#------------------------------------------------------------------------------ #$Date: 2017-09-08 04:59:02 +0300 (Fri, 08 Sep 2017) $ #$Revision: 200358 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/69/1546976.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_1546976 loop_ _publ_author_name 'Fieser, Megan E.' 'Palumbo, Chad T.' 'La Pierre, Henry Storms' 'Halter, Dominik P.' 'Voora, Vamsee K.' 'Ziller, Joseph W.' 'Furche, Filipp' 'Meyer, Karsten' 'Evans, William J.' _publ_section_title ; Comparisons of Lanthanide / Actinide +2 Ions in a Tris(aryloxide)arene Coordination Environment ; _journal_name_full 'Chem. Sci.' _journal_paper_doi 10.1039/C7SC02337E _journal_year 2017 _chemical_absolute_configuration ad _chemical_formula_sum 'C85 H121.37 Dy K N2 O10' _chemical_formula_weight 1532.80 _space_group_crystal_system cubic _space_group_IT_number 198 _space_group_name_Hall 'P 2ac 2ab 3' _space_group_name_H-M_alt 'P 21 3' _symmetry_space_group_name_Hall 'P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P 21 3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-08-01 deposited with the CCDC. 2017-09-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.798(3) _cell_length_b 19.798(3) _cell_length_c 19.798(3) _cell_measurement_reflns_used 9694 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 28.11 _cell_measurement_theta_min 2.30 _cell_volume 7760(2) _computing_cell_refinement 'Bruker SAINT 8.34a, 2013' _computing_data_collection 'Bruker APEX2 2014.11-0, 2014' _computing_data_reduction 'Bruker SAINT 8.34a, 2013' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'Bruker SHELXTL 2014/4' _diffrn_ambient_temperature 133(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_unetI/netI 0.0236 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 94001 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 25.500 _diffrn_reflns_theta_max 28.901 _diffrn_reflns_theta_min 1.455 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 1.076 _exptl_absorpt_correction_T_max 0.8015 _exptl_absorpt_correction_T_min 0.7436 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS 2014/5' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_meas ? _exptl_crystal_density_method not_measured _exptl_crystal_description block _exptl_crystal_F_000 3241 _exptl_crystal_size_max 0.566 _exptl_crystal_size_mid 0.438 _exptl_crystal_size_min 0.371 _refine_diff_density_max 0.613 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.071 _refine_ls_abs_structure_details ; Flack x determined using 2700 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.002(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.218 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 307 _refine_ls_number_reflns 6642 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.218 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0417 _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^)+(0.0193P)^2^+12.9912P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0959 _refine_ls_wR_factor_ref 0.0970 _reflns_Friedel_coverage 0.840 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.980 _reflns_number_gt 6365 _reflns_number_total 6642 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7sc02337e3.cif _cod_data_source_block ctp96 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not_measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_original_cell_volume 7760(3) _cod_database_code 1546976 _shelx_shelxl_version_number 2014/7 _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. ; _shelx_estimated_absorpt_t_min 0.581 _shelx_estimated_absorpt_t_max 0.691 _exptl_absorpt_special_details ; Reflections not merged 94046 Corrected reflections written to file ctp96s.hkl Estimated minimum and maximum transmission: 0.7436 0.8015 The ratio (0.9278) of these values is more reliable than their absolute values Additional spherical absorption correction applied with mu*r = 0.1500 Lambda/2 correction factor = 0.00150 ; _shelx_res_file ; ctp96.res created by SHELXL-2014/7 TITL ctp96 in P2(1)3 CELL 0.71073 19.79830 19.79830 19.79830 90.0000 90.0000 90.0000 ZERR 4.00 0.00280 0.00280 0.00280 0.0000 0.0000 0.0000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SYMM Z, X, Y SYMM 0.5+Z, 0.5-X, -Y SYMM 0.5-Z, -X, 0.5+Y SYMM -Z, 0.5+X, 0.5-Y SYMM Y, Z, X SYMM -Y, 0.5+Z, 0.5-X SYMM 0.5+Y, 0.5-Z, -X SYMM 0.5-Y, -Z, 0.5+X SFAC C H N O K DY UNIT 340 485.48 8 40 4 4 TEMP -140.000 SIZE 0.371 0.438 0.566 rem APEX2 2014.11-0, SAINT 8.34a, SADABS 2014/5 (multi), SHELXTL 2014/7 (dual) OMIT 0 2 2 OMIT 1 0 8 TWIN 0 1 0 1 0 0 0 0 -1 DFIX 1.90 0.05 DY2 H2 BIND DY2 H2 L.S. 16 FMAP 2 PLAN 10 ACTA 51 WGHT 0.019300 12.991200 BASF 0.01284 FVAR 0.08162 PART 1 DY1 6 0.310521 0.310521 0.310521 10.21000 0.01667 0.01667 = 0.01667 -0.00221 -0.00221 -0.00221 PART 2 DY2 6 0.293045 0.293045 0.293045 10.12333 0.01612 0.01612 = 0.01612 -0.00206 -0.00206 -0.00206 H2 2 0.236972 0.236972 0.236972 10.12333 10.04000 PART 0 O1 4 0.282960 0.223347 0.372046 11.00000 0.03073 0.01914 = 0.02277 0.00398 -0.00538 -0.00461 C1 1 0.359154 0.334059 0.431960 11.00000 0.02451 0.02228 = 0.02168 -0.00238 -0.00521 -0.00384 C2 1 0.417370 0.319778 0.392315 11.00000 0.02300 0.02002 = 0.03333 0.00073 -0.00311 -0.00583 C3 1 0.462742 0.263171 0.412439 11.00000 0.02510 0.04192 = 0.03753 0.01227 -0.00144 0.00349 AFIX 137 H3A 2 0.509290 0.273934 0.399492 11.00000 -1.50000 H3B 2 0.448445 0.221648 0.389602 11.00000 -1.50000 H3C 2 0.460324 0.256714 0.461456 11.00000 -1.50000 AFIX 0 C4 1 0.340126 0.288684 0.489851 11.00000 0.03158 0.02772 = 0.02335 -0.00562 -0.00391 -0.00343 AFIX 23 H4A 2 0.295565 0.303959 0.506628 11.00000 -1.20000 H4B 2 0.373050 0.296915 0.526575 11.00000 -1.20000 AFIX 0 C5 1 0.335827 0.212883 0.479784 11.00000 0.01910 0.02826 = 0.02415 -0.00030 0.00264 -0.00263 C6 1 0.304735 0.183189 0.422560 11.00000 0.02127 0.02416 = 0.02359 0.00227 -0.00198 -0.00269 C7 1 0.295389 0.112033 0.420798 11.00000 0.01716 0.02769 = 0.02375 0.00132 0.00050 -0.00267 C8 1 0.319262 0.074868 0.475794 11.00000 0.02489 0.02503 = 0.02585 0.00204 0.00298 0.00184 AFIX 43 H8A 2 0.313375 0.027255 0.474867 11.00000 -1.20000 AFIX 0 C9 1 0.350763 0.102576 0.531284 11.00000 0.02276 0.03455 = 0.02485 0.00584 0.00342 0.00051 C10 1 0.358194 0.171604 0.532251 11.00000 0.02201 0.04066 = 0.01667 0.00213 0.00286 -0.00418 AFIX 43 H10A 2 0.379406 0.191975 0.570166 11.00000 -1.20000 AFIX 0 C11 1 0.373349 0.058216 0.589497 11.00000 0.03581 0.04808 = 0.03087 0.01539 -0.00350 -0.00298 AFIX 137 H11A 2 0.337497 0.025908 0.600496 11.00000 -1.50000 H11B 2 0.382824 0.086443 0.629040 11.00000 -1.50000 H11C 2 0.414321 0.033630 0.576575 11.00000 -1.50000 AFIX 0 C12 1 0.258807 0.076202 0.362314 11.00000 0.02884 0.02024 = 0.02962 0.00140 -0.00840 -0.00252 C13 1 0.258184 -0.001203 0.372817 11.00000 0.05599 0.02019 = 0.04404 0.00032 -0.01776 0.00157 AFIX 23 H13A 2 0.305207 -0.018141 0.374376 11.00000 -1.20000 H13B 2 0.236445 -0.011863 0.416569 11.00000 -1.20000 AFIX 0 C14 1 0.219721 -0.036964 0.315454 11.00000 0.09050 0.02074 = 0.05086 -0.00170 -0.03410 -0.00428 AFIX 13 H14A 2 0.220512 -0.086797 0.323654 11.00000 -1.20000 AFIX 0 C15 1 0.147189 -0.013044 0.314354 11.00000 0.07312 0.03112 = 0.06769 0.00387 -0.02940 -0.02579 AFIX 23 H15A 2 0.125072 -0.023589 0.357944 11.00000 -1.20000 H15B 2 0.122080 -0.036341 0.277923 11.00000 -1.20000 AFIX 0 C16 1 0.146531 0.063701 0.302149 11.00000 0.03575 0.02907 = 0.05861 -0.00672 -0.01874 -0.01042 AFIX 13 H16A 2 0.098710 0.079891 0.300663 11.00000 -1.20000 AFIX 0 C17 1 0.180333 0.079452 0.235963 11.00000 0.05972 0.02450 = 0.04102 -0.00580 -0.02641 -0.00198 AFIX 23 H17A 2 0.179394 0.128816 0.228040 11.00000 -1.20000 H17B 2 0.155368 0.057274 0.198744 11.00000 -1.20000 AFIX 0 C18 1 0.253584 0.054713 0.236305 11.00000 0.05254 0.02926 = 0.03627 -0.01090 -0.00974 0.00208 AFIX 13 H18A 2 0.275139 0.064982 0.191796 11.00000 -1.20000 AFIX 0 C19 1 0.291333 0.092902 0.293159 11.00000 0.03360 0.06611 = 0.02463 -0.00758 -0.01181 0.00882 AFIX 23 H19A 2 0.288967 0.142155 0.284854 11.00000 -1.20000 H19B 2 0.339481 0.079410 0.293461 11.00000 -1.20000 AFIX 0 C20 1 0.184003 0.099634 0.360355 11.00000 0.02901 0.02395 = 0.04009 0.00139 -0.00643 -0.00550 AFIX 23 H20A 2 0.161824 0.088874 0.403861 11.00000 -1.20000 H20B 2 0.182019 0.149147 0.353651 11.00000 -1.20000 AFIX 0 C21 1 0.254071 -0.022064 0.248407 11.00000 0.08610 0.03017 = 0.04767 -0.01498 -0.03091 0.01165 AFIX 23 H21A 2 0.229837 -0.045286 0.211342 11.00000 -1.20000 H21B 2 0.301166 -0.038847 0.249317 11.00000 -1.20000 AFIX 0 K1 5 0.647719 0.147719 0.352281 10.33333 0.01951 0.01951 = 0.01951 0.00041 0.00041 -0.00041 O2 4 0.698033 0.270600 0.405521 11.00000 0.03021 0.02337 = 0.02777 -0.00249 0.00121 0.00009 O3 4 0.601914 0.199000 0.476073 11.00000 0.03283 0.02850 = 0.02053 -0.00396 0.00388 -0.00152 N1 3 0.734820 0.234820 0.265180 10.33333 0.02456 0.02456 = 0.02456 0.00276 0.00276 -0.00276 N2 3 0.562590 0.062590 0.437410 10.33333 0.02837 0.02837 = 0.02837 0.00458 0.00458 -0.00458 C22 1 0.766366 0.287536 0.307605 11.00000 0.02674 0.02382 = 0.03632 0.00082 0.00003 -0.00902 AFIX 23 H22A 2 0.785160 0.323048 0.277838 11.00000 -1.20000 H22B 2 0.804425 0.267218 0.332885 11.00000 -1.20000 AFIX 0 C23 1 0.718556 0.319875 0.357136 11.00000 0.03466 0.02015 = 0.03010 0.00194 -0.00407 -0.00305 AFIX 23 H23A 2 0.741222 0.357989 0.380244 11.00000 -1.20000 H23B 2 0.678554 0.337700 0.333001 11.00000 -1.20000 AFIX 0 C24 1 0.660430 0.301871 0.458153 11.00000 0.03512 0.02395 = 0.03153 -0.00646 -0.00215 0.00162 AFIX 23 H24A 2 0.619643 0.323732 0.439206 11.00000 -1.20000 H24B 2 0.688228 0.337048 0.480295 11.00000 -1.20000 AFIX 0 C25 1 0.640339 0.249536 0.508650 11.00000 0.03791 0.03317 = 0.02228 -0.00916 -0.00169 -0.00133 AFIX 23 H25A 2 0.681154 0.229222 0.529188 11.00000 -1.20000 H25B 2 0.613291 0.270589 0.545060 11.00000 -1.20000 AFIX 0 C26 1 0.568799 0.155797 0.522754 11.00000 0.03625 0.03694 = 0.01673 -0.00173 0.00657 0.00501 AFIX 23 H26A 2 0.540171 0.182990 0.553436 11.00000 -1.20000 H26B 2 0.602796 0.131725 0.550416 11.00000 -1.20000 AFIX 0 C27 1 0.525506 0.105109 0.485419 11.00000 0.02665 0.03671 = 0.03203 0.00486 0.00867 -0.00351 AFIX 23 H27A 2 0.503020 0.075551 0.518902 11.00000 -1.20000 H27B 2 0.489769 0.129786 0.460633 11.00000 -1.20000 AFIX 0 O4 4 0.539836 0.437705 0.490919 10.33333 0.07560 0.07560 = 0.08535 -0.00931 0.00966 -0.02389 part -1 C28 1 0.491259 0.430744 0.540986 10.66666 0.15983 AFIX 23 H28A 2 0.447665 0.426468 0.516867 10.66666 -1.20000 H28B 2 0.489818 0.474855 0.564492 10.66666 -1.20000 AFIX 0 C29 1 0.489486 0.381746 0.592337 10.66666 0.10782 AFIX 33 H29A 2 0.449443 0.388858 0.620554 10.66666 -1.50000 H29B 2 0.487571 0.336638 0.572044 10.66666 -1.50000 H29C 2 0.530208 0.385581 0.620216 10.66666 -1.50000 part 0 AFIX 0 HKLF 4 REM ctp96 in P2(1)3 REM R1 = 0.0417 for 6365 Fo > 4sig(Fo) and 0.0450 for all 6642 data REM 307 parameters refined using 1 restraints END WGHT 0.0193 12.9791 REM Highest difference peak 0.613, deepest hole -0.564, 1-sigma level 0.071 Q1 1 0.3097 0.3518 0.3093 11.00000 0.05 0.61 Q2 1 0.4791 0.4498 0.6406 11.00000 0.05 0.53 Q3 1 0.3268 0.0794 0.3309 11.00000 0.05 0.46 Q4 1 0.1096 0.0661 0.3085 11.00000 0.05 0.44 Q5 1 0.3169 0.3101 0.5236 11.00000 0.05 0.43 Q6 1 0.3176 0.0585 0.2827 11.00000 0.05 0.41 Q7 1 0.3148 0.0643 0.2655 11.00000 0.05 0.40 Q8 1 0.4889 0.4221 0.6171 11.00000 0.05 0.39 Q9 1 0.4924 0.3899 0.5378 11.00000 0.05 0.39 Q10 1 0.2682 0.0660 0.3243 11.00000 0.05 0.38 ; _shelx_res_checksum 93275 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' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 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 0.31052(2) 0.31052(2) 0.31052(2) 0.01667(14) Uani 0.63 3 d S T P . 1 Dy2 Dy 0.29304(4) 0.29304(4) 0.29304(4) 0.0161(3) Uani 0.37 3 d DS T P . 2 H2 H 0.237(2) 0.237(2) 0.237(2) 0.040 Uiso 0.37 3 d DS U P A 2 O1 O 0.28296(17) 0.22335(16) 0.37205(16) 0.0242(7) Uani 1 1 d . . . . . C1 C 0.3592(2) 0.3341(2) 0.4320(2) 0.0228(9) Uani 1 1 d . . . . . C2 C 0.4174(2) 0.3198(2) 0.3923(3) 0.0255(10) Uani 1 1 d . . . . . C3 C 0.4627(3) 0.2632(3) 0.4124(3) 0.0348(12) Uani 1 1 d . . . . . H3A H 0.5093 0.2739 0.3995 0.052 Uiso 1 1 calc R U . . . H3B H 0.4484 0.2216 0.3896 0.052 Uiso 1 1 calc R U . . . H3C H 0.4603 0.2567 0.4615 0.052 Uiso 1 1 calc R U . . . C4 C 0.3401(3) 0.2887(2) 0.4899(2) 0.0276(10) Uani 1 1 d . . . . . H4A H 0.2956 0.3040 0.5066 0.033 Uiso 1 1 calc R U . . . H4B H 0.3731 0.2969 0.5266 0.033 Uiso 1 1 calc R U . . . C5 C 0.3358(2) 0.2129(2) 0.4798(2) 0.0238(9) Uani 1 1 d . . . . . C6 C 0.3047(2) 0.1832(2) 0.4226(2) 0.0230(9) Uani 1 1 d . . . . . C7 C 0.2954(2) 0.1120(2) 0.4208(2) 0.0229(9) Uani 1 1 d . . . . . C8 C 0.3193(2) 0.0749(2) 0.4758(2) 0.0253(10) Uani 1 1 d . . . . . H8A H 0.3134 0.0273 0.4749 0.030 Uiso 1 1 calc R U . . . C9 C 0.3508(3) 0.1026(3) 0.5313(2) 0.0274(10) Uani 1 1 d . . . . . C10 C 0.3582(2) 0.1716(3) 0.5323(2) 0.0264(10) Uani 1 1 d . . . . . H10A H 0.3794 0.1920 0.5702 0.032 Uiso 1 1 calc R U . . . C11 C 0.3733(3) 0.0582(3) 0.5895(3) 0.0383(13) Uani 1 1 d . . . . . H11A H 0.3375 0.0259 0.6005 0.057 Uiso 1 1 calc R U . . . H11B H 0.3828 0.0864 0.6290 0.057 Uiso 1 1 calc R U . . . H11C H 0.4143 0.0336 0.5766 0.057 Uiso 1 1 calc R U . . . C12 C 0.2588(3) 0.0762(2) 0.3623(3) 0.0262(10) Uani 1 1 d . . . . . C13 C 0.2582(3) -0.0012(3) 0.3728(3) 0.0401(14) Uani 1 1 d . . . . . H13A H 0.3052 -0.0181 0.3744 0.048 Uiso 1 1 calc R U . . . H13B H 0.2364 -0.0119 0.4166 0.048 Uiso 1 1 calc R U . . . C14 C 0.2197(4) -0.0370(3) 0.3155(4) 0.0540(19) Uani 1 1 d . . . . . H14A H 0.2205 -0.0868 0.3237 0.065 Uiso 1 1 calc R U . . . C15 C 0.1472(4) -0.0130(3) 0.3144(4) 0.0573(19) Uani 1 1 d . . . . . H15A H 0.1251 -0.0236 0.3579 0.069 Uiso 1 1 calc R U . . . H15B H 0.1221 -0.0363 0.2779 0.069 Uiso 1 1 calc R U . . . C16 C 0.1465(3) 0.0637(3) 0.3021(4) 0.0411(14) Uani 1 1 d . . . . . H16A H 0.0987 0.0799 0.3007 0.049 Uiso 1 1 calc R U . . . C17 C 0.1803(3) 0.0795(3) 0.2360(3) 0.0417(15) Uani 1 1 d . . . . . H17A H 0.1794 0.1288 0.2280 0.050 Uiso 1 1 calc R U . . . H17B H 0.1554 0.0573 0.1987 0.050 Uiso 1 1 calc R U . . . C18 C 0.2536(3) 0.0547(3) 0.2363(3) 0.0394(13) Uani 1 1 d . . . . . H18A H 0.2751 0.0650 0.1918 0.047 Uiso 1 1 calc R U . . . C19 C 0.2913(3) 0.0929(3) 0.2932(3) 0.0414(15) Uani 1 1 d . . . . . H19A H 0.2890 0.1422 0.2849 0.050 Uiso 1 1 calc R U . . . H19B H 0.3395 0.0794 0.2935 0.050 Uiso 1 1 calc R U . . . C20 C 0.1840(3) 0.0996(2) 0.3604(3) 0.0310(10) Uani 1 1 d . . . . . H20A H 0.1618 0.0889 0.4039 0.037 Uiso 1 1 calc R U . . . H20B H 0.1820 0.1491 0.3537 0.037 Uiso 1 1 calc R U . . . C21 C 0.2541(4) -0.0221(3) 0.2484(4) 0.0546(19) Uani 1 1 d . . . . . H21A H 0.2298 -0.0453 0.2113 0.066 Uiso 1 1 calc R U . . . H21B H 0.3012 -0.0388 0.2493 0.066 Uiso 1 1 calc R U . . . K1 K 0.64772(5) 0.14772(5) 0.35228(5) 0.0195(3) Uani 1 3 d S T P . . O2 O 0.69803(19) 0.27060(16) 0.40552(17) 0.0271(7) Uani 1 1 d . . . . . O3 O 0.60191(17) 0.19900(18) 0.47607(16) 0.0273(7) Uani 1 1 d . . . . . N1 N 0.7348(2) 0.2348(2) 0.2652(2) 0.0246(14) Uani 1 3 d S T P . . N2 N 0.5626(2) 0.0626(2) 0.4374(2) 0.0284(15) Uani 1 3 d S T P . . C22 C 0.7664(2) 0.2875(2) 0.3076(3) 0.0290(10) Uani 1 1 d . . . . . H22A H 0.7852 0.3230 0.2778 0.035 Uiso 1 1 calc R U . . . H22B H 0.8044 0.2672 0.3329 0.035 Uiso 1 1 calc R U . . . C23 C 0.7186(3) 0.3199(2) 0.3571(3) 0.0283(10) Uani 1 1 d . . . . . H23A H 0.7412 0.3580 0.3802 0.034 Uiso 1 1 calc R U . . . H23B H 0.6786 0.3377 0.3330 0.034 Uiso 1 1 calc R U . . . C24 C 0.6604(3) 0.3019(3) 0.4582(3) 0.0302(10) Uani 1 1 d . . . . . H24A H 0.6196 0.3237 0.4392 0.036 Uiso 1 1 calc R U . . . H24B H 0.6882 0.3370 0.4803 0.036 Uiso 1 1 calc R U . . . C25 C 0.6403(3) 0.2495(3) 0.5087(3) 0.0311(11) Uani 1 1 d . . . . . H25A H 0.6812 0.2292 0.5292 0.037 Uiso 1 1 calc R U . . . H25B H 0.6133 0.2706 0.5451 0.037 Uiso 1 1 calc R U . . . C26 C 0.5688(3) 0.1558(3) 0.5228(2) 0.0300(11) Uani 1 1 d . . . . . H26A H 0.5402 0.1830 0.5534 0.036 Uiso 1 1 calc R U . . . H26B H 0.6028 0.1317 0.5504 0.036 Uiso 1 1 calc R U . . . C27 C 0.5255(3) 0.1051(3) 0.4854(3) 0.0318(11) Uani 1 1 d . . . . . H27A H 0.5030 0.0756 0.5189 0.038 Uiso 1 1 calc R U . . . H27B H 0.4898 0.1298 0.4606 0.038 Uiso 1 1 calc R U . . . O4 O 0.5398(10) 0.4377(10) 0.4909(11) 0.079(5) Uani 0.3333 1 d . . P . . C28 C 0.4913(15) 0.4307(14) 0.5410(14) 0.160(10) Uiso 0.6667 1 d . . P B -1 H28A H 0.4477 0.4265 0.5169 0.192 Uiso 0.6667 1 calc R U P B -1 H28B H 0.4898 0.4749 0.5645 0.192 Uiso 0.6667 1 calc R U P B -1 C29 C 0.4895(10) 0.3817(10) 0.5923(10) 0.108(6) Uiso 0.6667 1 d . . P B -1 H29A H 0.4494 0.3889 0.6206 0.162 Uiso 0.6667 1 calc R U P B -1 H29B H 0.4876 0.3366 0.5720 0.162 Uiso 0.6667 1 calc R U P B -1 H29C H 0.5302 0.3856 0.6202 0.162 Uiso 0.6667 1 calc R U P B -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 Dy1 0.01667(14) 0.01667(14) 0.01667(14) -0.00221(15) -0.00221(15) -0.00221(15) Dy2 0.0161(3) 0.0161(3) 0.0161(3) -0.0021(3) -0.0021(3) -0.0021(3) O1 0.0307(18) 0.0191(15) 0.0228(16) 0.0040(12) -0.0054(13) -0.0046(13) C1 0.025(2) 0.022(2) 0.022(2) -0.0024(16) -0.0052(17) -0.0038(17) C2 0.023(2) 0.020(2) 0.033(2) 0.0007(18) -0.0031(18) -0.0058(18) C3 0.025(3) 0.042(3) 0.038(3) 0.012(2) -0.001(2) 0.003(2) C4 0.032(3) 0.028(2) 0.023(2) -0.0056(19) -0.0039(19) -0.003(2) C5 0.019(2) 0.028(2) 0.024(2) -0.0003(18) 0.0026(17) -0.0026(18) C6 0.021(2) 0.024(2) 0.024(2) 0.0023(17) -0.0020(17) -0.0027(19) C7 0.017(2) 0.028(2) 0.024(2) 0.0013(18) 0.0005(16) -0.0027(17) C8 0.025(2) 0.025(2) 0.026(2) 0.0020(18) 0.0030(19) 0.0018(19) C9 0.023(2) 0.035(3) 0.025(2) 0.006(2) 0.0034(19) 0.001(2) C10 0.022(2) 0.041(3) 0.017(2) 0.0021(18) 0.0029(17) -0.0042(19) C11 0.036(3) 0.048(3) 0.031(3) 0.015(2) -0.003(2) -0.003(3) C12 0.029(2) 0.020(2) 0.030(2) 0.0014(19) -0.008(2) -0.0025(18) C13 0.056(4) 0.020(2) 0.044(3) 0.000(2) -0.018(3) 0.002(2) C14 0.091(5) 0.021(3) 0.051(4) -0.002(3) -0.034(4) -0.004(3) C15 0.073(5) 0.031(3) 0.068(5) 0.004(3) -0.029(4) -0.026(3) C16 0.036(3) 0.029(3) 0.059(4) -0.007(3) -0.019(3) -0.010(2) C17 0.060(4) 0.024(2) 0.041(3) -0.006(2) -0.026(3) -0.002(3) C18 0.053(4) 0.029(3) 0.036(3) -0.011(2) -0.010(3) 0.002(2) C19 0.034(3) 0.066(4) 0.025(3) -0.008(3) -0.012(2) 0.009(3) C20 0.029(3) 0.024(2) 0.040(3) 0.001(2) -0.006(2) -0.005(2) C21 0.086(5) 0.030(3) 0.048(4) -0.015(3) -0.031(4) 0.012(3) K1 0.0195(3) 0.0195(3) 0.0195(3) 0.0004(3) 0.0004(3) -0.0004(3) O2 0.0302(18) 0.0234(16) 0.0278(17) -0.0025(13) 0.0012(15) 0.0001(14) O3 0.0328(18) 0.0285(18) 0.0205(16) -0.0040(14) 0.0039(13) -0.0015(15) N1 0.0246(14) 0.0246(14) 0.0246(14) 0.0028(15) 0.0028(15) -0.0028(15) N2 0.0284(15) 0.0284(15) 0.0284(15) 0.0046(16) 0.0046(16) -0.0046(16) C22 0.027(2) 0.024(2) 0.036(3) 0.001(2) 0.000(2) -0.0090(17) C23 0.035(3) 0.020(2) 0.030(2) 0.0019(19) -0.0041(19) -0.0030(19) C24 0.035(3) 0.024(2) 0.032(2) -0.006(2) -0.002(2) 0.002(2) C25 0.038(3) 0.033(3) 0.022(2) -0.009(2) -0.002(2) -0.001(2) C26 0.036(3) 0.037(3) 0.017(2) -0.0017(19) 0.0066(19) 0.005(2) C27 0.027(2) 0.037(3) 0.032(3) 0.005(2) 0.009(2) -0.004(2) O4 0.076(12) 0.076(13) 0.085(13) -0.009(10) 0.010(10) -0.024(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 DY1 Cnt 106.1 . . O1 Dy1 O1 112.55(8) 9 5 O1 Dy1 O1 112.55(8) 9 . O1 Dy1 O1 112.55(8) 5 . O1 Dy1 C1 114.78(13) 9 . O1 Dy1 C1 124.24(14) 5 . O1 Dy1 C1 73.83(13) . . O1 Dy1 C1 73.83(13) 9 9 O1 Dy1 C1 114.78(14) 5 9 O1 Dy1 C1 124.25(14) . 9 C1 Dy1 C1 55.88(17) . 9 O1 Dy1 C1 124.25(14) 9 5 O1 Dy1 C1 73.83(13) 5 5 O1 Dy1 C1 114.78(14) . 5 C1 Dy1 C1 55.88(17) . 5 C1 Dy1 C1 55.88(17) 9 5 O1 Dy1 C2 137.73(14) 9 . O1 Dy1 C2 93.13(14) 5 . O1 Dy1 C2 85.06(13) . . C1 Dy1 C2 31.12(15) . . C1 Dy1 C2 64.86(14) 9 . C1 Dy1 C2 31.10(14) 5 . O1 Dy1 C2 85.06(13) 9 9 O1 Dy1 C2 137.73(14) 5 9 O1 Dy1 C2 93.13(14) . 9 C1 Dy1 C2 31.10(14) . 9 C1 Dy1 C2 31.12(15) 9 9 C1 Dy1 C2 64.86(14) 5 9 C2 Dy1 C2 54.80(17) . 9 O1 Dy1 C2 93.13(14) 9 5 O1 Dy1 C2 85.06(13) 5 5 O1 Dy1 C2 137.73(14) . 5 C1 Dy1 C2 64.86(14) . 5 C1 Dy1 C2 31.10(14) 9 5 C1 Dy1 C2 31.12(15) 5 5 C2 Dy1 C2 54.80(17) . 5 C2 Dy1 C2 54.80(17) 9 5 H2 Dy2 O1 89.76(10) . 9 H2 Dy2 O1 89.76(10) . 5 O1 Dy2 O1 119.998(1) 9 5 H2 Dy2 O1 89.76(10) . . O1 Dy2 O1 120.000(1) 9 . O1 Dy2 O1 119.996(1) 5 . C6 O1 Dy2 155.7(3) . . C6 O1 Dy1 143.2(3) . . C2 C1 C2 119.6(5) 9 . C2 C1 C4 120.1(4) 9 . C2 C1 C4 120.3(4) . . C2 C1 Dy1 76.0(3) 9 . C2 C1 Dy1 75.9(3) . . C4 C1 Dy1 119.9(3) . . C1 C2 C1 120.2(5) 5 . C1 C2 C3 120.4(5) 5 . C1 C2 C3 119.4(4) . . C1 C2 Dy1 72.9(3) 5 . C1 C2 Dy1 72.9(3) . . C3 C2 Dy1 126.0(3) . . C1 C4 C5 120.3(4) . . C10 C5 C6 119.4(4) . . C10 C5 C4 117.7(4) . . C6 C5 C4 122.7(4) . . O1 C6 C5 119.2(4) . . O1 C6 C7 121.6(4) . . C5 C6 C7 119.2(4) . . C8 C7 C6 117.3(4) . . C8 C7 C12 120.2(4) . . C6 C7 C12 122.5(4) . . C9 C8 C7 124.4(5) . . C10 C9 C8 117.1(5) . . C10 C9 C11 122.3(5) . . C8 C9 C11 120.6(5) . . C9 C10 C5 122.6(5) . . C7 C12 C13 111.1(4) . . C7 C12 C19 111.8(4) . . C13 C12 C19 109.5(5) . . C7 C12 C20 109.3(4) . . C13 C12 C20 107.0(4) . . C19 C12 C20 108.1(4) . . C14 C13 C12 111.1(5) . . C15 C14 C21 110.6(6) . . C15 C14 C13 109.6(6) . . C21 C14 C13 109.5(6) . . C14 C15 C16 108.6(5) . . C17 C16 C15 109.7(6) . . C17 C16 C20 109.9(5) . . C15 C16 C20 109.5(5) . . C16 C17 C18 110.6(5) . . C17 C18 C21 108.8(6) . . C17 C18 C19 107.7(5) . . C21 C18 C19 111.5(5) . . C18 C19 C12 109.7(5) . . C16 C20 C12 109.8(4) . . C14 C21 C18 109.0(5) . . O3 K1 O3 98.68(10) . 8_645 O3 K1 O3 98.68(10) . 11_556 O3 K1 O3 98.68(10) 8_645 11_556 O3 K1 O2 120.21(10) . 8_645 O3 K1 O2 58.49(10) 8_645 8_645 O3 K1 O2 136.06(10) 11_556 8_645 O3 K1 O2 136.06(10) . 11_556 O3 K1 O2 120.21(10) 8_645 11_556 O3 K1 O2 58.49(10) 11_556 11_556 O2 K1 O2 98.54(10) 8_645 11_556 O3 K1 O2 58.49(10) . . O3 K1 O2 136.06(10) 8_645 . O3 K1 O2 120.21(10) 11_556 . O2 K1 O2 98.54(10) 8_645 . O2 K1 O2 98.54(10) 11_556 . O3 K1 N2 61.16(8) . . O3 K1 N2 61.16(8) 8_645 . O3 K1 N2 61.16(8) 11_556 . O2 K1 N2 118.96(8) 8_645 . O2 K1 N2 118.96(8) 11_556 . O2 K1 N2 118.95(8) . . O3 K1 N1 118.84(8) . . O3 K1 N1 118.84(8) 8_645 . O3 K1 N1 118.84(8) 11_556 . O2 K1 N1 61.04(8) 8_645 . O2 K1 N1 61.04(8) 11_556 . O2 K1 N1 61.05(8) . . N2 K1 N1 180.00(9) . . C24 O2 C23 110.1(4) . . C24 O2 K1 117.5(3) . . C23 O2 K1 116.0(3) . . C25 O3 C26 112.2(4) . . C25 O3 K1 118.8(3) . . C26 O3 K1 120.0(3) . . C22 N1 C22 110.1(3) 8_645 11_556 C22 N1 C22 110.1(3) 8_645 . C22 N1 C22 110.1(3) 11_556 . C22 N1 K1 108.9(3) 8_645 . C22 N1 K1 108.9(3) 11_556 . C22 N1 K1 108.9(3) . . C27 N2 C27 109.6(3) . 8_645 C27 N2 C27 109.6(3) . 11_556 C27 N2 C27 109.6(3) 8_645 11_556 C27 N2 K1 109.4(3) . . C27 N2 K1 109.4(3) 8_645 . C27 N2 K1 109.4(3) 11_556 . N1 C22 C23 113.9(4) . . O2 C23 C22 109.0(4) . . O2 C24 C25 109.1(4) . . O3 C25 C24 109.2(4) . . O3 C26 C27 110.1(4) . . N2 C27 C26 114.4(4) . . O4 C28 C29 127(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Dy1 Cnt 2.238 . Dy1 O1 2.182(3) 9 Dy1 O1 2.182(3) 5 Dy1 O1 2.182(3) . Dy1 C1 2.632(4) . Dy1 C1 2.632(4) 9 Dy1 C1 2.632(4) 5 Dy1 C2 2.670(5) . Dy1 C2 2.671(5) 9 Dy1 C2 2.671(5) 5 Dy2 H2 1.92(7) . Dy2 O1 2.095(3) 9 Dy2 O1 2.095(3) 5 Dy2 O1 2.095(3) . O1 C6 1.348(5) . C1 C2 1.422(7) 9 C1 C2 1.423(7) . C1 C4 1.504(7) . C2 C1 1.422(7) 5 C2 C3 1.491(7) . C4 C5 1.516(7) . C5 C10 1.394(7) . C5 C6 1.417(6) . C6 C7 1.421(6) . C7 C8 1.397(6) . C7 C12 1.539(7) . C8 C9 1.377(7) . C9 C10 1.375(7) . C9 C11 1.516(7) . C12 C13 1.547(7) . C12 C19 1.549(8) . C12 C20 1.552(7) . C13 C14 1.540(8) . C14 C15 1.512(11) . C14 C21 1.520(11) . C15 C16 1.539(8) . C16 C17 1.504(10) . C16 C20 1.544(7) . C17 C18 1.531(9) . C18 C21 1.539(8) . C18 C19 1.548(7) . K1 O3 2.804(3) . K1 O3 2.804(3) 8_645 K1 O3 2.804(3) 11_556 K1 O2 2.832(3) 8_645 K1 O2 2.832(3) 11_556 K1 O2 2.832(3) . K1 N2 2.919(7) . K1 N1 2.987(7) . O2 C24 1.422(6) . O2 C23 1.426(6) . O3 C25 1.413(6) . O3 C26 1.420(6) . N1 C22 1.478(5) 8_645 N1 C22 1.478(5) 11_556 N1 C22 1.478(5) . N2 C27 1.467(6) . N2 C27 1.467(6) 8_645 N2 C27 1.467(6) 11_556 C22 C23 1.506(7) . C24 C25 1.494(7) . C26 C27 1.513(8) . O4 C28 1.39(3) . C28 C29 1.41(3) .