#------------------------------------------------------------------------------ #$Date: 2019-04-17 01:16:03 +0300 (Wed, 17 Apr 2019) $ #$Revision: 214658 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/08/1550898.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_1550898 loop_ _publ_author_name 'Peng, Yan' 'Singh, Mukesh Kumar' 'Mereacre, Valeriu' 'Anson, Christopher' 'Rajaraman, Gopalan' 'Powell, Annie K.' _publ_section_title ; Mechanism of Magnetization Relaxation in {MIII2DyIII2} (M = Cr, Mn, Fe, Al) “Butterfly” Complexes: How Important Are the Transition Metal Ions Here? ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C8SC05362F _journal_year 2019 _chemical_formula_moiety 'C68 H72 Dy2 Mn2 N4 O18, 2(C H4 O), C2 H3 N' _chemical_formula_sum 'C72 H83 Dy2 Mn2 N5 O20' _chemical_formula_weight 1773.31 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary 'intrinsic phasing' _atom_sites_solution_secondary difmap _audit_creation_date 2018-11-20 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2018-11-21 deposited with the CCDC. 2019-04-04 downloaded from the CCDC. ; _cell_angle_alpha 111.771(2) _cell_angle_beta 93.386(2) _cell_angle_gamma 110.092(2) _cell_formula_units_Z 1 _cell_length_a 11.1952(2) _cell_length_b 13.2472(3) _cell_length_c 14.6071(3) _cell_measurement_reflns_used 14388 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 70.7190 _cell_measurement_theta_min 3.9010 _cell_volume 1845.67(8) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 180.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0534 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -70.00 30.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -77.0000 -60.0000 100 #__ type_ start__ end____ width___ exp.time_ 2 omega -36.00 33.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 88.0000 84.0000 69 #__ type_ start__ end____ width___ exp.time_ 3 omega -21.00 69.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 57.0000 60.0000 90 #__ type_ start__ end____ width___ exp.time_ 4 omega 33.00 123.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.0000 57.0000 90.0000 90 #__ type_ start__ end____ width___ exp.time_ 5 omega -19.00 98.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.0000 -19.0000 -90.0000 117 #__ type_ start__ end____ width___ exp.time_ 6 omega 33.00 123.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.0000 57.0000 -120.0000 90 #__ type_ start__ end____ width___ exp.time_ 7 omega 23.00 111.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.0000 -125.0000 60.0000 88 #__ type_ start__ end____ width___ exp.time_ 8 omega -15.00 75.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.0000 -57.0000 120.0000 90 #__ type_ start__ end____ width___ exp.time_ 9 omega -16.00 84.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.0000 -77.0000 -120.0000 100 #__ type_ start__ end____ width___ exp.time_ 10 omega 23.00 111.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.0000 -125.0000 -180.0000 88 #__ type_ start__ end____ width___ exp.time_ 11 omega 36.00 116.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -111.0000 30.0000 80 #__ type_ start__ end____ width___ exp.time_ 12 omega 99.00 178.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 88.0000 84.0000 79 #__ type_ start__ end____ width___ exp.time_ 13 omega 36.00 93.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -38.0000 120.0000 57 #__ type_ start__ end____ width___ exp.time_ 14 omega 36.00 93.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -38.0000 -120.0000 57 #__ type_ start__ end____ width___ exp.time_ 15 omega 38.00 138.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -77.0000 0.0000 100 #__ type_ start__ end____ width___ exp.time_ 16 omega 35.00 94.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -25.0000 -180.0000 59 #__ type_ start__ end____ width___ exp.time_ 17 omega 86.00 178.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 50.0000 -120.0000 92 #__ type_ start__ end____ width___ exp.time_ 18 omega 36.00 93.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -38.0000 60.0000 57 #__ type_ start__ end____ width___ exp.time_ 19 omega 57.00 151.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 178.0000 60.0000 94 #__ type_ start__ end____ width___ exp.time_ 20 omega 36.00 116.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -111.0000 -150.0000 80 #__ type_ start__ end____ width___ exp.time_ 21 omega 36.00 93.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -38.0000 -60.0000 57 #__ type_ start__ end____ width___ exp.time_ 22 omega 36.00 116.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -111.0000 150.0000 80 #__ type_ start__ end____ width___ exp.time_ 23 omega 38.00 104.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -50.0000 60.0000 66 #__ type_ start__ end____ width___ exp.time_ 24 omega 36.00 93.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -38.0000 0.0000 57 #__ type_ start__ end____ width___ exp.time_ 25 omega 35.00 178.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 0.0000 60.0000 143 #__ type_ start__ end____ width___ exp.time_ 26 omega 40.00 130.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -63.0000 -180.0000 90 #__ type_ start__ end____ width___ exp.time_ 27 omega -26.00 72.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 38.0000 -30.0000 98 #__ type_ start__ end____ width___ exp.time_ 28 omega -44.00 73.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 19.0000 -150.0000 117 #__ type_ start__ end____ width___ exp.time_ 29 omega 24.00 124.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.0000 77.0000 0.0000 100 #__ type_ start__ end____ width___ exp.time_ 30 omega 28.00 126.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.0000 38.0000 0.0000 98 #__ type_ start__ end____ width___ exp.time_ 31 omega 24.00 124.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.0000 77.0000 -150.0000 100 #__ type_ start__ end____ width___ exp.time_ 32 omega 24.00 124.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.0000 77.0000 90.0000 100 #__ type_ start__ end____ width___ exp.time_ 33 omega 24.00 124.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.0000 77.0000 -90.0000 100 #__ type_ start__ end____ width___ exp.time_ 34 omega 24.00 124.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.0000 77.0000 150.0000 100 #__ type_ start__ end____ width___ exp.time_ 35 omega 82.00 178.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 38.0000 -150.0000 96 #__ type_ start__ end____ width___ exp.time_ 36 omega 78.00 178.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 0.0000 100 #__ type_ start__ end____ width___ exp.time_ 37 omega 82.00 178.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 38.0000 120.0000 96 #__ type_ start__ end____ width___ exp.time_ 38 omega 78.00 178.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 -90.0000 100 #__ type_ start__ end____ width___ exp.time_ 39 omega 82.00 178.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 38.0000 -180.0000 96 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0581744000 _diffrn_orient_matrix_UB_12 -0.0072214000 _diffrn_orient_matrix_UB_13 0.0945014000 _diffrn_orient_matrix_UB_21 -0.1175585000 _diffrn_orient_matrix_UB_22 0.0117953000 _diffrn_orient_matrix_UB_23 0.0458741000 _diffrn_orient_matrix_UB_31 -0.0727616000 _diffrn_orient_matrix_UB_32 -0.1355548000 _diffrn_orient_matrix_UB_33 -0.0498048000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_unetI/netI 0.0289 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 26827 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 70.895 _diffrn_reflns_theta_min 3.335 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 13.983 _exptl_absorpt_correction_T_max 0.542 _exptl_absorpt_correction_T_min 0.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.595 _exptl_crystal_description block _exptl_crystal_F_000 892 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.639 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 498 _refine_ls_number_reflns 7030 _refine_ls_number_restraints 25 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0254 _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^)+(0.0353P)^2^+0.6127P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.0648 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6602 _reflns_number_total 7030 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8sc05362f3.cif _cod_data_source_block pmn32dy2 _cod_original_cell_volume 1845.67(7) _cod_database_code 1550898 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C50H80Mn2Dy2N16O30 _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_max 0.542 _shelx_estimated_absorpt_t_min 0.308 _reflns_odcompleteness_completeness 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, H1 of O1, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, H41A of O41A, H42A of O42A 2. Restrained distances H41A-O42A 1.98 with sigma of 0.04 H42A-O9 1.92 with sigma of 0.04 O1-H1 0.88 with sigma of 0.04 O41A-C41A \\sim O42A-C42A with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C41B \\sim N41B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 4. Rigid body (RIGU) restrains O41A, C41A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O42A, C42A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N41B, C41B, C42B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Fixed Sof: O41A(0.5) H41A(0.5) C41A(0.5) H41B(0.5) H41C(0.5) H41D(0.5) O42A(0.5) H42A(0.5) C42A(0.5) H42B(0.5) H42C(0.5) H42D(0.5) N41B(0.5) C41B(0.5) C42B(0.5) H42E(0.5) H42F(0.5) H42G(0.5) 6.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B) 6.b Aromatic/amide H refined with riding coordinates: C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C16(H16), C17(H17), C21(H21), C22(H22), C24(H24), C25(H25), C29(H29), C30(H30), C32(H32), C33(H33) 6.c Idealised Me refined as rotating group: C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C34(H34A,H34B,H34C), C41A(H41B,H41C, H41D), C42A(H42B,H42C,H42D), C42B(H42E,H42F,H42G) 6.d Idealised tetrahedral OH refined as rotating group: O41A(H41A), O42A(H42A) ; _shelx_res_file ; TITL pMn32Dy2_a.res in P-1 pmn32dy2.res created by SHELXL-2018/3 at 16:52:38 on 20-Nov-2018 REM Old TITL pMn(III)2Dy2 in P1 REM SHELXT solution in P-1 REM R1 0.107, Rweak 0.014, Alpha 0.104, Orientation as input REM Formula found by SHELXT: C34 N4 O9 Mn Dy CELL 1.54184 11.1952 13.2472 14.6071 111.771 93.386 110.092 ZERR 1 0.0002 0.0003 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H Dy Mn N O UNIT 72 83 2 2 5 20 DFIX 1.98 0.04 H41A O42A DFIX 1.92 0.04 H42A O9 DFIX 0.88 0.04 O1 H1 SADI O41A C41A O42A C42A SIMU C41B N41B RIGU O41A C41A RIGU O42A C42A RIGU N41B C41B C42B L.S. 32 PLAN 30 SIZE 0.11 0.07 0.05 TEMP -93 HTAB O1 O41A HTAB O1 N41B HTAB O41A O42A HTAB O42A O9 HTAB C42B O9 BOND $H HTAB fmap 2 acta REM REM REM WGHT 0.035300 0.612700 FVAR 4.59278 DY1 3 0.457256 0.265012 0.334799 11.00000 0.03114 0.02902 = 0.01364 0.00566 0.00191 0.01627 MN1 4 0.565283 0.562426 0.426686 11.00000 0.02693 0.02753 = 0.01225 0.00665 0.00185 0.01466 O1 6 0.407502 0.431817 0.420542 11.00000 0.02677 0.03018 = 0.01354 0.00693 -0.00051 0.01492 H1 2 0.338849 0.421071 0.395130 11.00000 -1.20000 N1 5 0.681274 0.267215 0.402684 11.00000 0.03691 0.03398 = 0.02205 0.00923 0.00454 0.02152 C1 1 0.785927 0.385681 0.432153 11.00000 0.03134 0.04220 = 0.03379 0.01540 0.00252 0.01886 AFIX 23 H1A 2 0.869128 0.376852 0.422324 11.00000 -1.20000 H1B 2 0.795985 0.434035 0.504756 11.00000 -1.20000 AFIX 0 C2 1 0.758482 0.449911 0.371739 11.00000 0.03099 0.03848 = 0.02848 0.01325 0.00874 0.01957 AFIX 23 H2A 2 0.820101 0.533858 0.403038 11.00000 -1.20000 H2B 2 0.770132 0.413517 0.302066 11.00000 -1.20000 AFIX 0 O2 6 0.629068 0.442481 0.369726 11.00000 0.02803 0.03315 = 0.02077 0.00853 0.00592 0.01836 C3 1 0.662831 0.239027 0.491243 11.00000 0.03830 0.03977 = 0.02384 0.01349 0.00113 0.02400 AFIX 23 H3A 2 0.747430 0.248927 0.525972 11.00000 -1.20000 H3B 2 0.602443 0.155358 0.468116 11.00000 -1.20000 AFIX 0 C4 1 0.608764 0.317632 0.564746 11.00000 0.03220 0.03541 = 0.02124 0.01094 0.00092 0.01941 AFIX 23 H4A 2 0.579634 0.286002 0.614877 11.00000 -1.20000 H4B 2 0.677272 0.398279 0.601262 11.00000 -1.20000 AFIX 0 O3 6 0.502288 0.321978 0.511021 11.00000 0.03064 0.03224 = 0.01395 0.00835 -0.00023 0.01729 C5 1 0.709876 0.173570 0.325818 11.00000 0.04474 0.04280 = 0.03327 0.01332 0.01101 0.03087 AFIX 23 H5A 2 0.658490 0.096628 0.326888 11.00000 -1.20000 H5B 2 0.803201 0.189467 0.343741 11.00000 -1.20000 AFIX 0 C6 1 0.679705 0.164680 0.220969 11.00000 0.04049 0.03761 = 0.02838 0.00786 0.01050 0.02233 C7 1 0.743736 0.117857 0.148352 11.00000 0.05454 0.06849 = 0.03625 0.01471 0.01697 0.04072 AFIX 43 H7 2 0.810058 0.094611 0.165638 11.00000 -1.20000 AFIX 0 C8 1 0.710962 0.105350 0.051906 11.00000 0.06828 0.08932 = 0.03282 0.01253 0.02400 0.05247 AFIX 43 H8 2 0.751196 0.070085 0.000886 11.00000 -1.20000 AFIX 0 C9 1 0.617470 0.145229 0.029667 11.00000 0.06309 0.07894 = 0.02393 0.01274 0.01433 0.03855 AFIX 43 H9 2 0.596575 0.142706 -0.035345 11.00000 -1.20000 AFIX 0 C10 1 0.556479 0.188382 0.105140 11.00000 0.05058 0.05507 = 0.02511 0.01224 0.00879 0.02936 AFIX 43 H10 2 0.489791 0.212103 0.089513 11.00000 -1.20000 AFIX 0 N2 5 0.585891 0.198783 0.199303 11.00000 0.03994 0.03714 = 0.02198 0.00653 0.00626 0.02108 O4 6 0.472911 0.523288 0.276533 11.00000 0.04041 0.03681 = 0.01479 0.00937 0.00156 0.01948 O5 6 0.394630 0.324700 0.211929 11.00000 0.04148 0.03518 = 0.01507 0.00934 0.00170 0.01908 C11 1 0.415764 0.421542 0.205552 11.00000 0.02905 0.04138 = 0.01456 0.00932 0.00364 0.01884 C12 1 0.370518 0.415628 0.104079 11.00000 0.03168 0.04773 = 0.01713 0.01507 0.00395 0.01976 C13 1 0.318279 0.308505 0.020011 11.00000 0.04885 0.04985 = 0.02106 0.01030 -0.00182 0.01870 AFIX 43 H13 2 0.306916 0.237473 0.026994 11.00000 -1.20000 AFIX 0 C14 1 0.282367 0.304128 -0.074449 11.00000 0.05465 0.07020 = 0.01688 0.00864 -0.00585 0.01942 AFIX 43 H14 2 0.248233 0.229941 -0.131448 11.00000 -1.20000 AFIX 0 C15 1 0.295094 0.404902 -0.087426 11.00000 0.03761 0.08737 = 0.02374 0.03016 0.00233 0.02289 C16 1 0.343930 0.511367 -0.002681 11.00000 0.03951 0.07202 = 0.03699 0.03709 0.00722 0.02513 AFIX 43 H16 2 0.351353 0.581833 -0.009321 11.00000 -1.20000 AFIX 0 C17 1 0.382337 0.517057 0.092031 11.00000 0.03656 0.05018 = 0.02393 0.01629 0.00209 0.01953 AFIX 43 H17 2 0.417001 0.591326 0.148942 11.00000 -1.20000 AFIX 0 C18 1 0.257411 0.398318 -0.191149 11.00000 0.05913 0.13270 = 0.02895 0.04614 0.00248 0.03126 AFIX 137 H18A 2 0.311478 0.367592 -0.234764 11.00000 -1.50000 H18B 2 0.270770 0.477520 -0.185917 11.00000 -1.50000 H18C 2 0.165542 0.345572 -0.220050 11.00000 -1.50000 AFIX 0 O6 6 0.261742 0.314993 0.544139 11.00000 0.03150 0.03204 = 0.01765 0.00641 0.00366 0.01407 O7 6 0.248213 0.201386 0.381429 11.00000 0.03202 0.03645 = 0.01895 0.00574 0.00453 0.01568 C19 1 0.201833 0.227153 0.458129 11.00000 0.03301 0.03047 = 0.02016 0.00979 0.00194 0.01756 C20 1 0.064587 0.151744 0.452983 11.00000 0.03061 0.03037 = 0.02702 0.01288 0.00310 0.01773 C21 1 0.008957 0.175047 0.537352 11.00000 0.03540 0.04218 = 0.02544 0.01339 0.00491 0.01847 AFIX 43 H21 2 0.057574 0.241409 0.598773 11.00000 -1.20000 AFIX 0 C22 1 -0.116598 0.102207 0.532295 11.00000 0.03965 0.05122 = 0.03766 0.02462 0.01199 0.02392 AFIX 43 H22 2 -0.152485 0.118677 0.590829 11.00000 -1.20000 AFIX 0 C23 1 -0.190987 0.005737 0.443545 11.00000 0.03317 0.03458 = 0.05215 0.02704 0.00509 0.01464 C24 1 -0.135514 -0.015670 0.359686 11.00000 0.04213 0.02868 = 0.04143 0.00798 -0.00329 0.00825 AFIX 43 H24 2 -0.185041 -0.080823 0.297817 11.00000 -1.20000 AFIX 0 C25 1 -0.009657 0.055690 0.364033 11.00000 0.04214 0.03365 = 0.02958 0.00880 0.00456 0.01621 AFIX 43 H25 2 0.026167 0.038665 0.305494 11.00000 -1.20000 AFIX 0 C26 1 -0.327778 -0.073212 0.438755 11.00000 0.04093 0.04671 = 0.07451 0.03603 0.00663 0.01139 AFIX 137 H26A 2 -0.390011 -0.049491 0.410977 11.00000 -1.50000 H26B 2 -0.338080 -0.065919 0.506795 11.00000 -1.50000 H26C 2 -0.344089 -0.155505 0.395379 11.00000 -1.50000 AFIX 0 O8 6 0.421284 0.069612 0.318422 11.00000 0.04019 0.02943 = 0.02369 0.00469 -0.00239 0.01529 O9 6 0.298207 0.073532 0.197257 11.00000 0.04524 0.03609 = 0.01976 0.00720 0.00382 0.02155 C27 1 0.326603 0.017570 0.243434 11.00000 0.03364 0.03327 = 0.02070 0.00421 0.00619 0.01745 C28 1 0.247633 -0.110324 0.211684 11.00000 0.03749 0.03531 = 0.02066 0.00382 0.00537 0.01890 C29 1 0.125666 -0.166141 0.147160 11.00000 0.03989 0.04378 = 0.03969 0.00998 0.00076 0.01970 AFIX 43 H29 2 0.092725 -0.122882 0.120934 11.00000 -1.20000 AFIX 0 C30 1 0.052571 -0.284078 0.121234 11.00000 0.03767 0.04698 = 0.06360 0.00963 -0.00416 0.01055 AFIX 43 H30 2 -0.030360 -0.320856 0.076931 11.00000 -1.20000 AFIX 0 C31 1 0.096391 -0.350487 0.157815 11.00000 0.05031 0.03598 = 0.05316 0.00847 0.01167 0.01173 C32 1 0.218215 -0.293926 0.221981 11.00000 0.06158 0.03466 = 0.03875 0.01139 0.00814 0.02209 AFIX 43 H32 2 0.251191 -0.337437 0.247845 11.00000 -1.20000 AFIX 0 C33 1 0.292075 -0.176441 0.248867 11.00000 0.04558 0.03644 = 0.03021 0.00659 0.00061 0.01811 AFIX 43 H33 2 0.374724 -0.139838 0.293518 11.00000 -1.20000 AFIX 0 C34 1 0.015865 -0.479125 0.131331 11.00000 0.07886 0.04109 = 0.10443 0.01994 0.01308 0.00885 AFIX 137 H34A 2 0.069213 -0.525230 0.109411 11.00000 -1.50000 H34B 2 -0.059143 -0.508415 0.076666 11.00000 -1.50000 H34C 2 -0.014731 -0.487207 0.190729 11.00000 -1.50000 AFIX 0 PART 1 O41A 6 0.131602 0.356243 0.330275 10.50000 0.05933 0.05211 = 0.03704 0.01707 -0.01028 0.01967 AFIX 147 H41A 2 0.112382 0.283304 0.299461 10.50000 -1.50000 AFIX 0 C41A 1 0.082134 0.394641 0.269488 10.50000 0.05481 0.05665 = 0.05723 0.01647 -0.01004 0.01996 AFIX 137 H41B 2 0.075804 0.469501 0.310567 10.50000 -1.50000 H41C 2 -0.004667 0.335554 0.230855 10.50000 -1.50000 H41D 2 0.139374 0.406730 0.222936 10.50000 -1.50000 AFIX 0 O42A 6 0.076315 0.124427 0.172377 10.50000 0.05241 0.07091 = 0.04022 0.01489 -0.00444 0.03191 AFIX 147 H42A 2 0.139240 0.109312 0.188690 10.50000 -1.50000 AFIX 0 C42A 1 0.054629 0.095632 0.070828 10.50000 0.06943 0.12519 = 0.04686 0.02851 0.01084 0.05615 AFIX 137 H42B 2 0.134343 0.095372 0.046582 10.50000 -1.50000 H42C 2 0.029503 0.153977 0.058136 10.50000 -1.50000 H42D 2 -0.015464 0.016959 0.035164 10.50000 -1.50000 AFIX 0 PART 0 PART 2 N41B 5 0.120100 0.379025 0.312472 10.50000 0.21098 0.05886 = 0.05231 0.00743 -0.07065 0.04755 C41B 1 0.102571 0.297197 0.251627 10.50000 0.04468 0.06145 = 0.05487 0.02404 -0.00602 0.01594 C42B 1 0.088575 0.191715 0.164775 10.50000 0.04201 0.07024 = 0.05809 0.01757 0.00372 0.01131 AFIX 137 H42E 2 -0.003509 0.138010 0.140514 10.50000 -1.50000 H42F 2 0.138754 0.152195 0.183954 10.50000 -1.50000 H42G 2 0.121009 0.213565 0.111089 10.50000 -1.50000 AFIX 0 HKLF 4 REM pMn32Dy2_a.res in P-1 REM wR2 = 0.0648, GooF = S = 1.037, Restrained GooF = 1.038 for all data REM R1 = 0.0254 for 6602 Fo > 4sig(Fo) and 0.0282 for all 7030 data REM 498 parameters refined using 25 restraints END WGHT 0.0353 0.6127 REM Instructions for potential hydrogen bonds HTAB O1 O41A HTAB O1 N41B EQIV $1 -x+1, -y+1, -z+1 HTAB C2 O6_$1 HTAB C2 N2 HTAB C3 O8 HTAB C10 O5 HTAB O41A O7 HTAB O41A O42A HTAB O42A O7 HTAB O42A O9 HTAB C42B O9 REM Highest difference peak 0.639, deepest hole -0.690, 1-sigma level 0.060 Q1 1 0.4818 0.3025 0.4245 11.00000 0.05 0.64 Q2 1 0.4239 0.2146 0.2443 11.00000 0.05 0.56 Q3 1 0.5217 0.2390 0.3327 11.00000 0.05 0.53 Q4 1 0.3796 0.2831 0.3335 11.00000 0.05 0.50 Q5 1 0.4654 0.1751 0.3465 11.00000 0.05 0.38 Q6 1 0.4468 0.3570 0.3295 11.00000 0.05 0.33 Q7 1 0.1310 0.1757 0.4618 11.00000 0.05 0.27 Q8 1 0.0341 0.1744 0.4883 11.00000 0.05 0.26 Q9 1 0.2957 0.1621 0.3509 11.00000 0.05 0.26 Q10 1 0.5284 0.5108 0.3290 11.00000 0.05 0.26 Q11 1 0.1680 -0.3367 0.1658 11.00000 0.05 0.26 Q12 1 0.4951 0.5844 0.4265 11.00000 0.05 0.26 Q13 1 0.5266 0.2124 0.2279 11.00000 0.05 0.25 Q14 1 0.3100 0.1204 0.2371 11.00000 0.05 0.25 Q15 1 0.5611 0.3778 0.4377 11.00000 0.05 0.24 Q16 1 0.2415 0.0758 0.1901 11.00000 0.05 0.24 Q17 1 0.6650 0.1338 0.0431 11.00000 0.05 0.24 Q18 1 0.3812 0.4162 0.1567 11.00000 0.05 0.24 Q19 1 0.1931 -0.1346 0.1751 11.00000 0.05 0.24 Q20 1 -0.1937 0.0038 0.3916 11.00000 0.05 0.24 Q21 1 -0.3671 -0.0177 0.4827 11.00000 0.05 0.24 Q22 1 0.4995 0.4675 0.3365 11.00000 0.05 0.23 Q23 1 0.4187 0.4139 0.4822 11.00000 0.05 0.23 Q24 1 0.3704 0.4612 0.0926 11.00000 0.05 0.22 Q25 1 0.2595 -0.1286 0.2408 11.00000 0.05 0.22 Q26 1 0.3476 0.3543 0.5580 11.00000 0.05 0.22 Q27 1 0.7845 0.4234 0.4016 11.00000 0.05 0.21 Q28 1 -0.1583 0.0582 0.4745 11.00000 0.05 0.21 Q29 1 0.6220 0.5323 0.4244 11.00000 0.05 0.21 Q30 1 0.6197 0.2053 -0.0183 11.00000 0.05 0.21 ; _shelx_res_checksum 97784 _olex2_submission_special_instructions 'No special instructions were received' 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 0.45726(2) 0.26501(2) 0.33480(2) 0.02448(5) Uani 1 1 d . . . . . Mn1 Mn 0.56528(4) 0.56243(3) 0.42669(2) 0.02172(9) Uani 1 1 d . . . . . O1 O 0.40750(17) 0.43182(15) 0.42054(12) 0.0233(4) Uani 1 1 d D . . . . H1 H 0.339(2) 0.421(3) 0.395(2) 0.028 Uiso 1 1 d DR . . . . N1 N 0.6813(2) 0.2672(2) 0.40268(15) 0.0296(5) Uani 1 1 d . . . . . C1 C 0.7859(3) 0.3857(3) 0.4322(2) 0.0349(6) Uani 1 1 d . . . . . H1A H 0.869128 0.376852 0.422324 0.042 Uiso 1 1 calc R . . . . H1B H 0.795985 0.434035 0.504756 0.042 Uiso 1 1 calc R . . . . C2 C 0.7585(3) 0.4499(3) 0.3717(2) 0.0310(6) Uani 1 1 d . . . . . H2A H 0.820101 0.533858 0.403038 0.037 Uiso 1 1 calc R . . . . H2B H 0.770132 0.413517 0.302066 0.037 Uiso 1 1 calc R . . . . O2 O 0.62907(16) 0.44248(16) 0.36973(12) 0.0263(4) Uani 1 1 d . . . . . C3 C 0.6628(3) 0.2390(3) 0.49124(19) 0.0316(6) Uani 1 1 d . . . . . H3A H 0.747430 0.248927 0.525972 0.038 Uiso 1 1 calc R . . . . H3B H 0.602443 0.155358 0.468116 0.038 Uiso 1 1 calc R . . . . C4 C 0.6088(2) 0.3176(2) 0.56475(18) 0.0283(5) Uani 1 1 d . . . . . H4A H 0.579634 0.286002 0.614877 0.034 Uiso 1 1 calc R . . . . H4B H 0.677272 0.398279 0.601262 0.034 Uiso 1 1 calc R . . . . O3 O 0.50229(16) 0.32198(15) 0.51102(11) 0.0248(4) Uani 1 1 d . . . . . C5 C 0.7099(3) 0.1736(3) 0.3258(2) 0.0370(7) Uani 1 1 d . . . . . H5A H 0.658490 0.096628 0.326888 0.044 Uiso 1 1 calc R . . . . H5B H 0.803201 0.189467 0.343741 0.044 Uiso 1 1 calc R . . . . C6 C 0.6797(3) 0.1647(3) 0.2210(2) 0.0352(6) Uani 1 1 d . . . . . C7 C 0.7437(3) 0.1179(3) 0.1484(2) 0.0502(8) Uani 1 1 d . . . . . H7 H 0.810058 0.094611 0.165638 0.060 Uiso 1 1 calc R . . . . C8 C 0.7110(4) 0.1054(4) 0.0519(2) 0.0607(10) Uani 1 1 d . . . . . H8 H 0.751196 0.070085 0.000886 0.073 Uiso 1 1 calc R . . . . C9 C 0.6175(4) 0.1452(4) 0.0297(2) 0.0548(9) Uani 1 1 d . . . . . H9 H 0.596575 0.142706 -0.035345 0.066 Uiso 1 1 calc R . . . . C10 C 0.5565(3) 0.1884(3) 0.1051(2) 0.0425(7) Uani 1 1 d . . . . . H10 H 0.489791 0.212103 0.089513 0.051 Uiso 1 1 calc R . . . . N2 N 0.5859(2) 0.1988(2) 0.19930(16) 0.0332(5) Uani 1 1 d . . . . . O4 O 0.47291(18) 0.52329(16) 0.27653(12) 0.0301(4) Uani 1 1 d . . . . . O5 O 0.39463(18) 0.32470(16) 0.21193(12) 0.0300(4) Uani 1 1 d . . . . . C11 C 0.4158(2) 0.4215(2) 0.20555(17) 0.0277(6) Uani 1 1 d . . . . . C12 C 0.3705(3) 0.4156(3) 0.10408(18) 0.0305(6) Uani 1 1 d . . . . . C13 C 0.3183(3) 0.3085(3) 0.0200(2) 0.0420(7) Uani 1 1 d . . . . . H13 H 0.306916 0.237473 0.026994 0.050 Uiso 1 1 calc R . . . . C14 C 0.2824(3) 0.3041(3) -0.0744(2) 0.0524(9) Uani 1 1 d . . . . . H14 H 0.248233 0.229941 -0.131448 0.063 Uiso 1 1 calc R . . . . C15 C 0.2951(3) 0.4049(4) -0.0874(2) 0.0481(8) Uani 1 1 d . . . . . C16 C 0.3439(3) 0.5114(3) -0.0027(2) 0.0441(8) Uani 1 1 d . . . . . H16 H 0.351353 0.581833 -0.009321 0.053 Uiso 1 1 calc R . . . . C17 C 0.3823(3) 0.5171(3) 0.0920(2) 0.0361(6) Uani 1 1 d . . . . . H17 H 0.417001 0.591326 0.148942 0.043 Uiso 1 1 calc R . . . . C18 C 0.2574(4) 0.3983(4) -0.1911(2) 0.0719(13) Uani 1 1 d . . . . . H18A H 0.311478 0.367592 -0.234764 0.108 Uiso 1 1 calc GR . . . . H18B H 0.270770 0.477520 -0.185917 0.108 Uiso 1 1 calc GR . . . . H18C H 0.165542 0.345572 -0.220050 0.108 Uiso 1 1 calc GR . . . . O6 O 0.26174(17) 0.31499(16) 0.54414(12) 0.0279(4) Uani 1 1 d . . . . . O7 O 0.24821(17) 0.20139(16) 0.38143(12) 0.0304(4) Uani 1 1 d . . . . . C19 C 0.2018(2) 0.2272(2) 0.45813(18) 0.0268(5) Uani 1 1 d . . . . . C20 C 0.0646(2) 0.1517(2) 0.45298(19) 0.0275(5) Uani 1 1 d . . . . . C21 C 0.0090(3) 0.1750(3) 0.5374(2) 0.0337(6) Uani 1 1 d . . . . . H21 H 0.057574 0.241409 0.598773 0.040 Uiso 1 1 calc R . . . . C22 C -0.1166(3) 0.1022(3) 0.5323(2) 0.0390(7) Uani 1 1 d . . . . . H22 H -0.152485 0.118677 0.590829 0.047 Uiso 1 1 calc R . . . . C23 C -0.1910(3) 0.0057(3) 0.4435(2) 0.0369(6) Uani 1 1 d . . . . . C24 C -0.1355(3) -0.0157(3) 0.3597(2) 0.0418(7) Uani 1 1 d . . . . . H24 H -0.185041 -0.080823 0.297817 0.050 Uiso 1 1 calc R . . . . C25 C -0.0097(3) 0.0557(3) 0.3640(2) 0.0363(6) Uani 1 1 d . . . . . H25 H 0.026167 0.038665 0.305494 0.044 Uiso 1 1 calc R . . . . C26 C -0.3278(3) -0.0732(3) 0.4388(3) 0.0526(9) Uani 1 1 d . . . . . H26A H -0.390011 -0.049491 0.410977 0.079 Uiso 1 1 calc GR . . . . H26B H -0.338080 -0.065919 0.506795 0.079 Uiso 1 1 calc GR . . . . H26C H -0.344089 -0.155505 0.395379 0.079 Uiso 1 1 calc GR . . . . O8 O 0.42128(18) 0.06961(16) 0.31842(13) 0.0331(4) Uani 1 1 d . . . . . O9 O 0.29821(19) 0.07353(17) 0.19726(13) 0.0337(4) Uani 1 1 d D . . . . C27 C 0.3266(3) 0.0176(2) 0.24343(18) 0.0302(6) Uani 1 1 d . . . . . C28 C 0.2476(3) -0.1103(2) 0.21168(19) 0.0324(6) Uani 1 1 d . . . . . C29 C 0.1257(3) -0.1661(3) 0.1472(2) 0.0429(7) Uani 1 1 d . . . . . H29 H 0.092725 -0.122882 0.120934 0.052 Uiso 1 1 calc R . . . . C30 C 0.0526(3) -0.2841(3) 0.1212(3) 0.0562(9) Uani 1 1 d . . . . . H30 H -0.030360 -0.320856 0.076931 0.067 Uiso 1 1 calc R . . . . C31 C 0.0964(3) -0.3505(3) 0.1578(3) 0.0512(8) Uani 1 1 d . . . . . C32 C 0.2182(3) -0.2939(3) 0.2220(2) 0.0455(7) Uani 1 1 d . . . . . H32 H 0.251191 -0.337437 0.247845 0.055 Uiso 1 1 calc R . . . . C33 C 0.2921(3) -0.1764(3) 0.2489(2) 0.0395(7) Uani 1 1 d . . . . . H33 H 0.374724 -0.139838 0.293518 0.047 Uiso 1 1 calc R . . . . C34 C 0.0159(5) -0.4791(3) 0.1313(4) 0.0828(14) Uani 1 1 d . . . . . H34A H 0.069213 -0.525230 0.109411 0.124 Uiso 1 1 calc GR . . . . H34B H -0.059143 -0.508415 0.076666 0.124 Uiso 1 1 calc GR . . . . H34C H -0.014731 -0.487207 0.190729 0.124 Uiso 1 1 calc GR . . . . O41A O 0.1316(7) 0.3562(7) 0.3303(6) 0.0516(16) Uani 0.5 1 d D U P A 1 H41A H 0.112382 0.283304 0.299461 0.077 Uiso 0.5 1 calc DGR . P A 1 C41A C 0.0821(7) 0.3946(7) 0.2695(6) 0.060(2) Uani 0.5 1 d D U P A 1 H41B H 0.075804 0.469501 0.310567 0.090 Uiso 0.5 1 calc GR . P A 1 H41C H -0.004667 0.335554 0.230855 0.090 Uiso 0.5 1 calc GR . P A 1 H41D H 0.139374 0.406730 0.222936 0.090 Uiso 0.5 1 calc GR . P A 1 O42A O 0.0763(6) 0.1244(5) 0.1724(4) 0.0556(14) Uani 0.5 1 d D U P B 1 H42A H 0.139240 0.109312 0.188690 0.083 Uiso 0.5 1 calc DGR . P B 1 C42A C 0.0546(8) 0.0956(9) 0.0708(5) 0.078(3) Uani 0.5 1 d D U P B 1 H42B H 0.134343 0.095372 0.046582 0.117 Uiso 0.5 1 calc GR . P B 1 H42C H 0.029503 0.153977 0.058136 0.117 Uiso 0.5 1 calc GR . P B 1 H42D H -0.015464 0.016959 0.035164 0.117 Uiso 0.5 1 calc GR . P B 1 N41B N 0.1201(16) 0.3790(11) 0.3125(9) 0.119(6) Uani 0.5 1 d . U P C 2 C41B C 0.1026(7) 0.2972(7) 0.2516(6) 0.0560(18) Uani 0.5 1 d . U P C 2 C42B C 0.0886(8) 0.1917(8) 0.1648(7) 0.063(2) Uani 0.5 1 d . U P C 2 H42E H -0.003509 0.138010 0.140514 0.095 Uiso 0.5 1 calc GR . P C 2 H42F H 0.138754 0.152195 0.183954 0.095 Uiso 0.5 1 calc GR . P C 2 H42G H 0.121009 0.213565 0.111089 0.095 Uiso 0.5 1 calc GR . P C 2 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 0.03114(9) 0.02902(9) 0.01364(7) 0.00566(6) 0.00191(5) 0.01627(7) Mn1 0.02693(19) 0.0275(2) 0.01225(16) 0.00665(15) 0.00185(14) 0.01466(16) O1 0.0268(9) 0.0302(9) 0.0135(7) 0.0069(7) -0.0005(6) 0.0149(8) N1 0.0369(12) 0.0340(12) 0.0220(10) 0.0092(9) 0.0045(9) 0.0215(10) C1 0.0313(14) 0.0422(16) 0.0338(14) 0.0154(13) 0.0025(11) 0.0189(13) C2 0.0310(13) 0.0385(15) 0.0285(13) 0.0132(12) 0.0087(11) 0.0196(12) O2 0.0280(9) 0.0331(10) 0.0208(8) 0.0085(7) 0.0059(7) 0.0184(8) C3 0.0383(14) 0.0398(16) 0.0238(12) 0.0135(12) 0.0011(11) 0.0240(13) C4 0.0322(13) 0.0354(15) 0.0212(12) 0.0109(11) 0.0009(10) 0.0194(12) O3 0.0306(9) 0.0322(10) 0.0139(7) 0.0084(7) -0.0002(7) 0.0173(8) C5 0.0447(16) 0.0428(17) 0.0333(14) 0.0133(13) 0.0110(12) 0.0309(14) C6 0.0405(15) 0.0376(16) 0.0284(14) 0.0079(12) 0.0105(12) 0.0223(13) C7 0.0545(19) 0.068(2) 0.0362(16) 0.0147(16) 0.0170(15) 0.0407(19) C8 0.068(2) 0.089(3) 0.0328(17) 0.0125(18) 0.0240(16) 0.052(2) C9 0.063(2) 0.079(3) 0.0239(14) 0.0127(16) 0.0143(14) 0.039(2) C10 0.0506(18) 0.055(2) 0.0251(14) 0.0122(14) 0.0088(13) 0.0294(16) N2 0.0399(13) 0.0371(13) 0.0220(10) 0.0065(10) 0.0063(9) 0.0211(11) O4 0.0404(10) 0.0368(11) 0.0148(8) 0.0094(8) 0.0016(7) 0.0195(9) O5 0.0415(10) 0.0352(10) 0.0151(8) 0.0093(8) 0.0017(7) 0.0191(9) C11 0.0290(13) 0.0414(16) 0.0146(11) 0.0093(11) 0.0036(10) 0.0188(12) C12 0.0317(13) 0.0477(17) 0.0171(12) 0.0151(12) 0.0040(10) 0.0198(13) C13 0.0488(17) 0.0498(19) 0.0211(13) 0.0103(13) -0.0018(12) 0.0187(15) C14 0.055(2) 0.070(2) 0.0169(13) 0.0086(15) -0.0059(13) 0.0194(18) C15 0.0376(16) 0.087(3) 0.0237(14) 0.0302(17) 0.0023(12) 0.0229(17) C16 0.0395(16) 0.072(2) 0.0370(16) 0.0371(17) 0.0072(13) 0.0251(16) C17 0.0366(15) 0.0502(18) 0.0239(13) 0.0163(13) 0.0021(11) 0.0195(14) C18 0.059(2) 0.133(4) 0.0290(17) 0.046(2) 0.0025(15) 0.031(2) O6 0.0315(9) 0.0320(10) 0.0176(8) 0.0064(7) 0.0037(7) 0.0141(8) O7 0.0320(9) 0.0364(10) 0.0189(8) 0.0057(8) 0.0045(7) 0.0157(8) C19 0.0330(13) 0.0305(14) 0.0202(12) 0.0098(11) 0.0019(10) 0.0176(11) C20 0.0306(13) 0.0304(14) 0.0270(12) 0.0129(11) 0.0031(10) 0.0177(11) C21 0.0354(14) 0.0422(16) 0.0254(13) 0.0134(12) 0.0049(11) 0.0185(13) C22 0.0396(15) 0.0512(19) 0.0377(15) 0.0246(14) 0.0120(13) 0.0239(14) C23 0.0332(14) 0.0346(15) 0.0521(18) 0.0270(14) 0.0051(13) 0.0146(12) C24 0.0421(16) 0.0287(15) 0.0414(16) 0.0080(13) -0.0033(13) 0.0083(13) C25 0.0421(16) 0.0337(15) 0.0296(14) 0.0088(12) 0.0046(12) 0.0162(13) C26 0.0409(17) 0.047(2) 0.075(2) 0.0360(19) 0.0066(17) 0.0114(15) O8 0.0402(10) 0.0294(10) 0.0237(9) 0.0047(8) -0.0024(8) 0.0153(9) O9 0.0452(11) 0.0361(11) 0.0198(8) 0.0072(8) 0.0038(8) 0.0215(9) C27 0.0336(13) 0.0333(15) 0.0207(12) 0.0042(11) 0.0062(10) 0.0174(12) C28 0.0375(14) 0.0353(15) 0.0207(12) 0.0038(11) 0.0054(11) 0.0189(13) C29 0.0399(16) 0.0438(18) 0.0397(16) 0.0100(14) 0.0008(13) 0.0197(14) C30 0.0377(17) 0.047(2) 0.064(2) 0.0096(18) -0.0042(16) 0.0105(16) C31 0.0503(19) 0.0360(17) 0.053(2) 0.0085(15) 0.0117(16) 0.0117(15) C32 0.062(2) 0.0347(17) 0.0388(16) 0.0114(14) 0.0081(15) 0.0221(15) C33 0.0456(17) 0.0364(16) 0.0302(14) 0.0066(13) 0.0006(12) 0.0181(14) C34 0.079(3) 0.041(2) 0.104(4) 0.020(2) 0.013(3) 0.009(2) O41A 0.059(3) 0.052(4) 0.037(3) 0.017(3) -0.010(3) 0.020(3) C41A 0.055(4) 0.057(5) 0.057(5) 0.016(4) -0.010(4) 0.020(4) O42A 0.052(3) 0.071(4) 0.040(2) 0.015(3) -0.004(2) 0.032(3) C42A 0.069(5) 0.125(8) 0.047(4) 0.029(5) 0.011(4) 0.056(6) N41B 0.211(13) 0.059(6) 0.052(5) 0.007(4) -0.071(6) 0.048(6) C41B 0.045(4) 0.061(4) 0.055(4) 0.024(3) -0.006(3) 0.016(4) C42B 0.042(4) 0.070(6) 0.058(5) 0.018(4) 0.004(3) 0.011(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' Mn Mn -0.5299 2.8052 '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_ _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 N1 118.40(6) . . O1 Dy1 N2 138.89(7) . . O1 Dy1 O7 70.38(6) . . O1 Dy1 O8 143.41(6) . . O1 Dy1 O9 124.36(6) . . O2 Dy1 O1 67.38(6) . . O2 Dy1 N1 67.87(6) . . O2 Dy1 O3 85.23(6) . . O2 Dy1 N2 78.57(7) . . O2 Dy1 O5 76.55(6) . . O2 Dy1 O7 137.12(6) . . O2 Dy1 O8 139.31(6) . . O2 Dy1 O9 145.10(6) . . O3 Dy1 O1 69.58(5) . . O3 Dy1 N1 66.61(6) . . O3 Dy1 N2 131.13(6) . . O3 Dy1 O5 142.08(6) . . O3 Dy1 O7 73.43(6) . . O3 Dy1 O8 86.08(6) . . O3 Dy1 O9 129.27(6) . . N2 Dy1 N1 64.56(7) . . O5 Dy1 O1 72.75(6) . . O5 Dy1 N1 131.79(7) . . O5 Dy1 N2 77.62(6) . . O5 Dy1 O7 97.94(6) . . O5 Dy1 O8 128.76(6) . . O5 Dy1 O9 76.93(6) . . O7 Dy1 N1 130.27(6) . . O7 Dy1 N2 142.68(7) . . O7 Dy1 O9 69.04(6) . . O8 Dy1 N1 72.19(7) . . O8 Dy1 N2 77.69(7) . . O8 Dy1 O7 76.83(6) . . O8 Dy1 O9 53.29(6) . . O9 Dy1 N1 116.70(6) . . O9 Dy1 N2 73.91(7) . . O1 Mn1 O1 76.34(7) . 2_666 O1 Mn1 O4 85.53(7) . . O2 Mn1 O1 84.58(7) . . O2 Mn1 O1 94.85(7) . 2_666 O2 Mn1 O4 89.13(7) . . O2 Mn1 O6 90.99(8) . 2_666 O3 Mn1 O1 82.20(6) 2_666 2_666 O3 Mn1 O1 92.91(7) 2_666 . O3 Mn1 O2 176.52(7) 2_666 . O3 Mn1 O4 93.08(7) 2_666 . O3 Mn1 O6 90.97(8) 2_666 2_666 O4 Mn1 O1 160.95(7) . 2_666 O6 Mn1 O1 167.40(7) 2_666 . O6 Mn1 O1 92.34(7) 2_666 2_666 O6 Mn1 O4 106.24(7) 2_666 . Dy1 O1 H1 110(2) . . Mn1 O1 Dy1 101.55(7) . . Mn1 O1 Dy1 98.39(6) 2_666 . Mn1 O1 Mn1 103.66(7) . 2_666 Mn1 O1 H1 118(2) 2_666 . Mn1 O1 H1 122(2) . . C1 N1 Dy1 110.01(14) . . C3 N1 Dy1 105.22(15) . . C3 N1 C1 111.0(2) . . C5 N1 Dy1 110.10(15) . . C5 N1 C1 111.6(2) . . C5 N1 C3 108.7(2) . . N1 C1 H1A 109.1 . . N1 C1 H1B 109.1 . . N1 C1 C2 112.6(2) . . H1A C1 H1B 107.8 . . C2 C1 H1A 109.1 . . C2 C1 H1B 109.1 . . C1 C2 H2A 109.9 . . C1 C2 H2B 109.9 . . H2A C2 H2B 108.3 . . O2 C2 C1 109.1(2) . . O2 C2 H2A 109.9 . . O2 C2 H2B 109.9 . . Mn1 O2 Dy1 106.03(7) . . C2 O2 Dy1 121.33(15) . . C2 O2 Mn1 130.34(16) . . N1 C3 H3A 109.3 . . N1 C3 H3B 109.3 . . N1 C3 C4 111.8(2) . . H3A C3 H3B 107.9 . . C4 C3 H3A 109.3 . . C4 C3 H3B 109.3 . . C3 C4 H4A 109.8 . . C3 C4 H4B 109.8 . . H4A C4 H4B 108.3 . . O3 C4 C3 109.21(19) . . O3 C4 H4A 109.8 . . O3 C4 H4B 109.8 . . Mn1 O3 Dy1 108.46(7) 2_666 . C4 O3 Dy1 124.70(14) . . C4 O3 Mn1 120.74(14) . 2_666 N1 C5 H5A 108.9 . . N1 C5 H5B 108.9 . . N1 C5 C6 113.4(2) . . H5A C5 H5B 107.7 . . C6 C5 H5A 108.9 . . C6 C5 H5B 108.9 . . C7 C6 C5 120.5(3) . . N2 C6 C5 117.8(2) . . N2 C6 C7 121.7(3) . . C6 C7 H7 120.1 . . C8 C7 C6 119.8(3) . . C8 C7 H7 120.1 . . C7 C8 H8 120.5 . . C7 C8 C9 118.9(3) . . C9 C8 H8 120.5 . . C8 C9 H9 121.1 . . C10 C9 C8 117.8(3) . . C10 C9 H9 121.1 . . C9 C10 H10 118.1 . . N2 C10 C9 123.7(3) . . N2 C10 H10 118.1 . . C6 N2 Dy1 119.17(17) . . C10 N2 Dy1 122.66(18) . . C10 N2 C6 118.0(2) . . C11 O4 Mn1 125.91(16) . . C11 O5 Dy1 136.27(15) . . O4 C11 C12 116.8(2) . . O5 C11 O4 125.9(2) . . O5 C11 C12 117.2(2) . . C13 C12 C11 120.7(3) . . C17 C12 C11 120.9(2) . . C17 C12 C13 118.4(2) . . C12 C13 H13 119.8 . . C12 C13 C14 120.5(3) . . C14 C13 H13 119.8 . . C13 C14 H14 119.2 . . C15 C14 C13 121.5(3) . . C15 C14 H14 119.2 . . C14 C15 C16 117.8(3) . . C14 C15 C18 120.6(3) . . C16 C15 C18 121.6(3) . . C15 C16 H16 119.4 . . C15 C16 C17 121.2(3) . . C17 C16 H16 119.4 . . C12 C17 C16 120.6(3) . . C12 C17 H17 119.7 . . C16 C17 H17 119.7 . . C15 C18 H18A 109.5 . . C15 C18 H18B 109.5 . . C15 C18 H18C 109.5 . . H18A C18 H18B 109.5 . . H18A C18 H18C 109.5 . . H18B C18 H18C 109.5 . . C19 O6 Mn1 125.94(17) . 2_666 C19 O7 Dy1 138.18(17) . . O6 C19 C20 115.4(2) . . O7 C19 O6 125.7(2) . . O7 C19 C20 118.8(2) . . C21 C20 C19 121.2(2) . . C25 C20 C19 120.5(2) . . C25 C20 C21 118.4(3) . . C20 C21 H21 119.8 . . C22 C21 C20 120.5(3) . . C22 C21 H21 119.8 . . C21 C22 H22 119.4 . . C21 C22 C23 121.3(3) . . C23 C22 H22 119.4 . . C22 C23 C24 117.8(3) . . C22 C23 C26 120.9(3) . . C24 C23 C26 121.3(3) . . C23 C24 H24 119.3 . . C25 C24 C23 121.5(3) . . C25 C24 H24 119.3 . . C20 C25 H25 119.7 . . C24 C25 C20 120.6(3) . . C24 C25 H25 119.7 . . C23 C26 H26A 109.5 . . C23 C26 H26B 109.5 . . C23 C26 H26C 109.5 . . H26A C26 H26B 109.5 . . H26A C26 H26C 109.5 . . H26B C26 H26C 109.5 . . C27 O8 Dy1 95.34(16) . . C27 O9 Dy1 89.53(15) . . O8 C27 Dy1 58.04(14) . . O8 C27 O9 120.9(3) . . O8 C27 C28 118.4(2) . . O9 C27 Dy1 63.60(14) . . O9 C27 C28 120.7(2) . . C28 C27 Dy1 169.68(18) . . C29 C28 C27 121.2(3) . . C33 C28 C27 120.5(2) . . C33 C28 C29 118.2(3) . . C28 C29 H29 119.9 . . C30 C29 C28 120.1(3) . . C30 C29 H29 119.9 . . C29 C30 H30 119.0 . . C29 C30 C31 122.0(3) . . C31 C30 H30 119.0 . . C30 C31 C32 117.4(3) . . C30 C31 C34 122.3(3) . . C32 C31 C34 120.3(4) . . C31 C32 H32 119.3 . . C33 C32 C31 121.4(3) . . C33 C32 H32 119.3 . . C28 C33 H33 119.5 . . C32 C33 C28 120.9(3) . . C32 C33 H33 119.5 . . C31 C34 H34A 109.5 . . C31 C34 H34B 109.5 . . C31 C34 H34C 109.5 . . H34A C34 H34B 109.5 . . H34A C34 H34C 109.5 . . H34B C34 H34C 109.5 . . C41A O41A H41A 109.5 . . O41A C41A H41B 109.5 . . O41A C41A H41C 109.5 . . O41A C41A H41D 109.5 . . H41B C41A H41C 109.5 . . H41B C41A H41D 109.5 . . H41C C41A H41D 109.5 . . C42A O42A H42A 109.5 . . O42A C42A H42B 109.5 . . O42A C42A H42C 109.5 . . O42A C42A H42D 109.5 . . H42B C42A H42C 109.5 . . H42B C42A H42D 109.5 . . H42C C42A H42D 109.5 . . N41B C41B C42B 174.4(13) . . C41B C42B H42E 109.5 . . C41B C42B H42F 109.5 . . C41B C42B H42G 109.5 . . H42E C42B H42F 109.5 . . H42E C42B H42G 109.5 . . H42F C42B H42G 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Dy1 O1 2.3742(17) . Dy1 N1 2.628(2) . Dy1 O2 2.3183(18) . Dy1 O3 2.3652(15) . Dy1 N2 2.584(2) . Dy1 O5 2.3713(16) . Dy1 O7 2.4311(18) . Dy1 O8 2.3943(18) . Dy1 O9 2.5170(19) . Mn1 O1 1.9718(18) . Mn1 O1 2.2036(16) 2_666 Mn1 O2 1.8963(16) . Mn1 O3 1.8944(16) 2_666 Mn1 O4 2.1608(16) . Mn1 O6 1.9486(18) 2_666 O1 H1 0.78(2) . N1 C1 1.482(4) . N1 C3 1.481(3) . N1 C5 1.478(3) . C1 H1A 0.9900 . C1 H1B 0.9900 . C1 C2 1.517(4) . C2 H2A 0.9900 . C2 H2B 0.9900 . C2 O2 1.416(3) . C3 H3A 0.9900 . C3 H3B 0.9900 . C3 C4 1.511(3) . C4 H4A 0.9900 . C4 H4B 0.9900 . C4 O3 1.418(3) . C5 H5A 0.9900 . C5 H5B 0.9900 . C5 C6 1.500(4) . C6 C7 1.390(4) . C6 N2 1.342(3) . C7 H7 0.9500 . C7 C8 1.368(5) . C8 H8 0.9500 . C8 C9 1.395(5) . C9 H9 0.9500 . C9 C10 1.378(4) . C10 H10 0.9500 . C10 N2 1.339(3) . O4 C11 1.262(3) . O5 C11 1.262(3) . C11 C12 1.503(3) . C12 C13 1.384(4) . C12 C17 1.382(4) . C13 H13 0.9500 . C13 C14 1.389(4) . C14 H14 0.9500 . C14 C15 1.378(5) . C15 C16 1.384(5) . C15 C18 1.511(4) . C16 H16 0.9500 . C16 C17 1.391(4) . C17 H17 0.9500 . C18 H18A 0.9800 . C18 H18B 0.9800 . C18 H18C 0.9800 . O6 C19 1.289(3) . O7 C19 1.244(3) . C19 C20 1.497(4) . C20 C21 1.394(4) . C20 C25 1.385(4) . C21 H21 0.9500 . C21 C22 1.384(4) . C22 H22 0.9500 . C22 C23 1.386(4) . C23 C24 1.386(4) . C23 C26 1.509(4) . C24 H24 0.9500 . C24 C25 1.383(4) . C25 H25 0.9500 . C26 H26A 0.9800 . C26 H26B 0.9800 . C26 H26C 0.9800 . O8 C27 1.265(3) . O9 C27 1.270(3) . C27 C28 1.486(4) . C28 C29 1.392(4) . C28 C33 1.389(4) . C29 H29 0.9500 . C29 C30 1.378(5) . C30 H30 0.9500 . C30 C31 1.384(5) . C31 C32 1.388(5) . C31 C34 1.510(5) . C32 H32 0.9500 . C32 C33 1.373(4) . C33 H33 0.9500 . C34 H34A 0.9800 . C34 H34B 0.9800 . C34 H34C 0.9800 . O41A H41A 0.8400 . O41A C41A 1.351(8) . C41A H41B 0.9800 . C41A H41C 0.9800 . C41A H41D 0.9800 . O42A H42A 0.8400 . O42A C42A 1.371(8) . C42A H42B 0.9800 . C42A H42C 0.9800 . C42A H42D 0.9800 . N41B C41B 1.059(15) . C41B C42B 1.448(12) . C42B H42E 0.9800 . C42B H42F 0.9800 . C42B H42G 0.9800 . 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_publ_flag O1 H1 O41A 0.78(2) 2.19(3) 2.949(7) 167(3) yes O1 H1 N41B 0.78(2) 2.45(3) 3.220(14) 178(3) yes O41A H41A O42A 0.84 2.11 2.899(10) 155.5 yes O42A H42A O9 0.84 2.00 2.825(6) 166.8 yes C42B H42F O9 0.98 2.39 3.336(10) 162.8 yes