) -0.017(2) 0.013(2) O1F 0.0159(10) 0.0189(10) 0.0228(11) -0.0030(8) 0.0050(8) 0.0009(8) C2F 0.0196(15) 0.0277(17) 0.0364(19) -0.0010(15) 0.0056(14) 0.0033(13) O1G 0.0641(18) 0.0375(15) 0.0156(12) -0.0120(11) 0.0083(12) -0.0134(13) C2G 0.097(10) 0.069(8) 0.021(4) -0.011(4) 0.008(6) 0.015(6) C2G' 0.045(10) 0.018(7) 0.021(6) -0.014(5) 0.005(7) 0.004(6) O1H 0.0258(11) 0.0255(11) 0.0137(10) 0.0036(8) 0.0005(9) 0.0061(9) C2H 0.038(2) 0.039(2) 0.0187(16) 0.0077(14) -0.0037(14) 0.0119(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O2D 2.43(3) . ? La1 O4D 2.46(3) . ? La1 O4D' 2.46(3) . ? La1 O13 2.5058(19) 3_556 ? La1 O14 2.5317(18) . ? La1 O13 2.5532(19) . ? La1 O1E 2.556(2) . ? La1 O23A 2.586(2) . ? La1 O2D' 2.62(3) . ? La1 O1F 2.647(2) . ? La1 O1H 2.654(2) . ? La1 Mn1 3.5874(4) . ? Mn1 O1B 1.862(2) . ? Mn1 O13 1.890(2) 3_556 ? Mn1 O1H 1.928(2) . ? Mn1 N22B 1.999(3) . ? Mn1 O1F 2.241(2) 3_556 ? Mn1 O1G 2.329(2) . ? Mn1 Mn3 3.0584(6) 3_556 ? Mn1 Mn4 3.1294(6) 3_556 ? Mn1 La1 3.7191(4) 3_556 ? Mn3 O1A 1.79(3) 3_556 ? Mn3 O13 1.897(2) . ? Mn3 O1A' 1.925(17) 3_556 ? Mn3 O23B 1.931(2) 3_556 ? Mn3 N22A 2.013(3) 3_556 ? Mn3 O23A 2.116(2) . ? Mn3 Mn1 3.0586(6) 3_556 ? Mn4 O1C 1.854(2) 3_556 ? Mn4 O14 1.8838(16) . ? Mn4 O1F 1.967(2) . ? Mn4 N22C 2.022(3) 3_556 ? Mn4 O23C 2.165(2) . ? Mn4 O1H 2.380(2) 3_556 ? Mn4 Mn4 3.0838(9) 3_556 ? Mn4 Mn1 3.1294(6) 3_556 ? O13 Mn1 1.8896(19) 3_556 ? O13 La1 2.5059(19) 3_556 ? O14 Mn4 1.8838(16) 3_556 ? O14 La1 2.5316(18) 3_556 ? C2A C3A 1.30(3) . ? C2A C1A' 1.322(16) . ? C2A C21A 1.464(5) . ? C2A C3A' 1.479(16) . ? C2A C1A 1.57(2) . ? C1A O1A 1.33(2) . ? C1A C6A 1.39(4) . ? O1A Mn3 1.79(3) 3_556 ? C3A C4A 1.40(3) . ? C3A H3A 0.9500 . ? C4A C5A 1.39(2) . ? C4A H4A 0.9500 . ? C5A C6A 1.30(2) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? O1A' C1A' 1.326(11) . ? O1A' Mn3 1.925(17) 3_556 ? C1A' C6A' 1.42(2) . ? C3A' C4A' 1.357(19) . ? C3A' H3A' 0.9500 . ? C4A' C5A' 1.402(12) . ? C4A' H4A' 0.9500 . ? C5A' C6A' 1.366(12) . ? C5A' H5A' 0.9500 . ? C6A' H6A' 0.9500 . ? C21A N22A 1.299(4) . ? C21A C24A 1.504(5) . ? N22A O23A 1.378(3) . ? N22A Mn3 2.013(3) 3_556 ? C24A C25A 1.524(6) . ? C24A H24A 0.9900 . ? C24A H24B 0.9900 . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25C 0.9800 . ? C1B O1B 1.322(4) . ? C1B C2B 1.403(5) . ? C1B C6B 1.416(4) . ? C2B C3B' 1.410(12) . ? C2B C3B 1.45(2) . ? C2B C21B 1.470(5) . ? C3B C4B 1.30(4) . ? C3B H3B 0.9500 . ? C4B C5B 1.39(3) . ? C4B H4B 0.9500 . ? C3B' C4B' 1.415(16) . ? C3B' H3B' 0.9500 . ? C4B' C5B 1.383(15) . ? C4B' H4B' 0.9500 . ? C5B C6B 1.367(5) . ? C5B H5B 0.9500 . ? C5B H5B' 0.9501 . ? C6B H6B 0.9500 . ? C21B N22B 1.302(4) . ? C21B C24' 1.497(12) . ? C21B C24B 1.553(17) . ? N22B O23B 1.369(3) . ? O23B Mn3 1.931(2) 3_556 ? C24B C25B 1.509(14) . ? C24B H24C 0.9900 . ? C24B H24D 0.9900 . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? C24' C25' 1.573(13) . ? C24' H24E 0.9900 . ? C24' H24F 0.9900 . ? C25' H25G 0.9800 . ? C25' H25H 0.9800 . ? C25' H25I 0.9800 . ? C1C O1C 1.318(4) . ? C1C C2C' 1.325(19) . ? C1C C6C 1.388(5) . ? C1C C2C 1.517(19) . ? O1C Mn4 1.854(2) 3_556 ? C2C C3C 1.40(3) . ? C2C C21C 1.47(3) . ? C3C C4C 1.36(2) . ? C3C H3C 0.9500 . ? C4C C5C 1.40(3) . ? C4C H4C 0.9500 . ? C5C C6C 1.41(3) . ? C5C H5C 0.9500 . ? C2C' C3C' 1.44(2) . ? C2C' C21" 1.47(2) . ? C3C' C4C' 1.346(18) . ? C3C' H3C' 0.9500 . ? C4C' C5C' 1.38(2) . ? C4C' H4C' 0.9500 . ? C5C' C6C 1.37(2) . ? C5C' H5C' 0.9500 . ? C6C H6C 0.9500 . ? C6C H6C' 0.9500 . ? N22C C21" 1.315(16) . ? N22C C21C 1.320(18) . ? N22C O23C 1.378(3) . ? N22C Mn4 2.022(3) 3_556 ? C21C C24C 1.46(2) . ? C24C C25C 1.527(13) . ? C24C H24G 0.9900 . ? C24C H24H 0.9900 . ? C25C H25J 0.9800 . ? C25C H25K 0.9800 . ? C25C H25L 0.9800 . ? C21" C24" 1.554(17) . ? C24" C25" 1.493(13) . ? C24" H24I 0.9900 . ? C24" H24J 0.9900 . ? C25" H25M 0.9800 . ? C25" H25N 0.9800 . ? C25" H25O 0.9800 . ? C1D C2D 1.530(15) . ? C1D H1D1 0.9800 . ? C1D H1D2 0.9800 . ? C1D H1D3 0.9800 . ? C2D C3D 1.306(16) . ? C2D O2D 1.39(3) . ? C3D C4D 1.414(14) . ? C3D H3D 0.9500 . ? C4D O4D 1.25(2) . ? C4D C5D 1.545(18) . ? C5D H5D1 0.9800 . ? C5D H5D2 0.9800 . ? C5D H5D3 0.9800 . ? C1D' C2D' 1.524(14) . ? C1D' H1D4 0.9800 . ? C1D' H1D5 0.9800 . ? C1D' H1D6 0.9800 . ? C2D' O2D' 1.22(3) . ? C2D' C3D' 1.381(14) . ? C3D' C4D' 1.397(15) . ? C4D' O4D' 1.28(2) . ? C4D' C5D' 1.516(17) . ? C5D' H5D4 0.9800 . ? C5D' H5D5 0.9800 . ? C5D' H5D6 0.9800 . ? O1E C2E 1.426(4) . ? C2E H2E1 0.9800 . ? C2E H2E2 0.9800 . ? C2E H2E3 0.9800 . ? O1F C2F 1.450(4) . ? O1F Mn1 2.241(2) 3_556 ? C2F H2F1 0.9800 . ? C2F H2F2 0.9800 . ? C2F H2F3 0.9800 . ? O1G C2G' 1.43(3) . ? O1G C2G 1.479(15) . ? C2G H2G1 0.9800 . ? C2G H2G2 0.9800 . ? C2G H2G3 0.9800 . ? C2G' H2G4 0.9800 . ? C2G' H2G5 0.9800 . ? C2G' H2G6 0.9800 . ? O1H C2H 1.429(4) . ? O1H Mn4 2.381(2) 3_556 ? C2H H2H1 0.9800 . ? C2H H2H2 0.9800 . ? C2H H2H3 0.9800 . ? C1S C2S 1.661(15) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S C3S 1.448(14) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.552(14) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S C5S 1.535(14) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C5S C6S 1.600(15) . ? C5S H5S1 0.9900 . ? C5S H5S2 0.9900 . ? C6S H6S1 0.9800 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2D La1 O4D 72.2(7) . . ? O2D La1 O4D' 63.1(7) . . ? O4D La1 O4D' 9.3(6) . . ? O2D La1 O13 86.4(7) . 3_556 ? O4D La1 O13 144.5(6) . 3_556 ? O4D' La1 O13 140.2(6) . 3_556 ? O2D La1 O14 139.3(7) . . ? O4D La1 O14 141.7(5) . . ? O4D' La1 O14 148.2(6) . . ? O13 La1 O14 71.45(6) 3_556 . ? O2D La1 O13 135.4(7) . . ? O4D La1 O13 102.6(5) . . ? O4D' La1 O13 110.3(5) . . ? O13 La1 O13 72.98(7) 3_556 . ? O14 La1 O13 70.68(5) . . ? O2D La1 O1E 86.7(7) . . ? O4D La1 O1E 74.3(7) . . ? O4D' La1 O1E 72.8(7) . . ? O13 La1 O1E 133.57(7) 3_556 . ? O14 La1 O1E 84.93(7) . . ? O13 La1 O1E 135.90(7) . . ? O2D La1 O23A 73.8(7) . . ? O4D La1 O23A 75.6(7) . . ? O4D' La1 O23A 75.8(7) . . ? O13 La1 O23A 71.30(6) 3_556 . ? O14 La1 O23A 126.30(7) . . ? O13 La1 O23A 62.29(6) . . ? O1E La1 O23A 147.99(7) . . ? O2D La1 O2D' 5.8(12) . . ? O4D La1 O2D' 77.9(7) . . ? O4D' La1 O2D' 68.8(7) . . ? O13 La1 O2D' 81.9(7) 3_556 . ? O14 La1 O2D' 133.7(6) . . ? O13 La1 O2D' 136.1(7) . . ? O1E La1 O2D' 87.2(7) . . ? O23A La1 O2D' 75.8(7) . . ? O2D La1 O1F 149.9(7) . . ? O4D La1 O1F 81.7(4) . . ? O4D' La1 O1F 89.9(4) . . ? O13 La1 O1F 123.66(6) 3_556 . ? O14 La1 O1F 61.20(5) . . ? O13 La1 O1F 64.18(6) . . ? O1E La1 O1F 71.95(7) . . ? O23A La1 O1F 114.19(6) . . ? O2D' La1 O1F 154.1(7) . . ? O2D La1 O1H 75.3(7) . . ? O4D La1 O1H 134.3(5) . . ? O4D' La1 O1H 126.4(5) . . ? O13 La1 O1H 61.32(6) 3_556 . ? O14 La1 O1H 64.17(5) . . ? O13 La1 O1H 123.10(6) . . ? O1E La1 O1H 72.51(7) . . ? O23A La1 O1H 124.10(6) . . ? O2D' La1 O1H 70.0(6) . . ? O1F La1 O1H 115.96(6) . . ? O2D La1 Mn1 76.1(6) . . ? O4D La1 Mn1 148.3(3) . . ? O4D' La1 Mn1 139.2(3) . . ? O13 La1 Mn1 29.95(4) 3_556 . ? O14 La1 Mn1 67.627(17) . . ? O13 La1 Mn1 99.67(4) . . ? O1E La1 Mn1 104.24(5) . . ? O23A La1 Mn1 95.50(5) . . ? O2D' La1 Mn1 70.4(6) . . ? O1F La1 Mn1 128.83(4) . . ? O1H La1 Mn1 31.74(4) . . ? O1B Mn1 O13 175.65(10) . 3_556 ? O1B Mn1 O1H 91.92(10) . . ? O13 Mn1 O1H 87.26(8) 3_556 . ? O1B Mn1 N22B 88.07(10) . . ? O13 Mn1 N22B 92.58(9) 3_556 . ? O1H Mn1 N22B 177.71(11) . . ? O1B Mn1 O1F 100.72(9) . 3_556 ? O13 Mn1 O1F 83.52(8) 3_556 3_556 ? O1H Mn1 O1F 87.66(8) . 3_556 ? N22B Mn1 O1F 94.60(10) . 3_556 ? O1B Mn1 O1G 98.38(10) . . ? O13 Mn1 O1G 77.47(9) 3_556 . ? O1H Mn1 O1G 95.98(10) . . ? N22B Mn1 O1G 81.76(11) . . ? O1F Mn1 O1G 160.43(8) 3_556 . ? O1B Mn1 Mn3 141.70(7) . 3_556 ? O13 Mn1 Mn3 36.21(6) 3_556 3_556 ? O1H Mn1 Mn3 115.61(6) . 3_556 ? N22B Mn1 Mn3 63.36(7) . 3_556 ? O1F Mn1 Mn3 106.21(5) 3_556 3_556 ? O1G Mn1 Mn3 54.96(7) . 3_556 ? O1B Mn1 Mn4 94.07(7) . 3_556 ? O13 Mn1 Mn4 88.64(6) 3_556 3_556 ? O1H Mn1 Mn4 49.46(6) . 3_556 ? N22B Mn1 Mn4 132.83(9) . 3_556 ? O1F Mn1 Mn4 38.71(5) 3_556 3_556 ? O1G Mn1 Mn4 143.71(7) . 3_556 ? Mn3 Mn1 Mn4 123.889(17) 3_556 3_556 ? O1B Mn1 La1 136.94(8) . . ? O13 Mn1 La1 41.46(6) 3_556 . ? O1H Mn1 La1 46.39(6) . . ? N22B Mn1 La1 133.10(7) . . ? O1F Mn1 La1 89.44(5) 3_556 . ? O1G Mn1 La1 79.45(7) . . ? Mn3 Mn1 La1 70.656(12) 3_556 . ? Mn4 Mn1 La1 68.403(12) 3_556 . ? O1B Mn1 La1 145.07(8) . 3_556 ? O13 Mn1 La1 39.25(6) 3_556 3_556 ? O1H Mn1 La1 91.22(6) . 3_556 ? N22B Mn1 La1 90.10(8) . 3_556 ? O1F Mn1 La1 44.69(5) 3_556 3_556 ? O1G Mn1 La1 115.86(6) . 3_556 ? Mn3 Mn1 La1 64.656(12) 3_556 3_556 ? Mn4 Mn1 La1 62.661(11) 3_556 3_556 ? La1 Mn1 La1 61.312(8) . 3_556 ? O1A Mn3 O13 175.9(9) 3_556 . ? O1A Mn3 O1A' 10.0(11) 3_556 3_556 ? O13 Mn3 O1A' 170.9(5) . 3_556 ? O1A Mn3 O23B 85.9(9) 3_556 3_556 ? O13 Mn3 O23B 90.01(9) . 3_556 ? O1A' Mn3 O23B 89.7(5) 3_556 3_556 ? O1A Mn3 N22A 89.3(9) 3_556 3_556 ? O13 Mn3 N22A 94.70(9) . 3_556 ? O1A' Mn3 N22A 83.8(5) 3_556 3_556 ? O23B Mn3 N22A 167.65(12) 3_556 3_556 ? O1A Mn3 O23A 97.4(8) 3_556 . ? O13 Mn3 O23A 82.76(8) . . ? O1A' Mn3 O23A 106.3(5) 3_556 . ? O23B Mn3 O23A 94.23(11) 3_556 . ? N22A Mn3 O23A 97.68(9) 3_556 . ? O1A Mn3 Mn1 141.0(9) 3_556 3_556 ? O13 Mn3 Mn1 36.04(6) . 3_556 ? O1A' Mn3 Mn1 137.1(5) 3_556 3_556 ? O23B Mn3 Mn1 64.66(7) 3_556 3_556 ? N22A Mn3 Mn1 113.88(7) 3_556 3_556 ? O23A Mn3 Mn1 109.20(6) . 3_556 ? O1A Mn3 La1 138.2(7) 3_556 . ? O13 Mn3 La1 40.83(6) . . ? O1A' Mn3 La1 148.1(4) 3_556 . ? O23B Mn3 La1 83.58(9) 3_556 . ? N22A Mn3 La1 107.37(7) 3_556 . ? O23A Mn3 La1 43.59(5) . . ? Mn1 Mn3 La1 66.429(12) 3_556 . ? O1C Mn4 O14 176.35(10) 3_556 . ? O1C Mn4 O1F 91.03(10) 3_556 . ? O14 Mn4 O1F 86.43(8) . . ? O1C Mn4 N22C 89.33(11) 3_556 3_556 ? O14 Mn4 N22C 92.99(9) . 3_556 ? O1F Mn4 N22C 175.21(11) . 3_556 ? O1C Mn4 O23C 97.18(10) 3_556 . ? O14 Mn4 O23C 85.69(7) . . ? O1F Mn4 O23C 95.83(9) . . ? N22C Mn4 O23C 88.87(11) 3_556 . ? O1C Mn4 O1H 97.48(10) 3_556 3_556 ? O14 Mn4 O1H 79.62(7) . 3_556 ? O1F Mn4 O1H 82.94(8) . 3_556 ? N22C Mn4 O1H 92.27(10) 3_556 3_556 ? O23C Mn4 O1H 165.30(8) . 3_556 ? O1C Mn4 Mn4 148.52(7) 3_556 3_556 ? O14 Mn4 Mn4 35.07(7) . 3_556 ? O1F Mn4 Mn4 114.47(6) . 3_556 ? N22C Mn4 Mn4 66.84(7) 3_556 3_556 ? O23C Mn4 Mn4 63.62(6) . 3_556 ? O1H Mn4 Mn4 103.48(5) 3_556 3_556 ? O1C Mn4 Mn1 91.10(8) 3_556 3_556 ? O14 Mn4 Mn1 85.25(7) . 3_556 ? O1F Mn4 Mn1 45.42(6) . 3_556 ? N22C Mn4 Mn1 129.80(9) 3_556 3_556 ? O23C Mn4 Mn1 140.64(7) . 3_556 ? O1H Mn4 Mn1 38.00(5) 3_556 3_556 ? Mn4 Mn4 Mn1 119.771(12) 3_556 3_556 ? O1C Mn4 La1 136.14(8) 3_556 . ? O14 Mn4 La1 41.97(4) . . ? O1F Mn4 La1 46.16(6) . . ? N22C Mn4 La1 134.19(7) 3_556 . ? O23C Mn4 La1 81.25(6) . . ? O1H Mn4 La1 87.50(5) 3_556 . ? Mn4 Mn4 La1 68.730(11) 3_556 . ? Mn1 Mn4 La1 66.723(12) 3_556 . ? Mn1 O13 Mn3 107.75(9) 3_556 . ? Mn1 O13 La1 108.60(8) 3_556 3_556 ? Mn3 O13 La1 122.28(9) . 3_556 ? Mn1 O13 La1 112.83(9) 3_556 . ? Mn3 O13 La1 110.11(8) . . ? La1 O13 La1 94.90(6) 3_556 . ? Mn4 O14 Mn4 109.87(14) . 3_556 ? Mn4 O14 La1 117.74(2) . 3_556 ? Mn4 O14 La1 108.19(2) 3_556 3_556 ? Mn4 O14 La1 108.19(2) . . ? Mn4 O14 La1 117.74(2) 3_556 . ? La1 O14 La1 94.81(9) 3_556 . ? C3A C2A C1A' 107.4(15) . . ? C3A C2A C21A 127.0(14) . . ? C1A' C2A C21A 125.1(8) . . ? C3A C2A C3A' 14.9(16) . . ? C1A' C2A C3A' 117.9(10) . . ? C21A C2A C3A' 116.8(7) . . ? C3A C2A C1A 116.6(17) . . ? C1A' C2A C1A 10.5(16) . . ? C21A C2A C1A 115.3(11) . . ? C3A' C2A C1A 127.9(13) . . ? O1A C1A C6A 120(2) . . ? O1A C1A C2A 127(2) . . ? C6A C1A C2A 113(2) . . ? C1A O1A Mn3 116(2) . 3_556 ? C2A C3A C4A 127(2) . . ? C2A C3A H3A 116.7 . . ? C4A C3A H3A 116.7 . . ? C5A C4A C3A 115(2) . . ? C5A C4A H4A 122.7 . . ? C3A C4A H4A 122.7 . . ? C6A C5A C4A 124(2) . . ? C6A C5A H5A 117.9 . . ? C4A C5A H5A 117.9 . . ? C5A C6A C1A 124(3) . . ? C5A C6A H6A 118.0 . . ? C1A C6A H6A 118.0 . . ? C1A' O1A' Mn3 122.9(14) . 3_556 ? C2A C1A' O1A' 119.8(15) . . ? C2A C1A' C6A' 122.2(12) . . ? O1A' C1A' C6A' 118.0(14) . . ? C4A' C3A' C2A 119.6(11) . . ? C4A' C3A' H3A' 120.2 . . ? C2A C3A' H3A' 120.2 . . ? C3A' C4A' C5A' 120.4(12) . . ? C3A' C4A' H4A' 119.8 . . ? C5A' C4A' H4A' 119.8 . . ? C6A' C5A' C4A' 120.3(11) . . ? C6A' C5A' H5A' 119.8 . . ? C4A' C5A' H5A' 119.8 . . ? C5A' C6A' C1A' 119.3(13) . . ? C5A' C6A' H6A' 120.3 . . ? C1A' C6A' H6A' 120.3 . . ? N22A C21A C2A 118.3(3) . . ? N22A C21A C24A 121.7(3) . . ? C2A C21A C24A 120.0(3) . . ? C21A N22A O23A 117.5(3) . . ? C21A N22A Mn3 128.1(2) . 3_556 ? O23A N22A Mn3 114.45(18) . 3_556 ? N22A O23A Mn3 120.46(17) . . ? N22A O23A La1 114.81(15) . . ? Mn3 O23A La1 102.06(7) . . ? C21A C24A C25A 111.2(3) . . ? C21A C24A H24A 109.4 . . ? C25A C24A H24A 109.4 . . ? C21A C24A H24B 109.4 . . ? C25A C24A H24B 109.4 . . ? H24A C24A H24B 108.0 . . ? C24A C25A H25A 109.5 . . ? C24A C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? C24A C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? O1B C1B C2B 124.4(3) . . ? O1B C1B C6B 116.7(3) . . ? C2B C1B C6B 118.9(3) . . ? C1B O1B Mn1 130.8(2) . . ? C1B C2B C3B' 119.4(6) . . ? C1B C2B C3B 113.3(11) . . ? C3B' C2B C3B 20.1(9) . . ? C1B C2B C21B 122.0(3) . . ? C3B' C2B C21B 118.5(6) . . ? C3B C2B C21B 122.3(12) . . ? C4B C3B C2B 125(2) . . ? C4B C3B H3B 117.4 . . ? C2B C3B H3B 117.4 . . ? C3B C4B C5B 118(2) . . ? C3B C4B H4B 120.9 . . ? C5B C4B H4B 120.9 . . ? C2B C3B' C4B' 119.9(10) . . ? C2B C3B' H3B' 120.1 . . ? C4B' C3B' H3B' 120.1 . . ? C5B C4B' C3B' 119.6(10) . . ? C5B C4B' H4B' 120.2 . . ? C3B' C4B' H4B' 120.2 . . ? C6B C5B C4B' 120.5(6) . . ? C6B C5B C4B 119.0(13) . . ? C4B' C5B C4B 19.5(10) . . ? C6B C5B H5B 120.5 . . ? C4B' C5B H5B 115.4 . . ? C4B C5B H5B 120.5 . . ? C6B C5B H5B' 119.5 . . ? C4B' C5B H5B' 120.0 . . ? C4B C5B H5B' 117.8 . . ? H5B C5B H5B' 19.2 . . ? C5B C6B C1B 121.2(4) . . ? C5B C6B H6B 119.4 . . ? C1B C6B H6B 119.4 . . ? N22B C21B C2B 120.6(3) . . ? N22B C21B C24' 120.2(5) . . ? C2B C21B C24' 118.1(5) . . ? N22B C21B C24B 117.5(6) . . ? C2B C21B C24B 120.7(6) . . ? C24' C21B C24B 22.2(5) . . ? C21B N22B O23B 115.8(3) . . ? C21B N22B Mn1 131.0(2) . . ? O23B N22B Mn1 113.20(18) . . ? N22B O23B Mn3 115.30(19) . 3_556 ? C25B C24B C21B 117.9(10) . . ? C25B C24B H24C 107.8 . . ? C21B C24B H24C 107.8 . . ? C25B C24B H24D 107.8 . . ? C21B C24B H24D 107.8 . . ? H24C C24B H24D 107.2 . . ? C24B C25B H25D 109.5 . . ? C24B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C24B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C21B C24' C25' 113.9(8) . . ? C21B C24' H24E 108.8 . . ? C25' C24' H24E 108.8 . . ? C21B C24' H24F 108.8 . . ? C25' C24' H24F 108.8 . . ? H24E C24' H24F 107.7 . . ? C24' C25' H25G 109.5 . . ? C24' C25' H25H 109.5 . . ? H25G C25' H25H 109.5 . . ? C24' C25' H25I 109.5 . . ? H25G C25' H25I 109.5 . . ? H25H C25' H25I 109.5 . . ? O1C C1C C2C' 123.3(9) . . ? O1C C1C C6C 116.5(3) . . ? C2C' C1C C6C 119.6(9) . . ? O1C C1C C2C 123.5(10) . . ? C2C' C1C C2C 14.8(14) . . ? C6C C1C C2C 119.4(10) . . ? C1C O1C Mn4 132.3(2) . 3_556 ? C3C C2C C21C 120.2(16) . . ? C3C C2C C1C 117.2(17) . . ? C21C C2C C1C 122.6(17) . . ? C4C C3C C2C 120.5(18) . . ? C4C C3C H3C 119.7 . . ? C2C C3C H3C 119.7 . . ? C3C C4C C5C 122.4(17) . . ? C3C C4C H4C 118.8 . . ? C5C C4C H4C 118.8 . . ? C4C C5C C6C 120(2) . . ? C4C C5C H5C 119.8 . . ? C6C C5C H5C 119.8 . . ? C1C C2C' C3C' 118.6(14) . . ? C1C C2C' C21" 124.8(16) . . ? C3C' C2C' C21" 116.5(14) . . ? C4C' C3C' C2C' 121.6(12) . . ? C4C' C3C' H3C' 119.2 . . ? C2C' C3C' H3C' 119.2 . . ? C3C' C4C' C5C' 118.7(12) . . ? C3C' C4C' H4C' 120.6 . . ? C5C' C4C' H4C' 120.6 . . ? C6C C5C' C4C' 119.4(14) . . ? C6C C5C' H5C' 120.3 . . ? C4C' C5C' H5C' 120.3 . . ? C5C' C6C C1C 121.9(9) . . ? C5C' C6C C5C 19.2(12) . . ? C1C C6C C5C 119.3(12) . . ? C5C' C6C H6C 114.3 . . ? C1C C6C H6C 120.4 . . ? C5C C6C H6C 120.4 . . ? C5C' C6C H6C' 118.9 . . ? C1C C6C H6C' 119.2 . . ? C5C C6C H6C' 117.6 . . ? H6C C6C H6C' 19.9 . . ? C21" N22C C21C 21.4(7) . . ? C21" N22C O23C 118.2(7) . . ? C21C N22C O23C 112.7(7) . . ? C21" N22C Mn4 125.9(6) . 3_556 ? C21C N22C Mn4 132.4(8) . 3_556 ? O23C N22C Mn4 114.13(18) . 3_556 ? N22C O23C Mn4 110.69(18) . . ? N22C C21C C24C 121.5(13) . . ? N22C C21C C2C 118.2(14) . . ? C24C C21C C2C 118.8(14) . . ? C21C C24C C25C 115.8(10) . . ? C21C C24C H24G 108.3 . . ? C25C C24C H24G 108.3 . . ? C21C C24C H24H 108.3 . . ? C25C C24C H24H 108.3 . . ? H24G C24C H24H 107.4 . . ? C24C C25C H25J 109.5 . . ? C24C C25C H25K 109.5 . . ? H25J C25C H25K 109.5 . . ? C24C C25C H25L 109.5 . . ? H25J C25C H25L 109.5 . . ? H25K C25C H25L 109.5 . . ? N22C C21" C2C' 121.4(13) . . ? N22C C21" C24" 116.5(11) . . ? C2C' C21" C24" 121.9(13) . . ? C25" C24" C21" 108.4(9) . . ? C25" C24" H24I 110.0 . . ? C21" C24" H24I 110.0 . . ? C25" C24" H24J 110.0 . . ? C21" C24" H24J 110.0 . . ? H24I C24" H24J 108.4 . . ? C24" C25" H25M 109.5 . . ? C24" C25" H25N 109.5 . . ? H25M C25" H25N 109.5 . . ? C24" C25" H25O 109.5 . . ? H25M C25" H25O 109.5 . . ? H25N C25" H25O 109.5 . . ? C2D C1D H1D1 109.5 . . ? C2D C1D H1D2 109.5 . . ? H1D1 C1D H1D2 109.5 . . ? C2D C1D H1D3 109.5 . . ? H1D1 C1D H1D3 109.5 . . ? H1D2 C1D H1D3 109.5 . . ? C3D C2D O2D 126.7(14) . . ? C3D C2D C1D 121.5(13) . . ? O2D C2D C1D 111.5(14) . . ? C2D C3D C4D 126.8(15) . . ? C2D C3D H3D 116.6 . . ? C4D C3D H3D 116.6 . . ? O4D C4D C3D 125.7(15) . . ? O4D C4D C5D 116.0(13) . . ? C3D C4D C5D 118.3(13) . . ? C4D C5D H5D1 109.5 . . ? C4D C5D H5D2 109.5 . . ? H5D1 C5D H5D2 109.5 . . ? C4D C5D H5D3 109.5 . . ? H5D1 C5D H5D3 109.5 . . ? H5D2 C5D H5D3 109.5 . . ? C2D O2D La1 132.4(14) . . ? C4D O4D La1 135.9(13) . . ? C2D' C1D' H1D4 109.5 . . ? C2D' C1D' H1D5 109.5 . . ? H1D4 C1D' H1D5 109.5 . . ? C2D' C1D' H1D6 109.5 . . ? H1D4 C1D' H1D6 109.5 . . ? H1D5 C1D' H1D6 109.5 . . ? O2D' C2D' C3D' 128.2(15) . . ? O2D' C2D' C1D' 114.5(13) . . ? C3D' C2D' C1D' 117.2(11) . . ? C2D' C3D' C4D' 124.2(14) . . ? O4D' C4D' C3D' 126.4(15) . . ? O4D' C4D' C5D' 114.5(15) . . ? C3D' C4D' C5D' 119.1(13) . . ? C4D' C5D' H5D4 109.5 . . ? C4D' C5D' H5D5 109.5 . . ? H5D4 C5D' H5D5 109.5 . . ? C4D' C5D' H5D6 109.5 . . ? H5D4 C5D' H5D6 109.5 . . ? H5D5 C5D' H5D6 109.5 . . ? C2D' O2D' La1 133.8(16) . . ? C4D' O4D' La1 137.8(14) . . ? C2E O1E La1 137.9(2) . . ? O1E C2E H2E1 109.5 . . ? O1E C2E H2E2 109.5 . . ? H2E1 C2E H2E2 109.5 . . ? O1E C2E H2E3 109.5 . . ? H2E1 C2E H2E3 109.5 . . ? H2E2 C2E H2E3 109.5 . . ? C2F O1F Mn4 119.10(18) . . ? C2F O1F Mn1 116.23(18) . 3_556 ? Mn4 O1F Mn1 95.86(8) . 3_556 ? C2F O1F La1 120.88(18) . . ? Mn4 O1F La1 101.41(8) . . ? Mn1 O1F La1 98.77(7) 3_556 . ? O1F C2F H2F1 109.5 . . ? O1F C2F H2F2 109.5 . . ? H2F1 C2F H2F2 109.5 . . ? O1F C2F H2F3 109.5 . . ? H2F1 C2F H2F3 109.5 . . ? H2F2 C2F H2F3 109.5 . . ? C2G' O1G C2G 20.1(9) . . ? C2G' O1G Mn1 126.7(9) . . ? C2G O1G Mn1 121.4(7) . . ? O1G C2G H2G1 109.5 . . ? O1G C2G H2G2 109.5 . . ? H2G1 C2G H2G2 109.5 . . ? O1G C2G H2G3 109.5 . . ? H2G1 C2G H2G3 109.5 . . ? H2G2 C2G H2G3 109.5 . . ? O1G C2G' H2G4 109.5 . . ? O1G C2G' H2G5 109.5 . . ? H2G4 C2G' H2G5 109.5 . . ? O1G C2G' H2G6 109.5 . . ? H2G4 C2G' H2G6 109.5 . . ? H2G5 C2G' H2G6 109.5 . . ? C2H O1H Mn1 119.40(19) . . ? C2H O1H Mn4 115.8(2) . 3_556 ? Mn1 O1H Mn4 92.54(8) . 3_556 ? C2H O1H La1 123.47(19) . . ? Mn1 O1H La1 101.87(8) . . ? Mn4 O1H La1 97.67(7) 3_556 . ? O1H C2H H2H1 109.5 . . ? O1H C2H H2H2 109.5 . . ? H2H1 C2H H2H2 109.5 . . ? O1H C2H H2H3 109.5 . . ? H2H1 C2H H2H3 109.5 . . ? H2H2 C2H H2H3 109.5 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C3S C2S C1S 120.5(15) . . ? C3S C2S H2S1 107.2 . . ? C1S C2S H2S1 107.2 . . ? C3S C2S H2S2 107.2 . . ? C1S C2S H2S2 107.2 . . ? H2S1 C2S H2S2 106.8 . . ? C2S C3S C4S 143.3(19) . . ? C2S C3S H3S1 101.1 . . ? C4S C3S H3S1 101.1 . . ? C2S C3S H3S2 101.1 . . ? C4S C3S H3S2 101.1 . . ? H3S1 C3S H3S2 104.5 . . ? C5S C4S C3S 107.9(13) . . ? C5S C4S H4S1 110.1 . . ? C3S C4S H4S1 110.1 . . ? C5S C4S H4S2 110.1 . . ? C3S C4S H4S2 110.1 . . ? H4S1 C4S H4S2 108.4 . . ? C4S C5S C6S 115.4(12) . . ? C4S C5S H5S1 108.4 . . ? C6S C5S H5S1 108.4 . . ? C4S C5S H5S2 108.4 . . ? C6S C5S H5S2 108.4 . . ? H5S1 C5S H5S2 107.5 . . ? C5S C6S H6S1 109.5 . . ? C5S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.715 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.067 data_eb1013 _database_code_depnum_ccdc_archive 'CCDC 817029' #TrackingRef '- Complex 3.cif' _audit_creation_date 11-02-04 _audit_creation_method CRYSTALS_ver_14.05 _oxford_structure_analysis_title 'eb1013 in P2(1)/c' _chemical_name_systematic ? _chemical_melting_point ? _chemical_compound_source 'Ross Inglis' _exptl_crystal_recrystallization_method ; Slow evaporation of a MeOH/MeCN solution ; _publ_section_exptl_refinement ; The H atoms were all positioned geometrically. U~iso~(H) (in the range 1.2 times U~eq~ of the parent atom), the positions were refined with riding constraints. One of the aromatic rings is disordered over 2 orientations with 50% each of occupancy: the two componends had to be refined isotropically and restrained to be planar The tail of one of the solvent molecules attached to the main cluster had to be refined isotropically. see the bottom part of the file for the full list of the applied restraints. #-------------------------------------------------------------- CHECKCIF OUTPUT: #-------------------------------------------------------------- 301_ALERT_3_B Note: Main Residue Disorder ................... 4.00 Perc. One of the aromatic rings is disordered over two different orientations 302_ALERT_4_B Note: Anion/Solvent Disorder ................... 50.00 Perc. The only solvent molecule in the lattice is water molecule with 50% of occupancy. 201_ALERT_2_C Isotropic non-H Atoms in Main Residue(s) ....... 4 disordered carbon atoms on the disordered aromatic ring and the aliphatic tail of one solvent molecule had to be refined isotropically 041_ALERT_1_G Calc. and Reported SumFormula Strings Differ ? 042_ALERT_1_G Calc. and Reported MoietyFormula Strings Differ ? 045_ALERT_1_G Calculated and Reported Z Differ by ............ 0.50 Ratio the chemical formula and Z values have been tuned to have chemical sense. 601_ALERT_2_G Structure Contains Solvent Accessible VOIDS of . 38.00 A**3 No other reasonable peaks appear in the difference map 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 12 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 449 913_ALERT_3_G Missing # of Very Strong Reflections in FCF .... 1 INTENSITY STATISTICS FOR DATASET # 1 eb1013.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.24 789 792 99.6 5.25 49.4 21.11 0.0450 0.0333 2.24 - 1.76 809 809 100.0 4.77 28.1 14.83 0.0509 0.0436 1.76 - 1.53 821 821 100.0 4.07 29.2 12.79 0.0568 0.0503 1.53 - 1.39 804 804 100.0 3.85 17.4 10.22 0.0730 0.0650 1.39 - 1.29 800 800 100.0 5.45 12.2 15.48 0.0800 0.0442 1.29 - 1.21 853 853 100.0 5.16 12.6 15.54 0.0815 0.0450 1.21 - 1.15 803 803 100.0 4.04 12.7 14.50 0.0753 0.0469 1.15 - 1.10 814 814 100.0 2.29 10.9 12.98 0.0435 0.0555 1.10 - 1.05 967 967 100.0 2.27 9.9 12.33 0.0441 0.0576 1.05 - 1.01 918 919 99.9 2.20 7.5 11.06 0.0533 0.0639 1.01 - 0.98 800 800 100.0 2.09 7.5 10.63 0.0545 0.0667 0.98 - 0.95 897 897 100.0 2.05 5.1 9.37 0.0610 0.0754 0.95 - 0.92 1019 1019 100.0 1.95 5.7 9.72 0.0623 0.0712 0.92 - 0.89 1168 1168 100.0 1.85 4.9 9.32 0.0602 0.0742 0.89 - 0.87 853 853 100.0 1.71 5.3 9.39 0.0666 0.0725 0.87 - 0.85 955 957 99.8 1.60 4.6 9.22 0.0725 0.0751 0.85 - 0.83 972 1038 93.6 1.36 3.8 8.83 0.0770 0.0800 0.83 - 0.80 638 1041 61.3 0.74 3.6 8.44 0.0657 0.0814 #----------------------------------------------------------------------------- 0.90 - 0.80 4220 4691 90.0 1.41 4.4 9.04 0.0696 0.0765 Inf - 0.80 15680 16155 97.1 2.81 12.3 11.85 0.0582 0.0519 Merged [A], lowest resolution = 17.45 Angstroms, 885 outliers downweighted 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C28 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C35 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C50 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C64 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C71 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C83 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C96 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C95 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C105 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C104 The hydrogen atoms were all placed geometrically 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.43 Ratio 412_ALERT_2_C Short Intra XH3 .. XHn H4901 .. H501 .. 1.76 Ang. 413_ALERT_2_C Short Inter XH3 .. XHn H12 .. H151 .. 2.05 Ang. 413_ALERT_2_C Short Inter XH3 .. XHn H522 .. H890 .. 1.97 Ang. 062_ALERT_4_G Rescale T(min) & T(max) by ..................... 0.50 213_ALERT_2_G Atom C52 has ADP max/min Ratio ..... 3.20 prolat 241_ALERT_2_G Check High Ueq as Compared to Neighbors for C2 320_ALERT_2_G Check Hybridisation of C2 in Main Residue . ? 342_ALERT_3_G Low Bond Precision on C-C Bonds (x 1000) Ang .. 9 432_ALERT_2_B Short Inter X...Y Contact O1 .. C1 .. 2.63 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H12 .. H13 .. 1.82 Ang. 432_ALERT_2_B Short Inter X...Y Contact C1 .. C1 .. 2.78 Ang. 795_ALERT_4_B C-Atom in CIF Coordinate List out of Sequence .. C1 061_ALERT_4_C Tmax/Tmin Range Test RR' too Large ............. 0.74 412_ALERT_2_G Short Intra XH3 .. XHn H711 .. H721 .. 1.88 Ang. 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 16 796_ALERT_4_G O-Atom in CIF Coordinate List out of Sequence .. O23 No action taken here ; #end of refcif _cell_length_a 12.7152(3) _cell_length_b 25.6100(9) _cell_length_c 23.8804(7) _cell_angle_alpha 90 _cell_angle_beta 92.941(3) _cell_angle_gamma 90 _cell_volume 7766.1(4) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' 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 0.0181 0.0091 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' N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0492 0.0322 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' Cl 0.3639 0.7018 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' Mn -0.5299 2.8052 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Tb -9.1472 9.1891 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 = C85 Mn6 N17 O3 Tb2 # Dc = 1.67 Fooo = 4124.00 Mu = 169.19 M = 1954.47 # Found Formula = C67 H87 Mn6 N6 O27.50 Tb2 # Dc = 1.77 FOOO = 4124.00 Mu = 171.25 M = 2063.87 _chemical_formula_sum 'C67 H87 Mn6 N6 O27.50 Tb2' _chemical_formula_moiety '[Mn6Tb2O3(acac)2(MeSaO)6(MeO)4(MeOH)3(EtOH)].0.5H2O' _chemical_formula_weight 2063.87 _cell_measurement_temperature 100.0 _cell_measurement_reflns_used 16286 _cell_measurement_theta_min 2.5295 _cell_measurement_theta_max 73.8768 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.040 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_max 0.160 _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 4124 _exptl_absorpt_coefficient_mu 17.125 # Sheldrick geometric approximatio 0.36 0.50 _exptl_absorpt_correction_T_min 0.10893 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_device Serial _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_detector_area_resol_mean 5.1574 _diffrn_measurement_method '\w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _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 100.0 _diffrn_reflns_number 44617 _reflns_number_total 15309 _diffrn_reflns_av_R_equivalents 0.000 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 15309 # Theoretical number of reflections is about 31552 _diffrn_reflns_theta_min 2.532 _diffrn_reflns_theta_max 74.042 _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 69.600 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 31 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _oxford_diffrn_Wilson_B_factor 1.76 _oxford_diffrn_Wilson_scale 0.83 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.50 _refine_diff_density_max 1.92 # 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>-10.0\s(I) _refine_ls_number_reflns 15241 _refine_ls_number_restraints 667 _refine_ls_number_parameters 953 _oxford_refine_ls_R_factor_ref 0.0691 _refine_ls_wR_factor_ref 0.0637 _refine_ls_goodness_of_fit_ref 1.0007 _refine_ls_shift/su_max 0.0033713 _refine_ls_shift/su_mean 1.0608300 # The values computed from all data _oxford_reflns_number_all 15241 _refine_ls_R_factor_all 0.0691 _refine_ls_wR_factor_all 0.0637 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 12785 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_gt 0.0626 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # 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: 505. 451. 141. ; # 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, C., 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. 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 O1 O 0.6326(8) 0.4810(4) 0.6368(4) 0.057(3) 0.5000 Uiso . . . . . . . C2 C 0.5814(8) 0.4219(4) 0.4989(5) 0.098(2) 1.0000 Uiso . U . . . . . C1 C 0.5399(8) 0.4627(4) 0.5377(4) 0.101(2) 1.0000 Uiso . U . . . . . Tb1 Tb 0.44166(3) 0.296889(14) 0.472004(14) 0.0173 1.0000 Uani . . . . . . . Tb2 Tb 0.30112(3) 0.224756(14) 0.368695(14) 0.0169 1.0000 Uani . . . . . . . Mn1 Mn 0.30182(7) 0.36845(3) 0.36440(4) 0.0190 1.0000 Uani . . . . . . . Mn2 Mn 0.15607(7) 0.31367(3) 0.44519(4) 0.0205 1.0000 Uani . . . . . . . Mn3 Mn 0.22630(6) 0.22355(4) 0.52079(3) 0.0202 1.0000 Uani . . . . . . . Mn4 Mn 0.45718(7) 0.14889(3) 0.46856(4) 0.0184 1.0000 Uani . . . . . . . Mn5 Mn 0.58483(6) 0.21252(3) 0.38834(3) 0.0193 1.0000 Uani . . . . . . . Mn6 Mn 0.49687(7) 0.31029(3) 0.32348(4) 0.0187 1.0000 Uani . . . . . . . O3 O 0.4596(2) 0.21348(14) 0.42758(14) 0.0206 1.0000 Uani . . . . . . . O6 O 0.4753(3) 0.23490(14) 0.31646(15) 0.0256 1.0000 Uani . U . . . . . O8 O 0.5939(3) 0.28587(15) 0.40530(14) 0.0263 1.0000 Uani . U . . . . . O10 O 0.3876(3) 0.30812(13) 0.37434(14) 0.0199 1.0000 Uani . . . . . . . O12 O 0.1735(3) 0.30394(15) 0.36648(14) 0.0236 1.0000 Uani . U . . . . . O14 O 0.2941(3) 0.36699(14) 0.44576(15) 0.0237 1.0000 Uani . U . . . . . O16 O 0.2628(3) 0.26193(14) 0.45644(15) 0.0227 1.0000 Uani . . . . . . . O18 O 0.3891(3) 0.23053(15) 0.53969(14) 0.0242 1.0000 Uani . U . . . . . O29 O 0.1770(3) 0.18762(16) 0.58262(16) 0.0357 1.0000 Uani . U . . . . . O34 O 0.2969(3) 0.15102(15) 0.43924(15) 0.0242 1.0000 Uani . U . . . . . O40 O 0.1937(3) 0.28691(17) 0.55948(15) 0.0392 1.0000 Uani . U . . . . . O45 O 0.0453(3) 0.35967(18) 0.43285(17) 0.0390 1.0000 Uani . U . . . . . O51 O 0.0533(3) 0.23966(17) 0.45572(18) 0.0409 1.0000 Uani . U . . . . . O54 O 0.4493(3) 0.41296(14) 0.36362(16) 0.0299 1.0000 Uani . U . . . . . O59 O 0.6027(3) 0.31021(16) 0.27338(16) 0.0328 1.0000 Uani . U . . . . . O65 O 0.2149(3) 0.42722(16) 0.35775(16) 0.0345 1.0000 Uani . U . . . . . O70 O 0.3747(3) 0.33116(15) 0.26088(14) 0.0272 1.0000 Uani . U . . . . . O77 O 0.7155(3) 0.21015(16) 0.35688(15) 0.0312 1.0000 Uani . U . . . . . O82 O 0.5054(3) 0.11018(16) 0.40573(16) 0.0308 1.0000 Uani . U . . . . . O88 O 0.6445(3) 0.18320(16) 0.47774(16) 0.0335 1.0000 Uani . U . . . . . O90 O 0.3086(3) 0.14870(15) 0.31679(16) 0.0259 1.0000 Uani . U . . . . . O94 O 0.1289(3) 0.18892(15) 0.36732(15) 0.0286 1.0000 Uani . U . . . . . O97 O 0.2576(3) 0.24910(15) 0.27237(15) 0.0260 1.0000 Uani . U . . . . . O99 O 0.4261(3) 0.33994(16) 0.55621(16) 0.0314 1.0000 Uani . U . . . . . O103 O 0.5959(3) 0.27521(16) 0.52838(14) 0.0288 1.0000 Uani . U . . . . . O106 O 0.5243(3) 0.38112(18) 0.46360(18) 0.0425 1.0000 Uani . U . . . . . N19 N 0.4434(4) 0.18434(18) 0.54242(18) 0.0235 1.0000 Uani . U . . . . . O23 O 0.4625(3) 0.08676(15) 0.50964(16) 0.0317 1.0000 Uani . U . . . . . N33 N 0.2262(4) 0.15424(19) 0.48086(18) 0.0254 1.0000 Uani . U . . . . . N41 N 0.1361(4) 0.32154(19) 0.52742(19) 0.0292 1.0000 Uani . U . . . . . N55 N 0.5283(4) 0.38672(18) 0.33782(19) 0.0269 1.0000 Uani . U . . . . . N69 N 0.3049(4) 0.36696(18) 0.27952(19) 0.0248 1.0000 Uani . U . . . . . N81 N 0.5722(4) 0.13534(19) 0.37242(19) 0.0279 1.0000 Uani . U . . . . . C9 C 0.6969(4) 0.3091(2) 0.4168(2) 0.0323 1.0000 Uani . U . . . . . C15 C 0.2834(5) 0.4148(2) 0.4754(3) 0.0347 1.0000 Uani . U . . . . . C20 C 0.4803(4) 0.1702(2) 0.5916(2) 0.0228 1.0000 Uani . U . . . . . C21 C 0.5366(4) 0.1201(2) 0.5972(2) 0.0241 1.0000 Uani . U . . . . . C22 C 0.5216(4) 0.0800(2) 0.5573(2) 0.0257 1.0000 Uani . U . . . . . C24 C 0.5716(5) 0.0321(2) 0.5668(2) 0.0332 1.0000 Uani . U . . . . . C25 C 0.6342(5) 0.0238(3) 0.6149(3) 0.0418 1.0000 Uani . U . . . . . C26 C 0.6524(6) 0.0637(3) 0.6530(3) 0.0433 1.0000 Uani . U . . . . . C27 C 0.6019(5) 0.1106(2) 0.6451(3) 0.0339 1.0000 Uani . U . . . . . C28 C 0.4684(5) 0.2047(2) 0.6411(2) 0.0345 1.0000 Uani . U . . . . . C30 C 0.1000(5) 0.1516(3) 0.5772(3) 0.0357 1.0000 Uani . U . . . . . C31 C 0.0980(5) 0.1130(2) 0.5353(3) 0.0340 1.0000 Uani . U . . . . . C32 C 0.1796(5) 0.1113(2) 0.4935(2) 0.0316 1.0000 Uani . U . . . . . C35 C 0.2085(5) 0.0614(2) 0.4650(3) 0.0367 1.0000 Uani . U . . . . . C36 C 0.0189(5) 0.0758(3) 0.5358(3) 0.0464 1.0000 Uani . U . . . . . C37 C -0.0604(6) 0.0765(3) 0.5727(3) 0.0562 1.0000 Uani . U . . . . . C38 C -0.0561(6) 0.1141(3) 0.6140(3) 0.0534 1.0000 Uani . U . . . . . C39 C 0.0235(5) 0.1513(3) 0.6159(3) 0.0430 1.0000 Uani . U . . . . . C42 C 0.0738(5) 0.3519(3) 0.5543(3) 0.0416 1.0000 Uani . U . . . . . C50 C 0.0738(7) 0.3470(3) 0.6170(3) 0.0764 1.0000 Uani . U . . . . . C52 C -0.0581(5) 0.2430(3) 0.4631(4) 0.0790 1.0000 Uani . U . . . . . C53 C 0.0856(4) 0.3098(2) 0.3268(2) 0.0313 1.0000 Uani . U . . . . . C56 C 0.6103(5) 0.4140(3) 0.3254(3) 0.0331 1.0000 Uani . U . . . . . C57 C 0.6986(5) 0.3888(3) 0.2986(2) 0.0313 1.0000 Uani . U . . . . . C58 C 0.6887(5) 0.3390(2) 0.2730(2) 0.0322 1.0000 Uani . U . . . . . C60 C 0.7737(5) 0.3193(3) 0.2451(2) 0.0392 1.0000 Uani . U . . . . . C61 C 0.8666(5) 0.3436(3) 0.2440(3) 0.0471 1.0000 Uani . U . . . . . C62 C 0.8792(5) 0.3930(3) 0.2699(3) 0.0479 1.0000 Uani . U . . . . . C63 C 0.7956(5) 0.4145(3) 0.2960(3) 0.0404 1.0000 Uani . U . . . . . C64 C 0.6144(6) 0.4703(3) 0.3405(3) 0.0539 1.0000 Uani . U . . . . . C66 C 0.1630(5) 0.4480(2) 0.3133(3) 0.0284 1.0000 Uani . U . . . . . C67 C 0.1809(4) 0.4356(2) 0.2573(2) 0.0287 1.0000 Uani . U . . . . . C68 C 0.2632(4) 0.3980(2) 0.2427(2) 0.0280 1.0000 Uani . U . . . . . C71 C 0.2990(5) 0.3952(3) 0.1836(2) 0.0394 1.0000 Uani . U . . . . . C72 C 0.1210(5) 0.4608(3) 0.2142(3) 0.0403 1.0000 Uani . U . . . . . C73 C 0.0433(6) 0.4964(3) 0.2259(3) 0.0494 1.0000 Uani . U . . . . . C74 C 0.0275(5) 0.5086(3) 0.2807(3) 0.0447 1.0000 Uani . U . . . . . C75 C 0.0847(5) 0.4846(2) 0.3238(3) 0.0392 1.0000 Uani . U . . . . . C76 C 0.4893(4) 0.2107(2) 0.2631(2) 0.0266 1.0000 Uani . U . . . . . C78 C 0.7451(5) 0.1800(3) 0.3147(2) 0.0329 1.0000 Uani . U . . . . . C79 C 0.7008(5) 0.1302(3) 0.3033(3) 0.0386 1.0000 Uani . U . . . . . C80 C 0.6229(5) 0.1065(3) 0.3381(3) 0.0371 1.0000 Uani . U . . . . . C83 C 0.6042(6) 0.0493(3) 0.3361(3) 0.0568 1.0000 Uani . U . . . . . C84 C 0.7365(6) 0.1028(3) 0.2570(3) 0.0510 1.0000 Uani . U . . . . . C85 C 0.8171(6) 0.1225(3) 0.2262(3) 0.0574 1.0000 Uani . U . . . . . C86 C 0.8629(6) 0.1690(3) 0.2390(3) 0.0508 1.0000 Uani . U . . . . . C87 C 0.8293(5) 0.1979(3) 0.2842(3) 0.0450 1.0000 Uani . U . . . . . C89 C 0.7324(5) 0.1483(3) 0.4941(3) 0.0579 1.0000 Uani . U . . . . . C91 C 0.2462(5) 0.1115(2) 0.3036(2) 0.0303 1.0000 Uani . U . . . . . C92 C 0.1434(5) 0.1084(3) 0.3203(3) 0.0401 1.0000 Uani . U . . . . . C93 C 0.0931(5) 0.1442(3) 0.3539(3) 0.0346 1.0000 Uani . U . . . . . C95 C -0.0120(5) 0.1294(3) 0.3762(3) 0.0428 1.0000 Uani . U . . . . . C96 C 0.2881(6) 0.0693(2) 0.2672(3) 0.0457 1.0000 Uani . U . . . . . C98 C 0.2051(5) 0.2268(3) 0.2250(2) 0.0375 1.0000 Uani . U . . . . . C100 C 0.4862(5) 0.3481(2) 0.6007(2) 0.0356 1.0000 Uani . U . . . . . C101 C 0.5863(5) 0.3272(3) 0.6084(3) 0.0416 1.0000 Uani . U . . . . . C102 C 0.6354(4) 0.2929(3) 0.5747(2) 0.0336 1.0000 Uani . U . . . . . C104 C 0.7414(5) 0.2708(3) 0.5926(3) 0.0565 1.0000 Uani . U . . . . . C105 C 0.4382(6) 0.3806(3) 0.6448(3) 0.0496 1.0000 Uani . U . . . . . C491 C -0.0440(10) 0.4302(5) 0.5543(7) 0.0417(15) 0.5000 Uiso . U . . 1 . . C481 C -0.1060(10) 0.4672(5) 0.5288(6) 0.0423(16) 0.5000 Uiso . U . . 1 . . C471 C -0.1173(10) 0.4693(5) 0.4689(6) 0.0416(16) 0.5000 Uiso . U . . 1 . . C461 C -0.0640(11) 0.4323(6) 0.4388(7) 0.0400(15) 0.5000 Uiso . U . . 1 . . C44 C -0.0069(5) 0.3902(3) 0.4650(3) 0.0408(11) 1.0000 Uiso . U . . . . . C43 C 0.0043(5) 0.3889(3) 0.5248(3) 0.0421(11) 1.0000 Uiso . U . . . . . C490 C -0.0747(12) 0.4136(6) 0.5569(7) 0.053(2) 0.5000 Uiso . U . . 2 . . C480 C -0.1535(12) 0.4453(5) 0.5291(7) 0.054(2) 0.5000 Uiso . U . . 2 . . C470 C -0.1573(12) 0.4486(5) 0.4724(7) 0.053(2) 0.5000 Uiso . U . . 2 . . C460 C -0.0881(13) 0.4188(6) 0.4410(8) 0.052(2) 0.5000 Uiso . U . . 2 . . H21 H 0.6294 0.4023 0.5223 0.1184 1.0000 Uiso R . . . . . . H22 H 0.6192 0.4414 0.4728 0.1184 1.0000 Uiso R . . . . . . H11 H 0.5520 0.4518 0.5755 0.1210 1.0000 Uiso R . . . . . . H12 H 0.5747 0.4949 0.5321 0.1210 1.0000 Uiso R . . . . . . H13 H 0.4664 0.4669 0.5297 0.1210 1.0000 Uiso R . . . . . . H241 H 0.5624 0.0050 0.5399 0.0399 1.0000 Uiso R . . . . . . H251 H 0.6650 -0.0096 0.6218 0.0501 1.0000 Uiso R . . . . . . H261 H 0.6998 0.0587 0.6846 0.0521 1.0000 Uiso R . . . . . . H271 H 0.6113 0.1372 0.6726 0.0406 1.0000 Uiso R . . . . . . H281 H 0.4999 0.1886 0.6736 0.0415 1.0000 Uiso R . . . . . . H282 H 0.5021 0.2372 0.6349 0.0415 1.0000 Uiso R . . . . . . H283 H 0.3957 0.2105 0.6462 0.0415 1.0000 Uiso R . . . . . . H351 H 0.1676 0.0335 0.4787 0.0442 1.0000 Uiso R . . . . . . H352 H 0.2811 0.0543 0.4727 0.0442 1.0000 Uiso R . . . . . . H353 H 0.1949 0.0648 0.4257 0.0442 1.0000 Uiso R . . . . . . H361 H 0.0196 0.0484 0.5091 0.0558 1.0000 Uiso R . . . . . . H371 H -0.1163 0.0519 0.5698 0.0670 1.0000 Uiso R . . . . . . H381 H -0.1079 0.1146 0.6413 0.0638 1.0000 Uiso R . . . . . . H391 H 0.0251 0.1770 0.6445 0.0516 1.0000 Uiso R . . . . . . H501 H 0.0251 0.3712 0.6311 0.0917 1.0000 Uiso R . . . . . . H502 H 0.1423 0.3541 0.6328 0.0917 1.0000 Uiso R . . . . . . H503 H 0.0539 0.3125 0.6267 0.0917 1.0000 Uiso R . . . . . . H601 H 0.7654 0.2869 0.2260 0.0470 1.0000 Uiso R . . . . . . H611 H 0.9235 0.3280 0.2259 0.0564 1.0000 Uiso R . . . . . . H621 H 0.9445 0.4110 0.2694 0.0574 1.0000 Uiso R . . . . . . H631 H 0.8037 0.4480 0.3127 0.0484 1.0000 Uiso R . . . . . . H641 H 0.6784 0.4850 0.3289 0.0649 1.0000 Uiso R . . . . . . H642 H 0.6108 0.4740 0.3799 0.0649 1.0000 Uiso R . . . . . . H643 H 0.5565 0.4879 0.3222 0.0649 1.0000 Uiso R . . . . . . H711 H 0.2616 0.4202 0.1610 0.0473 1.0000 Uiso R . . . . . . H712 H 0.3724 0.4023 0.1836 0.0473 1.0000 Uiso R . . . . . . H713 H 0.2858 0.3612 0.1689 0.0473 1.0000 Uiso R . . . . . . H721 H 0.1340 0.4530 0.1763 0.0483 1.0000 Uiso R . . . . . . H731 H 0.0018 0.5122 0.1963 0.0592 1.0000 Uiso R . . . . . . H741 H -0.0239 0.5340 0.2890 0.0537 1.0000 Uiso R . . . . . . H751 H 0.0707 0.4930 0.3615 0.0471 1.0000 Uiso R . . . . . . H831 H 0.6470 0.0340 0.3090 0.0684 1.0000 Uiso R . . . . . . H832 H 0.6216 0.0346 0.3719 0.0684 1.0000 Uiso R . . . . . . H833 H 0.5322 0.0428 0.3260 0.0684 1.0000 Uiso R . . . . . . H841 H 0.7052 0.0703 0.2467 0.0613 1.0000 Uiso R . . . . . . H851 H 0.8406 0.1029 0.1954 0.0690 1.0000 Uiso R . . . . . . H861 H 0.9178 0.1819 0.2173 0.0607 1.0000 Uiso R . . . . . . H871 H 0.8635 0.2298 0.2945 0.0539 1.0000 Uiso R . . . . . . H921 H 0.1034 0.0789 0.3079 0.0482 1.0000 Uiso R . . . . . . H951 H -0.0310 0.0953 0.3636 0.0515 1.0000 Uiso R . . . . . . H952 H -0.0070 0.1299 0.4160 0.0515 1.0000 Uiso R . . . . . . H953 H -0.0640 0.1536 0.3630 0.0515 1.0000 Uiso R . . . . . . H961 H 0.2353 0.0436 0.2600 0.0549 1.0000 Uiso R . . . . . . H962 H 0.3480 0.0536 0.2857 0.0549 1.0000 Uiso R . . . . . . H963 H 0.3077 0.0841 0.2327 0.0549 1.0000 Uiso R . . . . . . H1011 H 0.6258 0.3382 0.6412 0.0501 1.0000 Uiso R . . . . . . H1041 H 0.7648 0.2861 0.6274 0.0677 1.0000 Uiso R . . . . . . H1042 H 0.7903 0.2786 0.5650 0.0677 1.0000 Uiso R . . . . . . H1043 H 0.7362 0.2341 0.5969 0.0677 1.0000 Uiso R . . . . . . H1051 H 0.4874 0.3847 0.6758 0.0595 1.0000 Uiso R . . . . . . H1052 H 0.4202 0.4140 0.6297 0.0595 1.0000 Uiso R . . . . . . H1053 H 0.3766 0.3639 0.6568 0.0595 1.0000 Uiso R . . . . . . H4911 H -0.0325 0.4317 0.5939 0.0501 0.5000 Uiso R . . . 1 . . H4811 H -0.1413 0.4920 0.5508 0.0510 0.5000 Uiso R . . . 1 . . H4711 H -0.1600 0.4951 0.4504 0.0501 0.5000 Uiso R . . . 1 . . H4611 H -0.0658 0.4351 0.3991 0.0483 0.5000 Uiso R . . . 1 . . H4901 H -0.0744 0.4087 0.5964 0.0637 0.5000 Uiso R . . . 2 . . H4801 H -0.2021 0.4642 0.5502 0.0650 0.5000 Uiso R . . . 2 . . H4701 H -0.2075 0.4708 0.4538 0.0636 0.5000 Uiso R . . . 2 . . H4601 H -0.0983 0.4186 0.4013 0.0616 0.5000 Uiso R . . . 2 . . H90 H 0.7268 0.2957 0.4511 0.0379 1.0000 Uiso R . . . . . . H91 H 0.6900 0.3460 0.4196 0.0379 1.0000 Uiso R . . . . . . H92 H 0.7413 0.3009 0.3872 0.0379 1.0000 Uiso R . . . . . . H150 H 0.2808 0.4078 0.5144 0.0417 1.0000 Uiso R . . . . . . H151 H 0.3420 0.4367 0.4691 0.0417 1.0000 Uiso R . . . . . . H152 H 0.2203 0.4318 0.4625 0.0417 1.0000 Uiso R . . . . . . H520 H -0.0947 0.2490 0.4281 0.0962 1.0000 Uiso R . . . . . . H521 H -0.0709 0.2711 0.4879 0.0962 1.0000 Uiso R . . . . . . H522 H -0.0821 0.2113 0.4788 0.0962 1.0000 Uiso R . . . . . . H530 H 0.0380 0.2817 0.3309 0.0373 1.0000 Uiso R . . . . . . H531 H 0.0509 0.3419 0.3335 0.0373 1.0000 Uiso R . . . . . . H532 H 0.1098 0.3097 0.2898 0.0373 1.0000 Uiso R . . . . . . H760 H 0.5573 0.2188 0.2509 0.0320 1.0000 Uiso R . . . . . . H761 H 0.4824 0.1739 0.2667 0.0320 1.0000 Uiso R . . . . . . H762 H 0.4373 0.2234 0.2365 0.0320 1.0000 Uiso R . . . . . . H890 H 0.7966 0.1673 0.4959 0.0686 1.0000 Uiso R . . . . . . H891 H 0.7213 0.1334 0.5298 0.0686 1.0000 Uiso R . . . . . . H892 H 0.7358 0.1214 0.4670 0.0686 1.0000 Uiso R . . . . . . H980 H 0.2059 0.2505 0.1945 0.0448 1.0000 Uiso R . . . . . . H981 H 0.1343 0.2194 0.2333 0.0448 1.0000 Uiso R . . . . . . H982 H 0.2395 0.1954 0.2155 0.0448 1.0000 Uiso R . . . . . . H970 H 0.2960 0.2759 0.2686 0.0312 1.0000 Uiso R . . . . . . H1060 H 0.5003 0.3913 0.4316 0.0514 1.0000 Uiso R . . . . . . H10 H 0.6087 0.5120 0.6367 0.0687 0.5000 Uiso R . . . . . . H1 H 0.6174 0.4701 0.6690 0.0687 0.5000 Uiso R . . . . . . H880 H 0.6291 0.2124 0.4939 0.0397 1.0000 Uiso . . . . . . . H510 H 0.0775 0.2233 0.4273 0.0480 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 0.01735(17) 0.01861(18) 0.01622(17) -0.00113(15) 0.00315(13) 0.00172(15) Tb2 0.01329(16) 0.02045(18) 0.01716(17) -0.00175(15) 0.00326(13) 0.00178(15) Mn1 0.0180(5) 0.0210(5) 0.0181(5) 0.0001(4) 0.0032(4) 0.0057(4) Mn2 0.0169(4) 0.0254(5) 0.0196(4) -0.0001(4) 0.0061(4) 0.0071(4) Mn3 0.0190(4) 0.0224(4) 0.0199(4) 0.0014(4) 0.0079(3) 0.0032(4) Mn4 0.0194(5) 0.0211(5) 0.0149(4) -0.0010(4) 0.0028(4) 0.0043(4) Mn5 0.0130(4) 0.0269(6) 0.0184(4) -0.0005(4) 0.0047(3) 0.0044(4) Mn6 0.0159(4) 0.0227(5) 0.0180(4) 0.0008(4) 0.0055(3) 0.0010(4) O3 0.0118(16) 0.023(2) 0.0272(19) 0.0001(16) 0.0025(14) 0.0113(15) O6 0.030(2) 0.025(2) 0.0211(18) 0.0002(16) -0.0006(16) 0.0050(17) O8 0.0175(17) 0.034(3) 0.0270(19) 0.0033(17) -0.0001(15) 0.0006(16) O10 0.0141(17) 0.020(2) 0.0257(19) -0.0029(15) 0.0009(15) 0.0014(15) O12 0.0183(17) 0.031(2) 0.0214(18) 0.0008(17) 0.0040(14) 0.0021(17) O14 0.025(2) 0.025(2) 0.021(2) -0.0020(16) 0.0060(17) 0.0046(16) O16 0.0218(19) 0.027(2) 0.0197(19) 0.0027(16) 0.0045(16) 0.0081(16) O18 0.0228(19) 0.025(2) 0.0244(19) 0.0017(17) 0.0031(15) 0.0031(15) O29 0.046(2) 0.040(3) 0.023(2) 0.0047(18) 0.0106(18) -0.0080(18) O34 0.0162(18) 0.036(2) 0.0206(19) 0.0019(17) 0.0001(14) 0.0070(16) O40 0.047(3) 0.043(3) 0.028(2) 0.0046(18) 0.0057(18) 0.024(2) O45 0.031(2) 0.054(3) 0.032(2) 0.0082(19) -0.0006(18) 0.018(2) O51 0.023(2) 0.052(3) 0.049(3) -0.009(2) 0.017(2) -0.003(2) O54 0.032(2) 0.023(2) 0.034(2) 0.0007(17) 0.0045(17) -0.0024(17) O59 0.0247(19) 0.038(2) 0.037(2) -0.0002(19) 0.0164(18) 0.0026(16) O65 0.045(3) 0.033(2) 0.025(2) 0.0012(18) 0.0008(18) 0.0118(19) O70 0.031(2) 0.032(2) 0.0180(19) -0.0013(16) 0.0037(16) 0.0095(16) O77 0.0168(18) 0.047(3) 0.030(2) -0.0046(17) 0.0020(15) 0.0045(18) O82 0.037(2) 0.034(2) 0.023(2) -0.0066(17) 0.0112(17) -0.0002(18) O88 0.035(2) 0.038(2) 0.028(2) 0.0000(19) 0.0037(18) 0.0118(18) O90 0.028(2) 0.021(2) 0.028(2) -0.0058(17) 0.0028(17) 0.0009(15) O94 0.0212(19) 0.034(2) 0.030(2) -0.0036(17) 0.0001(16) -0.0062(16) O97 0.026(2) 0.030(2) 0.0217(19) 0.0008(16) -0.0031(16) 0.0042(17) O99 0.041(2) 0.029(2) 0.025(2) -0.0032(17) 0.0048(16) -0.0016(19) O103 0.0244(19) 0.042(2) 0.0205(17) -0.0042(18) 0.0039(14) 0.0047(19) O106 0.040(3) 0.050(3) 0.039(3) 0.0249(18) 0.018(2) 0.014(2) N19 0.025(2) 0.022(2) 0.023(2) 0.0012(18) 0.0017(18) 0.0025(17) O23 0.041(2) 0.026(2) 0.027(2) -0.0017(17) -0.0032(17) 0.0005(18) N33 0.024(2) 0.034(2) 0.018(2) 0.000(2) 0.0030(17) -0.0018(19) N41 0.035(3) 0.033(3) 0.020(2) 0.0047(18) 0.0055(19) 0.0079(19) N55 0.026(2) 0.029(3) 0.025(3) 0.004(2) -0.0028(18) 0.0002(17) N69 0.025(2) 0.030(3) 0.020(2) 0.0026(18) 0.0080(18) 0.0048(17) N81 0.028(3) 0.033(3) 0.023(2) 0.0012(19) 0.0039(18) 0.005(2) C9 0.016(2) 0.047(4) 0.034(3) 0.002(3) 0.005(2) -0.003(2) C15 0.045(4) 0.026(3) 0.033(3) -0.004(2) 0.007(3) 0.004(3) C20 0.027(3) 0.024(2) 0.018(2) -0.0004(18) 0.006(2) -0.004(2) C21 0.029(3) 0.026(2) 0.017(2) 0.0020(17) 0.0035(19) 0.000(2) C22 0.031(3) 0.025(2) 0.022(2) 0.0011(18) 0.0054(19) -0.002(2) C24 0.045(4) 0.028(3) 0.027(3) -0.001(2) 0.005(2) 0.008(2) C25 0.055(4) 0.038(3) 0.033(3) -0.002(2) -0.001(3) 0.018(3) C26 0.055(4) 0.043(3) 0.031(3) -0.004(2) -0.009(3) 0.021(3) C27 0.044(4) 0.032(3) 0.025(3) -0.002(2) -0.006(2) 0.007(3) C28 0.052(4) 0.028(3) 0.024(3) -0.005(2) 0.006(3) 0.005(3) C30 0.037(3) 0.039(3) 0.031(3) 0.005(2) 0.005(2) -0.004(2) C31 0.033(3) 0.034(3) 0.035(3) 0.006(2) 0.005(2) -0.002(2) C32 0.032(3) 0.033(3) 0.030(3) 0.005(2) 0.002(2) -0.001(2) C35 0.033(3) 0.036(3) 0.042(4) -0.001(3) 0.009(3) -0.005(3) C36 0.049(4) 0.051(4) 0.040(4) -0.005(3) 0.014(3) -0.017(3) C37 0.046(4) 0.076(5) 0.048(4) -0.009(3) 0.015(3) -0.032(4) C38 0.052(4) 0.071(5) 0.039(4) -0.003(3) 0.016(3) -0.020(3) C39 0.042(4) 0.056(4) 0.032(3) 0.000(3) 0.008(3) -0.009(3) C42 0.048(4) 0.048(4) 0.030(2) 0.001(3) 0.014(3) 0.016(3) C50 0.119(8) 0.081(6) 0.031(3) 0.005(4) 0.023(4) 0.066(6) C52 0.026(3) 0.091(7) 0.123(8) -0.042(6) 0.033(4) -0.021(4) C53 0.017(3) 0.047(4) 0.030(3) 0.000(3) 0.0015(19) 0.011(3) C56 0.034(3) 0.036(3) 0.029(3) 0.004(2) 0.000(2) -0.008(2) C57 0.027(2) 0.044(3) 0.022(3) 0.011(2) -0.003(2) -0.006(2) C58 0.028(2) 0.041(3) 0.029(3) 0.011(2) 0.007(2) 0.000(2) C60 0.031(3) 0.060(4) 0.028(3) 0.011(3) 0.011(3) 0.003(2) C61 0.027(3) 0.081(4) 0.034(4) 0.013(3) 0.007(3) 0.002(3) C62 0.026(3) 0.071(4) 0.047(4) 0.023(3) 0.002(3) -0.009(3) C63 0.032(3) 0.050(4) 0.039(4) 0.017(3) -0.002(3) -0.011(2) C64 0.051(5) 0.042(3) 0.072(5) -0.010(4) 0.022(4) -0.021(3) C66 0.027(3) 0.023(3) 0.035(2) 0.001(2) -0.003(2) 0.004(2) C67 0.022(3) 0.031(3) 0.032(2) 0.005(2) 0.001(2) -0.0011(19) C68 0.027(3) 0.029(3) 0.028(2) 0.007(2) 0.004(2) 0.0004(19) C71 0.048(4) 0.045(4) 0.026(3) 0.008(3) 0.005(3) 0.011(3) C72 0.040(4) 0.046(4) 0.034(3) 0.011(3) 0.002(3) 0.009(3) C73 0.050(4) 0.052(4) 0.046(3) 0.012(3) -0.001(3) 0.019(3) C74 0.047(4) 0.035(4) 0.052(3) 0.005(3) 0.003(3) 0.019(3) C75 0.042(4) 0.034(4) 0.042(3) -0.006(3) 0.000(3) 0.014(2) C76 0.032(3) 0.029(3) 0.018(2) 0.001(2) 0.002(2) 0.000(3) C78 0.023(3) 0.047(3) 0.029(3) 0.002(2) 0.004(2) 0.016(2) C79 0.037(3) 0.042(3) 0.038(3) -0.001(2) 0.014(2) 0.017(2) C80 0.037(3) 0.039(3) 0.037(3) -0.003(3) 0.010(2) 0.012(2) C83 0.068(5) 0.042(3) 0.063(5) -0.012(4) 0.023(4) 0.004(3) C84 0.056(4) 0.047(4) 0.053(4) -0.009(3) 0.026(3) 0.016(3) C85 0.071(5) 0.061(4) 0.043(4) 0.000(3) 0.035(4) 0.020(3) C86 0.045(4) 0.066(4) 0.044(4) 0.011(3) 0.024(3) 0.019(3) C87 0.038(3) 0.057(4) 0.042(3) 0.008(3) 0.016(3) 0.014(3) C89 0.025(4) 0.069(5) 0.080(6) 0.012(4) 0.003(4) 0.016(3) C91 0.037(3) 0.025(3) 0.030(3) 0.000(2) 0.002(2) -0.005(2) C92 0.037(3) 0.037(4) 0.046(4) -0.012(3) 0.004(3) -0.017(3) C93 0.026(3) 0.036(3) 0.042(4) -0.002(3) 0.001(2) -0.008(2) C95 0.029(3) 0.053(4) 0.047(4) -0.003(3) 0.003(3) -0.016(3) C96 0.066(5) 0.031(3) 0.041(4) -0.011(3) 0.012(3) -0.008(3) C98 0.040(4) 0.037(4) 0.035(3) -0.013(3) -0.003(3) -0.001(3) C100 0.051(3) 0.033(4) 0.023(3) -0.001(2) 0.004(2) -0.002(3) C101 0.048(3) 0.045(4) 0.031(3) -0.012(3) -0.001(3) -0.004(3) C102 0.036(3) 0.045(4) 0.019(2) 0.000(2) -0.0026(19) 0.002(2) C104 0.034(3) 0.087(6) 0.047(4) -0.014(4) -0.010(3) 0.009(3) C105 0.076(5) 0.039(4) 0.034(3) -0.011(3) 0.004(3) 0.008(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.2480(15) 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 O1 . H10 . 0.850 no O1 . H1 . 0.850 no C2 . C1 . 1.508(13) yes C2 . O106 . 1.505(11) yes C2 . H21 . 0.950 no C2 . H22 . 0.950 no C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no Tb1 . Tb2 . 3.4986(5) yes Tb1 . Mn1 . 3.5573(10) yes Tb1 . Mn3 . 3.5652(9) yes Tb1 . Mn5 . 3.5139(9) yes Tb1 . O3 . 2.401(3) yes Tb1 . O8 . 2.585(3) yes Tb1 . O10 . 2.414(3) yes Tb1 . O14 . 2.648(4) yes Tb1 . O16 . 2.455(4) yes Tb1 . O18 . 2.461(4) yes Tb1 . O99 . 2.311(4) yes Tb1 . O103 . 2.387(4) yes Tb1 . O106 . 2.413(5) yes Tb2 . Mn2 . 3.5027(9) yes Tb2 . Mn4 . 3.5937(10) yes Tb2 . Mn6 . 3.5264(9) yes Tb2 . O3 . 2.415(3) yes Tb2 . O6 . 2.610(4) yes Tb2 . O10 . 2.402(3) yes Tb2 . O12 . 2.596(4) yes Tb2 . O16 . 2.375(3) yes Tb2 . O34 . 2.533(4) yes Tb2 . O90 . 2.313(4) yes Tb2 . O94 . 2.373(4) yes Tb2 . O97 . 2.420(4) yes Mn1 . Mn2 . 3.0809(12) yes Mn1 . Mn6 . 3.0941(12) yes Mn1 . O10 . 1.899(3) yes Mn1 . O12 . 2.324(4) yes Mn1 . O14 . 1.951(4) yes Mn1 . O54 . 2.196(4) yes Mn1 . O65 . 1.869(4) yes Mn1 . N69 . 2.030(5) yes Mn2 . Mn3 . 3.0360(13) yes Mn2 . O12 . 1.920(3) yes Mn2 . O14 . 2.224(4) yes Mn2 . O16 . 1.906(4) yes Mn2 . O45 . 1.849(4) yes Mn2 . O51 . 2.323(4) yes Mn2 . N41 . 2.003(4) yes Mn3 . O16 . 1.901(4) yes Mn3 . O18 . 2.103(4) yes Mn3 . O29 . 1.875(4) yes Mn3 . O40 . 1.923(4) yes Mn3 . O51 . 2.660(4) yes Mn3 . N33 . 2.015(5) yes Mn4 . Mn5 . 3.0460(12) yes Mn4 . O3 . 1.923(4) yes Mn4 . O34 . 2.121(4) yes Mn4 . O82 . 1.925(4) yes Mn4 . O88 . 2.538(4) yes Mn4 . N19 . 1.999(4) yes Mn4 . O23 . 1.869(4) yes Mn5 . Mn6 . 3.1213(12) yes Mn5 . O3 . 1.889(3) yes Mn5 . O6 . 2.229(4) yes Mn5 . O8 . 1.924(4) yes Mn5 . O77 . 1.859(3) yes Mn5 . O88 . 2.352(4) yes Mn5 . N81 . 2.018(5) yes Mn6 . O6 . 1.956(4) yes Mn6 . O8 . 2.342(4) yes Mn6 . O10 . 1.893(3) yes Mn6 . O59 . 1.846(3) yes Mn6 . O70 . 2.167(4) yes Mn6 . N55 . 2.024(5) yes O6 . C76 . 1.435(6) yes O8 . C9 . 1.452(6) yes O12 . C53 . 1.435(6) yes O14 . C15 . 1.425(6) yes O18 . N19 . 1.370(5) yes O29 . C30 . 1.346(7) yes O34 . N33 . 1.376(5) yes O40 . N41 . 1.361(6) yes O45 . C44 . 1.302(7) yes O51 . C52 . 1.439(7) yes O51 . H510 . 0.868 no O54 . N55 . 1.379(6) yes O59 . C58 . 1.319(7) yes O65 . C66 . 1.332(7) yes O70 . N69 . 1.366(5) yes O77 . C78 . 1.338(7) yes O82 . N81 . 1.356(6) yes O88 . C89 . 1.468(7) yes O88 . H880 . 0.868 no O90 . C91 . 1.269(7) yes O94 . C93 . 1.268(7) yes O97 . C98 . 1.404(6) yes O97 . H970 . 0.850 no O99 . C100 . 1.292(7) yes O103 . C102 . 1.273(6) yes O106 . H1060 . 0.850 no N19 . C20 . 1.295(7) yes O23 . C22 . 1.342(6) yes N33 . C32 . 1.293(7) yes N41 . C42 . 1.302(7) yes N55 . C56 . 1.302(7) yes N69 . C68 . 1.279(7) yes N81 . C80 . 1.299(7) yes C9 . H90 . 0.950 no C9 . H91 . 0.950 no C9 . H92 . 0.950 no C15 . H150 . 0.950 no C15 . H151 . 0.950 no C15 . H152 . 0.950 no C20 . C21 . 1.472(7) yes C20 . C28 . 1.489(7) yes C21 . C22 . 1.407(7) yes C21 . C27 . 1.398(8) yes C22 . C24 . 1.395(8) yes C24 . C25 . 1.381(8) yes C24 . H241 . 0.950 no C25 . C26 . 1.380(9) yes C25 . H251 . 0.950 no C26 . C27 . 1.372(8) yes C26 . H261 . 0.950 no C27 . H271 . 0.950 no C28 . H281 . 0.950 no C28 . H282 . 0.950 no C28 . H283 . 0.950 no C30 . C31 . 1.406(8) yes C30 . C39 . 1.374(8) yes C31 . C32 . 1.478(8) yes C31 . C36 . 1.385(8) yes C32 . C35 . 1.501(8) yes C35 . H351 . 0.950 no C35 . H352 . 0.950 no C35 . H353 . 0.950 no C36 . C37 . 1.373(9) yes C36 . H361 . 0.950 no C37 . C38 . 1.378(9) yes C37 . H371 . 0.950 no C38 . C39 . 1.388(9) yes C38 . H381 . 0.950 no C39 . H391 . 0.950 no C42 . C50 . 1.502(8) yes C42 . C43 . 1.454(9) yes C50 . H501 . 0.950 no C50 . H502 . 0.950 no C50 . H503 . 0.950 no C52 . H520 . 0.950 no C52 . H521 . 0.950 no C52 . H522 . 0.950 no C53 . H530 . 0.950 no C53 . H531 . 0.950 no C53 . H532 . 0.950 no C56 . C57 . 1.470(9) yes C56 . C64 . 1.486(9) yes C57 . C58 . 1.418(8) yes C57 . C63 . 1.402(8) yes C58 . C60 . 1.393(8) yes C60 . C61 . 1.337(9) yes C60 . H601 . 0.950 no C61 . C62 . 1.413(10) yes C61 . H611 . 0.950 no C62 . C63 . 1.375(9) yes C62 . H621 . 0.950 no C63 . H631 . 0.950 no C64 . H641 . 0.950 no C64 . H642 . 0.950 no C64 . H643 . 0.950 no C66 . C67 . 1.405(8) yes C66 . C75 . 1.400(8) yes C67 . C68 . 1.478(8) yes C67 . C72 . 1.405(8) yes C68 . C71 . 1.508(7) yes C71 . H711 . 0.950 no C71 . H712 . 0.950 no C71 . H713 . 0.950 no C72 . C73 . 1.384(8) yes C72 . H721 . 0.950 no C73 . C74 . 1.372(9) yes C73 . H731 . 0.950 no C74 . C75 . 1.374(8) yes C74 . H741 . 0.950 no C75 . H751 . 0.950 no C76 . H760 . 0.950 no C76 . H761 . 0.950 no C76 . H762 . 0.950 no C78 . C79 . 1.414(9) yes C78 . C87 . 1.403(8) yes C79 . C80 . 1.458(9) yes C79 . C84 . 1.405(8) yes C80 . C83 . 1.484(9) yes C83 . H831 . 0.950 no C83 . H832 . 0.950 no C83 . H833 . 0.950 no C84 . C85 . 1.386(9) yes C84 . H841 . 0.950 no C85 . C86 . 1.354(10) yes C85 . H851 . 0.950 no C86 . C87 . 1.395(9) yes C86 . H861 . 0.950 no C87 . H871 . 0.950 no C89 . H890 . 0.950 no C89 . H891 . 0.950 no C89 . H892 . 0.950 no C91 . C92 . 1.388(8) yes C91 . C96 . 1.502(8) yes C92 . C93 . 1.394(9) yes C92 . H921 . 0.950 no C93 . C95 . 1.512(8) yes C95 . H951 . 0.950 no C95 . H952 . 0.950 no C95 . H953 . 0.950 no C96 . H961 . 0.950 no C96 . H962 . 0.950 no C96 . H963 . 0.950 no C98 . H980 . 0.950 no C98 . H981 . 0.950 no C98 . H982 . 0.950 no C100 . C101 . 1.385(9) yes C100 . C105 . 1.498(8) yes C101 . C102 . 1.365(8) yes C101 . H1011 . 0.950 no C102 . C104 . 1.504(8) yes C104 . H1041 . 0.950 no C104 . H1042 . 0.950 no C104 . H1043 . 0.950 no C105 . H1051 . 0.950 no C105 . H1052 . 0.950 no C105 . H1053 . 0.950 no C491 . C481 . 1.357(19) yes C491 . C43 . 1.427(16) yes C491 . H4911 . 0.950 no C481 . C471 . 1.433(19) yes C481 . H4811 . 0.950 no C471 . C461 . 1.39(2) yes C471 . H4711 . 0.950 no C461 . C44 . 1.426(18) yes C461 . H4611 . 0.950 no C44 . C43 . 1.428(9) yes C490 . C480 . 1.43(2) yes C490 . H4901 . 0.950 no C480 . C470 . 1.35(2) yes C480 . H4801 . 0.950 no C470 . C460 . 1.41(2) yes C470 . H4701 . 0.950 no C460 . H4601 . 0.950 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 H10 . O1 . H1 . 102.3 no C1 . C2 . O106 . 130.6(9) yes C1 . C2 . H21 . 103.9 no O106 . C2 . H21 . 103.8 no C1 . C2 . H22 . 104.1 no O106 . C2 . H22 . 104.0 no H21 . C2 . H22 . 109.5 no C2 . C1 . H11 . 109.7 no C2 . C1 . H12 . 109.6 no H11 . C1 . H12 . 109.5 no C2 . C1 . H13 . 109.1 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no Tb2 . Tb1 . Mn1 . 62.892(17) yes Tb2 . Tb1 . Mn3 . 65.114(16) yes Mn1 . Tb1 . Mn3 . 98.26(2) yes Tb2 . Tb1 . Mn5 . 62.300(16) yes Mn1 . Tb1 . Mn5 . 99.23(2) yes Mn3 . Tb1 . Mn5 . 106.91(2) yes Tb2 . Tb1 . O3 . 43.56(8) yes Mn1 . Tb1 . O3 . 101.21(8) yes Mn3 . Tb1 . O3 . 76.57(8) yes Mn5 . Tb1 . O3 . 30.46(8) yes Tb2 . Tb1 . O8 . 83.07(8) yes Mn1 . Tb1 . O8 . 88.48(8) yes Mn3 . Tb1 . O8 . 139.11(9) yes Mn5 . Tb1 . O8 . 32.46(9) yes O3 . Tb1 . O8 . 62.57(11) yes Tb2 . Tb1 . O10 . 43.28(8) yes Mn1 . Tb1 . O10 . 29.99(8) yes Mn3 . Tb1 . O10 . 101.13(8) yes Mn5 . Tb1 . O10 . 69.77(8) yes O3 . Tb1 . O10 . 73.03(11) yes Tb2 . Tb1 . O14 . 82.02(8) yes Mn1 . Tb1 . O14 . 32.66(8) yes Mn3 . Tb1 . O14 . 83.56(8) yes Mn5 . Tb1 . O14 . 131.58(8) yes O3 . Tb1 . O14 . 125.51(11) yes Tb2 . Tb1 . O16 . 42.69(8) yes Mn1 . Tb1 . O16 . 69.73(8) yes Mn3 . Tb1 . O16 . 30.25(8) yes Mn5 . Tb1 . O16 . 101.11(8) yes O3 . Tb1 . O16 . 73.56(11) yes Tb2 . Tb1 . O18 . 87.27(8) yes Mn1 . Tb1 . O18 . 133.43(8) yes Mn3 . Tb1 . O18 . 35.17(8) yes Mn5 . Tb1 . O18 . 96.60(8) yes O3 . Tb1 . O18 . 73.21(12) yes Tb2 . Tb1 . O99 . 143.35(11) yes Mn1 . Tb1 . O99 . 108.72(10) yes Mn3 . Tb1 . O99 . 82.28(10) yes Mn5 . Tb1 . O99 . 149.10(11) yes O3 . Tb1 . O99 . 145.42(13) yes Tb2 . Tb1 . O103 . 130.55(10) yes Mn1 . Tb1 . O103 . 153.26(9) yes Mn3 . Tb1 . O103 . 108.42(9) yes Mn5 . Tb1 . O103 . 75.10(9) yes O3 . Tb1 . O103 . 87.03(12) yes Tb2 . Tb1 . O106 . 128.50(11) yes Mn1 . Tb1 . O106 . 71.52(11) yes Mn3 . Tb1 . O106 . 147.51(10) yes Mn5 . Tb1 . O106 . 105.18(10) yes O3 . Tb1 . O106 . 134.99(12) yes O8 . Tb1 . O10 . 66.60(11) yes O8 . Tb1 . O14 . 118.16(11) yes O10 . Tb1 . O14 . 61.81(11) yes O8 . Tb1 . O16 . 125.75(11) yes O10 . Tb1 . O16 . 71.43(11) yes O14 . Tb1 . O16 . 64.65(11) yes O8 . Tb1 . O18 . 124.51(12) yes O10 . Tb1 . O18 . 130.02(12) yes O14 . Tb1 . O18 . 114.23(11) yes O16 . Tb1 . O18 . 64.33(11) yes O8 . Tb1 . O99 . 133.51(13) yes O10 . Tb1 . O99 . 138.67(13) yes O14 . Tb1 . O99 . 77.96(13) yes O16 . Tb1 . O99 . 100.72(13) yes O18 . Tb1 . O99 . 73.73(13) yes O8 . Tb1 . O103 . 72.69(11) yes O10 . Tb1 . O103 . 139.24(11) yes O14 . Tb1 . O103 . 147.43(13) yes O16 . Tb1 . O103 . 136.78(13) yes O18 . Tb1 . O103 . 73.27(12) yes O8 . Tb1 . O106 . 72.73(13) yes O10 . Tb1 . O106 . 85.23(14) yes O14 . Tb1 . O106 . 71.37(13) yes O16 . Tb1 . O106 . 135.87(13) yes O18 . Tb1 . O106 . 143.72(14) yes O99 . Tb1 . O103 . 74.01(14) yes O99 . Tb1 . O106 . 72.70(14) yes O103 . Tb1 . O106 . 84.60(15) yes Tb1 . Tb2 . Mn2 . 63.419(17) yes Tb1 . Tb2 . Mn4 . 64.713(16) yes Mn2 . Tb2 . Mn4 . 107.04(2) yes Tb1 . Tb2 . Mn6 . 62.930(16) yes Mn2 . Tb2 . Mn6 . 98.90(2) yes Mn4 . Tb2 . Mn6 . 99.48(2) yes Tb1 . Tb2 . O3 . 43.25(8) yes Mn2 . Tb2 . O3 . 102.71(8) yes Mn4 . Tb2 . O3 . 29.89(8) yes Mn6 . Tb2 . O3 . 70.82(8) yes Tb1 . Tb2 . O6 . 82.48(8) yes Mn2 . Tb2 . O6 . 131.83(8) yes Mn4 . Tb2 . O6 . 85.28(8) yes Mn6 . Tb2 . O6 . 33.10(8) yes O3 . Tb2 . O6 . 65.60(11) yes Tb1 . Tb2 . O10 . 43.56(8) yes Mn2 . Tb2 . O10 . 69.19(8) yes Mn4 . Tb2 . O10 . 101.99(8) yes Mn6 . Tb2 . O10 . 30.33(8) yes O3 . Tb2 . O10 . 73.00(12) yes Tb1 . Tb2 . O12 . 84.15(8) yes Mn2 . Tb2 . O12 . 32.60(7) yes Mn4 . Tb2 . O12 . 139.39(8) yes Mn6 . Tb2 . O12 . 87.64(8) yes O3 . Tb2 . O12 . 127.40(11) yes Tb1 . Tb2 . O16 . 44.49(9) yes Mn2 . Tb2 . O16 . 30.88(9) yes Mn4 . Tb2 . O16 . 76.27(9) yes Mn6 . Tb2 . O16 . 101.61(9) yes O3 . Tb2 . O16 . 74.76(12) yes Tb1 . Tb2 . O34 . 87.26(8) yes Mn2 . Tb2 . O34 . 96.21(8) yes Mn4 . Tb2 . O34 . 35.45(8) yes Mn6 . Tb2 . O34 . 134.92(8) yes O3 . Tb2 . O34 . 64.47(11) yes Tb1 . Tb2 . O90 . 142.08(10) yes Mn2 . Tb2 . O90 . 149.77(9) yes Mn4 . Tb2 . O90 . 82.17(10) yes Mn6 . Tb2 . O90 . 108.05(9) yes O3 . Tb2 . O90 . 98.94(12) yes Tb1 . Tb2 . O94 . 130.66(9) yes Mn2 . Tb2 . O94 . 75.43(9) yes Mn4 . Tb2 . O94 . 106.13(9) yes Mn6 . Tb2 . O94 . 154.34(9) yes O3 . Tb2 . O94 . 134.73(12) yes Tb1 . Tb2 . O97 . 128.16(9) yes Mn2 . Tb2 . O97 . 103.15(9) yes Mn4 . Tb2 . O97 . 149.50(9) yes Mn6 . Tb2 . O97 . 71.29(9) yes O3 . Tb2 . O97 . 136.68(12) yes O6 . Tb2 . O10 . 62.69(11) yes O6 . Tb2 . O12 . 117.22(11) yes O10 . Tb2 . O12 . 65.84(11) yes O6 . Tb2 . O16 . 126.83(12) yes O10 . Tb2 . O16 . 73.04(12) yes O12 . Tb2 . O16 . 63.16(11) yes O6 . Tb2 . O34 . 116.07(11) yes O10 . Tb2 . O34 . 130.58(12) yes O12 . Tb2 . O34 . 124.15(11) yes O16 . Tb2 . O34 . 72.53(12) yes O6 . Tb2 . O90 . 76.62(12) yes O10 . Tb2 . O90 . 138.35(12) yes O12 . Tb2 . O90 . 133.60(12) yes O16 . Tb2 . O90 . 145.72(13) yes O34 . Tb2 . O90 . 74.42(12) yes O6 . Tb2 . O94 . 146.82(12) yes O10 . Tb2 . O94 . 139.81(12) yes O12 . Tb2 . O94 . 74.13(12) yes O16 . Tb2 . O94 . 86.34(12) yes O34 . Tb2 . O94 . 70.72(12) yes O6 . Tb2 . O97 . 71.22(12) yes O10 . Tb2 . O97 . 84.60(12) yes O12 . Tb2 . O97 . 70.56(11) yes O16 . Tb2 . O97 . 133.49(12) yes O34 . Tb2 . O97 . 144.37(13) yes O90 . Tb2 . O94 . 74.35(13) yes O90 . Tb2 . O97 . 73.82(13) yes O94 . Tb2 . O97 . 85.46(13) yes Tb1 . Mn1 . Mn2 . 66.89(2) yes Tb1 . Mn1 . Mn6 . 66.49(2) yes Mn2 . Mn1 . Mn6 . 119.75(3) yes Tb1 . Mn1 . O10 . 39.46(10) yes Mn2 . Mn1 . O10 . 84.91(11) yes Mn6 . Mn1 . O10 . 35.25(10) yes Tb1 . Mn1 . O12 . 86.78(9) yes Mn2 . Mn1 . O12 . 38.51(8) yes Mn6 . Mn1 . O12 . 103.86(9) yes O10 . Mn1 . O12 . 79.54(13) yes Tb1 . Mn1 . O14 . 47.11(11) yes Mn2 . Mn1 . O14 . 45.98(11) yes Mn6 . Mn1 . O14 . 112.78(11) yes O10 . Mn1 . O14 . 85.27(15) yes O12 . Mn1 . O14 . 83.92(14) yes Tb1 . Mn1 . O54 . 82.99(10) yes Mn2 . Mn1 . O54 . 141.55(11) yes Mn6 . Mn1 . O54 . 63.15(10) yes O10 . Mn1 . O54 . 86.45(15) yes O12 . Mn1 . O54 . 165.94(14) yes Tb1 . Mn1 . O65 . 138.38(12) yes Mn2 . Mn1 . O65 . 92.75(13) yes Mn6 . Mn1 . O65 . 147.22(13) yes O10 . Mn1 . O65 . 177.42(17) yes O12 . Mn1 . O65 . 99.31(16) yes Tb1 . Mn1 . N69 . 132.62(13) yes Mn2 . Mn1 . N69 . 131.30(14) yes Mn6 . Mn1 . N69 . 67.58(13) yes O10 . Mn1 . N69 . 93.97(17) yes O12 . Mn1 . N69 . 93.31(16) yes O14 . Mn1 . O54 . 96.01(15) yes O14 . Mn1 . O65 . 92.31(16) yes O54 . Mn1 . O65 . 94.74(17) yes O14 . Mn1 . N69 . 177.22(18) yes O54 . Mn1 . N69 . 86.61(17) yes O65 . Mn1 . N69 . 88.40(18) yes Mn1 . Mn2 . Tb2 . 67.65(2) yes Mn1 . Mn2 . Mn3 . 123.40(3) yes Tb2 . Mn2 . Mn3 . 70.69(2) yes Mn1 . Mn2 . O12 . 48.91(11) yes Tb2 . Mn2 . O12 . 46.75(11) yes Mn3 . Mn2 . O12 . 115.99(12) yes Mn1 . Mn2 . O14 . 39.12(9) yes Tb2 . Mn2 . O14 . 88.04(9) yes Mn3 . Mn2 . O14 . 104.78(10) yes O12 . Mn2 . O14 . 87.42(14) yes Mn1 . Mn2 . O16 . 87.60(11) yes Tb2 . Mn2 . O16 . 39.77(11) yes Mn3 . Mn2 . O16 . 37.06(11) yes O12 . Mn2 . O16 . 86.03(15) yes O14 . Mn2 . O16 . 82.53(14) yes Mn1 . Mn2 . O45 . 95.05(14) yes Tb2 . Mn2 . O45 . 138.46(14) yes Mn3 . Mn2 . O45 . 141.05(14) yes O12 . Mn2 . O45 . 92.98(17) yes O14 . Mn2 . O45 . 101.81(17) yes Mn1 . Mn2 . O51 . 143.04(11) yes Tb2 . Mn2 . O51 . 80.81(10) yes Mn3 . Mn2 . O51 . 57.68(11) yes O12 . Mn2 . O51 . 95.39(16) yes O14 . Mn2 . O51 . 161.56(15) yes Mn1 . Mn2 . N41 . 132.75(15) yes Tb2 . Mn2 . N41 . 132.33(14) yes Mn3 . Mn2 . N41 . 62.73(14) yes O12 . Mn2 . N41 . 178.20(19) yes O14 . Mn2 . N41 . 94.13(17) yes O16 . Mn2 . O45 . 175.51(19) yes O16 . Mn2 . O51 . 79.50(15) yes O45 . Mn2 . O51 . 96.24(17) yes O16 . Mn2 . N41 . 93.26(17) yes O45 . Mn2 . N41 . 87.60(19) yes O51 . Mn2 . N41 . 82.85(18) yes Mn2 . Mn3 . Tb1 . 67.21(2) yes Mn2 . Mn3 . O16 . 37.16(11) yes Tb1 . Mn3 . O16 . 40.57(11) yes Mn2 . Mn3 . O18 . 108.61(10) yes Tb1 . Mn3 . O18 . 42.39(10) yes O16 . Mn3 . O18 . 81.45(15) yes Mn2 . Mn3 . O29 . 137.84(14) yes Tb1 . Mn3 . O29 . 144.05(13) yes O16 . Mn3 . O29 . 174.52(17) yes O18 . Mn3 . O29 . 103.77(16) yes Mn2 . Mn3 . O40 . 65.19(12) yes Tb1 . Mn3 . O40 . 84.29(13) yes O16 . Mn3 . O40 . 91.13(16) yes O18 . Mn3 . O40 . 93.38(17) yes O29 . Mn3 . O40 . 86.95(18) yes Mn2 . Mn3 . O51 . 47.58(10) yes Tb1 . Mn3 . O51 . 110.70(9) yes O16 . Mn3 . O51 . 71.12(14) yes O18 . Mn3 . O51 . 152.57(13) yes O29 . Mn3 . O51 . 103.65(16) yes Mn2 . Mn3 . N33 . 113.28(13) yes Tb1 . Mn3 . N33 . 106.93(13) yes O16 . Mn3 . N33 . 93.85(17) yes O18 . Mn3 . N33 . 98.80(17) yes O29 . Mn3 . N33 . 87.03(18) yes O40 . Mn3 . O51 . 87.58(15) yes O40 . Mn3 . N33 . 167.40(19) yes O51 . Mn3 . N33 . 83.10(16) yes Tb2 . Mn4 . Mn5 . 65.63(2) yes Tb2 . Mn4 . O3 . 38.74(10) yes Mn5 . Mn4 . O3 . 36.57(9) yes Tb2 . Mn4 . O34 . 43.83(10) yes Mn5 . Mn4 . O34 . 108.21(10) yes O3 . Mn4 . O34 . 81.38(14) yes Tb2 . Mn4 . O82 . 87.05(13) yes Mn5 . Mn4 . O82 . 65.40(12) yes O3 . Mn4 . O82 . 91.85(16) yes O34 . Mn4 . O82 . 95.47(16) yes Tb2 . Mn4 . O88 . 110.73(9) yes Mn5 . Mn4 . O88 . 48.78(9) yes O3 . Mn4 . O88 . 72.94(13) yes O34 . Mn4 . O88 . 154.31(14) yes O82 . Mn4 . O88 . 84.85(15) yes Tb2 . Mn4 . N19 . 105.63(13) yes Mn5 . Mn4 . N19 . 112.68(14) yes O3 . Mn4 . N19 . 93.60(17) yes O34 . Mn4 . N19 . 98.81(16) yes O82 . Mn4 . N19 . 165.33(18) yes Tb2 . Mn4 . O23 . 144.36(13) yes Mn5 . Mn4 . O23 . 141.22(13) yes O3 . Mn4 . O23 . 176.87(17) yes O34 . Mn4 . O23 . 101.74(17) yes O82 . Mn4 . O23 . 88.07(17) yes O88 . Mn4 . N19 . 83.75(16) yes O88 . Mn4 . O23 . 103.94(16) yes N19 . Mn4 . O23 . 85.75(18) yes Mn4 . Mn5 . Tb1 . 70.31(2) yes Mn4 . Mn5 . Mn6 . 123.53(3) yes Tb1 . Mn5 . Mn6 . 66.79(2) yes Mn4 . Mn5 . O3 . 37.34(11) yes Tb1 . Mn5 . O3 . 40.12(11) yes Mn6 . Mn5 . O3 . 86.91(11) yes Mn4 . Mn5 . O6 . 106.86(10) yes Tb1 . Mn5 . O6 . 87.62(9) yes Mn6 . Mn5 . O6 . 38.53(9) yes O3 . Mn5 . O6 . 82.51(14) yes Mn4 . Mn5 . O8 . 114.72(10) yes Tb1 . Mn5 . O8 . 46.15(10) yes Mn6 . Mn5 . O8 . 48.49(10) yes O3 . Mn5 . O8 . 85.74(15) yes O6 . Mn5 . O8 . 86.52(14) yes Mn4 . Mn5 . O77 . 138.83(13) yes Tb1 . Mn5 . O77 . 138.56(13) yes Mn6 . Mn5 . O77 . 97.49(13) yes O3 . Mn5 . O77 . 174.01(15) yes O6 . Mn5 . O77 . 103.46(15) yes Mn4 . Mn5 . O88 . 54.26(10) yes Tb1 . Mn5 . O88 . 80.37(9) yes Mn6 . Mn5 . O88 . 142.87(10) yes O3 . Mn5 . O88 . 78.16(14) yes O6 . Mn5 . O88 . 160.21(14) yes Mn4 . Mn5 . N81 . 63.56(13) yes Tb1 . Mn5 . N81 . 132.16(13) yes Mn6 . Mn5 . N81 . 132.02(14) yes O3 . Mn5 . N81 . 92.61(17) yes O6 . Mn5 . N81 . 93.81(17) yes O8 . Mn5 . O77 . 94.11(17) yes O8 . Mn5 . O88 . 96.18(15) yes O77 . Mn5 . O88 . 95.91(15) yes O8 . Mn5 . N81 . 178.27(17) yes O77 . Mn5 . N81 . 87.46(19) yes O88 . Mn5 . N81 . 82.95(17) yes Mn1 . Mn6 . Tb2 . 67.20(2) yes Mn1 . Mn6 . Mn5 . 120.13(3) yes Tb2 . Mn6 . Mn5 . 65.81(2) yes Mn1 . Mn6 . O6 . 113.03(12) yes Tb2 . Mn6 . O6 . 46.78(11) yes Mn5 . Mn6 . O6 . 45.23(11) yes Mn1 . Mn6 . O8 . 105.17(9) yes Tb2 . Mn6 . O8 . 85.90(9) yes Mn5 . Mn6 . O8 . 37.97(10) yes O6 . Mn6 . O8 . 82.73(14) yes Mn1 . Mn6 . O10 . 35.38(11) yes Tb2 . Mn6 . O10 . 39.85(11) yes Mn5 . Mn6 . O10 . 85.07(11) yes O6 . Mn6 . O10 . 85.52(15) yes O8 . Mn6 . O10 . 80.18(13) yes Mn1 . Mn6 . O59 . 145.90(13) yes Tb2 . Mn6 . O59 . 138.36(13) yes Mn5 . Mn6 . O59 . 93.79(13) yes O6 . Mn6 . O59 . 92.69(17) yes O8 . Mn6 . O59 . 99.79(15) yes Mn1 . Mn6 . O70 . 62.70(9) yes Tb2 . Mn6 . O70 . 82.66(10) yes Mn5 . Mn6 . O70 . 140.01(11) yes O6 . Mn6 . O70 . 95.28(15) yes O8 . Mn6 . O70 . 165.91(13) yes Mn1 . Mn6 . N55 . 68.62(13) yes Tb2 . Mn6 . N55 . 133.27(14) yes Mn5 . Mn6 . N55 . 129.00(13) yes O6 . Mn6 . N55 . 174.22(18) yes O8 . Mn6 . N55 . 91.49(16) yes O10 . Mn6 . O59 . 178.20(17) yes O10 . Mn6 . O70 . 85.76(14) yes O59 . Mn6 . O70 . 94.23(16) yes O10 . Mn6 . N55 . 93.72(17) yes O59 . Mn6 . N55 . 88.08(18) yes O70 . Mn6 . N55 . 90.38(17) yes Tb2 . O3 . Tb1 . 93.18(11) yes Tb2 . O3 . Mn4 . 111.38(16) yes Tb1 . O3 . Mn4 . 122.42(16) yes Tb2 . O3 . Mn5 . 114.34(15) yes Tb1 . O3 . Mn5 . 109.42(16) yes Mn4 . O3 . Mn5 . 106.09(16) yes Tb2 . O6 . Mn5 . 96.79(13) yes Tb2 . O6 . Mn6 . 100.13(15) yes Mn5 . O6 . Mn6 . 96.24(16) yes Tb2 . O6 . C76 . 121.9(3) yes Mn5 . O6 . C76 . 118.1(3) yes Mn6 . O6 . C76 . 118.6(3) yes Tb1 . O8 . Mn6 . 96.08(12) yes Tb1 . O8 . Mn5 . 101.40(14) yes Mn6 . O8 . Mn5 . 93.55(14) yes Tb1 . O8 . C9 . 122.4(3) yes Mn6 . O8 . C9 . 118.7(3) yes Mn5 . O8 . C9 . 119.0(3) yes Tb1 . O10 . Tb2 . 93.16(12) yes Tb1 . O10 . Mn1 . 110.55(15) yes Tb2 . O10 . Mn1 . 117.24(15) yes Tb1 . O10 . Mn6 . 116.19(15) yes Tb2 . O10 . Mn6 . 109.82(15) yes Mn1 . O10 . Mn6 . 109.37(17) yes Tb2 . O12 . Mn1 . 96.72(12) yes Tb2 . O12 . Mn2 . 100.65(14) yes Mn1 . O12 . Mn2 . 92.59(15) yes Tb2 . O12 . C53 . 124.1(3) yes Mn1 . O12 . C53 . 115.8(3) yes Mn2 . O12 . C53 . 120.5(3) yes Mn2 . O14 . Tb1 . 97.73(13) yes Mn2 . O14 . Mn1 . 94.90(16) yes Tb1 . O14 . Mn1 . 100.23(14) yes Mn2 . O14 . C15 . 115.8(3) yes Tb1 . O14 . C15 . 123.4(3) yes Mn1 . O14 . C15 . 119.3(3) yes Tb1 . O16 . Tb2 . 92.82(12) yes Tb1 . O16 . Mn2 . 114.53(16) yes Tb2 . O16 . Mn2 . 109.34(16) yes Tb1 . O16 . Mn3 . 109.19(16) yes Tb2 . O16 . Mn3 . 125.13(17) yes Mn2 . O16 . Mn3 . 105.78(17) yes Mn3 . O18 . Tb1 . 102.43(14) yes Mn3 . O18 . N19 . 115.1(3) yes Tb1 . O18 . N19 . 118.3(3) yes Mn3 . O29 . C30 . 122.1(4) yes Tb2 . O34 . Mn4 . 100.72(14) yes Tb2 . O34 . N33 . 118.2(3) yes Mn4 . O34 . N33 . 114.5(3) yes Mn3 . O40 . N41 . 113.7(3) yes Mn2 . O45 . C44 . 134.1(4) yes Mn2 . O51 . Mn3 . 74.74(12) yes Mn2 . O51 . C52 . 121.9(4) yes Mn3 . O51 . C52 . 136.7(5) yes Mn2 . O51 . H510 . 94.9 no Mn3 . O51 . H510 . 93.8 no C52 . O51 . H510 . 121.1 no Mn1 . O54 . N55 . 113.1(3) yes Mn6 . O59 . C58 . 129.5(4) yes Mn1 . O65 . C66 . 131.0(4) yes Mn6 . O70 . N69 . 113.3(3) yes Mn5 . O77 . C78 . 127.9(4) yes Mn4 . O82 . N81 . 116.5(3) yes Mn5 . O88 . Mn4 . 76.96(12) yes Mn5 . O88 . C89 . 129.9(4) yes Mn4 . O88 . C89 . 120.7(4) yes Mn5 . O88 . H880 . 93.3 no Mn4 . O88 . H880 . 96.0 no C89 . O88 . H880 . 126.3 no Tb2 . O90 . C91 . 136.3(4) yes Tb2 . O94 . C93 . 132.2(4) yes Tb2 . O97 . C98 . 137.5(4) yes Tb2 . O97 . H970 . 101.8 no C98 . O97 . H970 . 119.7 no Tb1 . O99 . C100 . 136.0(4) yes Tb1 . O103 . C102 . 133.1(4) yes C2 . O106 . Tb1 . 140.6(5) yes C2 . O106 . H1060 . 115.6 no Tb1 . O106 . H1060 . 102.2 no O18 . N19 . Mn4 . 114.6(3) yes O18 . N19 . C20 . 116.4(4) yes Mn4 . N19 . C20 . 129.0(4) yes Mn4 . O23 . C22 . 123.9(4) yes O34 . N33 . Mn3 . 114.2(3) yes O34 . N33 . C32 . 116.2(5) yes Mn3 . N33 . C32 . 129.0(4) yes O40 . N41 . Mn2 . 113.2(3) yes O40 . N41 . C42 . 115.8(5) yes Mn2 . N41 . C42 . 130.9(4) yes O54 . N55 . Mn6 . 113.9(3) yes O54 . N55 . C56 . 116.7(5) yes Mn6 . N55 . C56 . 129.4(4) yes O70 . N69 . Mn1 . 112.6(3) yes O70 . N69 . C68 . 116.5(4) yes Mn1 . N69 . C68 . 130.2(4) yes O82 . N81 . Mn5 . 113.6(3) yes O82 . N81 . C80 . 116.5(5) yes Mn5 . N81 . C80 . 129.7(4) yes O8 . C9 . H90 . 109.4 no O8 . C9 . H91 . 109.6 no H90 . C9 . H91 . 109.5 no O8 . C9 . H92 . 109.5 no H90 . C9 . H92 . 109.5 no H91 . C9 . H92 . 109.5 no O14 . C15 . H150 . 109.5 no O14 . C15 . H151 . 109.5 no H150 . C15 . H151 . 109.5 no O14 . C15 . H152 . 109.5 no H150 . C15 . H152 . 109.5 no H151 . C15 . H152 . 109.5 no N19 . C20 . C21 . 118.6(5) yes N19 . C20 . C28 . 120.4(5) yes C21 . C20 . C28 . 121.0(5) yes C20 . C21 . C22 . 121.7(5) yes C20 . C21 . C27 . 119.4(5) yes C22 . C21 . C27 . 118.8(5) yes C21 . C22 . O23 . 122.2(5) yes C21 . C22 . C24 . 119.0(5) yes O23 . C22 . C24 . 118.8(5) yes C22 . C24 . C25 . 120.7(6) yes C22 . C24 . H241 . 119.6 no C25 . C24 . H241 . 119.7 no C24 . C25 . C26 . 120.2(6) yes C24 . C25 . H251 . 119.9 no C26 . C25 . H251 . 119.9 no C25 . C26 . C27 . 119.8(6) yes C25 . C26 . H261 . 120.1 no C27 . C26 . H261 . 120.1 no C21 . C27 . C26 . 121.2(6) yes C21 . C27 . H271 . 119.4 no C26 . C27 . H271 . 119.4 no C20 . C28 . H281 . 109.4 no C20 . C28 . H282 . 109.4 no H281 . C28 . H282 . 109.5 no C20 . C28 . H283 . 109.5 no H281 . C28 . H283 . 109.5 no H282 . C28 . H283 . 109.5 no O29 . C30 . C31 . 122.4(5) yes O29 . C30 . C39 . 118.5(6) yes C31 . C30 . C39 . 119.1(6) yes C30 . C31 . C32 . 121.0(6) yes C30 . C31 . C36 . 117.7(6) yes C32 . C31 . C36 . 121.3(6) yes C31 . C32 . N33 . 118.5(5) yes C31 . C32 . C35 . 121.9(5) yes N33 . C32 . C35 . 119.6(5) yes C32 . C35 . H351 . 109.4 no C32 . C35 . H352 . 109.5 no H351 . C35 . H352 . 109.5 no C32 . C35 . H353 . 109.5 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no C31 . C36 . C37 . 123.6(7) yes C31 . C36 . H361 . 118.2 no C37 . C36 . H361 . 118.2 no C36 . C37 . C38 . 117.7(7) yes C36 . C37 . H371 . 121.1 no C38 . C37 . H371 . 121.2 no C37 . C38 . C39 . 120.2(6) yes C37 . C38 . H381 . 119.8 no C39 . C38 . H381 . 119.9 no C38 . C39 . C30 . 121.5(7) yes C38 . C39 . H391 . 119.2 no C30 . C39 . H391 . 119.3 no N41 . C42 . C50 . 118.2(6) yes N41 . C42 . C43 . 121.3(6) yes C50 . C42 . C43 . 120.4(6) yes C42 . C50 . H501 . 109.4 no C42 . C50 . H502 . 109.5 no H501 . C50 . H502 . 109.5 no C42 . C50 . H503 . 109.5 no H501 . C50 . H503 . 109.5 no H502 . C50 . H503 . 109.5 no O51 . C52 . H520 . 110.0 no O51 . C52 . H521 . 108.8 no H520 . C52 . H521 . 109.5 no O51 . C52 . H522 . 109.6 no H520 . C52 . H522 . 109.5 no H521 . C52 . H522 . 109.5 no O12 . C53 . H530 . 109.3 no O12 . C53 . H531 . 109.4 no H530 . C53 . H531 . 109.5 no O12 . C53 . H532 . 109.6 no H530 . C53 . H532 . 109.5 no H531 . C53 . H532 . 109.5 no N55 . C56 . C57 . 120.1(6) yes N55 . C56 . C64 . 119.0(6) yes C57 . C56 . C64 . 120.9(6) yes C56 . C57 . C58 . 122.0(5) yes C56 . C57 . C63 . 120.4(6) yes C58 . C57 . C63 . 117.5(6) yes C57 . C58 . O59 . 123.7(5) yes C57 . C58 . C60 . 118.6(6) yes O59 . C58 . C60 . 117.7(6) yes C58 . C60 . C61 . 123.3(7) yes C58 . C60 . H601 . 118.4 no C61 . C60 . H601 . 118.3 no C60 . C61 . C62 . 119.3(7) yes C60 . C61 . H611 . 120.4 no C62 . C61 . H611 . 120.3 no C61 . C62 . C63 . 118.9(6) yes C61 . C62 . H621 . 120.6 no C63 . C62 . H621 . 120.5 no C57 . C63 . C62 . 122.3(7) yes C57 . C63 . H631 . 118.9 no C62 . C63 . H631 . 118.8 no C56 . C64 . H641 . 109.5 no C56 . C64 . H642 . 109.5 no H641 . C64 . H642 . 109.5 no C56 . C64 . H643 . 109.4 no H641 . C64 . H643 . 109.5 no H642 . C64 . H643 . 109.5 no O65 . C66 . C67 . 124.8(5) yes O65 . C66 . C75 . 116.9(5) yes C67 . C66 . C75 . 118.3(6) yes C66 . C67 . C68 . 121.5(5) yes C66 . C67 . C72 . 119.1(6) yes C68 . C67 . C72 . 119.4(5) yes C67 . C68 . N69 . 121.2(5) yes C67 . C68 . C71 . 120.2(5) yes N69 . C68 . C71 . 118.6(5) yes C68 . C71 . H711 . 109.5 no C68 . C71 . H712 . 109.4 no H711 . C71 . H712 . 109.5 no C68 . C71 . H713 . 109.5 no H711 . C71 . H713 . 109.5 no H712 . C71 . H713 . 109.5 no C67 . C72 . C73 . 121.4(6) yes C67 . C72 . H721 . 119.2 no C73 . C72 . H721 . 119.4 no C72 . C73 . C74 . 118.9(6) yes C72 . C73 . H731 . 120.5 no C74 . C73 . H731 . 120.6 no C73 . C74 . C75 . 121.0(6) yes C73 . C74 . H741 . 119.5 no C75 . C74 . H741 . 119.5 no C66 . C75 . C74 . 121.3(6) yes C66 . C75 . H751 . 119.4 no C74 . C75 . H751 . 119.4 no O6 . C76 . H760 . 109.5 no O6 . C76 . H761 . 109.4 no H760 . C76 . H761 . 109.5 no O6 . C76 . H762 . 109.4 no H760 . C76 . H762 . 109.5 no H761 . C76 . H762 . 109.5 no O77 . C78 . C79 . 122.7(5) yes O77 . C78 . C87 . 116.9(6) yes C79 . C78 . C87 . 120.1(6) yes C78 . C79 . C80 . 122.7(6) yes C78 . C79 . C84 . 117.4(6) yes C80 . C79 . C84 . 119.8(6) yes C79 . C80 . N81 . 119.8(6) yes C79 . C80 . C83 . 120.3(6) yes N81 . C80 . C83 . 119.8(6) yes C80 . C83 . H831 . 109.5 no C80 . C83 . H832 . 109.4 no H831 . C83 . H832 . 109.5 no C80 . C83 . H833 . 109.5 no H831 . C83 . H833 . 109.5 no H832 . C83 . H833 . 109.5 no C79 . C84 . C85 . 120.9(7) yes C79 . C84 . H841 . 119.5 no C85 . C84 . H841 . 119.6 no C84 . C85 . C86 . 121.3(7) yes C84 . C85 . H851 . 119.3 no C86 . C85 . H851 . 119.4 no C85 . C86 . C87 . 119.9(7) yes C85 . C86 . H861 . 120.1 no C87 . C86 . H861 . 120.0 no C78 . C87 . C86 . 120.0(7) yes C78 . C87 . H871 . 119.9 no C86 . C87 . H871 . 120.1 no O88 . C89 . H890 . 109.9 no O88 . C89 . H891 . 109.7 no H890 . C89 . H891 . 109.5 no O88 . C89 . H892 . 108.7 no H890 . C89 . H892 . 109.5 no H891 . C89 . H892 . 109.5 no O90 . C91 . C92 . 123.9(6) yes O90 . C91 . C96 . 116.6(5) yes C92 . C91 . C96 . 119.5(6) yes C91 . C92 . C93 . 126.4(6) yes C91 . C92 . H921 . 116.8 no C93 . C92 . H921 . 116.7 no C92 . C93 . O94 . 124.7(6) yes C92 . C93 . C95 . 118.5(6) yes O94 . C93 . C95 . 116.7(6) yes C93 . C95 . H951 . 109.5 no C93 . C95 . H952 . 109.5 no H951 . C95 . H952 . 109.5 no C93 . C95 . H953 . 109.4 no H951 . C95 . H953 . 109.5 no H952 . C95 . H953 . 109.5 no C91 . C96 . H961 . 109.5 no C91 . C96 . H962 . 109.5 no H961 . C96 . H962 . 109.5 no C91 . C96 . H963 . 109.4 no H961 . C96 . H963 . 109.5 no H962 . C96 . H963 . 109.5 no O97 . C98 . H980 . 109.6 no O97 . C98 . H981 . 109.3 no H980 . C98 . H981 . 109.5 no O97 . C98 . H982 . 109.4 no H980 . C98 . H982 . 109.5 no H981 . C98 . H982 . 109.5 no O99 . C100 . C101 . 123.2(6) yes O99 . C100 . C105 . 115.0(6) yes C101 . C100 . C105 . 121.7(6) yes C100 . C101 . C102 . 128.0(6) yes C100 . C101 . H1011 . 116.0 no C102 . C101 . H1011 . 116.0 no C101 . C102 . O103 . 124.7(6) yes C101 . C102 . C104 . 120.2(6) yes O103 . C102 . C104 . 115.0(5) yes C102 . C104 . H1041 . 109.3 no C102 . C104 . H1042 . 109.5 no H1041 . C104 . H1042 . 109.5 no C102 . C104 . H1043 . 109.6 no H1041 . C104 . H1043 . 109.5 no H1042 . C104 . H1043 . 109.5 no C100 . C105 . H1051 . 109.5 no C100 . C105 . H1052 . 109.4 no H1051 . C105 . H1052 . 109.5 no C100 . C105 . H1053 . 109.5 no H1051 . C105 . H1053 . 109.5 no H1052 . C105 . H1053 . 109.5 no C481 . C491 . C43 . 123.4(13) yes C481 . C491 . H4911 . 118.3 no C43 . C491 . H4911 . 118.2 no C491 . C481 . C471 . 120.0(13) yes C491 . C481 . H4811 . 120.0 no C471 . C481 . H4811 . 120.0 no C481 . C471 . C461 . 117.8(14) yes C481 . C471 . H4711 . 121.0 no C461 . C471 . H4711 . 121.2 no C471 . C461 . C44 . 122.7(14) yes C471 . C461 . H4611 . 118.5 no C44 . C461 . H4611 . 118.7 no C461 . C44 . O45 . 117.3(8) yes C461 . C44 . C43 . 118.6(9) yes O45 . C44 . C43 . 123.2(6) yes C42 . C43 . C44 . 121.8(6) yes C42 . C43 . C491 . 120.7(8) yes C44 . C43 . C491 . 116.9(8) yes C43 . C490 . C480 . 119.6(14) yes C43 . C490 . H4901 . 120.3 no C480 . C490 . H4901 . 120.1 no C490 . C480 . C470 . 119.2(16) yes C490 . C480 . H4801 . 120.3 no C470 . C480 . H4801 . 120.4 no C480 . C470 . C460 . 120.5(16) yes C480 . C470 . H4701 . 119.6 no C460 . C470 . H4701 . 119.9 no C470 . C460 . C44 . 123.0(16) yes C470 . C460 . H4601 . 118.5 no C44 . C460 . H4601 . 118.5 no