#------------------------------------------------------------------------------ #$Date: 2021-09-01 02:02:28 +0300 (Wed, 01 Sep 2021) $ #$Revision: 268337 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/81/7708159.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_7708159 loop_ _publ_author_name 'Ye, Hua-Jian' 'Zhang, Tian' 'Huang, Shu-Yuan' 'Liu, Xiao-Ling' 'Chen, Wen-Bin' 'Zhang, Yi-Quan' 'Tang, Jinkui' 'Dong, Wen' _publ_section_title ; Syntheses, structural modulation and slow magnetic relaxation of three dysprosium(III) complexes with mononuclear, dinuclear and one-dimensional structures ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT02532E _journal_year 2021 _chemical_formula_moiety 'C32 H28 Dy2 N10 O20, 5(H2 O), 2(C2 H3 N)' _chemical_formula_sum 'C36 H44 Dy2 N12 O25' _chemical_formula_weight 1369.83 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2021-08-25 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _audit_update_record ; 2021-08-26 deposited with the CCDC. 2021-08-30 downloaded from the CCDC. ; _cell_angle_alpha 103.705(2) _cell_angle_beta 90.636(2) _cell_angle_gamma 106.159(2) _cell_formula_units_Z 1 _cell_length_a 9.6507(3) _cell_length_b 11.3380(2) _cell_length_c 11.8034(4) _cell_measurement_reflns_used 9688 _cell_measurement_temperature 105.88(10) _cell_measurement_theta_max 75.7670 _cell_measurement_theta_min 3.8760 _cell_volume 1201.07(6) _computing_cell_refinement 'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 105.88(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.957 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 24.00 117.00 0.50 0.05 -- 45.87 77.00 -90.00 186 2 \w 92.00 119.00 0.50 0.05 -- 45.87 77.00-150.00 54 3 \w 69.00 94.00 0.50 0.05 -- 45.87 142.00-101.00 50 4 \w 24.00 87.00 0.50 0.05 -- 45.87 77.00-150.00 126 5 \w 90.00 178.00 0.50 0.05 -- 106.06 15.00 -30.00 176 6 \w 117.00 164.00 0.50 0.05 -- 106.06 45.00 0.00 94 7 \w 95.00 120.00 0.50 0.05 -- 106.06 142.00-101.00 50 8 \w 85.00 128.00 0.50 0.05 -- 106.06 127.00 88.00 86 9 \w 37.00 73.00 0.50 0.05 -- 106.06 -61.00-150.00 72 10 \w 68.00 102.00 0.50 0.05 -- 106.06 -94.00-150.00 68 11 \w 92.00 123.00 0.50 0.05 -- 106.06-142.00-157.00 62 12 \w 55.00 111.00 0.50 0.05 -- 106.06-125.00-120.00 112 13 \w 58.00 112.00 0.50 0.05 -- 106.06-125.00 -30.00 108 14 \w 71.00 97.00 0.50 0.05 -- 106.06 -94.00 30.00 52 15 \w 46.00 112.00 0.50 0.05 -- 106.06-127.00 12.00 132 16 \w 53.00 93.00 0.50 0.05 -- 45.87-127.00 12.00 80 17 \w 36.00 111.00 0.50 0.05 -- 106.06-125.00 30.00 150 18 \w 34.00 66.00 0.50 0.05 -- 106.06 -94.00 30.00 64 19 \w 33.00 69.00 0.50 0.05 -- 106.06 -61.00 30.00 72 20 \w 34.00 73.00 0.50 0.05 -- 106.06 -61.00 150.00 78 21 \w 40.00 73.00 0.50 0.05 -- 106.06 -61.00-120.00 66 22 \w 33.00 67.00 0.50 0.05 -- 106.06 -77.00-150.00 68 23 \w 47.00 87.00 0.50 0.05 -- 106.06-142.00-157.00 80 24 \w 35.00 100.00 0.50 0.05 -- 45.87-142.00-157.00 130 25 \w -55.00 -29.00 0.50 0.05 -- -102.00 61.00 120.00 52 26 \w -68.00 -30.00 0.50 0.05 -- -102.00 61.00 60.00 76 27 \w -88.00 -38.00 0.50 0.05 -- -45.87 127.00 88.00 100 28 \w -63.00 -31.00 0.50 0.05 -- -102.00 61.00-150.00 64 29 \w -86.00 -61.00 0.50 0.05 -- -45.87 142.00-101.00 50 30 \w -124.00 -98.00 0.50 0.05 -- -102.00 142.00-101.00 52 31 \w -111.00 -35.00 0.50 0.05 -- -102.00 127.00 88.00 152 32 \w -97.00 -29.00 0.50 0.05 -- -102.00 77.00 120.00 136 33 \w -141.00 -93.00 0.50 0.05 -- -102.00 -30.00 60.00 96 34 \w -104.00 -78.00 0.50 0.05 -- -45.87-127.00 12.00 52 35 \w -101.00 -76.00 0.50 0.05 -- -45.87-125.00 30.00 50 36 \w -111.00 -86.00 0.50 0.05 -- -45.87-125.00 90.00 50 37 \w -110.00 -85.00 0.50 0.05 -- -102.00-127.00 12.00 50 38 \w -145.00-112.00 0.50 0.05 -- -102.00 -77.00 -60.00 66 39 \w -117.00 -63.00 0.50 0.05 -- -45.87-142.00-157.00 108 40 \w -142.00-116.00 0.50 0.05 -- -102.00-142.00-157.00 52 41 \w -172.00 -29.00 0.50 0.05 -- -102.00 0.00-180.00 286 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1133099000 _diffrn_orient_matrix_UB_12 -0.0130545000 _diffrn_orient_matrix_UB_13 0.0855329000 _diffrn_orient_matrix_UB_21 -0.0819719000 _diffrn_orient_matrix_UB_22 0.0481737000 _diffrn_orient_matrix_UB_23 0.1039214000 _diffrn_orient_matrix_UB_31 -0.0908461000 _diffrn_orient_matrix_UB_32 -0.1373102000 _diffrn_orient_matrix_UB_33 -0.0075151000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_unetI/netI 0.0519 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.957 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 14773 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.957 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.391 _diffrn_reflns_theta_min 3.868 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 17.346 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.17858 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.894 _exptl_crystal_description block _exptl_crystal_F_000 676 _exptl_crystal_size_max 0.287 _exptl_crystal_size_mid 0.199 _exptl_crystal_size_min 0.092 _refine_diff_density_max 2.654 _refine_diff_density_min -1.277 _refine_diff_density_rms 0.147 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 350 _refine_ls_number_reflns 4814 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0419 _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^)+(0.0827P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1138 _refine_ls_wR_factor_ref 0.1150 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4539 _reflns_number_total 4814 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02532e2.cif _cod_data_source_block exp_646 _cod_database_code 7708159 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C H O N Dy' _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. ; _reflns_odcompleteness_completeness 99.98 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, {H9A,H9B} of O9, H13B of O13, All N(H) groups At 1.5 times of: All C(H,H,H) groups, H8 of O8, H5 of O5, {H10A,H10B} of O10, H1 of O1, {H11A,H11B} of O11, {H12A,H12B} of O12, H13A of O13 2. Restrained distances O9-H9B 0.85 with sigma of 0.02 H10B-H9B 3 with sigma of 0.02 H9B-H9A 1.38 with sigma of 0.02 O10-H9B 3 with sigma of 0.02 3. Others Fixed Sof: O11(0.5) H11A(0.5) H11B(0.5) 4.a Riding coordinates: O9(H9A,H9B), O10(H10A,H10B), O12(H12A,H12B), O13(H13A,H13B) 4.b Free rotating group: O11(H11A,H11B) 4.c Aromatic/amide H refined with riding coordinates: N5(H5A), C4(H4), C5(H5B), C9(H9), C13(H13), C14(H14), C15(H15) 4.d Idealised Me refined as rotating group: C17(H17A,H17B,H17C) 4.e Idealised tetrahedral OH refined as rotating group: O1(H1), O5(H5), O8(H8) ; _shelx_res_file ; TITL exp_646_a.res in P-1 exp_646.res created by SHELXL-2018/3 at 23:59:02 on 25-Aug-2021 REM Old TITL exp_646 in P-1 #2 REM SHELXT solution in P-1: R1 0.061, Rweak 0.013, Alpha 0.043 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C18 N10 O9 Dy CELL 1.54184 9.6507 11.338 11.8034 103.705 90.636 106.159 ZERR 1 0.0003 0.0002 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H Dy N O UNIT 36 44 2 12 25 DFIX 0.85 O9 H9b DFIX 3 H10b H9b DFIX 1.38 H9b H9a DFIX 3 O10 H9b L.S. 100 PLAN 5 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.082700 FVAR 0.49810 DY1 3 0.580576 0.676694 0.554791 11.00000 0.01824 0.01326 = 0.01688 0.00429 0.00169 0.00410 O1 5 1.127693 0.582780 0.690053 11.00000 0.01917 0.02270 = 0.03055 0.01154 -0.00140 0.00244 AFIX 147 H1 2 1.138079 0.641636 0.658741 11.00000 -1.50000 AFIX 0 O2 5 1.058020 0.724127 0.584635 11.00000 0.01896 0.01889 = 0.03113 0.01097 0.00242 0.00218 O3 5 0.828175 0.718195 0.559992 11.00000 0.01668 0.01853 = 0.02864 0.00917 0.00152 0.00361 O4 5 0.635882 0.480543 0.531762 11.00000 0.01872 0.01473 = 0.01745 0.00304 0.00129 0.00724 O5 5 0.534651 0.295226 0.080774 11.00000 0.04505 0.02602 = 0.02445 0.00376 0.00776 0.01068 AFIX 147 H5 2 0.488583 0.306309 0.138334 11.00000 -1.50000 AFIX 0 O6 5 0.513233 0.414514 0.288344 11.00000 0.02835 0.02017 = 0.01687 0.00539 0.00438 0.00896 O7 5 0.630814 0.620363 0.354133 11.00000 0.02493 0.01784 = 0.02082 0.00457 0.00320 0.00641 O8 5 0.750848 0.747355 0.214838 11.00000 0.05333 0.02439 = 0.02708 0.00926 0.01359 0.00559 AFIX 147 H8 2 0.719810 0.733819 0.276346 11.00000 -1.50000 AFIX 0 O9 5 0.402825 0.774221 0.652149 11.00000 0.02750 0.02116 = 0.02209 0.00983 0.00757 0.01063 AFIX 3 H9A 2 0.405045 0.842451 0.633099 11.00000 -1.20000 H9B 2 0.356075 0.753031 0.702059 11.00000 -1.20000 AFIX 0 O10 5 0.685244 0.821639 0.742460 11.00000 0.02950 0.02462 = 0.02464 -0.00015 -0.00116 0.01160 AFIX 3 H10A 2 0.766534 0.818259 0.767930 11.00000 -1.50000 H10B 2 0.661944 0.881309 0.781440 11.00000 -1.50000 AFIX 0 N1 4 0.578821 0.261220 0.587139 11.00000 0.01957 0.01497 = 0.01796 0.00273 0.00258 0.00430 N2 4 0.541126 0.157762 0.622584 11.00000 0.01988 0.01610 = 0.02117 0.00611 0.00382 0.00424 N3 4 0.324353 0.116148 0.495063 11.00000 0.02134 0.01522 = 0.02583 0.00696 0.00004 0.00713 N4 4 0.334572 -0.018448 0.606253 11.00000 0.01846 0.01566 = 0.02549 0.00660 0.00360 0.00553 N5 4 0.206051 -0.057513 0.541107 11.00000 0.01740 0.01865 = 0.02851 0.00976 0.00226 0.00254 AFIX 43 H5A 2 0.137424 -0.124678 0.541505 11.00000 -1.20000 AFIX 0 C1 1 0.922622 0.669634 0.583213 11.00000 0.02107 0.01629 = 0.01863 0.00351 0.00473 0.00393 C2 1 0.884038 0.545249 0.614820 11.00000 0.01889 0.01597 = 0.01691 0.00392 0.00233 0.00598 C3 1 0.990897 0.510517 0.670087 11.00000 0.02054 0.01889 = 0.01974 0.00404 0.00292 0.00265 C4 1 0.957784 0.397800 0.709743 11.00000 0.02230 0.02340 = 0.02113 0.00905 0.00004 0.00711 AFIX 43 H4 2 1.028209 0.380255 0.751992 11.00000 -1.20000 AFIX 0 C5 1 0.821938 0.315539 0.685375 11.00000 0.02448 0.01979 = 0.02096 0.00711 0.00194 0.00693 AFIX 43 H5B 2 0.800197 0.241071 0.710385 11.00000 -1.20000 AFIX 0 C6 1 0.713609 0.342128 0.622469 11.00000 0.01905 0.01702 = 0.01981 0.00669 0.00462 0.00423 C7 1 0.740964 0.458914 0.587322 11.00000 0.01813 0.01714 = 0.01327 0.00327 0.00351 0.00494 C8 1 0.401816 0.086319 0.575321 11.00000 0.01892 0.01837 = 0.01903 0.00559 0.00575 0.00602 C9 1 0.201345 0.023262 0.476262 11.00000 0.02030 0.01804 = 0.02654 0.00622 0.00384 0.00369 AFIX 43 H9 2 0.123221 0.015489 0.425372 11.00000 -1.20000 AFIX 0 C10 1 0.592924 0.518219 0.273114 11.00000 0.01903 0.02390 = 0.02008 0.00866 0.00371 0.00946 C11 1 0.642130 0.521479 0.155228 11.00000 0.02548 0.02598 = 0.02010 0.00942 0.00689 0.01220 C12 1 0.719639 0.635695 0.130812 11.00000 0.03263 0.02943 = 0.02415 0.00597 0.00408 0.01342 C13 1 0.764180 0.639147 0.019875 11.00000 0.04320 0.03405 = 0.03013 0.01837 0.01356 0.00968 AFIX 43 H13 2 0.813745 0.715639 0.003921 11.00000 -1.20000 AFIX 0 C14 1 0.733599 0.526757 -0.066741 11.00000 0.04087 0.04313 = 0.02077 0.01169 0.01343 0.01665 AFIX 43 H14 2 0.765009 0.528907 -0.140628 11.00000 -1.20000 AFIX 0 C15 1 0.658439 0.412379 -0.046969 11.00000 0.04446 0.03933 = 0.01815 0.00555 0.00962 0.01979 AFIX 43 H15 2 0.638998 0.338145 -0.106382 11.00000 -1.20000 AFIX 0 C16 1 0.611731 0.409914 0.064483 11.00000 0.03308 0.02888 = 0.02343 0.00938 0.00522 0.01146 AFIX 6 O11 5 1.023044 0.914701 0.234488 10.50000 0.03040 0.03974 = 0.04309 0.01983 -0.00619 -0.00363 H11A 2 0.944553 0.854712 0.216993 10.50000 -1.50000 H11B 2 1.009712 0.981631 0.221709 10.50000 -1.50000 AFIX 0 O12 5 0.616566 0.043224 0.805865 11.00000 0.06568 0.03613 = 0.04914 0.00640 0.00142 0.02368 AFIX 3 H12A 2 0.603706 0.091684 0.764885 11.00000 -1.50000 H12B 2 0.543966 0.032164 0.851665 11.00000 -1.50000 AFIX 0 O13 5 0.365923 0.081764 0.904400 11.00000 0.07642 0.04679 = 0.03477 -0.00306 -0.00488 0.01977 AFIX 3 H13A 2 0.315773 0.098194 0.853780 11.00000 -1.50000 H13B 2 0.415443 0.147004 0.952470 11.00000 -1.20000 AFIX 0 N6 4 1.029972 0.140148 0.149091 11.00000 0.03917 0.08651 = 0.04674 0.01866 -0.00151 0.01766 C17 1 0.837756 0.197450 0.038609 11.00000 0.06955 0.13987 = 0.05135 -0.00789 -0.02008 0.06076 AFIX 137 H17A 2 0.823969 0.149028 -0.041388 11.00000 -1.50000 H17B 2 0.868720 0.286274 0.041312 11.00000 -1.50000 H17C 2 0.748226 0.177970 0.074549 11.00000 -1.50000 AFIX 0 C18 1 0.947085 0.165833 0.101097 11.00000 0.03338 0.09112 = 0.03554 0.00287 0.00305 0.01534 HKLF 4 REM exp_646_a.res in P-1 REM wR2 = 0.1150, GooF = S = 1.077, Restrained GooF = 1.080 for all data REM R1 = 0.0419 for 4539 Fo > 4sig(Fo) and 0.0438 for all 4814 data REM 350 parameters refined using 4 restraints END WGHT 0.0827 0.0000 REM Highest difference peak 2.654, deepest hole -1.277, 1-sigma level 0.147 Q1 1 0.5803 0.6997 0.6408 11.00000 0.05 2.65 Q2 1 0.5829 0.6551 0.4609 11.00000 0.05 2.38 Q3 1 0.4601 0.0360 0.8933 11.00000 0.05 0.88 Q4 1 0.5066 0.5984 0.5458 11.00000 0.05 0.88 Q5 1 0.6568 0.7540 0.5628 11.00000 0.05 0.86 ; _shelx_res_checksum 3997 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 4.136 _oxdiff_exptl_absorpt_empirical_full_min 0.448 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 Dy1 Dy 0.58058(2) 0.67669(2) 0.55479(2) 0.01613(11) Uani 1 1 d . . . . . O1 O 1.1277(3) 0.5828(3) 0.6901(3) 0.0241(6) Uani 1 1 d . . . . . H1 H 1.138079 0.641636 0.658741 0.036 Uiso 1 1 calc R U . . . O2 O 1.0580(3) 0.7241(3) 0.5846(3) 0.0228(6) Uani 1 1 d . . . . . O3 O 0.8282(3) 0.7182(3) 0.5600(3) 0.0210(6) Uani 1 1 d . . . . . O4 O 0.6359(3) 0.4805(3) 0.5318(2) 0.0166(5) Uani 1 1 d . . . . . O5 O 0.5347(4) 0.2952(3) 0.0808(3) 0.0322(8) Uani 1 1 d . . . . . H5 H 0.488583 0.306309 0.138334 0.048 Uiso 1 1 calc R U . . . O6 O 0.5132(3) 0.4145(3) 0.2883(2) 0.0212(6) Uani 1 1 d . . . . . O7 O 0.6308(3) 0.6204(3) 0.3541(3) 0.0212(6) Uani 1 1 d . . . . . O8 O 0.7508(5) 0.7474(3) 0.2148(3) 0.0355(8) Uani 1 1 d . . . . . H8 H 0.719810 0.733819 0.276346 0.053 Uiso 1 1 calc R U . . . O9 O 0.4028(3) 0.7742(3) 0.6521(3) 0.0220(6) Uani 1 1 d D . . . . H9A H 0.405045 0.842451 0.633099 0.026 Uiso 1 1 d DR U . . . H9B H 0.356075 0.753031 0.702059 0.026 Uiso 1 1 d DR U . . . O10 O 0.6852(3) 0.8216(3) 0.7425(3) 0.0266(7) Uani 1 1 d D . . . . H10A H 0.766534 0.818259 0.767930 0.040 Uiso 1 1 d R U . . . H10B H 0.661944 0.881309 0.781440 0.040 Uiso 1 1 d DR U . . . N1 N 0.5788(4) 0.2612(3) 0.5871(3) 0.0179(7) Uani 1 1 d . . . . . N2 N 0.5411(4) 0.1578(3) 0.6226(3) 0.0190(7) Uani 1 1 d . . . . . N3 N 0.3244(4) 0.1161(3) 0.4951(3) 0.0201(7) Uani 1 1 d . . . . . N4 N 0.3346(4) -0.0184(3) 0.6063(3) 0.0195(7) Uani 1 1 d . . . . . N5 N 0.2061(4) -0.0575(3) 0.5411(3) 0.0214(7) Uani 1 1 d . . . . . H5A H 0.137424 -0.124678 0.541505 0.026 Uiso 1 1 calc R U . . . C1 C 0.9226(5) 0.6696(4) 0.5832(4) 0.0191(8) Uani 1 1 d . . . . . C2 C 0.8840(4) 0.5452(4) 0.6148(3) 0.0171(8) Uani 1 1 d . . . . . C3 C 0.9909(5) 0.5105(4) 0.6701(4) 0.0205(8) Uani 1 1 d . . . . . C4 C 0.9578(5) 0.3978(4) 0.7097(4) 0.0216(8) Uani 1 1 d . . . . . H4 H 1.028209 0.380255 0.751992 0.026 Uiso 1 1 calc R U . . . C5 C 0.8219(5) 0.3155(4) 0.6854(4) 0.0213(8) Uani 1 1 d . . . . . H5B H 0.800197 0.241071 0.710385 0.026 Uiso 1 1 calc R U . . . C6 C 0.7136(4) 0.3421(4) 0.6225(4) 0.0184(8) Uani 1 1 d . . . . . C7 C 0.7410(4) 0.4589(4) 0.5873(3) 0.0163(7) Uani 1 1 d . . . . . C8 C 0.4018(4) 0.0863(4) 0.5753(4) 0.0184(8) Uani 1 1 d . . . . . C9 C 0.2013(5) 0.0233(4) 0.4763(4) 0.0219(8) Uani 1 1 d . . . . . H9 H 0.123221 0.015489 0.425372 0.026 Uiso 1 1 calc R U . . . C10 C 0.5929(4) 0.5182(4) 0.2731(4) 0.0198(8) Uani 1 1 d . . . . . C11 C 0.6421(5) 0.5215(4) 0.1552(4) 0.0222(9) Uani 1 1 d . . . . . C12 C 0.7196(5) 0.6357(5) 0.1308(4) 0.0279(10) Uani 1 1 d . . . . . C13 C 0.7642(6) 0.6391(5) 0.0199(4) 0.0342(11) Uani 1 1 d . . . . . H13 H 0.813745 0.715639 0.003921 0.041 Uiso 1 1 calc R U . . . C14 C 0.7336(6) 0.5268(5) -0.0667(4) 0.0333(11) Uani 1 1 d . . . . . H14 H 0.765009 0.528907 -0.140628 0.040 Uiso 1 1 calc R U . . . C15 C 0.6584(6) 0.4124(5) -0.0470(4) 0.0326(11) Uani 1 1 d . . . . . H15 H 0.638998 0.338145 -0.106382 0.039 Uiso 1 1 calc R U . . . C16 C 0.6117(5) 0.4099(5) 0.0645(4) 0.0274(10) Uani 1 1 d . . . . . O11 O 1.0230(8) 0.9147(8) 0.2345(7) 0.0390(17) Uani 0.5 1 d G . P . . H11A H 0.944553 0.854712 0.216993 0.059 Uiso 0.5 1 d G U P . . H11B H 1.009712 0.981631 0.221709 0.059 Uiso 0.5 1 d G U P . . O12 O 0.6166(5) 0.0432(4) 0.8059(4) 0.0492(10) Uani 1 1 d . . . . . H12A H 0.603706 0.091684 0.764885 0.074 Uiso 1 1 d R U . . . H12B H 0.543966 0.032164 0.851665 0.074 Uiso 1 1 d R U . . . O13 O 0.3659(6) 0.0818(4) 0.9044(4) 0.0547(11) Uani 1 1 d . . . . . H13A H 0.315773 0.098194 0.853780 0.082 Uiso 1 1 d R U . . . H13B H 0.415443 0.147004 0.952470 0.066 Uiso 1 1 d R U . . . N6 N 1.0300(6) 0.1401(7) 0.1491(5) 0.0573(15) Uani 1 1 d . . . . . C17 C 0.8378(10) 0.1974(11) 0.0386(7) 0.086(3) Uani 1 1 d . . . . . H17A H 0.823969 0.149028 -0.041388 0.130 Uiso 1 1 calc R U . . . H17B H 0.868720 0.286274 0.041312 0.130 Uiso 1 1 calc R U . . . H17C H 0.748226 0.177970 0.074549 0.130 Uiso 1 1 calc R U . . . C18 C 0.9471(7) 0.1658(8) 0.1011(5) 0.0562(18) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01824(15) 0.01326(15) 0.01688(15) 0.00429(9) 0.00169(9) 0.00410(10) O1 0.0192(15) 0.0227(15) 0.0305(17) 0.0115(13) -0.0014(12) 0.0024(12) O2 0.0190(15) 0.0189(14) 0.0311(16) 0.0110(12) 0.0024(12) 0.0022(12) O3 0.0167(14) 0.0185(14) 0.0286(16) 0.0092(12) 0.0015(11) 0.0036(11) O4 0.0187(14) 0.0147(13) 0.0175(13) 0.0030(10) 0.0013(10) 0.0072(11) O5 0.045(2) 0.0260(17) 0.0245(17) 0.0038(13) 0.0078(15) 0.0107(15) O6 0.0283(16) 0.0202(14) 0.0169(14) 0.0054(11) 0.0044(11) 0.0090(12) O7 0.0249(15) 0.0178(14) 0.0208(15) 0.0046(11) 0.0032(11) 0.0064(12) O8 0.053(2) 0.0244(17) 0.0271(18) 0.0093(14) 0.0136(16) 0.0056(16) O9 0.0275(16) 0.0212(14) 0.0221(15) 0.0098(12) 0.0076(12) 0.0106(12) O10 0.0295(17) 0.0246(15) 0.0246(16) -0.0001(12) -0.0012(12) 0.0116(13) N1 0.0196(17) 0.0150(16) 0.0180(17) 0.0027(13) 0.0026(13) 0.0043(13) N2 0.0199(17) 0.0161(16) 0.0212(17) 0.0061(13) 0.0038(13) 0.0042(13) N3 0.0213(17) 0.0152(16) 0.0258(18) 0.0070(14) 0.0000(14) 0.0071(14) N4 0.0185(17) 0.0157(16) 0.0255(18) 0.0066(14) 0.0036(14) 0.0055(13) N5 0.0174(17) 0.0186(17) 0.0285(19) 0.0098(14) 0.0023(14) 0.0025(14) C1 0.021(2) 0.0163(19) 0.0186(19) 0.0035(15) 0.0047(15) 0.0039(16) C2 0.0189(19) 0.0160(18) 0.0169(19) 0.0039(15) 0.0023(14) 0.0060(15) C3 0.021(2) 0.019(2) 0.020(2) 0.0040(15) 0.0029(15) 0.0027(16) C4 0.022(2) 0.023(2) 0.021(2) 0.0090(16) 0.0000(15) 0.0071(17) C5 0.024(2) 0.020(2) 0.021(2) 0.0071(16) 0.0019(16) 0.0069(17) C6 0.019(2) 0.0170(18) 0.020(2) 0.0067(15) 0.0046(15) 0.0042(15) C7 0.0181(19) 0.0171(18) 0.0133(18) 0.0033(14) 0.0035(14) 0.0049(15) C8 0.0189(19) 0.0184(19) 0.0190(19) 0.0056(15) 0.0058(15) 0.0060(16) C9 0.020(2) 0.0180(19) 0.027(2) 0.0062(17) 0.0038(16) 0.0037(16) C10 0.019(2) 0.024(2) 0.020(2) 0.0087(16) 0.0037(15) 0.0095(17) C11 0.025(2) 0.026(2) 0.020(2) 0.0094(17) 0.0069(16) 0.0122(18) C12 0.033(2) 0.029(2) 0.024(2) 0.0060(19) 0.0041(18) 0.013(2) C13 0.043(3) 0.034(3) 0.030(3) 0.018(2) 0.014(2) 0.010(2) C14 0.041(3) 0.043(3) 0.021(2) 0.012(2) 0.013(2) 0.017(2) C15 0.044(3) 0.039(3) 0.018(2) 0.0056(19) 0.0096(19) 0.020(2) C16 0.033(2) 0.029(2) 0.023(2) 0.0094(18) 0.0052(18) 0.011(2) O11 0.030(4) 0.040(4) 0.043(4) 0.020(3) -0.006(3) -0.004(3) O12 0.066(3) 0.036(2) 0.049(2) 0.0064(18) 0.001(2) 0.024(2) O13 0.076(3) 0.047(2) 0.035(2) -0.0031(18) -0.005(2) 0.020(2) N6 0.039(3) 0.087(4) 0.047(3) 0.019(3) -0.002(2) 0.018(3) C17 0.070(5) 0.140(9) 0.051(4) -0.008(5) -0.020(4) 0.061(6) C18 0.033(3) 0.091(5) 0.036(3) 0.003(3) 0.003(2) 0.015(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 -6 1 0.1294 -1 -3 7 0.0915 1 0 7 0.0496 0 0 -7 0.0325 0 0 7 0.0548 6 0 2 0.1026 1 -7 3 0.1193 -3 -3 6 0.1163 -5 -2 -1 0.1179 -4 6 -4 0.0805 3 5 -1 0.1453 2 6 -1 0.1447 3 5 -5 0.1302 -2 2 6 0.0556 2 -3 -6 0.0545 0 -6 -3 0.0998 -6 0 0 0.1071 5 -5 4 0.0818 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Dy1 Dy1 107.29(7) . 2_666 ? O3 Dy1 O4 141.57(10) . 2_666 ? O3 Dy1 O4 72.04(10) . . ? O3 Dy1 O6 110.94(10) . 2_666 ? O3 Dy1 O7 75.17(11) . . ? O3 Dy1 O9 138.16(10) . . ? O3 Dy1 O10 71.61(11) . . ? O3 Dy1 N1 125.68(11) . 2_666 ? O3 Dy1 N3 73.47(11) . 2_666 ? O4 Dy1 Dy1 37.73(7) 2_666 2_666 ? O4 Dy1 Dy1 37.42(7) . 2_666 ? O4 Dy1 O4 75.15(11) 2_666 . ? O4 Dy1 O6 76.15(10) 2_666 2_666 ? O4 Dy1 O6 71.61(10) . 2_666 ? O4 Dy1 O7 77.67(10) 2_666 . ? O4 Dy1 O7 75.34(10) . . ? O4 Dy1 O9 136.77(10) . . ? O4 Dy1 O9 80.15(10) 2_666 . ? O4 Dy1 O10 110.93(10) . . ? O4 Dy1 O10 140.54(10) 2_666 . ? O4 Dy1 N1 128.01(10) . 2_666 ? O4 Dy1 N1 63.77(10) 2_666 2_666 ? O4 Dy1 N3 139.56(11) . 2_666 ? O4 Dy1 N3 124.91(11) 2_666 2_666 ? O6 Dy1 Dy1 69.50(7) 2_666 2_666 ? O6 Dy1 O9 68.32(10) 2_666 . ? O6 Dy1 O10 69.79(11) 2_666 . ? O6 Dy1 N1 123.12(11) 2_666 2_666 ? O6 Dy1 N3 142.03(11) 2_666 2_666 ? O7 Dy1 Dy1 72.88(7) . 2_666 ? O7 Dy1 O6 141.97(10) . 2_666 ? O7 Dy1 O9 132.68(10) . . ? O7 Dy1 O10 141.71(11) . . ? O7 Dy1 N1 66.21(11) . 2_666 ? O7 Dy1 N3 75.98(11) . 2_666 ? O9 Dy1 Dy1 110.72(7) . 2_666 ? O9 Dy1 N1 66.52(10) . 2_666 ? O9 Dy1 N3 83.60(11) . 2_666 ? O10 Dy1 Dy1 135.36(8) . 2_666 ? O10 Dy1 O9 69.30(10) . . ? O10 Dy1 N1 120.99(11) . 2_666 ? O10 Dy1 N3 76.78(11) . 2_666 ? N1 Dy1 Dy1 96.43(7) 2_666 2_666 ? N3 Dy1 Dy1 147.31(8) 2_666 2_666 ? N3 Dy1 N1 61.44(11) 2_666 2_666 ? C3 O1 H1 109.5 . . ? C1 O3 Dy1 138.6(3) . . ? Dy1 O4 Dy1 104.85(11) 2_666 . ? C7 O4 Dy1 124.3(2) . 2_666 ? C7 O4 Dy1 127.5(2) . . ? C16 O5 H5 109.5 . . ? C10 O6 Dy1 139.4(3) . 2_666 ? C10 O7 Dy1 134.0(3) . . ? C12 O8 H8 109.5 . . ? Dy1 O9 H9A 111.6 . . ? Dy1 O9 H9B 126.2 . . ? H9A O9 H9B 121.6 . . ? Dy1 O10 H10A 116.6 . . ? Dy1 O10 H10B 130.4 . . ? H10A O10 H10B 112.2 . . ? N2 N1 Dy1 124.9(3) . 2_666 ? N2 N1 C6 118.3(4) . . ? C6 N1 Dy1 116.7(3) . 2_666 ? N1 N2 C8 109.9(3) . . ? C8 N3 Dy1 119.2(3) . 2_666 ? C9 N3 Dy1 137.2(3) . 2_666 ? C9 N3 C8 102.9(4) . . ? C8 N4 N5 102.3(3) . . ? N4 N5 H5A 124.9 . . ? C9 N5 N4 110.2(3) . . ? C9 N5 H5A 124.9 . . ? O2 C1 C2 115.8(4) . . ? O3 C1 O2 122.5(4) . . ? O3 C1 C2 121.7(4) . . ? C3 C2 C1 119.4(4) . . ? C3 C2 C7 119.3(4) . . ? C7 C2 C1 121.3(4) . . ? O1 C3 C2 121.8(4) . . ? O1 C3 C4 116.5(4) . . ? C2 C3 C4 121.7(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 120.3 . . ? C4 C5 H5B 119.6 . . ? C4 C5 C6 120.7(4) . . ? C6 C5 H5B 119.6 . . ? N1 C6 C5 124.5(4) . . ? N1 C6 C7 114.2(4) . . ? C5 C6 C7 121.3(4) . . ? O4 C7 C2 123.7(4) . . ? O4 C7 C6 119.0(4) . . ? C2 C7 C6 117.3(4) . . ? N3 C8 N2 124.1(4) . . ? N4 C8 N2 121.3(4) . . ? N4 C8 N3 114.6(4) . . ? N3 C9 N5 110.0(4) . . ? N3 C9 H9 125.0 . . ? N5 C9 H9 125.0 . . ? O6 C10 O7 123.0(4) . . ? O6 C10 C11 118.6(4) . . ? O7 C10 C11 118.4(4) . . ? C12 C11 C10 121.0(4) . . ? C12 C11 C16 118.2(4) . . ? C16 C11 C10 120.9(4) . . ? O8 C12 C11 120.9(4) . . ? O8 C12 C13 118.0(4) . . ? C13 C12 C11 121.0(5) . . ? C12 C13 H13 120.5 . . ? C14 C13 C12 119.0(5) . . ? C14 C13 H13 120.5 . . ? C13 C14 H14 118.9 . . ? C15 C14 C13 122.1(4) . . ? C15 C14 H14 118.9 . . ? C14 C15 H15 120.7 . . ? C14 C15 C16 118.6(5) . . ? C16 C15 H15 120.7 . . ? O5 C16 C11 121.7(4) . . ? O5 C16 C15 117.2(4) . . ? C15 C16 C11 121.1(5) . . ? H11A O11 H11B 109.4 . . ? H12A O12 H12B 107.7 . . ? H13A O13 H13B 112.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? N6 C18 C17 179.2(10) . . ? 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 Dy1 Dy1 3.7652(4) 2_666 ? Dy1 O3 2.300(3) . ? Dy1 O4 2.384(3) . ? Dy1 O4 2.367(3) 2_666 ? Dy1 O6 2.396(3) 2_666 ? Dy1 O7 2.394(3) . ? Dy1 O9 2.446(3) . ? Dy1 O10 2.435(3) . ? Dy1 N1 2.602(4) 2_666 ? Dy1 N3 2.484(3) 2_666 ? O1 H1 0.8200 . ? O1 C3 1.330(5) . ? O2 C1 1.279(5) . ? O3 C1 1.247(5) . ? O4 C7 1.311(5) . ? O5 H5 0.8200 . ? O5 C16 1.365(6) . ? O6 C10 1.267(5) . ? O7 C10 1.273(5) . ? O8 H8 0.8200 . ? O8 C12 1.365(6) . ? O9 H9A 0.8502 . ? O9 H9B 0.7880 . ? O10 H10A 0.8510 . ? O10 H10B 0.8121 . ? N1 N2 1.297(5) . ? N1 C6 1.360(5) . ? N2 C8 1.392(5) . ? N3 C8 1.359(5) . ? N3 C9 1.325(6) . ? N4 N5 1.356(5) . ? N4 C8 1.322(5) . ? N5 H5A 0.8600 . ? N5 C9 1.335(6) . ? C1 C2 1.492(6) . ? C2 C3 1.406(6) . ? C2 C7 1.434(6) . ? C3 C4 1.419(6) . ? C4 H4 0.9300 . ? C4 C5 1.362(6) . ? C5 H5B 0.9300 . ? C5 C6 1.414(6) . ? C6 C7 1.436(6) . ? C9 H9 0.9300 . ? C10 C11 1.481(6) . ? C11 C12 1.401(7) . ? C11 C16 1.406(7) . ? C12 C13 1.389(7) . ? C13 H13 0.9300 . ? C13 C14 1.387(8) . ? C14 H14 0.9300 . ? C14 C15 1.373(8) . ? C15 H15 0.9300 . ? C15 C16 1.399(7) . ? O11 H11A 0.8499 . ? O11 H11B 0.8505 . ? O12 H12A 0.8449 . ? O12 H12B 0.8891 . ? O13 H13A 0.8500 . ? O13 H13B 0.8342 . ? N6 C18 1.115(9) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C17 C18 1.451(10) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Dy1 O3 C1 O2 -175.1(3) . . . . ? Dy1 O3 C1 C2 3.0(7) . . . . ? Dy1 O4 C7 C2 -39.6(5) . . . . ? Dy1 O4 C7 C2 164.5(3) 2_666 . . . ? Dy1 O4 C7 C6 140.9(3) . . . . ? Dy1 O4 C7 C6 -15.0(5) 2_666 . . . ? Dy1 O6 C10 O7 -12.1(7) 2_666 . . . ? Dy1 O6 C10 C11 169.1(3) 2_666 . . . ? Dy1 O7 C10 O6 -1.5(6) . . . . ? Dy1 O7 C10 C11 177.3(3) . . . . ? Dy1 N1 N2 C8 -1.2(4) 2_666 . . . ? Dy1 N1 C6 C5 -170.6(3) 2_666 . . . ? Dy1 N1 C6 C7 7.6(4) 2_666 . . . ? Dy1 N3 C8 N2 -8.0(5) 2_666 . . . ? Dy1 N3 C8 N4 172.2(3) 2_666 . . . ? Dy1 N3 C9 N5 -170.1(3) 2_666 . . . ? O1 C3 C4 C5 -175.8(4) . . . . ? O2 C1 C2 C3 15.3(6) . . . . ? O2 C1 C2 C7 -163.2(4) . . . . ? O3 C1 C2 C3 -162.9(4) . . . . ? O3 C1 C2 C7 18.6(6) . . . . ? O6 C10 C11 C12 174.4(4) . . . . ? O6 C10 C11 C16 -5.4(6) . . . . ? O7 C10 C11 C12 -4.5(6) . . . . ? O7 C10 C11 C16 175.7(4) . . . . ? O8 C12 C13 C14 180.0(5) . . . . ? N1 N2 C8 N3 6.0(5) . . . . ? N1 N2 C8 N4 -174.3(4) . . . . ? N1 C6 C7 O4 3.5(5) . . . . ? N1 C6 C7 C2 -176.0(3) . . . . ? N2 N1 C6 C5 7.0(6) . . . . ? N2 N1 C6 C7 -174.8(3) . . . . ? N4 N5 C9 N3 0.5(5) . . . . ? N5 N4 C8 N2 -179.7(4) . . . . ? N5 N4 C8 N3 0.1(5) . . . . ? C1 C2 C3 O1 -3.3(6) . . . . ? C1 C2 C3 C4 175.3(4) . . . . ? C1 C2 C7 O4 1.3(6) . . . . ? C1 C2 C7 C6 -179.3(4) . . . . ? C2 C3 C4 C5 5.5(7) . . . . ? C3 C2 C7 O4 -177.1(4) . . . . ? C3 C2 C7 C6 2.3(6) . . . . ? C3 C4 C5 C6 -0.8(7) . . . . ? C4 C5 C6 N1 175.0(4) . . . . ? C4 C5 C6 C7 -3.1(6) . . . . ? C5 C6 C7 O4 -178.3(4) . . . . ? C5 C6 C7 C2 2.2(6) . . . . ? C6 N1 N2 C8 -178.6(3) . . . . ? C7 C2 C3 O1 175.1(4) . . . . ? C7 C2 C3 C4 -6.2(6) . . . . ? C8 N3 C9 N5 -0.4(5) . . . . ? C8 N4 N5 C9 -0.3(4) . . . . ? C9 N3 C8 N2 179.9(4) . . . . ? C9 N3 C8 N4 0.2(5) . . . . ? C10 C11 C12 O8 -0.6(7) . . . . ? C10 C11 C12 C13 -179.1(5) . . . . ? C10 C11 C16 O5 0.8(7) . . . . ? C10 C11 C16 C15 -179.8(4) . . . . ? C11 C12 C13 C14 -1.4(8) . . . . ? C12 C11 C16 O5 -178.9(4) . . . . ? C12 C11 C16 C15 0.5(7) . . . . ? C12 C13 C14 C15 1.2(9) . . . . ? C13 C14 C15 C16 -0.1(8) . . . . ? C14 C15 C16 O5 178.7(5) . . . . ? C14 C15 C16 C11 -0.8(8) . . . . ? C16 C11 C12 O8 179.2(5) . . . . ? C16 C11 C12 C13 0.6(7) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -1.5327 -6.2844 0.8443 -0.0194 -0.0894 0.9958 -0.5115 -3.2933 7.3843 0.6166 0.6507 0.4432 1.3483 0.4307 6.9320 0.7401 0.6306 -0.2337 -0.4429 0.2200 -7.4136 -0.6872 -0.7235 0.0657 -0.1950 0.1513 7.3930 0.6083 0.7916 -0.0586 5.5288 -0.1026 2.4569 0.8380 -0.2028 -0.5066 0.6499 -7.1757 2.8975 0.4151 -0.0978 0.9045 -3.2393 -2.9258 5.9010 0.1759 0.7378 0.6517 -4.9421 -2.0116 -1.4580 -0.6584 0.1567 0.7361 -4.4778 5.5485 -3.9679 -0.9192 0.2220 -0.3253 2.8994 5.2276 -0.5980 0.2091 -0.0480 -0.9767 1.6538 6.2417 -1.1279 0.0094 0.0479 -0.9988 2.9142 4.6061 -4.5599 -0.1199 -0.4909 -0.8629 -2.3554 2.4898 6.1990 0.2308 0.9572 -0.1745 2.3503 -2.5172 -6.1852 -0.2299 -0.9567 0.1786 0.1808 -5.8182 -2.7390 -0.1378 -0.5797 0.8031 -5.9355 -0.0672 -0.4652 -0.7115 0.4350 0.5519 4.9427 -4.7868 3.9062 0.9567 -0.2298 0.1789