#------------------------------------------------------------------------------ #$Date: 2026-06-18 00:07:14 +0100 (Thu, 18 Jun 2026) $ #$Revision: 306589 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/11/7721140.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7721140 loop_ _publ_author_name 'Diodati, Alexander' 'Brantley, ChristiAnna L' 'Peralta, Juan E.' 'Figueroa, Amelia' 'Dobrzycki, Lukasz' 'Abboud, Khalil A.' 'Christou, George' _publ_section_title ; Novel Fe4 cluster topology from a new hexadentate chelate: magnetic analysis by experimental, DFT, and magnetostructural correlation methods. ; _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_paper_doi 10.1039/d6dt01053a _journal_year 2026 _chemical_absolute_configuration ad _chemical_formula_sum 'C37 H56.4 Ce Fe2 N14 O24.7' _chemical_formula_weight 1344.38 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary 'Intrinsic Phasing' _audit_creation_method ;FinalCif 2024.9-0 by Daniel Kratzert, Freiburg 2026, https://dkratzert.de/finalcif.html ; _audit_update_record ; 2026-05-22 deposited with the CCDC. 2026-05-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.6621(3) _cell_length_b 16.9239(4) _cell_length_c 19.0133(4) _cell_measurement_reflns_used 9834 _cell_measurement_temperature 100.14999999999998 _cell_measurement_theta_max 28.2838 _cell_measurement_theta_min 2.7359 _cell_measurement_wavelength 0.71073 _cell_volume 5039.74(19) _computing_cell_refinement 'SAINT V8.41 (Bruker AXS LLC)' _computing_data_collection 'APEX5 V2023.9-4 (Bruker AXS, 2023)' _computing_data_reduction 'SAINT V8.41 (Bruker AXS LLC)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 1503)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick G. M., 2015)' _computing_structure_solution 'SHELXT-2018/2 (Sheldrick G. M., 2015)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'charge integrating pixel array detector' _diffrn_detector_area_resol_mean 7.391 _diffrn_detector_type 'Bruker PHOTON III' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ;[mo_diod115_01_####.sfrm, Phi run, Counterclockwise Eulerian angles: dx= 70.00 mm theta= 0.000 deg phi= 0.000 deg omega= 0.000 deg chi= 54.740 deg, width= 1.000, images= 180, first= 1, secs/image= 1.000, secs/degree= 1.000, wavelength= 0.71073, kilovolts= 50.000, milliamps= 1.400, temperature= 100.0] [mo_diod115_02_####.sfrm, Phi run, Counterclockwise Eulerian angles: dx= 70.00 mm theta= 0.000 deg phi= 180.000 deg omega= 0.000 deg chi= 54.740 deg, width= 1.000, images= 180, first= 1, secs/image= 1.000, secs/degree= 1.000, wavelength= 0.71073, kilovolts= 50.000, milliamps= 1.401, temperature= 100.0] [mo_diod115_03_####.sfrm, Omega run, Counterclockwise Eulerian angles: dx= 70.00 mm theta= 9.819 deg phi= 360.000 deg omega= 358.373 deg chi= -44.500 deg, width= 0.500, images= 272, first= 1, secs/image= 5.000, secs/degree= 10.000, wavelength= 0.71073, kilovolts= 50.000, milliamps= 1.401, temperature= 100.0] [mo_diod115_04_####.sfrm, Phi run, Counterclockwise Eulerian angles: dx= 70.00 mm theta= 9.819 deg phi= 345.267 deg omega= 358.373 deg chi= -44.500 deg, width= 0.500, images= 269, first= 1, secs/image= 5.000, secs/degree= 10.000, wavelength= 0.71073, kilovolts= 50.000, milliamps= 1.400, temperature= 100.0] [mo_diod115_05_####.sfrm, Omega run, Counterclockwise Eulerian angles: dx= 70.00 mm theta= 9.819 deg phi= 51.001 deg omega= 358.373 deg chi= -44.500 deg, width= 0.500, images= 272, first= 1, secs/image= 5.000, secs/degree= 10.000, wavelength= 0.71073, kilovolts= 50.000, milliamps= 1.402, temperature= 100.0] [mo_diod115_06_####.sfrm, Phi run, Counterclockwise Eulerian angles: dx= 70.00 mm theta= 9.819 deg phi= 103.567 deg omega= 340.647 deg chi= -24.000 deg, width= -0.500, images= 269, first= 1, secs/image= 5.000, secs/degree= 10.000, wavelength= 0.71073, kilovolts= 50.000, milliamps= 1.400, temperature= 100.0] ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER D8 Venture with PHOTON III' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'HELIOS multilayer optics' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_unetI/netI 0.0272 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 76464 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_reduction_process narrow-frame _diffrn_reflns_theta_full 28.299 _diffrn_reflns_theta_max 28.299 _diffrn_reflns_theta_min 2.07 _diffrn_source 'micro-focus X-ray tube' _diffrn_source_current 1.4 _diffrn_source_target Mo _diffrn_source_type 'INCOATEC I\mS 3.0' _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 1.557 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_correction_T_min 0.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.772 _exptl_crystal_description plate _exptl_crystal_F_000 2736 _exptl_crystal_size_max 0.199 _exptl_crystal_size_mid 0.111 _exptl_crystal_size_min 0.108 _refine_diff_density_max 1.063 _refine_diff_density_min -0.955 _refine_diff_density_rms 0.074 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.546(12) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 866 _refine_ls_number_reflns 12503 _refine_ls_number_restraints 161 _refine_ls_restrained_S_all 1.103 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0312 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+5.7570P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.0709 _reflns_Friedel_coverage 0.826 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 11849 _reflns_number_total 12503 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt01053a2.cif _cod_data_source_block diod115 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_original_formula_sum 'C37 H56.40 Ce Fe2 N14 O24.70' _cod_database_code 7721140 _shelx_shelxl_version_number 2019/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _exptl_bruker_absorpt_correction_t_ratio 0.864 _shelx_estimated_absorpt_t_min 0.747 _shelx_estimated_absorpt_t_max 0.850 _bruker_diffrn_measurement_temperature_device 'Oxford Cryostream 800' _diffrn_measurement_bruker_total_exposure_time 5770.0 _diffrn_reflns_bruker_av_norm_i 2508.44 _diffrn_reflns_bruker_number_gt 68809 _computing_bruker_data_scaling 'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction' _geom_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. ; _shelx_res_file ; TITL diod115 in P2(1)2(1)2(1) mo_diod115_0m_a.res created by SHELXL-2019/3 at 16:29:09 on 20-May-2026 CELL 0.71073 15.6621 16.9239 19.0133 90.000 90.000 90.000 ZERR 4.000 0.0003 0.0004 0.0004 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H CE FE N O UNIT 148 225.6 4 8 56 98.8 LIST 4 TEMP -173.150 L.S. 11 SIZE 0.108 0.111 0.199 OMIT -2 56.6 ACTA 56.6 BOND $H HTAB EQIV $1 -x, y+1/2, -z+3/2 HTAB O2 O3 HTAB O3B O2B HTAB O4 O14 HTAB O5 N11 HTAB O5 O13 HTAB O5 O14 HTAB O5' O23'_$1 HTAB O311 O22 HTAB O312 N9' HTAB O312 O6' HTAB O312 O22' HTAB O1W O311 FMAP 2 TWIN -1 0 0 0 -1 0 0 0 -1 PLAN 20 SADI 0.01 Ce1 O6 Ce1 O6' SADI 0.01 Ce1 O7 Ce1 O7' SIMU 0.01 0.01 2 N9 N9' SIMU 0.01 0.01 2 O8 O8' SADI 0.01 Ce1 O9 Ce1 O9' SADI 0.01 Ce1 O10 Ce1 O10' SIMU 0.01 0.01 2 N10 N10' SADI 0.01 Ce1 O12 Ce1 O12' SADI 0.01 Ce1 O13 Ce1 O13' SIMU 0.01 0.01 2 O14 O14' SIMU 0.01 0.01 2 O13 O13' SADI 0.01 Ce1 O15 Ce1 O15' SADI 0.01 Ce1 O16 Ce1 O16' SIMU 0.01 0.01 2 O17 O17' SADI 0.01 Ce1 O18 Ce1 O18' SADI 0.01 Ce1 O19 Ce1 O19' SIMU 0.01 0.01 2 N13 N13' SIMU 0.01 0.01 2 O20 O20' SADI 0.01 Ce1 O21 Ce1 O21' SADI 0.01 Ce1 O22 Ce1 O22' EXYZ N6 N6' EADP N6 N6' EXYZ N7' N7" EADP N7' N7" EXYZ C38' C38" EADP C38' C38" SADI 0.01 C25 C26 C25 C26' SADI 0.01 Fe2 N7 Fe2 N7' SIMU 0.01 0.01 2 C26 C26' SIMU 0.01 0.01 2 C37' C37" C37 SIMU 0.01 0.01 2 C28' C28 SADI O312 C312 O311 C311 EXYZ O2 O2B EADP O2 O2B EXYZ O3 O3B EADP O3 O3B DFIX 0.95 0.01 O2 H2O O3B H3OB DFIX 1.47 0.01 O2B H3OB O3 H2O DFIX 0.95 0.01 O1W H1WA O1W H1WB DFIX 1.5 0.01 H1WA H1WB WGHT 0.026500 5.757000 BASF 0.54585 FVAR 0.29122 CE1 3 0.238882 0.205320 0.688625 11.00000 0.01566 0.02187 = 0.02523 0.00389 0.00027 -0.00217 FE1 4 0.277118 0.702979 0.603544 11.00000 0.03144 0.01610 = 0.01669 -0.00158 -0.00410 0.00022 FE2 4 0.271920 0.701580 0.776747 11.00000 0.01796 0.01422 = 0.01730 -0.00057 -0.00038 -0.00167 O1 6 0.238067 0.675445 0.689421 11.00000 0.02294 0.01656 = 0.02137 -0.00248 -0.00314 -0.00092 PART 1 10.5 O2 6 0.356553 0.788032 0.628916 10.50000 0.03859 0.01955 = 0.01677 -0.00041 0.00057 -0.01014 H2O 2 0.366110 0.795413 0.677999 10.50000 -1.50000 O3 6 0.365823 0.776209 0.753613 10.50000 0.02184 0.01986 = 0.01819 -0.00141 -0.00182 -0.00632 PART 2 10.5 O2B 6 0.356553 0.788032 0.628916 10.50000 0.03859 0.01955 = 0.01677 -0.00041 0.00057 -0.01014 O3B 6 0.365823 0.776209 0.753613 10.50000 0.02184 0.01986 = 0.01819 -0.00141 -0.00182 -0.00632 H3OB 2 0.370753 0.792850 0.705808 10.50000 -1.50000 PART 0 O4 6 0.103648 0.464228 0.507030 11.00000 0.05145 0.02295 = 0.03739 -0.00669 -0.00824 -0.00324 AFIX 83 H4A 2 0.115070 0.449477 0.548151 11.00000 -1.50000 AFIX 0 N1 5 0.377838 0.617606 0.600033 11.00000 0.03241 0.02044 = 0.01765 -0.00238 0.00156 -0.00107 N2 5 0.221876 0.609285 0.533530 11.00000 0.03285 0.01962 = 0.02219 -0.00378 -0.00555 0.00269 N3 5 0.315020 0.751970 0.498126 11.00000 0.04576 0.02285 = 0.02031 0.00000 -0.00140 -0.00259 N4 5 0.172511 0.779732 0.580021 11.00000 0.04060 0.01752 = 0.02408 -0.00009 -0.01538 -0.00181 N5 5 0.343250 0.593048 0.787154 11.00000 0.02231 0.01651 = 0.01809 0.00015 0.00226 0.00149 N8 5 0.185968 0.800635 0.785834 11.00000 0.01978 0.01663 = 0.02069 -0.00237 -0.00174 -0.00250 PART 1 10.9 N9 5 0.319512 0.042670 0.697486 10.90000 0.02086 0.02614 = 0.03877 0.00981 0.00896 -0.00111 O6 6 0.260348 0.057121 0.654083 10.90000 0.02786 0.02477 = 0.03266 0.00343 0.00161 -0.00045 O7 6 0.341827 0.098836 0.737810 10.90000 0.02750 0.03061 = 0.04265 0.01300 -0.00758 -0.00059 O8 6 0.354174 -0.022459 0.699859 10.90000 0.02810 0.02553 = 0.08036 0.01828 0.00841 0.00357 PART 2 10.1 SAME N9 O6 O7 O8 FLAT N9' O6' O7' O8' N9' 5 0.325334 0.041826 0.690185 10.10000 0.02511 O6' 6 0.346219 0.096035 0.648001 10.10000 0.03572 O7' 6 0.272239 0.064322 0.736341 10.10000 0.04113 O8' 6 0.353466 -0.025649 0.686439 10.10000 0.03873 PART 0 PART 1 10.9 N10 5 0.374249 0.257341 0.583272 10.90000 0.01912 0.04071 = 0.03939 0.01591 -0.00190 -0.00765 O9 6 0.370528 0.185830 0.605203 10.90000 0.02239 0.02815 = 0.03330 0.00842 0.00677 -0.00145 O10 6 0.316487 0.303858 0.600763 10.90000 0.02179 0.03094 = 0.03068 0.00993 0.00251 -0.00164 O11 6 0.434058 0.280434 0.547025 10.90000 0.03065 0.04225 = 0.05452 0.01801 0.01560 -0.00879 PART 2 10.1 SAME N10 O9 O10 O11 FLAT N10' O9' O10' O11' N10' 5 0.378235 0.250893 0.582883 10.10000 0.03307 O9' 6 0.384749 0.266872 0.649199 10.10000 0.06207 O10' 6 0.307354 0.224429 0.562895 10.10000 0.07130 O11' 6 0.426902 0.255145 0.531833 10.10000 0.03355 PART 0 PART 1 10.9 N11 5 0.162973 0.371473 0.668084 10.90000 0.02198 0.02729 = 0.03746 0.01308 0.00398 -0.00128 O12 6 0.143232 0.316319 0.628102 10.90000 0.02156 0.02697 = 0.03428 0.00434 -0.00248 -0.00184 O13 6 0.210165 0.357503 0.718966 10.90000 0.02019 0.02928 = 0.05437 0.00445 -0.00351 -0.00313 O14 6 0.134797 0.439804 0.657392 10.90000 0.03249 0.02344 = 0.04477 0.00996 0.00432 0.00172 PART 2 10.1 SAME N11 O12 O13 O14 FLAT N11' O12' O13' O14' N11' 5 0.162801 0.370663 0.720172 10.10000 0.02755 O12' 6 0.134800 0.310455 0.748257 10.10000 0.06847 O13' 6 0.241273 0.360136 0.717292 10.10000 0.03367 O14' 6 0.140123 0.438482 0.701157 10.10000 0.04983 PART 0 PART 1 10.9 N12 5 0.364221 0.262134 0.801324 10.90000 0.03179 0.01897 = 0.02489 0.00828 -0.00544 0.00171 O15 6 0.288140 0.240088 0.814724 10.90000 0.02848 0.03620 = 0.02135 0.00526 -0.00011 -0.00769 O16 6 0.384608 0.266063 0.737479 10.90000 0.02241 0.02646 = 0.03090 0.00602 0.00080 -0.00397 O17 6 0.415379 0.278678 0.848547 10.90000 0.03696 0.03470 = 0.03683 -0.00070 -0.01420 0.00212 PART 2 10.1 SAME N12 O15 O16 O17 FLAT N12' O15' O16' O17' N12' 5 0.365104 0.248284 0.811221 10.10000 0.01799 O15' 6 0.303606 0.289938 0.789704 10.10000 0.04186 O16' 6 0.364173 0.181383 0.782467 10.10000 0.05929 O17' 6 0.417199 0.267132 0.856254 10.10000 0.03294 PART 0 PART 1 10.9 N13 5 0.100134 0.164159 0.796390 10.90000 0.03286 0.03603 = 0.03520 -0.00907 0.01233 -0.00771 O18 6 0.163362 0.119218 0.783485 10.90000 0.03472 0.02389 = 0.02960 0.00427 0.00728 -0.00294 O19 6 0.100974 0.231690 0.767096 10.90000 0.03223 0.02622 = 0.03853 0.00071 0.01098 0.00153 O20 6 0.042312 0.141103 0.835403 10.90000 0.05022 0.04764 = 0.05460 -0.01251 0.03523 -0.01744 PART 2 10.1 SAME N13 O18 O19 O20 FLAT N13' O18' O19' O20' N13' 5 0.104769 0.156474 0.799394 10.10000 0.03688 O18' 6 0.182390 0.170372 0.814560 10.10000 0.05617 O19' 6 0.095257 0.137441 0.735327 10.10000 0.04670 O20' 6 0.047826 0.161832 0.843646 10.10000 0.04531 PART 0 PART 1 10.9 N14 5 0.120212 0.135519 0.576658 10.90000 0.02358 0.02107 = 0.02679 0.00658 -0.00416 -0.00339 O21 6 0.098855 0.140234 0.640014 10.90000 0.01748 0.03299 = 0.03046 0.00155 0.00049 -0.00478 O22 6 0.190432 0.167678 0.559076 10.90000 0.02646 0.02771 = 0.02376 0.00306 0.00174 -0.00551 O23 6 0.074779 0.101740 0.533644 10.90000 0.04625 0.03436 = 0.03192 0.01057 -0.01899 -0.01470 PART 2 10.1 SAME N14 O21 O22 O23 FLAT N14' O21' O22' O23' N14' 5 0.120445 0.144379 0.579357 10.10000 0.04770 O21' 6 0.112573 0.214256 0.599994 10.10000 0.03810 O22' 6 0.173877 0.095540 0.605447 10.10000 0.04170 O23' 6 0.072317 0.122938 0.532289 10.10000 0.02763 PART 0 C1 1 0.454755 0.628438 0.631028 11.00000 0.03203 0.02767 = 0.02168 -0.00110 -0.00099 -0.00556 AFIX 43 H1 2 0.466680 0.677991 0.652346 11.00000 -1.20000 AFIX 0 C2 1 0.516471 0.570391 0.632878 11.00000 0.02897 0.03200 = 0.02609 0.00304 -0.00045 -0.00059 AFIX 43 H2 2 0.569348 0.578932 0.656147 11.00000 -1.20000 AFIX 0 C3 1 0.499043 0.498951 0.599674 11.00000 0.03850 0.02390 = 0.02804 0.00297 0.00291 0.00910 AFIX 43 H3 2 0.541236 0.458656 0.598224 11.00000 -1.20000 AFIX 0 C4 1 0.420509 0.486696 0.568886 11.00000 0.03860 0.02158 = 0.02051 -0.00244 0.00219 0.00001 AFIX 43 H4 2 0.407489 0.437756 0.546890 11.00000 -1.20000 AFIX 0 C5 1 0.360722 0.547342 0.570646 11.00000 0.03234 0.02045 = 0.01644 0.00055 0.00279 -0.00016 C6 1 0.271106 0.534798 0.544882 11.00000 0.03463 0.01839 = 0.02339 -0.00475 -0.00509 0.00140 AFIX 23 H6A 2 0.273274 0.505178 0.500017 11.00000 -1.20000 H6B 2 0.240180 0.501726 0.579459 11.00000 -1.20000 AFIX 0 C7 1 0.229376 0.639143 0.459695 11.00000 0.05377 0.02659 = 0.01791 -0.00399 -0.00924 0.00534 AFIX 23 H7A 2 0.180761 0.674657 0.449296 11.00000 -1.20000 H7B 2 0.226718 0.594022 0.426629 11.00000 -1.20000 AFIX 0 C8 1 0.312489 0.683557 0.448857 11.00000 0.05478 0.02896 = 0.01854 -0.00097 -0.00068 -0.00128 AFIX 23 H8A 2 0.361497 0.648062 0.457977 11.00000 -1.20000 H8B 2 0.316342 0.702476 0.399688 11.00000 -1.20000 AFIX 0 C9 1 0.256242 0.816643 0.476086 11.00000 0.05612 0.02348 = 0.02377 0.00569 -0.01089 -0.00545 AFIX 23 H9A 2 0.231262 0.802955 0.429833 11.00000 -1.20000 H9B 2 0.289745 0.865786 0.470075 11.00000 -1.20000 AFIX 0 C10 1 0.184099 0.832288 0.527875 11.00000 0.04360 0.02634 = 0.02182 -0.00055 -0.01463 -0.00103 C11 1 0.130124 0.896881 0.520259 11.00000 0.05207 0.03964 = 0.04464 0.02004 -0.01262 0.00488 AFIX 43 H11 2 0.140727 0.935123 0.484740 11.00000 -1.20000 AFIX 0 C12 1 0.061178 0.905049 0.564557 11.00000 0.05006 0.04689 = 0.05919 0.01610 -0.01538 0.01662 AFIX 43 H12 2 0.024192 0.949269 0.560197 11.00000 -1.20000 AFIX 0 C13 1 0.046161 0.848251 0.615559 11.00000 0.03474 0.04218 = 0.04227 0.00149 -0.01106 0.00757 AFIX 43 H13 2 -0.002830 0.851118 0.644908 11.00000 -1.20000 AFIX 0 C14 1 0.103943 0.787670 0.622602 11.00000 0.03819 0.02692 = 0.02820 -0.00198 -0.01129 0.00119 AFIX 43 H14 2 0.095354 0.749858 0.658847 11.00000 -1.20000 AFIX 0 C15 1 0.402233 0.782618 0.509813 11.00000 0.04547 0.02958 = 0.02184 0.00364 0.00368 -0.00562 AFIX 23 H15A 2 0.420002 0.815775 0.469491 11.00000 -1.20000 H15B 2 0.442996 0.738189 0.514256 11.00000 -1.20000 AFIX 0 C16 1 0.402079 0.831649 0.577196 11.00000 0.04569 0.02869 = 0.01991 0.00642 -0.00079 -0.01176 AFIX 23 H16A 2 0.461333 0.841435 0.593100 11.00000 -1.20000 H16B 2 0.374020 0.883226 0.568871 11.00000 -1.20000 AFIX 0 C17 1 0.130469 0.597821 0.554339 11.00000 0.03257 0.02206 = 0.03380 -0.00694 -0.00742 0.00147 AFIX 23 H17A 2 0.102769 0.650381 0.555650 11.00000 -1.20000 H17B 2 0.129412 0.576512 0.602822 11.00000 -1.20000 AFIX 0 C18 1 0.076400 0.543905 0.508167 11.00000 0.04059 0.02246 = 0.03639 -0.00432 -0.01267 -0.00050 AFIX 23 H18A 2 0.016630 0.545743 0.525032 11.00000 -1.20000 H18B 2 0.077119 0.564640 0.459482 11.00000 -1.20000 AFIX 0 C21 1 0.329680 0.528155 0.747461 11.00000 0.02815 0.02125 = 0.02187 -0.00061 0.00005 -0.00047 AFIX 43 H21 2 0.283637 0.528675 0.714938 11.00000 -1.20000 AFIX 0 C22 1 0.379039 0.461671 0.751812 11.00000 0.03783 0.02096 = 0.02145 -0.00047 0.00746 0.00188 AFIX 43 H22 2 0.367038 0.416597 0.723721 11.00000 -1.20000 AFIX 0 C23 1 0.447211 0.461999 0.798499 11.00000 0.03157 0.02272 = 0.03038 0.00640 0.01070 0.00830 AFIX 43 H23 2 0.483400 0.417147 0.802240 11.00000 -1.20000 AFIX 0 C24 1 0.461948 0.527550 0.839193 11.00000 0.02054 0.02827 = 0.02745 0.00816 0.00165 0.00339 AFIX 43 H24 2 0.508333 0.528444 0.871378 11.00000 -1.20000 AFIX 0 C25 1 0.408306 0.592701 0.832871 11.00000 0.02356 0.02000 = 0.02048 0.00404 0.00366 -0.00145 PART 1 10.7 C26 1 0.426957 0.668942 0.869477 10.70000 0.03469 0.02075 = 0.02107 0.00622 -0.01216 -0.00305 AFIX 23 H26A 2 0.469841 0.699273 0.842377 10.70000 -1.20000 H26B 2 0.450745 0.658196 0.916760 10.70000 -1.20000 AFIX 0 N6 5 0.345622 0.716742 0.876223 10.70000 0.02911 0.01903 = 0.01715 -0.00213 -0.00102 -0.00570 C27 1 0.298817 0.686952 0.938293 10.70000 0.04380 0.02010 = 0.01367 0.00040 -0.00087 -0.00342 AFIX 23 H27A 2 0.318031 0.714619 0.981354 10.70000 -1.20000 H27B 2 0.308893 0.629605 0.944352 10.70000 -1.20000 AFIX 0 C28 1 0.206642 0.702590 0.925276 10.70000 0.03602 0.02923 = 0.02048 0.00341 0.00561 -0.00354 AFIX 23 H28A 2 0.197254 0.760404 0.923517 10.70000 -1.20000 H28B 2 0.172947 0.681357 0.965069 10.70000 -1.20000 AFIX 0 N7 5 0.174610 0.666077 0.857527 10.70000 0.01655 0.01741 = 0.02602 0.00525 0.00369 -0.00399 C37 1 0.160590 0.580880 0.871392 10.70000 0.03359 0.02551 = 0.02781 0.00315 0.00391 -0.00576 AFIX 23 H37A 2 0.124780 0.575670 0.914048 10.70000 -1.20000 H37B 2 0.216460 0.556110 0.881732 10.70000 -1.20000 AFIX 0 C38 1 0.118803 0.535603 0.812663 10.70000 0.04012 0.02902 = 0.03176 0.00392 0.00182 -0.00226 AFIX 23 H38A 2 0.057267 0.548643 0.810018 10.70000 -1.20000 H38B 2 0.145702 0.549031 0.767085 10.70000 -1.20000 AFIX 0 O5 6 0.130146 0.453500 0.827930 10.70000 0.05508 0.02165 = 0.04833 0.00063 0.00900 -0.00972 AFIX 83 H5A 2 0.154156 0.431281 0.793732 10.70000 -1.50000 AFIX 0 PART 2 10.3 SAME C26 N6 C27 C28 N7 C37 C38 O5 C26' 1 0.415522 0.662087 0.881792 10.30000 0.02840 AFIX 23 H26C 2 0.418614 0.642411 0.930761 10.30000 -1.20000 H26D 2 0.469419 0.690461 0.871682 10.30000 -1.20000 AFIX 0 N6' 5 0.345622 0.716742 0.876223 10.30000 0.02911 0.01903 = 0.01715 -0.00213 -0.00102 -0.00570 C27' 1 0.271757 0.706852 0.930636 10.30000 0.02307 AFIX 23 H27C 2 0.295954 0.698875 0.978212 10.30000 -1.20000 H27D 2 0.236421 0.755345 0.931506 10.30000 -1.20000 AFIX 0 C28' 1 0.216365 0.636148 0.910817 10.30000 0.01532 AFIX 23 H28C 2 0.252735 0.588434 0.907673 10.30000 -1.20000 H28D 2 0.173637 0.627120 0.948337 10.30000 -1.20000 AFIX 0 PART 2 10.15 N7' 5 0.171846 0.647611 0.843415 10.15000 0.02494 C37' 1 0.125951 0.588895 0.805535 10.15000 0.01708 AFIX 23 H37C 2 0.167770 0.560628 0.775679 10.15000 -1.20000 H37D 2 0.086576 0.616900 0.773322 10.15000 -1.20000 AFIX 0 C38' 1 0.074380 0.527163 0.843310 10.15000 0.01851 AFIX 23 H38D 2 0.014265 0.534181 0.828480 10.15000 -1.20000 H38C 2 0.093050 0.475172 0.825062 10.15000 -1.20000 AFIX 0 O5' 6 0.074331 0.521944 0.913930 10.15000 0.02633 AFIX 83 H5'A 2 0.031746 0.546050 0.930080 10.15000 -1.50000 AFIX 0 PART 3 10.15 SAME N7 C37 C38 O5 N7" 5 0.171846 0.647611 0.843415 10.15000 0.02494 C37" 1 0.153097 0.571102 0.811560 10.15000 0.01714 AFIX 23 H37E 2 0.203926 0.536800 0.816636 10.15000 -1.20000 H37F 2 0.143130 0.578995 0.760624 10.15000 -1.20000 AFIX 0 C38" 1 0.074380 0.527163 0.843310 10.15000 0.01851 AFIX 23 H38E 2 0.041198 0.560146 0.876508 10.15000 -1.20000 H38F 2 0.036401 0.504172 0.807066 10.15000 -1.20000 AFIX 0 O5" 6 0.127204 0.468618 0.878223 10.15000 0.02561 AFIX 83 H5"A 2 0.150186 0.439366 0.847966 10.15000 -1.50000 AFIX 0 PART 0 PART 0 C29 1 0.094882 0.705193 0.843884 11.00000 0.02455 0.03230 = 0.05433 0.01314 0.00950 -0.00143 AFIX 23 H29A 2 0.059601 0.705676 0.887086 11.00000 -1.20000 H29B 2 0.063091 0.676451 0.806859 11.00000 -1.20000 AFIX 0 C30 1 0.112207 0.789248 0.820137 11.00000 0.02368 0.02331 = 0.02647 0.00186 0.00213 -0.00059 C31 1 0.052345 0.849364 0.828112 11.00000 0.02426 0.03787 = 0.04721 0.00220 0.00709 0.00670 AFIX 43 H31 2 0.001032 0.840302 0.853505 11.00000 -1.20000 AFIX 0 C32 1 0.068548 0.922057 0.798706 11.00000 0.02911 0.02699 = 0.04992 -0.00449 -0.00270 0.01017 AFIX 43 H32 2 0.028726 0.963983 0.803982 11.00000 -1.20000 AFIX 0 C33 1 0.142739 0.933546 0.761664 11.00000 0.02976 0.01807 = 0.04465 -0.00106 -0.00221 -0.00053 AFIX 43 H33 2 0.154238 0.982836 0.739712 11.00000 -1.20000 AFIX 0 C34 1 0.199950 0.872378 0.756995 11.00000 0.02700 0.01858 = 0.02993 -0.00070 -0.00132 -0.00326 AFIX 43 H34 2 0.251865 0.880910 0.732297 11.00000 -1.20000 AFIX 0 C35 1 0.368184 0.801717 0.877531 11.00000 0.02515 0.01867 = 0.02466 -0.00620 -0.00240 -0.00295 AFIX 23 H35A 2 0.409844 0.812165 0.915570 11.00000 -1.20000 H35B 2 0.316543 0.833948 0.886395 11.00000 -1.20000 AFIX 0 C36 1 0.406726 0.823265 0.806640 11.00000 0.02811 0.01885 = 0.02163 -0.00011 -0.00453 -0.00851 AFIX 23 H36A 2 0.397693 0.880105 0.796838 11.00000 -1.20000 H36B 2 0.468911 0.812778 0.806898 11.00000 -1.20000 AFIX 0 PART 1 10.7 O311 6 0.296051 0.092385 0.461251 10.70000 0.08563 0.05677 = 0.04452 -0.00119 0.00310 0.03344 AFIX 83 H311 2 0.290403 0.135757 0.482223 10.70000 -1.50000 AFIX 0 C311 1 0.367966 0.054687 0.485429 10.70000 0.09329 0.04308 = 0.04239 -0.00362 0.01026 0.03321 AFIX 137 H31A 2 0.412110 0.093921 0.496141 10.70000 -1.50000 H31B 2 0.389064 0.018328 0.449272 10.70000 -1.50000 H31C 2 0.354029 0.024916 0.528122 10.70000 -1.50000 AFIX 0 PART 2 10.3 O312 6 0.322996 -0.000836 0.520782 10.30000 0.04740 AFIX 83 H312 2 0.305432 0.028431 0.553399 10.30000 -1.50000 AFIX 0 C312 1 0.328413 0.041031 0.461206 10.30000 0.07621 AFIX 133 H31D 2 0.272374 0.063459 0.449930 10.30000 -1.50000 H31E 2 0.346931 0.006443 0.422785 10.30000 -1.50000 H31F 2 0.369900 0.083836 0.467292 10.30000 -1.50000 AFIX 0 PART 1 10.7 O1W 6 0.208902 -0.011252 0.379802 10.70000 0.08243 0.07516 = 0.06022 0.00263 0.00426 -0.02094 H1WA 2 0.238200 0.020678 0.413915 10.70000 -1.50000 H1WB 2 0.225633 0.012262 0.336132 10.70000 -1.50000 PART 0 HKLF 4 REM diod115 in P2(1)2(1)2(1) REM wR2 = 0.0709, GooF = S = 1.089, Restrained GooF = 1.103 for all data REM R1 = 0.0312 for 11849 Fo > 4sig(Fo) and 0.0336 for all 12503 data REM 866 parameters refined using 161 restraints END WGHT 0.0265 5.7571 REM Instructions for potential hydrogen bonds HTAB O2 O3 HTAB O3 O2 HTAB O3B O2B HTAB O4 O14 HTAB C1 O2 EQIV $2 -x+1, y+1/2, -z+3/2 HTAB C1 O17_$2 HTAB C1 O17'_$2 HTAB C2 O7_$2 HTAB C2 O16'_$2 EQIV $3 x+1/2, -y+1/2, -z+1 HTAB C2 O1W_$3 HTAB C6 O14 EQIV $4 -x+1/2, -y+1, z-1/2 HTAB C7 O17_$4 HTAB C7 O17'_$4 HTAB C8 O5"_$4 HTAB C8 O15_$4 HTAB C9 O15_$4 HTAB C9 O18'_$4 EQIV $5 x, y+1, z HTAB C9 O312_$5 HTAB C11 O1W_$5 HTAB C14 O1 HTAB C15 O20'_$4 HTAB C16 O17_$2 HTAB C17 N4 HTAB C17 O14 HTAB C22 O13 HTAB C22 O13' HTAB C22 O16 HTAB C24 O6'_$2 HTAB C24 O8'_$2 EQIV $6 -x+1/2, -y+1, z+1/2 HTAB C27 O22_$6 HTAB C27 O4_$6 HTAB C28 O311_$6 HTAB C28 N10_$6 HTAB C28 O10_$6 HTAB C28 O11_$6 HTAB O5 N11 HTAB O5 O13 HTAB O5 O14 HTAB C26' O4_$6 HTAB C26' O9'_$2 HTAB C28' O5' HTAB C37' O14' HTAB C38' O14' HTAB O5' O23'_$1 HTAB C37" N5 HTAB C37" O1 HTAB C31 N11_$1 HTAB C31 O12_$1 HTAB C33 O6_$5 HTAB C33 O7'_$5 HTAB C33 O18_$5 HTAB C34 O3 HTAB C34 O8_$5 HTAB C34 O8'_$5 HTAB C35 O11_$2 HTAB C35 O311_$6 HTAB C36 O8_$5 HTAB C36 O16_$2 HTAB O311 O22 HTAB O312 N9' HTAB O312 O6' HTAB O312 O22' HTAB O1W O311 REM Highest difference peak 1.063, deepest hole -0.955, 1-sigma level 0.074 Q1 1 0.2347 0.1901 0.7273 11.00000 0.05 1.06 Q2 1 0.2727 0.1839 0.7138 11.00000 0.05 0.72 Q3 1 0.2800 0.1885 0.6696 11.00000 0.05 0.61 Q4 1 0.2728 0.2378 0.7008 11.00000 0.05 0.55 Q5 1 0.1815 0.2057 0.6891 11.00000 0.05 0.48 Q6 1 0.2189 0.6156 0.4322 11.00000 0.05 0.45 Q7 1 0.2680 0.8124 0.4064 11.00000 0.05 0.43 Q8 1 0.2161 0.3592 0.6659 11.00000 0.05 0.43 Q9 1 0.2780 0.2011 0.8590 11.00000 0.05 0.42 Q10 1 0.2207 0.6996 0.7480 11.00000 0.05 0.38 Q11 1 0.2359 0.6811 0.5876 11.00000 0.05 0.37 Q12 1 0.2390 0.4020 0.7169 11.00000 0.05 0.37 Q13 1 0.1462 0.4332 0.7381 11.00000 0.05 0.36 Q14 1 0.2936 0.0001 0.5079 11.00000 0.05 0.36 Q15 1 0.2622 0.1121 0.5176 11.00000 0.05 0.36 Q16 1 0.2569 0.7174 0.8137 11.00000 0.05 0.35 Q17 1 0.2584 0.7963 0.9438 11.00000 0.05 0.33 Q18 1 0.1593 0.7973 0.8229 11.00000 0.05 0.32 Q19 1 0.2253 0.7210 0.7981 11.00000 0.05 0.32 Q20 1 0.3007 0.7915 0.4442 11.00000 0.05 0.30 ; _shelx_res_checksum 17886 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.23888(2) 0.20532(2) 0.68862(2) 0.02092(6) Uani 1 1 d D . . . . Fe1 Fe 0.27712(4) 0.70298(4) 0.60354(3) 0.02141(13) Uani 1 1 d . . . . . Fe2 Fe 0.27192(3) 0.70158(4) 0.77675(3) 0.01649(11) Uani 1 1 d D . . . . O1 O 0.23807(18) 0.67545(15) 0.68942(15) 0.0203(5) Uani 1 1 d . . . . . O2 O 0.3566(2) 0.78803(19) 0.62892(15) 0.0250(6) Uani 0.5 1 d D . P A 1 H2O H 0.366(8) 0.795(4) 0.6780(9) 0.037 Uiso 0.5 1 d D U P B 1 O3 O 0.36582(19) 0.77621(17) 0.75361(15) 0.0200(6) Uani 0.5 1 d D . P C 1 O2B O 0.3566(2) 0.78803(19) 0.62892(15) 0.0250(6) Uani 0.5 1 d D . P A 2 O3B O 0.36582(19) 0.77621(17) 0.75361(15) 0.0200(6) Uani 0.5 1 d D . P C 2 H3OB H 0.371(7) 0.793(5) 0.7058(9) 0.030 Uiso 0.5 1 d D U P D 2 O4 O 0.1036(3) 0.4642(2) 0.5070(2) 0.0373(8) Uani 1 1 d . . . . . H4A H 0.115070 0.449477 0.548151 0.056 Uiso 1 1 calc R U . . . N1 N 0.3778(3) 0.6176(2) 0.60003(18) 0.0235(8) Uani 1 1 d . . . . . N2 N 0.2219(2) 0.6093(2) 0.53353(19) 0.0249(8) Uani 1 1 d . . . . . N3 N 0.3150(3) 0.7520(2) 0.4981(2) 0.0296(9) Uani 1 1 d . . . . . N4 N 0.1725(3) 0.7797(2) 0.58002(19) 0.0274(9) Uani 1 1 d . . . . . N5 N 0.3432(2) 0.5930(2) 0.78715(18) 0.0190(7) Uani 1 1 d . . . . . N8 N 0.1860(2) 0.8006(2) 0.78583(17) 0.0190(6) Uani 1 1 d . . . . . N9 N 0.3195(5) 0.0427(4) 0.6975(4) 0.0286(12) Uani 0.9 1 d D U P E 1 O6 O 0.2603(2) 0.0571(2) 0.65408(18) 0.0284(7) Uani 0.9 1 d D . P E 1 O7 O 0.3418(3) 0.0988(2) 0.7378(2) 0.0336(9) Uani 0.9 1 d D . P E 1 O8 O 0.3542(9) -0.0225(4) 0.6999(6) 0.045(3) Uani 0.9 1 d D U P E 1 N9' N 0.325(4) 0.042(3) 0.690(2) 0.025(7) Uiso 0.1 1 d D U P E 2 O6' O 0.3462(19) 0.0960(16) 0.6480(17) 0.036(8) Uiso 0.1 1 d D . P E 2 O7' O 0.272(2) 0.0643(12) 0.7363(18) 0.041(9) Uiso 0.1 1 d D . P E 2 O8' O 0.353(10) -0.026(4) 0.686(5) 0.039(8) Uiso 0.1 1 d D U P E 2 N10 N 0.3742(4) 0.2573(4) 0.5833(3) 0.0331(13) Uani 0.9 1 d D U P E 1 O9 O 0.3705(2) 0.1858(2) 0.60520(19) 0.0279(8) Uani 0.9 1 d D . P E 1 O10 O 0.3165(2) 0.3039(2) 0.60076(18) 0.0278(8) Uani 0.9 1 d D . P E 1 O11 O 0.4341(3) 0.2804(3) 0.5470(3) 0.0425(13) Uani 0.9 1 d D . P E 1 N10' N 0.378(3) 0.251(3) 0.583(2) 0.033(8) Uiso 0.1 1 d D U P E 2 O9' O 0.3847(17) 0.267(3) 0.6492(18) 0.062(13) Uiso 0.1 1 d D . P E 2 O10' O 0.307(3) 0.224(3) 0.5629(11) 0.071(14) Uiso 0.1 1 d D . P E 2 O11' O 0.427(3) 0.255(3) 0.532(2) 0.034(13) Uiso 0.1 1 d D . P E 2 N11 N 0.1630(3) 0.3715(3) 0.6681(2) 0.0289(10) Uani 0.9 1 d D . P F 1 O12 O 0.1432(2) 0.3163(2) 0.6281(2) 0.0276(8) Uani 0.9 1 d D . P F 1 O13 O 0.2102(3) 0.3575(2) 0.7190(3) 0.0346(10) Uani 0.9 1 d D U P F 1 O14 O 0.1348(3) 0.4398(2) 0.6574(2) 0.0336(9) Uani 0.9 1 d D U P F 1 N11' N 0.163(2) 0.3707(18) 0.7202(16) 0.028(9) Uiso 0.1 1 d D . P G 2 O12' O 0.135(2) 0.3105(16) 0.748(2) 0.068(14) Uiso 0.1 1 d D . P G 2 O13' O 0.241(2) 0.3601(10) 0.717(2) 0.034(7) Uiso 0.1 1 d D U P G 2 O14' O 0.140(3) 0.438(2) 0.701(2) 0.050(7) Uiso 0.1 1 d D U P G 2 N12 N 0.3642(4) 0.2621(4) 0.8013(3) 0.0252(15) Uani 0.9 1 d D . P E 1 O15 O 0.2881(2) 0.2401(2) 0.81472(19) 0.0287(7) Uani 0.9 1 d D . P E 1 O16 O 0.3846(2) 0.2661(2) 0.73748(19) 0.0266(8) Uani 0.9 1 d D . P E 1 O17 O 0.4154(6) 0.2787(4) 0.8485(5) 0.0362(16) Uani 0.9 1 d D U P E 1 N12' N 0.365(3) 0.248(2) 0.811(2) 0.018(16) Uiso 0.1 1 d D . P E 2 O15' O 0.304(2) 0.2899(18) 0.7897(15) 0.042(8) Uiso 0.1 1 d D . P E 2 O16' O 0.364(2) 0.181(2) 0.7825(19) 0.059(13) Uiso 0.1 1 d D . P E 2 O17' O 0.417(5) 0.267(5) 0.856(4) 0.033(8) Uiso 0.1 1 d D U P E 2 N13 N 0.1001(4) 0.1642(4) 0.7964(3) 0.0347(13) Uani 0.9 1 d D U P E 1 O18 O 0.1634(2) 0.1192(2) 0.78349(19) 0.0294(8) Uani 0.9 1 d D . P E 1 O19 O 0.1010(3) 0.2317(2) 0.7671(2) 0.0323(9) Uani 0.9 1 d D . P E 1 O20 O 0.0423(4) 0.1411(3) 0.8354(3) 0.0508(16) Uani 0.9 1 d D U P E 1 N13' N 0.105(3) 0.156(3) 0.799(2) 0.037(8) Uiso 0.1 1 d D U P E 2 O18' O 0.182(2) 0.170(3) 0.8146(11) 0.056(11) Uiso 0.1 1 d D . P E 2 O19' O 0.0953(16) 0.137(2) 0.7353(18) 0.047(10) Uiso 0.1 1 d D . P E 2 O20' O 0.048(3) 0.162(4) 0.844(3) 0.045(7) Uiso 0.1 1 d D U P E 2 N14 N 0.1202(3) 0.1355(5) 0.5767(3) 0.024(3) Uani 0.9 1 d D . P E 1 O21 O 0.0989(2) 0.1402(2) 0.64001(19) 0.0270(8) Uani 0.9 1 d D . P E 1 O22 O 0.1904(2) 0.1677(2) 0.55908(18) 0.0260(8) Uani 0.9 1 d D . P E 1 O23 O 0.0748(4) 0.1017(4) 0.5336(3) 0.0375(15) Uani 0.9 1 d D . P E 1 N14' N 0.120(3) 0.144(2) 0.579(2) 0.05(4) Uiso 0.1 1 d D . P E 2 O21' O 0.1126(16) 0.214(2) 0.6000(15) 0.038(8) Uiso 0.1 1 d D . P E 2 O22' O 0.174(2) 0.0955(15) 0.6054(17) 0.042(9) Uiso 0.1 1 d D . P E 2 O23' O 0.072(4) 0.123(3) 0.532(3) 0.028(15) Uiso 0.1 1 d D . P E 2 C1 C 0.4548(3) 0.6284(3) 0.6310(2) 0.0271(9) Uani 1 1 d . . . . . H1 H 0.466680 0.677991 0.652346 0.033 Uiso 1 1 calc R U . . . C2 C 0.5165(3) 0.5704(3) 0.6329(2) 0.0290(10) Uani 1 1 d . . . . . H2 H 0.569348 0.578932 0.656147 0.035 Uiso 1 1 calc R U . . . C3 C 0.4990(3) 0.4990(3) 0.5997(2) 0.0301(10) Uani 1 1 d . . . . . H3 H 0.541236 0.458656 0.598224 0.036 Uiso 1 1 calc R U . . . C4 C 0.4205(3) 0.4867(3) 0.5689(2) 0.0269(9) Uani 1 1 d . . . . . H4 H 0.407489 0.437756 0.546890 0.032 Uiso 1 1 calc R U . . . C5 C 0.3607(3) 0.5473(3) 0.5706(2) 0.0231(9) Uani 1 1 d . . . . . C6 C 0.2711(3) 0.5348(2) 0.5449(2) 0.0255(9) Uani 1 1 d . . . . . H6A H 0.273274 0.505178 0.500017 0.031 Uiso 1 1 calc R U . . . H6B H 0.240180 0.501726 0.579459 0.031 Uiso 1 1 calc R U . . . C7 C 0.2294(4) 0.6391(3) 0.4597(2) 0.0328(11) Uani 1 1 d . . . . . H7A H 0.180761 0.674657 0.449296 0.039 Uiso 1 1 calc R U . . . H7B H 0.226718 0.594022 0.426629 0.039 Uiso 1 1 calc R U . . . C8 C 0.3125(4) 0.6836(3) 0.4489(2) 0.0341(12) Uani 1 1 d . . . . . H8A H 0.361497 0.648062 0.457977 0.041 Uiso 1 1 calc R U . . . H8B H 0.316342 0.702476 0.399688 0.041 Uiso 1 1 calc R U . . . C9 C 0.2562(4) 0.8166(3) 0.4761(2) 0.0345(11) Uani 1 1 d . . . . . H9A H 0.231262 0.802955 0.429833 0.041 Uiso 1 1 calc R U . . . H9B H 0.289745 0.865786 0.470075 0.041 Uiso 1 1 calc R U . . . C10 C 0.1841(3) 0.8323(3) 0.5279(2) 0.0306(10) Uani 1 1 d . . . . . C11 C 0.1301(4) 0.8969(4) 0.5203(3) 0.0454(14) Uani 1 1 d . . . . . H11 H 0.140727 0.935123 0.484740 0.055 Uiso 1 1 calc R U . . . C12 C 0.0612(4) 0.9050(4) 0.5646(4) 0.0520(16) Uani 1 1 d . . . . . H12 H 0.024192 0.949269 0.560197 0.062 Uiso 1 1 calc R U . . . C13 C 0.0462(4) 0.8483(3) 0.6156(3) 0.0397(12) Uani 1 1 d . . . . . H13 H -0.002830 0.851118 0.644908 0.048 Uiso 1 1 calc R U . . . C14 C 0.1039(3) 0.7877(3) 0.6226(3) 0.0311(10) Uani 1 1 d . . . . . H14 H 0.095354 0.749858 0.658847 0.037 Uiso 1 1 calc R U . . . C15 C 0.4022(3) 0.7826(3) 0.5098(2) 0.0323(11) Uani 1 1 d . . . . . H15A H 0.420002 0.815775 0.469491 0.039 Uiso 1 1 calc R U . . . H15B H 0.442996 0.738189 0.514256 0.039 Uiso 1 1 calc R U . . . C16 C 0.4021(4) 0.8316(3) 0.5772(2) 0.0314(11) Uani 1 1 d . . . . . H16A H 0.461333 0.841435 0.593100 0.038 Uiso 1 1 calc R U . A 1 H16B H 0.374020 0.883226 0.568871 0.038 Uiso 1 1 calc R U . A 1 C17 C 0.1305(3) 0.5978(3) 0.5543(3) 0.0295(10) Uani 1 1 d . . . . . H17A H 0.102769 0.650381 0.555650 0.035 Uiso 1 1 calc R U . . . H17B H 0.129412 0.576512 0.602822 0.035 Uiso 1 1 calc R U . . . C18 C 0.0764(3) 0.5439(3) 0.5082(3) 0.0331(11) Uani 1 1 d . . . . . H18A H 0.016630 0.545743 0.525032 0.040 Uiso 1 1 calc R U . . . H18B H 0.077119 0.564640 0.459482 0.040 Uiso 1 1 calc R U . . . C21 C 0.3297(3) 0.5282(3) 0.7475(2) 0.0238(9) Uani 1 1 d . . . . . H21 H 0.283637 0.528675 0.714938 0.029 Uiso 1 1 calc R U . . . C22 C 0.3790(3) 0.4617(3) 0.7518(2) 0.0267(10) Uani 1 1 d . . . . . H22 H 0.367038 0.416597 0.723721 0.032 Uiso 1 1 calc R U . . . C23 C 0.4472(3) 0.4620(3) 0.7985(2) 0.0282(10) Uani 1 1 d . . . . . H23 H 0.483400 0.417147 0.802240 0.034 Uiso 1 1 calc R U . . . C24 C 0.4619(3) 0.5275(3) 0.8392(2) 0.0254(9) Uani 1 1 d . . . . . H24 H 0.508333 0.528444 0.871378 0.031 Uiso 1 1 calc R U . . . C25 C 0.4083(3) 0.5927(3) 0.8329(2) 0.0213(9) Uani 1 1 d D . . . . C26 C 0.4270(6) 0.6689(4) 0.8695(5) 0.026(2) Uani 0.7 1 d D U P C 1 H26A H 0.469841 0.699273 0.842377 0.031 Uiso 0.7 1 calc R U P C 1 H26B H 0.450745 0.658196 0.916760 0.031 Uiso 0.7 1 calc R U P C 1 N6 N 0.3456(2) 0.7167(2) 0.87622(18) 0.0218(7) Uani 0.7 1 d D . P C 1 C27 C 0.2988(5) 0.6870(4) 0.9383(3) 0.0259(15) Uani 0.7 1 d D . P C 1 H27A H 0.318031 0.714619 0.981354 0.031 Uiso 0.7 1 calc R U P C 1 H27B H 0.308893 0.629605 0.944352 0.031 Uiso 0.7 1 calc R U P C 1 C28 C 0.2066(4) 0.7026(5) 0.9253(3) 0.0286(13) Uani 0.7 1 d D U P C 1 H28A H 0.197254 0.760404 0.923517 0.034 Uiso 0.7 1 calc R U P C 1 H28B H 0.172947 0.681357 0.965069 0.034 Uiso 0.7 1 calc R U P C 1 N7 N 0.1746(4) 0.6661(4) 0.8575(4) 0.0200(13) Uani 0.7 1 d D . P C 1 C37 C 0.1606(5) 0.5809(4) 0.8714(3) 0.0290(14) Uani 0.7 1 d D U P C 1 H37A H 0.124780 0.575670 0.914048 0.035 Uiso 0.7 1 calc R U P C 1 H37B H 0.216460 0.556110 0.881732 0.035 Uiso 0.7 1 calc R U P C 1 C38 C 0.1188(5) 0.5356(4) 0.8127(4) 0.0336(14) Uani 0.7 1 d D . P C 1 H38A H 0.057267 0.548643 0.810018 0.040 Uiso 0.7 1 calc R U P C 1 H38B H 0.145702 0.549031 0.767085 0.040 Uiso 0.7 1 calc R U P C 1 O5 O 0.1301(4) 0.4535(3) 0.8279(3) 0.0417(13) Uani 0.7 1 d D . P C 1 H5A H 0.154156 0.431281 0.793732 0.063 Uiso 0.7 1 calc R U P C 1 C26' C 0.4155(14) 0.6621(11) 0.8818(13) 0.028(6) Uiso 0.3 1 d D U P C 2 H26C H 0.418614 0.642411 0.930761 0.034 Uiso 0.3 1 calc R U P C 2 H26D H 0.469419 0.690461 0.871682 0.034 Uiso 0.3 1 calc R U P C 2 N6' N 0.3456(2) 0.7167(2) 0.87622(18) 0.0218(7) Uani 0.3 1 d D . P C 2 C27' C 0.2718(10) 0.7069(10) 0.9306(9) 0.023(4) Uiso 0.3 1 d D . P C 2 H27C H 0.295954 0.698875 0.978212 0.028 Uiso 0.3 1 calc R U P C 2 H27D H 0.236421 0.755345 0.931506 0.028 Uiso 0.3 1 calc R U P C 2 C28' C 0.2164(8) 0.6361(7) 0.9108(6) 0.015(2) Uiso 0.3 1 d D U P C 2 H28C H 0.252735 0.588434 0.907673 0.018 Uiso 0.3 1 calc R U P C 2 H28D H 0.173637 0.627120 0.948337 0.018 Uiso 0.3 1 calc R U P C 2 N7' N 0.1718(10) 0.6476(10) 0.8434(8) 0.025(5) Uiso 0.15 1 d D . P C 2 C37' C 0.1260(17) 0.5889(14) 0.8055(11) 0.017(4) Uiso 0.15 1 d D U P C 2 H37C H 0.167770 0.560628 0.775679 0.020 Uiso 0.15 1 calc R U P C 2 H37D H 0.086576 0.616900 0.773322 0.020 Uiso 0.15 1 calc R U P C 2 C38' C 0.0744(9) 0.5272(8) 0.8433(7) 0.019(3) Uiso 0.15 1 d D . P C 2 H38D H 0.014265 0.534181 0.828480 0.022 Uiso 0.15 1 calc R U P C 2 H38C H 0.093050 0.475172 0.825062 0.022 Uiso 0.15 1 calc R U P C 2 O5' O 0.0743(13) 0.5219(12) 0.9139(9) 0.026(4) Uiso 0.15 1 d D . P C 2 H5'A H 0.031746 0.546050 0.930080 0.039 Uiso 0.15 1 calc R U P C 2 N7" N 0.1718(10) 0.6476(10) 0.8434(8) 0.025(5) Uiso 0.15 1 d D . P C 3 C37" C 0.1531(16) 0.5711(12) 0.8116(14) 0.017(4) Uiso 0.15 1 d D U P C 3 H37E H 0.203926 0.536800 0.816636 0.021 Uiso 0.15 1 calc R U P C 3 H37F H 0.143130 0.578995 0.760624 0.021 Uiso 0.15 1 calc R U P C 3 C38" C 0.0744(9) 0.5272(8) 0.8433(7) 0.019(3) Uiso 0.15 1 d D . P C 3 H38E H 0.041198 0.560146 0.876508 0.022 Uiso 0.15 1 calc R U P C 3 H38F H 0.036401 0.504172 0.807066 0.022 Uiso 0.15 1 calc R U P C 3 O5" O 0.1272(13) 0.4686(11) 0.8782(11) 0.026(4) Uiso 0.15 1 d D . P C 3 H5"A H 0.150186 0.439366 0.847966 0.038 Uiso 0.15 1 calc R U P C 3 C29 C 0.0949(3) 0.7052(3) 0.8439(3) 0.0371(11) Uani 1 1 d . . . . . H29A H 0.059601 0.705676 0.887086 0.044 Uiso 1 1 calc R U . C 1 H29B H 0.063091 0.676451 0.806859 0.044 Uiso 1 1 calc R U . C 1 C30 C 0.1122(3) 0.7892(3) 0.8201(2) 0.0245(8) Uani 1 1 d . . . . . C31 C 0.0523(3) 0.8494(3) 0.8281(3) 0.0364(12) Uani 1 1 d . . . . . H31 H 0.001032 0.840302 0.853505 0.044 Uiso 1 1 calc R U . . . C32 C 0.0685(3) 0.9221(3) 0.7987(3) 0.0353(12) Uani 1 1 d . . . . . H32 H 0.028726 0.963983 0.803982 0.042 Uiso 1 1 calc R U . . . C33 C 0.1427(3) 0.9335(3) 0.7617(3) 0.0308(10) Uani 1 1 d . . . . . H33 H 0.154238 0.982836 0.739712 0.037 Uiso 1 1 calc R U . . . C34 C 0.1999(3) 0.8724(3) 0.7570(2) 0.0252(9) Uani 1 1 d . . . . . H34 H 0.251865 0.880910 0.732297 0.030 Uiso 1 1 calc R U . . . C35 C 0.3682(3) 0.8017(3) 0.8775(2) 0.0228(8) Uani 1 1 d . . . . . H35A H 0.409844 0.812165 0.915570 0.027 Uiso 1 1 calc R U . C 1 H35B H 0.316543 0.833948 0.886395 0.027 Uiso 1 1 calc R U . C 1 C36 C 0.4067(3) 0.8233(2) 0.8066(2) 0.0229(8) Uani 1 1 d . . . . . H36A H 0.397693 0.880105 0.796838 0.027 Uiso 1 1 calc R U . C 1 H36B H 0.468911 0.812778 0.806898 0.027 Uiso 1 1 calc R U . C 1 O311 O 0.2961(5) 0.0924(4) 0.4613(3) 0.0623(19) Uani 0.7 1 d D . P H 1 H311 H 0.290403 0.135757 0.482223 0.093 Uiso 0.7 1 calc R U P H 1 C311 C 0.3680(8) 0.0547(6) 0.4854(5) 0.060(3) Uani 0.7 1 d D . P H 1 H31A H 0.412110 0.093921 0.496141 0.089 Uiso 0.7 1 calc R U P H 1 H31B H 0.389064 0.018328 0.449272 0.089 Uiso 0.7 1 calc R U P H 1 H31C H 0.354029 0.024916 0.528122 0.089 Uiso 0.7 1 calc R U P H 1 O312 O 0.3230(9) -0.0008(8) 0.5208(7) 0.047(3) Uiso 0.3 1 d D . P I 2 H312 H 0.305432 0.028431 0.553399 0.071 Uiso 0.3 1 calc R U P I 2 C312 C 0.328(2) 0.041(2) 0.4612(14) 0.076(9) Uiso 0.3 1 d D . P I 2 H31D H 0.272374 0.063459 0.449930 0.114 Uiso 0.3 1 calc R U P I 2 H31E H 0.346931 0.006443 0.422785 0.114 Uiso 0.3 1 calc R U P I 2 H31F H 0.369900 0.083836 0.467292 0.114 Uiso 0.3 1 calc R U P I 2 O1W O 0.2089(5) -0.0113(5) 0.3798(4) 0.073(2) Uani 0.7 1 d D . P J 1 H1WA H 0.238(8) 0.021(6) 0.414(4) 0.109 Uiso 0.7 1 d D U P K 1 H1WB H 0.226(8) 0.012(6) 0.336(3) 0.109 Uiso 0.7 1 d D U P L 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 Ce1 0.01566(9) 0.02187(10) 0.02523(10) 0.00389(10) 0.00027(9) -0.00217(8) Fe1 0.0314(3) 0.0161(3) 0.0167(2) -0.0016(2) -0.0041(2) 0.0002(3) Fe2 0.0180(3) 0.0142(2) 0.0173(2) -0.0006(2) -0.0004(2) -0.0017(3) O1 0.0229(13) 0.0166(11) 0.0214(12) -0.0025(11) -0.0031(14) -0.0009(10) O2 0.0386(17) 0.0195(15) 0.0168(13) -0.0004(13) 0.0006(12) -0.0101(15) O3 0.0218(14) 0.0199(15) 0.0182(14) -0.0014(11) -0.0018(11) -0.0063(11) O2B 0.0386(17) 0.0195(15) 0.0168(13) -0.0004(13) 0.0006(12) -0.0101(15) O3B 0.0218(14) 0.0199(15) 0.0182(14) -0.0014(11) -0.0018(11) -0.0063(11) O4 0.051(2) 0.0229(17) 0.0374(19) -0.0067(14) -0.0082(18) -0.0032(16) N1 0.032(2) 0.0204(18) 0.0176(17) -0.0024(14) 0.0016(15) -0.0011(16) N2 0.033(2) 0.0196(17) 0.0222(17) -0.0038(14) -0.0055(15) 0.0027(15) N3 0.046(3) 0.023(2) 0.0203(17) 0.0000(15) -0.0014(17) -0.0026(17) N4 0.041(2) 0.0175(19) 0.0241(18) -0.0001(14) -0.0154(16) -0.0018(15) N5 0.0223(17) 0.0165(16) 0.0181(16) 0.0001(13) 0.0023(13) 0.0015(13) N8 0.0198(15) 0.0166(16) 0.0207(15) -0.0024(14) -0.0017(12) -0.0025(14) N9 0.021(2) 0.026(2) 0.039(3) 0.010(2) 0.009(2) -0.0011(16) O6 0.0279(18) 0.0248(16) 0.0327(18) 0.0034(14) 0.0016(16) -0.0004(16) O7 0.0275(19) 0.031(2) 0.043(2) 0.0130(18) -0.0076(17) -0.0006(16) O8 0.028(2) 0.026(2) 0.080(7) 0.018(3) 0.008(5) 0.0036(18) N10 0.019(2) 0.041(3) 0.039(3) 0.016(2) -0.0019(19) -0.008(2) O9 0.0224(17) 0.028(2) 0.0333(19) 0.0084(15) 0.0068(14) -0.0015(14) O10 0.0218(16) 0.031(2) 0.0307(18) 0.0099(16) 0.0025(13) -0.0016(15) O11 0.031(2) 0.042(3) 0.055(3) 0.018(3) 0.016(2) -0.009(2) N11 0.022(2) 0.027(2) 0.037(2) 0.0131(18) 0.0040(18) -0.0013(17) O12 0.0216(17) 0.0270(19) 0.0343(19) 0.0043(15) -0.0025(15) -0.0018(14) O13 0.020(2) 0.029(2) 0.054(3) 0.0044(17) -0.004(2) -0.0031(16) O14 0.032(2) 0.0234(19) 0.045(2) 0.0100(17) 0.0043(18) 0.0017(16) N12 0.032(3) 0.019(2) 0.025(3) 0.008(2) -0.005(2) 0.002(2) O15 0.0285(17) 0.0362(19) 0.0214(16) 0.0053(16) -0.0001(15) -0.0077(14) O16 0.0224(17) 0.0265(18) 0.0309(19) 0.0060(15) 0.0008(15) -0.0040(14) O17 0.037(2) 0.035(4) 0.037(3) -0.001(3) -0.014(2) 0.002(2) N13 0.033(3) 0.036(3) 0.035(3) -0.009(2) 0.012(2) -0.008(2) O18 0.035(2) 0.0239(18) 0.0296(18) 0.0043(15) 0.0073(16) -0.0029(16) O19 0.032(2) 0.0262(19) 0.039(2) 0.0007(16) 0.0110(17) 0.0015(15) O20 0.050(3) 0.048(4) 0.055(3) -0.013(2) 0.035(2) -0.017(2) N14 0.024(4) 0.021(3) 0.027(4) 0.0066(17) -0.0042(17) -0.0034(17) O21 0.0175(16) 0.033(2) 0.0305(19) 0.0016(15) 0.0005(14) -0.0048(14) O22 0.0265(18) 0.0277(18) 0.0238(17) 0.0031(14) 0.0017(14) -0.0055(14) O23 0.046(3) 0.034(3) 0.032(3) 0.011(2) -0.0190(19) -0.015(3) C1 0.032(2) 0.028(2) 0.022(2) -0.0011(18) -0.0010(18) -0.0056(19) C2 0.029(2) 0.032(3) 0.026(2) 0.0030(19) -0.0004(19) -0.0006(19) C3 0.038(3) 0.024(2) 0.028(2) 0.0030(18) 0.003(2) 0.009(2) C4 0.039(3) 0.022(2) 0.021(2) -0.0024(17) 0.0022(19) 0.0000(19) C5 0.032(2) 0.020(2) 0.0164(18) 0.0006(16) 0.0028(17) -0.0002(17) C6 0.035(2) 0.0184(19) 0.023(2) -0.0048(15) -0.0051(18) 0.0014(18) C7 0.054(3) 0.027(2) 0.0179(19) -0.0040(17) -0.009(2) 0.005(2) C8 0.055(3) 0.029(3) 0.019(2) -0.0010(18) -0.001(2) -0.001(2) C9 0.056(3) 0.023(2) 0.024(2) 0.0057(16) -0.011(2) -0.005(2) C10 0.044(3) 0.026(2) 0.022(2) -0.0006(18) -0.015(2) -0.001(2) C11 0.052(3) 0.040(3) 0.045(3) 0.020(3) -0.013(3) 0.005(3) C12 0.050(4) 0.047(4) 0.059(4) 0.016(3) -0.015(3) 0.017(3) C13 0.035(3) 0.042(3) 0.042(3) 0.001(2) -0.011(2) 0.008(2) C14 0.038(2) 0.027(2) 0.028(2) -0.002(2) -0.0113(19) 0.001(2) C15 0.045(3) 0.030(3) 0.022(2) 0.0036(18) 0.0037(19) -0.006(2) C16 0.046(3) 0.029(2) 0.020(2) 0.0064(19) -0.001(2) -0.012(2) C17 0.033(2) 0.022(2) 0.034(3) -0.0069(19) -0.007(2) 0.0015(19) C18 0.041(3) 0.022(2) 0.036(3) -0.004(2) -0.013(2) 0.000(2) C21 0.028(2) 0.021(2) 0.022(2) -0.0006(17) 0.0000(17) -0.0005(17) C22 0.038(3) 0.021(2) 0.021(2) -0.0005(17) 0.0075(19) 0.0019(18) C23 0.032(2) 0.023(2) 0.030(3) 0.0064(18) 0.0107(19) 0.0083(18) C24 0.021(2) 0.028(2) 0.027(2) 0.0082(18) 0.0017(17) 0.0034(17) C25 0.024(2) 0.020(2) 0.0205(19) 0.0040(15) 0.0037(16) -0.0015(16) C26 0.035(4) 0.021(3) 0.021(4) 0.006(3) -0.012(3) -0.003(3) N6 0.0291(18) 0.0190(18) 0.0171(16) -0.0021(14) -0.0010(14) -0.0057(15) C27 0.044(4) 0.020(3) 0.014(3) 0.000(2) -0.001(3) -0.003(3) C28 0.036(3) 0.029(3) 0.020(3) 0.003(3) 0.006(2) -0.004(3) N7 0.017(3) 0.017(3) 0.026(3) 0.005(3) 0.004(2) -0.004(2) C37 0.034(3) 0.026(3) 0.028(3) 0.003(3) 0.004(3) -0.006(3) C38 0.040(4) 0.029(4) 0.032(3) 0.004(3) 0.002(4) -0.002(3) O5 0.055(3) 0.022(2) 0.048(4) 0.001(2) 0.009(3) -0.010(2) N6' 0.0291(18) 0.0190(18) 0.0171(16) -0.0021(14) -0.0010(14) -0.0057(15) C29 0.025(2) 0.032(2) 0.054(3) 0.013(3) 0.009(2) -0.001(2) C30 0.0237(18) 0.023(2) 0.026(2) 0.002(2) 0.0021(16) -0.0006(17) C31 0.024(2) 0.038(3) 0.047(3) 0.002(2) 0.007(2) 0.007(2) C32 0.029(2) 0.027(2) 0.050(3) -0.004(2) -0.003(2) 0.0102(19) C33 0.030(2) 0.018(2) 0.045(3) -0.0011(19) -0.002(2) -0.0005(18) C34 0.027(2) 0.019(2) 0.030(2) -0.0007(17) -0.0013(19) -0.0033(17) C35 0.0252(19) 0.019(2) 0.025(2) -0.0062(17) -0.0024(16) -0.0030(18) C36 0.028(2) 0.0188(18) 0.022(2) -0.0001(18) -0.005(2) -0.0085(15) O311 0.086(5) 0.057(4) 0.045(4) -0.001(3) 0.003(3) 0.033(4) C311 0.093(8) 0.043(5) 0.042(5) -0.004(4) 0.010(6) 0.033(5) O1W 0.082(5) 0.075(5) 0.060(4) 0.003(4) 0.004(4) -0.021(4) 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -2 -1 2 0.077 -2 1 0 0.054 -2 1 -2 0.043 -1 0 -2 0.038 -1 -1 0 0.082 -1 2 -2 0.057 0 0 1 0.051 0 -2 -1 0.088 0 2 1 0.065 1 1 -1 0.052 1 0 -1 0.048 1 1 0 0.062 2 -1 1 0.029 2 -1 2 0.031 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 O15 Ce1 O7 68.79(13) . . ? O15 Ce1 O18 67.70(12) . . ? O7 Ce1 O18 69.12(13) . . ? O15' Ce1 O21' 137.9(10) . . ? O15' Ce1 O7' 99.7(12) . . ? O21' Ce1 O7' 115.5(12) . . ? O15 Ce1 O6 114.38(11) . . ? O7 Ce1 O6 48.99(12) . . ? O18 Ce1 O6 72.27(11) . . ? O15' Ce1 O6' 110.9(11) . . ? O21' Ce1 O6' 109.8(11) . . ? O7' Ce1 O6' 47.7(9) . . ? O15' Ce1 O18' 65.2(13) . . ? O21' Ce1 O18' 110.4(11) . . ? O7' Ce1 O18' 62.8(13) . . ? O6' Ce1 O18' 109.1(12) . . ? O15' Ce1 O9' 69.7(12) . . ? O21' Ce1 O9' 117.0(12) . . ? O7' Ce1 O9' 106.8(14) . . ? O6' Ce1 O9' 68.7(14) . . ? O18' Ce1 O9' 130.2(12) . . ? O15 Ce1 O9 110.78(11) . . ? O7 Ce1 O9 69.01(12) . . ? O18 Ce1 O9 134.91(11) . . ? O6 Ce1 O9 68.05(11) . . ? O15 Ce1 O21 132.20(11) . . ? O7 Ce1 O21 110.81(12) . . ? O18 Ce1 O21 68.23(12) . . ? O6 Ce1 O21 67.42(12) . . ? O9 Ce1 O21 113.05(12) . . ? O1 Fe1 O2B 100.47(12) . . ? O1 Fe1 O2 100.47(12) . . ? O1 Fe1 N4 94.96(14) . . ? O2B Fe1 N4 95.25(14) . . ? O2 Fe1 N4 95.25(14) . . ? O1 Fe1 N1 95.95(13) . . ? O2B Fe1 N1 92.04(15) . . ? O2 Fe1 N1 92.04(15) . . ? N4 Fe1 N1 165.56(14) . . ? O1 Fe1 N2 102.92(13) . . ? O2B Fe1 N2 155.29(14) . . ? O2 Fe1 N2 155.29(14) . . ? N4 Fe1 N2 90.56(13) . . ? N1 Fe1 N2 77.80(14) . . ? O1 Fe1 N3 172.31(14) . . ? O2B Fe1 N3 77.37(13) . . ? O2 Fe1 N3 77.37(13) . . ? N4 Fe1 N3 77.99(16) . . ? N1 Fe1 N3 91.52(15) . . ? N2 Fe1 N3 80.42(14) . . ? O1 Fe2 O3B 99.79(12) . . ? O1 Fe2 O3 99.79(12) . . ? O1 Fe2 N8 94.65(12) . . ? O3B Fe2 N8 89.18(13) . . ? O3 Fe2 N8 89.18(13) . . ? O1 Fe2 N5 91.60(13) . . ? O3B Fe2 N5 100.25(13) . . ? O3 Fe2 N5 100.25(13) . . ? N8 Fe2 N5 167.65(13) . . ? O1 Fe2 N7" 102.6(4) . . ? N8 Fe2 N7" 80.4(5) . . ? N5 Fe2 N7" 87.9(5) . . ? O1 Fe2 N7' 102.6(4) . . ? O3B Fe2 N7' 155.9(4) . . ? N8 Fe2 N7' 80.4(5) . . ? N5 Fe2 N7' 87.9(5) . . ? O1 Fe2 N6 164.54(13) . . ? O3 Fe2 N6 74.43(12) . . ? N8 Fe2 N6 99.54(13) . . ? N5 Fe2 N6 75.66(13) . . ? O1 Fe2 N6' 164.54(13) . . ? O3B Fe2 N6' 74.43(12) . . ? N8 Fe2 N6' 99.54(13) . . ? N5 Fe2 N6' 75.66(13) . . ? N7' Fe2 N6' 85.9(4) . . ? O1 Fe2 N7 111.4(2) . . ? O3 Fe2 N7 145.4(2) . . ? N8 Fe2 N7 74.3(2) . . ? N5 Fe2 N7 93.5(2) . . ? N6 Fe2 N7 78.6(2) . . ? Fe2 O1 Fe1 132.22(15) . . ? C16 O2 Fe1 121.9(3) . . ? C16 O2 H2O 122(4) . . ? Fe1 O2 H2O 116(4) . . ? C36 O3 Fe2 121.8(3) . . ? C36 O3 H2O 124(2) . . ? Fe2 O3 H2O 111(3) . . ? C16 O2B Fe1 121.9(3) . . ? C36 O3B Fe2 121.8(3) . . ? C36 O3B H3OB 118(3) . . ? Fe2 O3B H3OB 117(4) . . ? C18 O4 H4A 109.5 . . ? C5 N1 C1 118.6(4) . . ? C5 N1 Fe1 117.7(3) . . ? C1 N1 Fe1 123.4(3) . . ? C6 N2 C7 112.3(4) . . ? C6 N2 C17 110.2(4) . . ? C7 N2 C17 111.5(4) . . ? C6 N2 Fe1 108.2(2) . . ? C7 N2 Fe1 106.7(3) . . ? C17 N2 Fe1 107.7(3) . . ? C15 N3 C8 113.1(4) . . ? C15 N3 C9 110.8(4) . . ? C8 N3 C9 112.2(4) . . ? C15 N3 Fe1 103.8(3) . . ? C8 N3 Fe1 105.5(3) . . ? C9 N3 Fe1 111.0(3) . . ? C10 N4 C14 118.9(4) . . ? C10 N4 Fe1 116.9(4) . . ? C14 N4 Fe1 123.0(3) . . ? C25 N5 C21 118.6(4) . . ? C25 N5 Fe2 117.2(3) . . ? C21 N5 Fe2 124.0(3) . . ? C30 N8 C34 117.8(4) . . ? C30 N8 Fe2 117.7(3) . . ? C34 N8 Fe2 124.4(3) . . ? O8 N9 O6 121.4(7) . . ? O8 N9 O7 121.8(6) . . ? O6 N9 O7 116.8(5) . . ? N9 O6 Ce1 96.7(4) . . ? N9 O7 Ce1 97.5(4) . . ? O8' N9' O6' 123(4) . . ? O8' N9' O7' 124(4) . . ? O6' N9' O7' 113(3) . . ? N9' O6' Ce1 99(2) . . ? N9' O7' Ce1 100(2) . . ? O11 N10 O10 120.2(6) . . ? O11 N10 O9 121.2(6) . . ? O10 N10 O9 118.5(5) . . ? N10 O9 Ce1 96.5(3) . . ? N10 O10 Ce1 95.9(3) . . ? O11' N10' O10' 109(3) . . ? O11' N10' O9' 135(4) . . ? O10' N10' O9' 116(3) . . ? N10' O9' Ce1 97(2) . . ? N10' O10' Ce1 97(2) . . ? O13 N11 O12 118.8(4) . . ? O13 N11 O14 120.8(5) . . ? O12 N11 O14 120.4(4) . . ? N11 O12 Ce1 97.2(3) . . ? N11 O13 Ce1 96.6(3) . . ? O12' N11' O13' 105(3) . . ? O12' N11' O14' 141(4) . . ? O13' N11' O14' 113(3) . . ? N11' O12' Ce1 98.6(18) . . ? N11' O13' Ce1 97.8(17) . . ? O17 N12 O16 121.7(6) . . ? O17 N12 O15 121.8(7) . . ? O16 N12 O15 116.5(5) . . ? N12 O15 Ce1 99.2(3) . . ? N12 O16 Ce1 95.7(3) . . ? O17' N12' O16' 123(4) . . ? O17' N12' O15' 126(4) . . ? O16' N12' O15' 111(3) . . ? N12' O15' Ce1 103(2) . . ? N12' O16' Ce1 99(2) . . ? O20 N13 O19 123.7(6) . . ? O20 N13 O18 119.9(6) . . ? O19 N13 O18 116.4(5) . . ? N13 O18 Ce1 98.8(3) . . ? N13 O19 Ce1 95.9(3) . . ? O20' N13' O19' 126(4) . . ? O20' N13' O18' 122(4) . . ? O19' N13' O18' 112(3) . . ? N13' O18' Ce1 99(2) . . ? N13' O19' Ce1 96(2) . . ? O23 N14 O21 121.1(5) . . ? O23 N14 O22 121.8(6) . . ? O21 N14 O22 117.2(6) . . ? N14 O21 Ce1 98.2(3) . . ? N14 O22 Ce1 96.1(3) . . ? O23' N14' O21' 117(3) . . ? O23' N14' O22' 120(4) . . ? O21' N14' O22' 124(3) . . ? O23' N14' Ce1 177(3) . . ? O21' N14' Ce1 60.9(18) . . ? O22' N14' Ce1 62.8(18) . . ? N14' O21' Ce1 94(2) . . ? N14' O22' Ce1 92(2) . . ? N1 C1 C2 122.6(4) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 118.0(4) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C4 C3 C2 119.9(4) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 118.7(4) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 122.0(4) . . ? N1 C5 C6 116.6(4) . . ? C4 C5 C6 121.2(4) . . ? N2 C6 C5 114.2(4) . . ? N2 C6 H6A 108.7 . . ? C5 C6 H6A 108.7 . . ? N2 C6 H6B 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? N2 C7 C8 111.2(4) . . ? N2 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? N2 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N3 C8 C7 108.8(4) . . ? N3 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? N3 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? N3 C9 C10 113.9(4) . . ? N3 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? N3 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? N4 C10 C11 121.0(5) . . ? N4 C10 C9 117.5(4) . . ? C11 C10 C9 121.4(5) . . ? C12 C11 C10 119.5(5) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 119.5(5) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 118.3(6) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? N4 C14 C13 122.6(5) . . ? N4 C14 H14 118.7 . . ? C13 C14 H14 118.7 . . ? N3 C15 C16 108.4(4) . . ? N3 C15 H15A 110.0 . . ? C16 C15 H15A 110.0 . . ? N3 C15 H15B 110.0 . . ? C16 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? O2B C16 C15 107.4(4) . . ? O2 C16 C15 107.4(4) . . ? O2 C16 H16A 110.2 . . ? C15 C16 H16A 110.2 . . ? O2 C16 H16B 110.2 . . ? C15 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? N2 C17 C18 117.2(4) . . ? N2 C17 H17A 108.0 . . ? C18 C17 H17A 108.0 . . ? N2 C17 H17B 108.0 . . ? C18 C17 H17B 108.0 . . ? H17A C17 H17B 107.2 . . ? O4 C18 C17 114.3(4) . . ? O4 C18 H18A 108.7 . . ? C17 C18 H18A 108.7 . . ? O4 C18 H18B 108.7 . . ? C17 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? N5 C21 C22 123.1(4) . . ? N5 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C21 C22 C23 118.0(4) . . ? C21 C22 H22 121.0 . . ? C23 C22 H22 121.0 . . ? C24 C23 C22 119.5(4) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 119.4(4) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? N5 C25 C24 121.3(4) . . ? N5 C25 C26 116.6(4) . . ? C24 C25 C26 121.7(5) . . ? N5 C25 C26' 117.1(9) . . ? C24 C25 C26' 121.4(9) . . ? C25 C26 N6 109.6(5) . . ? C25 C26 H26A 109.7 . . ? N6 C26 H26A 109.7 . . ? C25 C26 H26B 109.7 . . ? N6 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C27 N6 C35 115.9(4) . . ? C27 N6 C26 107.6(6) . . ? C35 N6 C26 108.6(4) . . ? C27 N6 Fe2 112.4(3) . . ? C35 N6 Fe2 104.4(2) . . ? C26 N6 Fe2 107.6(3) . . ? N6 C27 C28 106.7(6) . . ? N6 C27 H27A 110.4 . . ? C28 C27 H27A 110.4 . . ? N6 C27 H27B 110.4 . . ? C28 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? C27 C28 N7 113.0(6) . . ? C27 C28 H28A 109.0 . . ? N7 C28 H28A 109.0 . . ? C27 C28 H28B 109.0 . . ? N7 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C29 N7 C37 110.6(5) . . ? C29 N7 C28 104.7(6) . . ? C37 N7 C28 107.1(5) . . ? C29 N7 Fe2 110.1(4) . . ? C37 N7 Fe2 118.8(5) . . ? C28 N7 Fe2 104.3(4) . . ? N7 C37 C38 115.3(6) . . ? N7 C37 H37A 108.4 . . ? C38 C37 H37A 108.4 . . ? N7 C37 H37B 108.4 . . ? C38 C37 H37B 108.4 . . ? H37A C37 H37B 107.5 . . ? O5 C38 C37 106.9(6) . . ? O5 C38 H38A 110.3 . . ? C37 C38 H38A 110.3 . . ? O5 C38 H38B 110.3 . . ? C37 C38 H38B 110.3 . . ? H38A C38 H38B 108.6 . . ? C38 O5 H5A 109.5 . . ? N6' C26' C25 113.6(13) . . ? N6' C26' H26C 108.8 . . ? C25 C26' H26C 108.8 . . ? N6' C26' H26D 108.8 . . ? C25 C26' H26D 108.8 . . ? H26C C26' H26D 107.7 . . ? C26' N6' C35 116.2(9) . . ? C26' N6' C27' 116.5(14) . . ? C35 N6' C27' 105.7(7) . . ? C26' N6' Fe2 112.5(7) . . ? C35 N6' Fe2 104.4(2) . . ? C27' N6' Fe2 99.6(7) . . ? C28' C27' N6' 110.0(11) . . ? C28' C27' H27C 109.7 . . ? N6' C27' H27C 109.7 . . ? C28' C27' H27D 109.7 . . ? N6' C27' H27D 109.7 . . ? H27C C27' H27D 108.2 . . ? N7' C28' C27' 112.4(11) . . ? N7' C28' H28C 109.1 . . ? C27' C28' H28C 109.1 . . ? N7' C28' H28D 109.1 . . ? C27' C28' H28D 109.1 . . ? H28C C28' H28D 107.9 . . ? C37' N7' C28' 126.0(15) . . ? C37' N7' C29 92.8(15) . . ? C28' N7' C29 116.5(11) . . ? C37' N7' Fe2 110.9(12) . . ? C28' N7' Fe2 102.6(8) . . ? C29 N7' Fe2 107.1(8) . . ? N7' C37' C38' 121.0(16) . . ? N7' C37' H37C 107.1 . . ? C38' C37' H37C 107.1 . . ? N7' C37' H37D 107.1 . . ? C38' C37' H37D 107.1 . . ? H37C C37' H37D 106.8 . . ? O5' C38' C37' 121.5(15) . . ? O5' C38' H38D 107.0 . . ? C37' C38' H38D 107.0 . . ? O5' C38' H38C 107.0 . . ? C37' C38' H38C 107.0 . . ? H38D C38' H38C 106.7 . . ? C38' O5' H5'A 109.5 . . ? C37" N7" C29 113.8(15) . . ? C37" N7" Fe2 105.7(11) . . ? C29 N7" Fe2 107.1(8) . . ? N7" C37" C38" 114.9(15) . . ? N7" C37" H37E 108.5 . . ? C38" C37" H37E 108.5 . . ? N7" C37" H37F 108.5 . . ? C38" C37" H37F 108.5 . . ? H37E C37" H37F 107.5 . . ? O5" C38" C37" 93.0(15) . . ? O5" C38" H38E 113.1 . . ? C37" C38" H38E 113.1 . . ? O5" C38" H38F 113.1 . . ? C37" C38" H38F 113.1 . . ? H38E C38" H38F 110.5 . . ? C38" O5" H5"A 109.5 . . ? N7 C29 C30 109.3(4) . . ? C30 C29 N7' 116.7(5) . . ? C30 C29 N7" 116.7(5) . . ? N7 C29 H29A 109.8 . . ? C30 C29 H29A 109.8 . . ? N7 C29 H29B 109.8 . . ? C30 C29 H29B 109.8 . . ? H29A C29 H29B 108.3 . . ? N8 C30 C31 121.9(4) . . ? N8 C30 C29 115.7(4) . . ? C31 C30 C29 122.2(4) . . ? C32 C31 C30 119.0(4) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C33 C32 C31 119.4(4) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C34 C33 C32 118.6(5) . . ? C34 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? N8 C34 C33 123.1(4) . . ? N8 C34 H34 118.4 . . ? C33 C34 H34 118.4 . . ? N6' C35 C36 108.2(3) . . ? N6 C35 C36 108.2(3) . . ? N6 C35 H35A 110.1 . . ? C36 C35 H35A 110.1 . . ? N6 C35 H35B 110.1 . . ? C36 C35 H35B 110.1 . . ? H35A C35 H35B 108.4 . . ? O3B C36 C35 108.2(3) . . ? O3 C36 C35 108.2(3) . . ? O3 C36 H36A 110.1 . . ? C35 C36 H36A 110.1 . . ? O3 C36 H36B 110.1 . . ? C35 C36 H36B 110.1 . . ? H36A C36 H36B 108.4 . . ? C311 O311 H311 109.5 . . ? O311 C311 H31A 109.5 . . ? O311 C311 H31B 109.5 . . ? H31A C311 H31B 109.5 . . ? O311 C311 H31C 109.5 . . ? H31A C311 H31C 109.5 . . ? H31B C311 H31C 109.5 . . ? C312 O312 H312 109.5 . . ? O312 C312 H31D 109.5 . . ? O312 C312 H31E 109.5 . . ? H31D C312 H31E 109.5 . . ? O312 C312 H31F 109.5 . . ? H31D C312 H31F 109.5 . . ? H31E C312 H31F 109.5 . . ? H1WA O1W H1WB 103(2) . . ? 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 Ce1 O15 2.586(4) . ? Ce1 O7 2.593(4) . ? Ce1 O15' 2.602(14) . ? Ce1 O18 2.603(3) . ? Ce1 O21' 2.603(14) . ? Ce1 O7' 2.606(14) . ? Ce1 O6 2.614(3) . ? Ce1 O6' 2.616(14) . ? Ce1 O18' 2.620(14) . ? Ce1 O9' 2.620(14) . ? Ce1 O9 2.622(3) . ? Ce1 O21 2.622(3) . ? Fe1 O1 1.805(3) . ? Fe1 O2B 1.963(3) . ? Fe1 O2 1.963(3) . ? Fe1 N4 2.138(4) . ? Fe1 N1 2.140(4) . ? Fe1 N2 2.244(4) . ? Fe1 N3 2.249(4) . ? Fe2 O1 1.798(3) . ? Fe2 O3B 1.988(3) . ? Fe2 O3 1.988(3) . ? Fe2 N8 2.157(4) . ? Fe2 N5 2.159(3) . ? Fe2 N7" 2.213(11) . ? Fe2 N7' 2.213(11) . ? Fe2 N6 2.231(3) . ? Fe2 N6' 2.231(3) . ? Fe2 N7 2.246(5) . ? O2 C16 1.421(5) . ? O2 H2O 0.953(14) . ? O3 C36 1.436(5) . ? O3 H2O 1.474(14) . ? O2B C16 1.421(5) . ? O3B C36 1.436(5) . ? O3B H3OB 0.955(14) . ? O4 C18 1.415(6) . ? O4 H4A 0.8400 . ? N1 C5 1.341(6) . ? N1 C1 1.354(6) . ? N2 C6 1.493(5) . ? N2 C7 1.497(6) . ? N2 C17 1.498(6) . ? N3 C15 1.478(7) . ? N3 C8 1.490(6) . ? N3 C9 1.490(6) . ? N4 C10 1.344(6) . ? N4 C14 1.352(7) . ? N5 C25 1.339(6) . ? N5 C21 1.349(5) . ? N8 C30 1.341(5) . ? N8 C34 1.350(6) . ? N9 O8 1.230(6) . ? N9 O6 1.265(9) . ? N9 O7 1.270(9) . ? N9' O8' 1.23(2) . ? N9' O6' 1.26(3) . ? N9' O7' 1.27(3) . ? N10 O11 1.227(6) . ? N10 O10 1.245(8) . ? N10 O9 1.281(8) . ? N10' O11' 1.24(2) . ? N10' O10' 1.26(3) . ? N10' O9' 1.29(3) . ? N11 O13 1.240(7) . ? N11 O12 1.243(6) . ? N11 O14 1.254(6) . ? N11' O12' 1.23(2) . ? N11' O13' 1.24(3) . ? N11' O14' 1.25(2) . ? N12 O17 1.236(6) . ? N12 O16 1.257(8) . ? N12 O15 1.274(7) . ? N12' O17' 1.22(2) . ? N12' O16' 1.26(3) . ? N12' O15' 1.26(3) . ? N13 O20 1.234(6) . ? N13 O19 1.271(8) . ? N13 O18 1.273(7) . ? N13' O20' 1.23(2) . ? N13' O19' 1.27(3) . ? N13' O18' 1.27(3) . ? N14 O23 1.226(7) . ? N14 O21 1.253(7) . ? N14 O22 1.272(6) . ? N14' O23' 1.23(3) . ? N14' O21' 1.25(3) . ? N14' O22' 1.28(3) . ? C1 C2 1.379(7) . ? C1 H1 0.9500 . ? C2 C3 1.391(7) . ? C2 H2 0.9500 . ? C3 C4 1.378(7) . ? C3 H3 0.9500 . ? C4 C5 1.390(6) . ? C4 H4 0.9500 . ? C5 C6 1.502(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.517(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.522(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.389(7) . ? C11 C12 1.376(9) . ? C11 H11 0.9500 . ? C12 C13 1.386(8) . ? C12 H12 0.9500 . ? C13 C14 1.374(7) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.526(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.523(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C21 C22 1.368(6) . ? C21 H21 0.9500 . ? C22 C23 1.389(7) . ? C22 H22 0.9500 . ? C23 C24 1.372(7) . ? C23 H23 0.9500 . ? C24 C25 1.391(6) . ? C24 H24 0.9500 . ? C25 C26 1.495(7) . ? C25 C26' 1.502(12) . ? C26 N6 1.514(9) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? N6 C27 1.478(7) . ? N6 C35 1.481(5) . ? C27 C28 1.488(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 N7 1.514(10) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? N7 C29 1.437(8) . ? N7 C37 1.482(9) . ? C37 C38 1.504(9) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 O5 1.431(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? O5 H5A 0.8400 . ? C26' N6' 1.437(19) . ? C26' H26C 0.9900 . ? C26' H26D 0.9900 . ? N6' C35 1.481(5) . ? N6' C27' 1.561(15) . ? C27' C28' 1.525(17) . ? C27' H27C 0.9900 . ? C27' H27D 0.9900 . ? C28' N7' 1.472(18) . ? C28' H28C 0.9900 . ? C28' H28D 0.9900 . ? N7' C37' 1.42(2) . ? N7' C29 1.55(2) . ? C37' C38' 1.503(19) . ? C37' H37C 0.9900 . ? C37' H37D 0.9900 . ? C38' O5' 1.346(18) . ? C38' H38D 0.9900 . ? C38' H38C 0.9900 . ? O5' H5'A 0.8400 . ? N7" C37" 1.46(2) . ? N7" C29 1.55(2) . ? C37" C38" 1.56(2) . ? C37" H37E 0.9900 . ? C37" H37F 0.9900 . ? C38" O5" 1.451(19) . ? C38" H38E 0.9900 . ? C38" H38F 0.9900 . ? O5" H5"A 0.8400 . ? C29 C30 1.517(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.392(6) . ? C31 C32 1.375(7) . ? C31 H31 0.9500 . ? C32 C33 1.373(7) . ? C32 H32 0.9500 . ? C33 C34 1.372(6) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.521(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? O311 C311 1.374(12) . ? O311 H311 0.8400 . ? C311 H31A 0.9800 . ? C311 H31B 0.9800 . ? C311 H31C 0.9800 . ? O312 C312 1.34(2) . ? O312 H312 0.8400 . ? C312 H31D 0.9800 . ? C312 H31E 0.9800 . ? C312 H31F 0.9800 . ? O1W H1WA 0.961(14) . ? O1W H1WB 0.957(14) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O2^a H2O^a O3^a 0.953(14) 1.474(14) 2.384(4) 158(5) . yes O3B^b H3OB^b O2B^b 0.955(14) 1.481(14) 2.384(4) 156(4) . yes O4 H4A O14^a 0.84 2.11 2.930(6) 166.5 . yes O5^a H5A^a N11^a 0.84 2.60 3.381(7) 155.5 . yes O5^a H5A^a O13^a 0.84 2.09 2.916(7) 169.7 . yes O5^a H5A^a O14^a 0.84 2.61 3.252(7) 133.7 . yes O5'^b H5'A^b O23'^b 0.84 2.20 3.04(7) 172.8 3_556 yes O311^a H311^a O22^a 0.84 2.21 2.796(8) 127.0 . yes O312^b H312^b N9'^b 0.84 2.63 3.30(5) 137.9 . yes O312^b H312^b O6'^b 0.84 2.23 2.94(3) 143.7 . yes O312^b H312^b O22'^b 0.84 2.55 3.27(4) 144.4 . yes O1W^a H1WA^a O311^a 0.961(14) 1.76(3) 2.709(11) 168(10) . yes loop_ _bruker_diffrn_runs_axis _bruker_diffrn_runs_distance _bruker_diffrn_runs_theta _bruker_diffrn_runs_omega _bruker_diffrn_runs_phi _bruker_diffrn_runs_chi _bruker_diffrn_runs_width _bruker_diffrn_runs_images _bruker_diffrn_runs_time _bruker_diffrn_runs_wavelength _bruker_diffrn_runs_voltage _bruker_diffrn_runs_current _bruker_diffrn_runs_temperature Phi 70.00102999999999 0.0 3.1e-05 0.0 54.73995 1.0 180 1.0 0.71073 50.0 1.400488 99.99999999999997 Phi 70.00102999999999 0.0 3.1e-05 180.0 54.73995 1.0 180 1.0 0.71073 50.0 1.401418 99.99999999999997 Omega 70.00102999999999 9.819 358.373 359.9999 -44.49990000000004 0.5 272 5.0 0.71073 50.0 1.40065 99.99999999999997 Phi 70.00102999999999 9.819 358.373 345.2669 -44.49990000000004 0.5 269 5.0 0.71073 50.0 1.40034 99.99999999999997 Omega 70.00102999999999 9.819 358.373 51.00053 -44.49990000000004 0.5 272 5.0 0.71073 50.0 1.401636 99.99999999999997 Phi 70.00102999999999 9.819 340.6472 103.5671 -23.999899999999993 -0.5 269 5.0 0.71073 50.0 1.400114 99.99999999999997