# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_mnekb5 _database_code_depnum_ccdc_archive 'CCDC 259056' #Note to referee: final shelx res file and cifcheck comments are #under refine special details. # Organic groups: # 1 EtC(CH2O-)3 # 2 and 3 tBuCOO- = pivalate (PIV). # 4 and 5 NO3- # 6 NMe4+ cation # 7 MeCN of crystallisation # 8 solvent water? _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[NMe4]2[Mn2Dy2(NO3)4(PIV)4(C6H11O3)2].2MeCN.0.5H2O' _chemical_formula_sum 'C44 H89 Dy2 Mn2 N8 O26.50' _chemical_compound_source 'EKB; reaction number EKB5' _exptl_crystal_recrystallization_method 'Et2O diffusion into MeCN' _chemical_formula_weight 1589.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.6304(4) _cell_length_b 13.3520(4) _cell_length_c 17.0340(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.689(2) _cell_angle_gamma 90.00 _cell_volume 3258.50(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6424 _cell_measurement_theta_min 2 _cell_measurement_theta_max 38 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1606 _exptl_absorpt_coefficient_mu 2.726 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.180 _exptl_absorpt_correction_T_max 0.310 _exptl_absorpt_process_details 'Sadabs v. 2004/1' _exptl_special_details ; Data collection strategy obatined with COSMO. Oxford Cryosystems LT device. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method 'omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47521 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 38.57 _reflns_number_total 9572 _reflns_number_gt 8000 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution Dirdif _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-XP _computing_publication_material SHELXTL-XCIF _refine_special_details ; The two tBu groups are disordered. In both cases the disorder is a ca 60 deg rotation about C1-C2. 'Opposite' C-atoms were contarined to have equal adps, and neighbouring C's were lightly REStrained to have EADPs as well. The disorder about ligand 2 seems to be about an inversion centre, so the occupancies must be 0.5:0.5. That in ligand 3 is also associated with disorder in the nitrate ligand, #4. The occupancies of these groups were fixed at 0.7:0.3 after refinement. Th Uij's on all part weight atoms are high implying that the disorder is more extensive than modelled by part-weight atoms, with extra density is being mopped-up by the adps. 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.88 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.67 Ratio 242_ALERT_2_A Check Low U(eq) as Compared to Neighbors for C22 912_ALERT_3_A Missing FCF Reflections Above STH/L=0.6 ........ 8867 910_ALERT_3_C Missing FCF Reflections Below TH(Min) .......... 3 911_ALERT_3_C Missing FCF Refl. Between TH(Min) & STH/L=0.6 .. 5 The data collection strategy used aimed to obtain a complete data-set to 2\q=54\%. Some higher angle data were also collected, and these have been included in the refinement. Statistics are below. #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 0.998 3416 3408 8 23.01 0.550 0.998 4538 4530 8 25.24 0.600 0.999 5891 5883 8 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 0.999 7495 7487 8 29.84 0.700 0.937 9359 8774 585 32.21 0.750 0.782 11503 8998 2505 34.65 0.800 0.660 13993 9230 4763 37.17 0.850 0.566 16756 9477 7279 39.77 0.900 0.519 18447 9572 8875 061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.66 Sadabs corrects for all systematic errors which lead to disparities in the intensities of equivalent reflections. Such errors include absorption by the fibre and crystal decay. 220_ALERT_2_B Large Non-Solvent O Ueq(max)/Ueq(min) ... 4.36 Ratio 241_ALERT_2_B Check High U(eq) as Compared to Neighbors for C32 241_ALERT_2_B Check High U(eq) as Compared to Neighbors for C52 241_ALERT_2_B Check High U(eq) as Compared to Neighbors for C62 241_ALERT_2_B Check High U(eq) as Compared to Neighbors for C82 215_ALERT_3_C Disordered C52 has ADP max/min Ratio ....... 3.50 215_ALERT_3_C Disordered C82 has ADP max/min Ratio ....... 3.50 242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for C23 242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for C42 242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for C72 301_ALERT_3_C Main Residue Disorder ......................... 18.00 Perc. 302_ALERT_4_C Anion/Solvent Disorder ......................... 5.00 Perc. 413_ALERT_2_C Short Inter XH3 .. XHn H37A .. H73C .. 2.14 Ang. 432_ALERT_2_C Short Inter X...Y Contact O44 .. C63 .. 2.98 Ang. 779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 39.00 Deg. C63 -C23 -C53 1.555 1.555 1.555 779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 26.00 Deg. O44 -N14 -O34 1.555 1.555 1.555 See note on disorder above. 041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? 045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio 068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? This reflects (1) our choice of formula unit, (2) the format of our moiety formula, which is more chemically meaningful and (3) the absence of H-atoms on the part weight water molecule located near an inversion centre (O8). 242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for N14 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for N16 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for C27 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C12 796_ALERT_4_C O-Atom in CIF Coordinate List out of Sequence .. O12 No action taken. Final shelx res file: #TITL MNEKB5 IN P21/C SOLVED DIRDIF #CELL 0.71073 14.63040 13.35200 17.03400 90.0000 101.6890 90.0000 #ZERR 2.000 0.00040 0.00040 0.00050 0.0000 0.0020 0.0000 #LATT +1 #SYMM -X , 1/2+Y , 1/2-Z #SFAC C H N O MN DY #UNIT 88 178 16 53 4 4 REM Organic groups: REM 1 EtC(CH2O-)3 REM 2 and 3 tBuCOO- = pivalate (PIV). REM 4 and 5 NO3- REM 6 NMe4+ cation REM 7 MeCN of crystallisation REM 8 solvent water? (H's not placed) TEMP -123 OMIT 0 1 2 OMIT 1 1 1 OMIT 3 2 2 OMIT 1 1 0 OMIT -2 1 1 L.S. 12 ACTA BOND $H FMAP 2 PLAN 10 REM constrain 'opposite' C's in tBu groups to be equal EADP C32 C62 EADP C42 C72 EADP C52 C82 EADP C33 C63 EADP C43 C73 EADP C53 C83 SIMU 0.05 0.05 C32 > C82 SIMU 0.05 0.05 C33 > C83 REM res/con-traints for disordered nitrate EADP O34 O44 SADI 0.01 N14 O34 N14 O44 WGHT 0.044200 2.317800 FVAR 0.24937 DY1 6 0.200477 0.034565 0.081070 11.00000 0.03009 0.02950 = 0.02338 0.00203 -0.00256 0.00074 MN1 5 -0.021211 0.114141 0.010846 11.00000 0.03046 0.02176 = 0.02272 -0.00145 -0.00132 0.00483 C11 1 0.012218 0.041392 -0.175620 11.00000 0.03558 0.02740 = 0.01965 -0.00026 0.00285 0.00312 C21 1 -0.061921 0.117237 -0.163582 11.00000 0.03715 0.02881 = 0.02138 0.00529 0.00142 0.00549 AFIX 23 H21A 2 -0.034544 0.185226 -0.161569 11.00000 -1.20000 H21B 2 -0.114130 0.114527 -0.210681 11.00000 -1.20000 AFIX 0 O21 4 -0.098568 0.101983 -0.092660 11.00000 0.03228 0.02581 = 0.02107 0.00095 -0.00063 0.00316 C31 1 0.098646 0.050201 -0.109159 11.00000 0.03436 0.03477 = 0.02093 0.00250 0.00355 0.00169 AFIX 23 H31A 2 0.146898 0.003333 -0.120283 11.00000 -1.20000 H31B 2 0.123917 0.118986 -0.109130 11.00000 -1.20000 AFIX 0 O31 4 0.079984 0.028595 -0.031099 11.00000 0.03231 0.03937 = 0.01889 0.00413 0.00013 0.00130 C41 1 -0.025933 -0.066198 -0.180129 11.00000 0.04213 0.02825 = 0.02260 -0.00294 0.00327 0.00261 AFIX 23 H41A 2 -0.077297 -0.071527 -0.227719 11.00000 -1.20000 H41B 2 0.024253 -0.112290 -0.188451 11.00000 -1.20000 AFIX 0 O41 4 -0.059619 -0.099015 -0.111995 11.00000 0.03579 0.02477 = 0.02008 -0.00039 0.00062 0.00204 C51 1 0.040913 0.061904 -0.257159 11.00000 0.05183 0.03959 = 0.02131 0.00090 0.00605 0.00154 AFIX 23 H51A 2 0.092936 0.016161 -0.261436 11.00000 -1.20000 H51B 2 -0.012466 0.043713 -0.300490 11.00000 -1.20000 AFIX 0 C61 1 0.070738 0.167618 -0.272937 11.00000 0.05230 0.04527 = 0.03487 0.00705 0.01216 -0.00135 AFIX 33 H61A 2 0.086557 0.170728 -0.326104 11.00000 -1.50000 H61B 2 0.125428 0.186262 -0.232108 11.00000 -1.50000 H61C 2 0.019491 0.214138 -0.270790 11.00000 -1.50000 AFIX 0 O12 4 0.043952 0.242072 -0.014395 11.00000 0.04448 0.03562 = 0.02955 -0.00075 0.00033 0.00631 O22 4 0.188974 0.205153 0.050268 11.00000 0.04172 0.03435 = 0.03805 0.00866 0.00230 0.00109 C12 1 0.130279 0.262552 0.009529 11.00000 0.04754 0.02903 = 0.02327 -0.00076 0.00268 0.00033 SAME 0.01 C22 C52 C32 C42 SAME 0.01 C22 C62 C72 C82 REM Short Inter X...Y Contact C32 .. C32 .. 3.16 Ang. => occ's C22 1 0.163869 0.363250 -0.015705 11.00000 0.06668 0.03422 = 0.03524 0.00535 -0.00685 -0.00598 PART 1 10.5 C32 1 0.093665 0.442095 -0.005743 10.50000 0.20112 0.04982 = 0.16453 0.02702 0.11844 0.00202 AFIX 33 H32A 2 0.035355 0.430389 -0.044533 10.50000 -1.50000 H32B 2 0.118220 0.508403 -0.014962 10.50000 -1.50000 H32C 2 0.081683 0.438863 0.048758 10.50000 -1.50000 AFIX 0 C42 1 0.170970 0.358525 -0.100278 10.50000 0.15064 0.06014 = 0.04063 0.00230 0.01512 -0.04919 AFIX 33 H42A 2 0.115216 0.325928 -0.131383 10.50000 -1.50000 H42B 2 0.226492 0.319967 -0.105303 10.50000 -1.50000 H42C 2 0.175946 0.426522 -0.120663 10.50000 -1.50000 AFIX 0 C52 1 0.254672 0.391528 0.034569 10.50000 0.14556 0.05798 = 0.15000 0.05965 -0.10121 -0.05025 AFIX 33 H52A 2 0.247192 0.402733 0.089775 10.50000 -1.50000 H52B 2 0.277266 0.453088 0.013591 10.50000 -1.50000 H52C 2 0.299831 0.337533 0.033709 10.50000 -1.50000 AFIX 0 PART 2 10.5 C62 1 0.248907 0.341437 -0.050874 10.50000 0.20112 0.04982 = 0.16453 0.02702 0.11844 0.00202 AFIX 33 H62A 2 0.299945 0.318000 -0.008382 10.50000 -1.50000 H62B 2 0.268188 0.402626 -0.074841 10.50000 -1.50000 H62C 2 0.233615 0.289569 -0.092156 10.50000 -1.50000 AFIX 0 C72 1 0.191227 0.428246 0.053136 10.50000 0.15064 0.06014 = 0.04063 0.00230 0.01512 -0.04919 AFIX 33 H72A 2 0.227917 0.390005 0.097720 10.50000 -1.50000 H72B 2 0.135315 0.455081 0.069019 10.50000 -1.50000 H72C 2 0.228959 0.483625 0.039244 10.50000 -1.50000 AFIX 0 C82 1 0.097304 0.407717 -0.082341 10.50000 0.14556 0.05798 = 0.15000 0.05965 -0.10121 -0.05025 AFIX 33 H82A 2 0.090830 0.364178 -0.129463 10.50000 -1.50000 H82B 2 0.119986 0.473639 -0.095005 10.50000 -1.50000 H82C 2 0.036518 0.415114 -0.067180 10.50000 -1.50000 AFIX 0 PART 0 C13 1 -0.210360 0.166421 0.035633 11.00000 0.03873 0.03226 = 0.02727 0.00327 -0.00025 0.00603 O13 4 -0.123213 0.182551 0.055123 11.00000 0.03878 0.03289 = 0.03106 -0.00018 -0.00167 0.00279 O23 4 -0.248195 0.104676 -0.016462 11.00000 0.03829 0.03718 = 0.03186 -0.00382 0.00243 0.00296 SAME 0.01 C23 C53 C33 C43 SAME 0.01 C23 C63 C73 C83 C23 1 -0.272756 0.223997 0.081882 11.00000 0.04728 0.04949 = 0.03454 -0.00750 -0.00075 0.01551 PART 1 10.7 C33 1 -0.220464 0.292305 0.142911 10.70000 0.05505 0.13139 = 0.10823 -0.09145 0.00580 0.00053 AFIX 33 H33A 2 -0.171084 0.254959 0.178487 10.70000 -1.50000 H33B 2 -0.263037 0.321293 0.174380 10.70000 -1.50000 H33C 2 -0.192527 0.346046 0.116415 10.70000 -1.50000 AFIX 0 C43 1 -0.322378 0.143400 0.124598 10.70000 0.10866 0.06594 = 0.07505 0.00910 0.05976 0.02596 AFIX 33 H43A 2 -0.357932 0.098010 0.084502 10.70000 -1.50000 H43B 2 -0.364875 0.176388 0.154131 10.70000 -1.50000 H43C 2 -0.275530 0.105118 0.162024 10.70000 -1.50000 AFIX 0 C53 1 -0.351535 0.275013 0.024281 10.70000 0.06322 0.08165 = 0.05375 0.01177 0.01690 0.03572 AFIX 33 H53A 2 -0.381732 0.226670 -0.016030 10.70000 -1.50000 H53B 2 -0.326436 0.330680 -0.002340 10.70000 -1.50000 H53C 2 -0.397379 0.300678 0.053966 10.70000 -1.50000 AFIX 0 PART 2 10.3 C63 1 -0.373574 0.214831 0.049916 10.30000 0.05505 0.13139 = 0.10823 -0.09145 0.00580 0.00053 AFIX 33 H63A 2 -0.388488 0.242457 -0.004483 10.30000 -1.50000 H63B 2 -0.407882 0.251877 0.084370 10.30000 -1.50000 H63C 2 -0.391551 0.144050 0.048555 10.30000 -1.50000 AFIX 0 C73 1 -0.241390 0.333962 0.075279 10.30000 0.10866 0.06594 = 0.07505 0.00910 0.05976 0.02596 AFIX 33 H73A 2 -0.178131 0.342711 0.107072 10.30000 -1.50000 H73B 2 -0.284318 0.378826 0.095549 10.30000 -1.50000 H73C 2 -0.241878 0.349911 0.019038 10.30000 -1.50000 AFIX 0 C83 1 -0.244130 0.199872 0.169811 10.30000 0.06322 0.08165 = 0.05375 0.01177 0.01690 0.03572 AFIX 33 H83A 2 -0.175959 0.202487 0.185939 10.30000 -1.50000 H83B 2 -0.265983 0.132570 0.179758 10.30000 -1.50000 H83C 2 -0.271821 0.248863 0.200949 10.30000 -1.50000 AFIX 0 PART 0 N14 3 0.368892 0.106389 0.030649 11.00000 0.03898 0.09963 = 0.04945 0.01957 0.00213 -0.01231 O14 4 0.363492 0.086544 0.102712 11.00000 0.03729 0.08545 = 0.04049 0.01835 -0.00431 -0.00885 O24 4 0.298749 0.086544 -0.022944 11.00000 0.04049 0.05327 = 0.03675 0.00451 0.00334 -0.00048 PART 1 10.7 O34 4 0.443708 0.135015 0.015625 10.70000 0.04086 0.23786 = 0.07263 0.05441 0.00317 -0.03972 PART 2 10.3 O44 4 0.422525 0.170139 0.013903 10.30000 0.04086 0.23786 = 0.07263 0.05441 0.00317 -0.03972 PART 0 N15 3 0.299939 0.008011 0.244373 11.00000 0.03925 0.05022 = 0.02755 0.00504 -0.00451 -0.00592 O15 4 0.252749 0.086987 0.222090 11.00000 0.04904 0.04613 = 0.03092 -0.00258 -0.00461 0.00477 O25 4 0.287933 -0.064321 0.194846 11.00000 0.04685 0.03674 = 0.03400 0.00244 -0.00716 -0.00042 O35 4 0.353577 0.001630 0.308973 11.00000 0.05966 0.06709 = 0.03431 0.00542 -0.01959 -0.00383 N16 3 0.566577 0.826128 0.211882 11.00000 0.04130 0.05154 = 0.04418 0.00498 -0.00323 0.00218 C16 1 0.668412 0.844945 0.221712 11.00000 0.04503 0.07602 = 0.07044 -0.00780 -0.00446 0.00154 AFIX 33 H16A 2 0.703140 0.787884 0.249115 11.00000 -1.50000 H16B 2 0.685061 0.905758 0.253620 11.00000 -1.50000 H16C 2 0.684168 0.853598 0.168881 11.00000 -1.50000 AFIX 0 C26 1 0.543950 0.814015 0.291658 11.00000 0.08075 0.17010 = 0.05763 0.03338 0.01218 -0.01595 AFIX 33 H26A 2 0.476808 0.802175 0.285870 11.00000 -1.50000 H26B 2 0.561390 0.874937 0.323231 11.00000 -1.50000 H26C 2 0.578579 0.756865 0.319011 11.00000 -1.50000 AFIX 0 C36 1 0.544258 0.735753 0.161232 11.00000 0.09396 0.05290 = 0.09785 0.00017 -0.02836 -0.01044 AFIX 33 H36A 2 0.477237 0.721794 0.153122 11.00000 -1.50000 H36B 2 0.579424 0.678477 0.187835 11.00000 -1.50000 H36C 2 0.561343 0.747178 0.109221 11.00000 -1.50000 AFIX 0 C46 1 0.514743 0.913254 0.169945 11.00000 0.06440 0.06837 = 0.06601 0.01086 0.00124 0.02579 AFIX 33 H46A 2 0.447473 0.901554 0.163198 11.00000 -1.50000 H46B 2 0.530896 0.921503 0.117226 11.00000 -1.50000 H46C 2 0.531761 0.974023 0.201823 11.00000 -1.50000 AFIX 0 N17 3 0.347096 0.583810 0.177005 11.00000 0.09303 0.08236 = 0.07536 0.00877 -0.00108 0.01698 C27 1 0.279638 0.628364 0.157511 11.00000 0.09533 0.04184 = 0.04333 0.00038 0.01002 0.00798 C37 1 0.193486 0.682285 0.131097 11.00000 0.11500 0.05821 = 0.07294 0.01222 0.03014 0.03898 AFIX 137 H37A 2 0.165967 0.663251 0.075795 11.00000 -1.50000 H37B 2 0.206011 0.754440 0.133587 11.00000 -1.50000 H37C 2 0.149934 0.665806 0.165960 11.00000 -1.50000 AFIX 0 PART -1 O8 4 0.476883 0.473148 0.017238 10.25000 0.09370 HKLF 4 REM MNEKB5 IN P21/C SOLVED DIRDIF REM R1 = 0.0295 for 8000 Fo > 4sig(Fo) and 0.0385 for all 9572 data REM 396 parameters refined using 127 restraints END WGHT 0.0443 2.3064 REM Highest difference peak 1.327, deepest hole -0.939, 1-sigma level 0.114 Q1 1 0.1784 -0.0157 0.0958 11.00000 0.05 1.33 Q2 1 0.2286 0.0755 0.0569 11.00000 0.05 1.19 Q3 1 0.2405 0.0515 0.0584 11.00000 0.05 1.17 Q4 1 0.2281 -0.0110 0.0575 11.00000 0.05 1.09 Q5 1 0.1757 0.0808 0.0972 11.00000 0.05 1.04 Q6 1 0.6001 0.9657 0.2441 11.00000 0.05 1.02 Q7 1 -0.2011 0.1034 -0.0805 11.00000 0.05 1.00 Q8 1 0.0622 0.4394 -0.0186 11.00000 0.05 0.76 Q9 1 0.0208 0.1831 -0.0083 11.00000 0.05 0.75 Q10 1 0.4693 0.5058 0.0564 11.00000 0.05 0.73 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+2.3178P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ; riding; not placed on part-weight water - O8 ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9572 _refine_ls_number_parameters 396 _refine_ls_number_restraints 127 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.200477(8) 0.034565(9) 0.081070(7) 0.02878(5) Uani 1 1 d . . . Mn1 Mn -0.02121(2) 0.11414(3) 0.01085(2) 0.02592(8) Uani 1 1 d . . . C11 C 0.01222(18) 0.04139(17) -0.17562(15) 0.0279(5) Uani 1 1 d . . . C21 C -0.06192(18) 0.11724(19) -0.16358(14) 0.0297(5) Uani 1 1 d . . . H21A H -0.0345 0.1852 -0.1616 0.036 Uiso 1 1 calc R . . H21B H -0.1141 0.1145 -0.2107 0.036 Uiso 1 1 calc R . . O21 O -0.09857(12) 0.10198(13) -0.09266(10) 0.0272(3) Uani 1 1 d . . . C31 C 0.09865(18) 0.0502(2) -0.10916(15) 0.0303(5) Uani 1 1 d . . . H31A H 0.1469 0.0033 -0.1203 0.036 Uiso 1 1 calc R . . H31B H 0.1239 0.1190 -0.1091 0.036 Uiso 1 1 calc R . . O31 O 0.07998(13) 0.02859(13) -0.03110(11) 0.0309(4) Uani 1 1 d . . . C41 C -0.02593(19) -0.0662(2) -0.18013(15) 0.0315(5) Uani 1 1 d . . . H41A H -0.0773 -0.0715 -0.2277 0.038 Uiso 1 1 calc R . . H41B H 0.0243 -0.1123 -0.1885 0.038 Uiso 1 1 calc R . . O41 O -0.05962(12) -0.09902(13) -0.11199(10) 0.0276(3) Uani 1 1 d . . . C51 C 0.0409(2) 0.0619(2) -0.25716(16) 0.0378(6) Uani 1 1 d . . . H51A H 0.0929 0.0162 -0.2614 0.045 Uiso 1 1 calc R . . H51B H -0.0125 0.0437 -0.3005 0.045 Uiso 1 1 calc R . . C61 C 0.0707(2) 0.1676(2) -0.27294(18) 0.0437(7) Uani 1 1 d . . . H61A H 0.0866 0.1707 -0.3261 0.066 Uiso 1 1 calc R . . H61B H 0.1254 0.1863 -0.2321 0.066 Uiso 1 1 calc R . . H61C H 0.0195 0.2141 -0.2708 0.066 Uiso 1 1 calc R . . O12 O 0.04395(14) 0.24207(15) -0.01439(11) 0.0376(4) Uani 1 1 d . . . O22 O 0.18897(14) 0.20515(15) 0.05027(13) 0.0389(4) Uani 1 1 d . . . C12 C 0.1303(2) 0.2626(2) 0.00953(15) 0.0339(5) Uani 1 1 d . A . C22 C 0.1639(2) 0.3633(2) -0.01571(17) 0.0478(7) Uani 1 1 d D . . C32 C 0.0937(9) 0.4421(7) -0.0057(10) 0.127(4) Uani 0.50 1 d PDU A 1 H32A H 0.0354 0.4304 -0.0445 0.191 Uiso 0.50 1 calc PR A 1 H32B H 0.1182 0.5084 -0.0150 0.191 Uiso 0.50 1 calc PR A 1 H32C H 0.0817 0.4389 0.0488 0.191 Uiso 0.50 1 calc PR A 1 C42 C 0.1710(10) 0.3585(7) -0.1003(4) 0.084(3) Uani 0.50 1 d PDU A 1 H42A H 0.1152 0.3259 -0.1314 0.127 Uiso 0.50 1 calc PR A 1 H42B H 0.2265 0.3200 -0.1053 0.127 Uiso 0.50 1 calc PR A 1 H42C H 0.1759 0.4265 -0.1207 0.127 Uiso 0.50 1 calc PR A 1 C52 C 0.2547(8) 0.3915(8) 0.0346(8) 0.136(5) Uani 0.50 1 d PDU A 1 H52A H 0.2472 0.4027 0.0898 0.204 Uiso 0.50 1 calc PR A 1 H52B H 0.2773 0.4531 0.0136 0.204 Uiso 0.50 1 calc PR A 1 H52C H 0.2998 0.3375 0.0337 0.204 Uiso 0.50 1 calc PR A 1 C62 C 0.2489(9) 0.3414(7) -0.0509(9) 0.127(4) Uani 0.50 1 d PDU A 2 H62A H 0.2999 0.3180 -0.0084 0.191 Uiso 0.50 1 calc PR A 2 H62B H 0.2682 0.4026 -0.0748 0.191 Uiso 0.50 1 calc PR A 2 H62C H 0.2336 0.2896 -0.0922 0.191 Uiso 0.50 1 calc PR A 2 C72 C 0.1912(9) 0.4282(7) 0.0531(4) 0.084(3) Uani 0.50 1 d PDU A 2 H72A H 0.2279 0.3900 0.0977 0.127 Uiso 0.50 1 calc PR A 2 H72B H 0.1353 0.4551 0.0690 0.127 Uiso 0.50 1 calc PR A 2 H72C H 0.2290 0.4836 0.0392 0.127 Uiso 0.50 1 calc PR A 2 C82 C 0.0973(9) 0.4077(7) -0.0823(8) 0.136(5) Uani 0.50 1 d PDU A 2 H82A H 0.0908 0.3642 -0.1295 0.204 Uiso 0.50 1 calc PR A 2 H82B H 0.1200 0.4736 -0.0950 0.204 Uiso 0.50 1 calc PR A 2 H82C H 0.0365 0.4151 -0.0672 0.204 Uiso 0.50 1 calc PR A 2 C13 C -0.21036(19) 0.1664(2) 0.03563(16) 0.0337(5) Uani 1 1 d . B . O13 O -0.12321(13) 0.18255(14) 0.05512(11) 0.0355(4) Uani 1 1 d . . . O23 O -0.24820(13) 0.10468(15) -0.01646(12) 0.0364(4) Uani 1 1 d . . . C23 C -0.2728(2) 0.2240(2) 0.08188(17) 0.0450(7) Uani 1 1 d D . . C33 C -0.2205(4) 0.2923(6) 0.1429(5) 0.100(3) Uani 0.70 1 d PDU B 1 H33A H -0.1711 0.2550 0.1785 0.150 Uiso 0.70 1 calc PR B 1 H33B H -0.2630 0.3213 0.1744 0.150 Uiso 0.70 1 calc PR B 1 H33C H -0.1925 0.3460 0.1164 0.150 Uiso 0.70 1 calc PR B 1 C43 C -0.3224(5) 0.1434(4) 0.1246(4) 0.0774(18) Uani 0.70 1 d PDU B 1 H43A H -0.3579 0.0980 0.0845 0.116 Uiso 0.70 1 calc PR B 1 H43B H -0.3649 0.1764 0.1541 0.116 Uiso 0.70 1 calc PR B 1 H43C H -0.2755 0.1051 0.1620 0.116 Uiso 0.70 1 calc PR B 1 C53 C -0.3515(4) 0.2750(5) 0.0243(3) 0.0655(15) Uani 0.70 1 d PDU B 1 H53A H -0.3817 0.2267 -0.0160 0.098 Uiso 0.70 1 calc PR B 1 H53B H -0.3264 0.3307 -0.0023 0.098 Uiso 0.70 1 calc PR B 1 H53C H -0.3974 0.3007 0.0540 0.098 Uiso 0.70 1 calc PR B 1 C63 C -0.3736(6) 0.2148(13) 0.0499(9) 0.100(3) Uani 0.30 1 d PDU B 2 H63A H -0.3885 0.2425 -0.0045 0.150 Uiso 0.30 1 calc PR B 2 H63B H -0.4079 0.2519 0.0844 0.150 Uiso 0.30 1 calc PR B 2 H63C H -0.3916 0.1440 0.0486 0.150 Uiso 0.30 1 calc PR B 2 C73 C -0.2414(10) 0.3340(6) 0.0753(9) 0.0774(18) Uani 0.30 1 d PDU B 2 H73A H -0.1781 0.3427 0.1071 0.116 Uiso 0.30 1 calc PR B 2 H73B H -0.2843 0.3788 0.0955 0.116 Uiso 0.30 1 calc PR B 2 H73C H -0.2419 0.3499 0.0190 0.116 Uiso 0.30 1 calc PR B 2 C83 C -0.2441(9) 0.1999(11) 0.1698(5) 0.0655(15) Uani 0.30 1 d PDU B 2 H83A H -0.1760 0.2025 0.1859 0.098 Uiso 0.30 1 calc PR B 2 H83B H -0.2660 0.1326 0.1798 0.098 Uiso 0.30 1 calc PR B 2 H83C H -0.2718 0.2489 0.2009 0.098 Uiso 0.30 1 calc PR B 2 N14 N 0.3689(2) 0.1064(3) 0.03065(19) 0.0637(9) Uani 1 1 d D . . O14 O 0.36349(15) 0.0865(2) 0.10271(14) 0.0561(6) Uani 1 1 d . C . O24 O 0.29875(15) 0.08654(18) -0.02294(13) 0.0441(5) Uani 1 1 d . C . O34 O 0.4437(4) 0.1350(9) 0.0156(10) 0.118(5) Uani 0.70 1 d PD C 1 O44 O 0.4225(14) 0.170(3) 0.014(3) 0.118(5) Uani 0.30 1 d PD C 2 N15 N 0.29994(18) 0.0080(2) 0.24437(15) 0.0406(5) Uani 1 1 d . . . O15 O 0.25275(15) 0.08699(17) 0.22209(12) 0.0438(5) Uani 1 1 d . C . O25 O 0.28793(15) -0.06432(16) 0.19485(12) 0.0414(5) Uani 1 1 d . C . O35 O 0.35358(18) 0.0016(2) 0.30897(14) 0.0578(6) Uani 1 1 d . C . N16 N 0.56658(18) 0.8261(2) 0.21188(17) 0.0473(6) Uani 1 1 d . . . C16 C 0.6684(3) 0.8449(3) 0.2217(3) 0.0661(10) Uani 1 1 d . . . H16A H 0.7031 0.7879 0.2491 0.099 Uiso 1 1 calc R . . H16B H 0.6851 0.9058 0.2536 0.099 Uiso 1 1 calc R . . H16C H 0.6842 0.8536 0.1689 0.099 Uiso 1 1 calc R . . C26 C 0.5439(4) 0.8140(5) 0.2917(3) 0.103(2) Uani 1 1 d . . . H26A H 0.4768 0.8022 0.2859 0.155 Uiso 1 1 calc R . . H26B H 0.5614 0.8749 0.3232 0.155 Uiso 1 1 calc R . . H26C H 0.5786 0.7569 0.3190 0.155 Uiso 1 1 calc R . . C36 C 0.5443(4) 0.7358(3) 0.1612(3) 0.0883(16) Uani 1 1 d . . . H36A H 0.4772 0.7218 0.1531 0.132 Uiso 1 1 calc R . . H36B H 0.5794 0.6785 0.1878 0.132 Uiso 1 1 calc R . . H36C H 0.5613 0.7472 0.1092 0.132 Uiso 1 1 calc R . . C46 C 0.5147(3) 0.9133(3) 0.1699(3) 0.0679(11) Uani 1 1 d . . . H46A H 0.4475 0.9016 0.1632 0.102 Uiso 1 1 calc R . . H46B H 0.5309 0.9215 0.1172 0.102 Uiso 1 1 calc R . . H46C H 0.5318 0.9740 0.2018 0.102 Uiso 1 1 calc R . . N17 N 0.3471(3) 0.5838(4) 0.1770(3) 0.0861(12) Uani 1 1 d . . . C27 C 0.2796(3) 0.6284(3) 0.1575(2) 0.0607(10) Uani 1 1 d . . . C37 C 0.1935(4) 0.6823(3) 0.1311(3) 0.0805(14) Uani 1 1 d . . . H37A H 0.1660 0.6633 0.0758 0.121 Uiso 1 1 calc R . . H37B H 0.2060 0.7544 0.1336 0.121 Uiso 1 1 calc R . . H37C H 0.1499 0.6658 0.1660 0.121 Uiso 1 1 calc R . . O8 O 0.4769(12) 0.4731(11) 0.0172(10) 0.094(5) Uiso 0.25 1 d P D -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 0.03009(7) 0.02950(7) 0.02338(7) 0.00203(4) -0.00256(4) 0.00074(4) Mn1 0.03046(17) 0.02176(17) 0.02272(17) -0.00145(13) -0.00132(13) 0.00483(13) C11 0.0356(12) 0.0274(12) 0.0196(11) -0.0003(8) 0.0029(9) 0.0031(9) C21 0.0371(12) 0.0288(12) 0.0214(11) 0.0053(9) 0.0014(9) 0.0055(10) O21 0.0323(8) 0.0258(8) 0.0211(8) 0.0010(6) -0.0006(6) 0.0032(7) C31 0.0344(12) 0.0348(13) 0.0209(11) 0.0025(9) 0.0036(9) 0.0017(10) O31 0.0323(9) 0.0394(10) 0.0189(8) 0.0041(7) 0.0001(6) 0.0013(7) C41 0.0421(13) 0.0282(12) 0.0226(11) -0.0029(9) 0.0033(9) 0.0026(10) O41 0.0358(8) 0.0248(8) 0.0201(8) -0.0004(6) 0.0006(6) 0.0020(7) C51 0.0518(16) 0.0396(14) 0.0213(12) 0.0009(10) 0.0061(11) 0.0015(12) C61 0.0523(17) 0.0453(17) 0.0349(15) 0.0071(12) 0.0122(12) -0.0014(13) O12 0.0445(10) 0.0356(10) 0.0296(9) -0.0007(8) 0.0003(8) 0.0063(8) O22 0.0417(10) 0.0344(10) 0.0380(11) 0.0087(8) 0.0023(8) 0.0011(8) C12 0.0475(14) 0.0290(12) 0.0233(12) -0.0008(9) 0.0027(10) 0.0003(11) C22 0.067(2) 0.0342(14) 0.0352(15) 0.0053(12) -0.0069(13) -0.0060(14) C32 0.201(11) 0.050(4) 0.165(9) 0.027(5) 0.118(9) 0.002(5) C42 0.151(8) 0.060(4) 0.041(3) 0.002(3) 0.015(4) -0.049(4) C52 0.146(8) 0.058(4) 0.150(8) 0.060(5) -0.101(7) -0.050(5) C62 0.201(11) 0.050(4) 0.165(9) 0.027(5) 0.118(9) 0.002(5) C72 0.151(8) 0.060(4) 0.041(3) 0.002(3) 0.015(4) -0.049(4) C82 0.146(8) 0.058(4) 0.150(8) 0.060(5) -0.101(7) -0.050(5) C13 0.0387(13) 0.0323(13) 0.0273(12) 0.0033(10) -0.0002(10) 0.0060(10) O13 0.0388(9) 0.0329(9) 0.0311(9) -0.0002(7) -0.0017(7) 0.0028(8) O23 0.0383(9) 0.0372(10) 0.0319(10) -0.0038(8) 0.0024(7) 0.0030(8) C23 0.0473(15) 0.0495(18) 0.0345(15) -0.0075(12) -0.0008(11) 0.0155(14) C33 0.055(3) 0.131(6) 0.108(5) -0.091(5) 0.006(3) 0.001(3) C43 0.109(5) 0.066(3) 0.075(4) 0.009(3) 0.060(4) 0.026(3) C53 0.063(3) 0.082(4) 0.054(3) 0.012(3) 0.017(2) 0.036(3) C63 0.055(3) 0.131(6) 0.108(5) -0.091(5) 0.006(3) 0.001(3) C73 0.109(5) 0.066(3) 0.075(4) 0.009(3) 0.060(4) 0.026(3) C83 0.063(3) 0.082(4) 0.054(3) 0.012(3) 0.017(2) 0.036(3) N14 0.0390(14) 0.100(3) 0.0495(17) 0.0196(17) 0.0021(12) -0.0123(16) O14 0.0373(11) 0.0854(18) 0.0405(12) 0.0183(12) -0.0043(9) -0.0088(11) O24 0.0405(10) 0.0533(13) 0.0368(11) 0.0045(9) 0.0033(8) -0.0005(9) O34 0.041(4) 0.238(11) 0.073(2) 0.054(7) 0.003(4) -0.040(6) O44 0.041(4) 0.238(11) 0.073(2) 0.054(7) 0.003(4) -0.040(6) N15 0.0393(12) 0.0502(14) 0.0276(12) 0.0050(10) -0.0045(9) -0.0059(11) O15 0.0490(11) 0.0461(12) 0.0309(10) -0.0026(9) -0.0046(8) 0.0048(9) O25 0.0469(11) 0.0367(10) 0.0340(11) 0.0024(8) -0.0072(8) -0.0004(9) O35 0.0597(14) 0.0671(15) 0.0343(12) 0.0054(11) -0.0196(10) -0.0038(13) N16 0.0413(13) 0.0515(15) 0.0442(15) 0.0050(12) -0.0032(10) 0.0022(11) C16 0.0450(18) 0.076(3) 0.070(3) -0.008(2) -0.0045(17) 0.0015(18) C26 0.081(3) 0.170(6) 0.058(3) 0.033(3) 0.012(2) -0.016(4) C36 0.094(3) 0.053(2) 0.098(4) 0.000(2) -0.028(3) -0.010(2) C46 0.064(2) 0.068(3) 0.066(3) 0.011(2) 0.0012(19) 0.026(2) N17 0.093(3) 0.082(3) 0.075(3) 0.009(2) -0.001(2) 0.017(2) C27 0.095(3) 0.0418(18) 0.0433(19) 0.0004(15) 0.0100(19) 0.0080(19) C37 0.115(4) 0.058(2) 0.073(3) 0.012(2) 0.030(3) 0.039(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O31 2.3238(18) . ? Dy1 O22 2.336(2) . ? Dy1 O23 2.3381(19) 3 ? Dy1 O41 2.3884(17) 3 ? Dy1 O21 2.3885(17) 3 ? Dy1 O14 2.439(2) . ? Dy1 O15 2.470(2) . ? Dy1 O25 2.476(2) . ? Dy1 O24 2.592(2) . ? Dy1 N15 2.888(2) . ? Dy1 N14 2.930(3) . ? Dy1 Mn1 3.3922(4) . ? Mn1 O41 1.8926(17) 3 ? Mn1 O21 1.8993(16) . ? Mn1 O13 2.021(2) . ? Mn1 O12 2.044(2) . ? Mn1 O31 2.1061(19) . ? Mn1 O31 2.1472(18) 3 ? Mn1 Mn1 3.1473(7) 3 ? Mn1 Dy1 3.4071(4) 3 ? C11 C31 1.521(4) . ? C11 C21 1.528(3) . ? C11 C41 1.537(3) . ? C11 C51 1.555(4) . ? C21 O21 1.432(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? O21 Dy1 2.3885(17) 3 ? C31 O31 1.440(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? O31 Mn1 2.1472(18) 3 ? C41 O41 1.419(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? O41 Mn1 1.8926(17) 3 ? O41 Dy1 2.3884(17) 3 ? C51 C61 1.517(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? O12 C12 1.276(3) . ? O22 C12 1.251(3) . ? C12 C22 1.523(4) . ? C22 C72 1.449(6) . ? C22 C82 1.463(6) . ? C22 C42 1.467(6) . ? C22 C52 1.476(6) . ? C22 C32 1.504(7) . ? C22 C62 1.514(7) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C13 O23 1.255(3) . ? C13 O13 1.269(3) . ? C13 C23 1.529(4) . ? O23 Dy1 2.3380(19) 3 ? C23 C63 1.470(7) . ? C23 C33 1.475(5) . ? C23 C83 1.506(7) . ? C23 C53 1.516(5) . ? C23 C73 1.549(7) . ? C23 C43 1.558(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? N14 O44 1.230(10) . ? N14 O34 1.234(6) . ? N14 O24 1.256(4) . ? N14 O14 1.274(4) . ? N15 O35 1.218(3) . ? N15 O25 1.271(3) . ? N15 O15 1.275(3) . ? N16 C26 1.471(5) . ? N16 C36 1.481(5) . ? N16 C16 1.487(4) . ? N16 C46 1.490(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? N17 C27 1.143(6) . ? C27 C37 1.442(6) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O31 Dy1 O22 80.83(7) . . ? O31 Dy1 O23 80.49(6) . 3 ? O22 Dy1 O23 133.19(7) . 3 ? O31 Dy1 O41 69.45(6) . 3 ? O22 Dy1 O41 70.86(7) . 3 ? O23 Dy1 O41 138.04(6) 3 3 ? O31 Dy1 O21 70.09(6) . 3 ? O22 Dy1 O21 138.17(6) . 3 ? O23 Dy1 O21 71.51(6) 3 3 ? O41 Dy1 O21 71.09(6) 3 3 ? O31 Dy1 O14 133.61(7) . . ? O22 Dy1 O14 77.30(8) . . ? O23 Dy1 O14 85.49(9) 3 . ? O41 Dy1 O14 136.48(8) 3 . ? O21 Dy1 O14 144.32(8) 3 . ? O31 Dy1 O15 147.48(7) . . ? O22 Dy1 O15 86.34(7) . . ? O23 Dy1 O15 128.31(7) 3 . ? O41 Dy1 O15 78.14(6) 3 . ? O21 Dy1 O15 102.21(7) 3 . ? O14 Dy1 O15 70.84(8) . . ? O31 Dy1 O25 144.18(6) . . ? O22 Dy1 O25 134.27(7) . . ? O23 Dy1 O25 77.77(7) 3 . ? O41 Dy1 O25 110.59(7) 3 . ? O21 Dy1 O25 76.15(6) 3 . ? O14 Dy1 O25 72.49(8) . . ? O15 Dy1 O25 51.75(7) . . ? O31 Dy1 O24 83.14(7) . . ? O22 Dy1 O24 67.05(7) . . ? O23 Dy1 O24 68.36(7) 3 . ? O41 Dy1 O24 132.61(6) 3 . ? O21 Dy1 O24 134.65(7) 3 . ? O14 Dy1 O24 50.68(7) . . ? O15 Dy1 O24 118.92(7) . . ? O25 Dy1 O24 114.05(7) . . ? O31 Dy1 N15 159.72(7) . . ? O22 Dy1 N15 109.60(8) . . ? O23 Dy1 N15 102.45(8) 3 . ? O41 Dy1 N15 96.93(7) 3 . ? O21 Dy1 N15 91.60(6) 3 . ? O14 Dy1 N15 66.60(7) . . ? O15 Dy1 N15 26.07(8) . . ? O25 Dy1 N15 25.98(8) . . ? O24 Dy1 N15 116.75(7) . . ? O31 Dy1 N14 108.25(8) . . ? O22 Dy1 N14 69.00(9) . . ? O23 Dy1 N14 76.89(9) 3 . ? O41 Dy1 N14 139.56(9) 3 . ? O21 Dy1 N14 148.22(9) 3 . ? O14 Dy1 N14 25.40(8) . . ? O15 Dy1 N14 94.55(9) . . ? O25 Dy1 N14 94.13(8) . . ? O24 Dy1 N14 25.35(7) . . ? N15 Dy1 N14 91.89(8) . . ? O31 Dy1 Mn1 37.72(5) . . ? O22 Dy1 Mn1 66.12(5) . . ? O23 Dy1 Mn1 116.00(5) 3 . ? O41 Dy1 Mn1 32.74(4) 3 . ? O21 Dy1 Mn1 72.54(4) 3 . ? O14 Dy1 Mn1 143.12(6) . . ? O15 Dy1 Mn1 109.86(5) . . ? O25 Dy1 Mn1 138.46(5) . . ? O24 Dy1 Mn1 107.35(5) . . ? N15 Dy1 Mn1 129.59(6) . . ? N14 Dy1 Mn1 126.50(6) . . ? O41 Mn1 O21 168.77(7) 3 . ? O41 Mn1 O13 94.64(8) 3 . ? O21 Mn1 O13 92.23(7) . . ? O41 Mn1 O12 92.79(8) 3 . ? O21 Mn1 O12 95.27(8) . . ? O13 Mn1 O12 96.43(8) . . ? O41 Mn1 O31 84.17(7) 3 . ? O21 Mn1 O31 88.07(7) . . ? O13 Mn1 O31 173.97(8) . . ? O12 Mn1 O31 89.54(7) . . ? O41 Mn1 O31 87.47(7) 3 3 ? O21 Mn1 O31 83.72(7) . 3 ? O13 Mn1 O31 89.50(8) . 3 ? O12 Mn1 O31 174.03(8) . 3 ? O31 Mn1 O31 84.55(8) . 3 ? O41 Mn1 Mn1 84.37(5) 3 3 ? O21 Mn1 Mn1 84.42(5) . 3 ? O13 Mn1 Mn1 131.26(6) . 3 ? O12 Mn1 Mn1 132.31(6) . 3 ? O31 Mn1 Mn1 42.78(5) . 3 ? O31 Mn1 Mn1 41.77(5) 3 3 ? O41 Mn1 Dy1 43.04(5) 3 . ? O21 Mn1 Dy1 130.39(5) . . ? O13 Mn1 Dy1 137.34(5) . . ? O12 Mn1 Dy1 83.25(5) . . ? O31 Mn1 Dy1 42.45(5) . . ? O31 Mn1 Dy1 92.91(5) 3 . ? Mn1 Mn1 Dy1 62.669(11) 3 . ? O41 Mn1 Dy1 129.57(5) 3 3 ? O21 Mn1 Dy1 42.70(5) . 3 ? O13 Mn1 Dy1 82.94(5) . 3 ? O12 Mn1 Dy1 137.63(5) . 3 ? O31 Mn1 Dy1 93.25(5) . 3 ? O31 Mn1 Dy1 42.32(5) 3 3 ? Mn1 Mn1 Dy1 62.187(12) 3 3 ? Dy1 Mn1 Dy1 124.856(11) . 3 ? C31 C11 C21 110.8(2) . . ? C31 C11 C41 110.4(2) . . ? C21 C11 C41 111.4(2) . . ? C31 C11 C51 108.5(2) . . ? C21 C11 C51 109.3(2) . . ? C41 C11 C51 106.3(2) . . ? O21 C21 C11 114.60(19) . . ? O21 C21 H21A 108.6 . . ? C11 C21 H21A 108.6 . . ? O21 C21 H21B 108.6 . . ? C11 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C21 O21 Mn1 121.09(15) . . ? C21 O21 Dy1 121.66(14) . 3 ? Mn1 O21 Dy1 104.66(7) . 3 ? O31 C31 C11 112.8(2) . . ? O31 C31 H31A 109.0 . . ? C11 C31 H31A 109.0 . . ? O31 C31 H31B 109.0 . . ? C11 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C31 O31 Mn1 118.85(15) . . ? C31 O31 Mn1 118.90(15) . 3 ? Mn1 O31 Mn1 95.45(8) . 3 ? C31 O31 Dy1 119.89(15) . . ? Mn1 O31 Dy1 99.83(7) . . ? Mn1 O31 Dy1 99.22(7) 3 . ? O41 C41 C11 115.5(2) . . ? O41 C41 H41A 108.4 . . ? C11 C41 H41A 108.4 . . ? O41 C41 H41B 108.4 . . ? C11 C41 H41B 108.4 . . ? H41A C41 H41B 107.5 . . ? C41 O41 Mn1 121.40(16) . 3 ? C41 O41 Dy1 121.82(14) . 3 ? Mn1 O41 Dy1 104.22(7) 3 3 ? C61 C51 C11 117.5(2) . . ? C61 C51 H51A 107.9 . . ? C11 C51 H51A 107.9 . . ? C61 C51 H51B 107.9 . . ? C11 C51 H51B 107.9 . . ? H51A C51 H51B 107.2 . . ? C51 C61 H61A 109.5 . . ? C51 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C51 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C12 O12 Mn1 125.85(17) . . ? C12 O22 Dy1 137.07(18) . . ? O22 C12 O12 124.7(3) . . ? O22 C12 C22 118.2(3) . . ? O12 C12 C22 117.0(2) . . ? C72 C22 C82 114.6(6) . . ? C72 C22 C42 139.3(5) . . ? C82 C22 C42 54.8(7) . . ? C72 C22 C52 46.3(7) . . ? C82 C22 C52 136.5(5) . . ? C42 C22 C52 110.3(7) . . ? C72 C22 C32 64.7(7) . . ? C82 C22 C32 56.0(7) . . ? C42 C22 C32 109.1(6) . . ? C52 C22 C32 108.1(7) . . ? C72 C22 C62 108.7(6) . . ? C82 C22 C62 104.0(7) . . ? C42 C22 C62 51.4(6) . . ? C52 C22 C62 64.1(7) . . ? C32 C22 C62 144.5(6) . . ? C72 C22 C12 110.6(4) . . ? C82 C22 C12 112.0(4) . . ? C42 C22 C12 109.3(4) . . ? C52 C22 C12 111.5(4) . . ? C32 C22 C12 108.6(5) . . ? C62 C22 C12 106.2(4) . . ? C22 C32 H32A 109.5 . . ? C22 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C22 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C22 C42 H42A 109.5 . . ? C22 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C22 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C22 C52 H52A 109.5 . . ? C22 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C22 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C22 C62 H62A 109.5 . . ? C22 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C22 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C22 C72 H72A 109.5 . . ? C22 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C22 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C22 C82 H82A 109.5 . . ? C22 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C22 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? O23 C13 O13 124.9(3) . . ? O23 C13 C23 118.1(2) . . ? O13 C13 C23 116.9(2) . . ? C13 O13 Mn1 127.17(18) . . ? C13 O23 Dy1 136.41(17) . 3 ? C63 C23 C33 130.6(6) . . ? C63 C23 C83 114.0(8) . . ? C33 C23 C83 55.3(6) . . ? C63 C23 C53 39.0(7) . . ? C33 C23 C53 113.3(5) . . ? C83 C23 C53 139.6(5) . . ? C63 C23 C13 115.2(6) . . ? C33 C23 C13 113.3(3) . . ? C83 C23 C13 109.3(5) . . ? C53 C23 C13 110.3(3) . . ? C63 C23 C73 110.0(7) . . ? C33 C23 C73 49.2(6) . . ? C83 C23 C73 104.4(7) . . ? C53 C23 C73 74.0(6) . . ? C13 C23 C73 102.9(5) . . ? C63 C23 C43 65.7(8) . . ? C33 C23 C43 108.8(5) . . ? C83 C23 C43 56.6(6) . . ? C53 C23 C43 104.3(4) . . ? C13 C23 C43 106.1(3) . . ? C73 C23 C43 149.5(6) . . ? C23 C33 H33A 109.5 . . ? C23 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C23 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C23 C43 H43A 109.5 . . ? C23 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C23 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C23 C53 H53A 109.5 . . ? C23 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C23 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C23 C63 H63A 109.5 . . ? C23 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C23 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C23 C73 H73A 109.5 . . ? C23 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C23 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C23 C83 H83A 109.5 . . ? C23 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C23 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? O44 N14 O34 26(2) . . ? O44 N14 O24 116.3(17) . . ? O34 N14 O24 122.9(8) . . ? O44 N14 O14 122(2) . . ? O34 N14 O14 119.7(7) . . ? O24 N14 O14 117.1(3) . . ? O44 N14 Dy1 155(2) . . ? O34 N14 Dy1 174.8(6) . . ? O24 N14 Dy1 62.11(15) . . ? O14 N14 Dy1 55.21(14) . . ? N14 O14 Dy1 99.39(17) . . ? N14 O24 Dy1 92.54(18) . . ? O35 N15 O25 121.6(3) . . ? O35 N15 O15 122.5(3) . . ? O25 N15 O15 115.9(2) . . ? O35 N15 Dy1 170.2(2) . . ? O25 N15 Dy1 58.60(13) . . ? O15 N15 Dy1 58.34(13) . . ? N15 O15 Dy1 95.59(16) . . ? N15 O25 Dy1 95.41(16) . . ? C26 N16 C36 112.6(4) . . ? C26 N16 C16 108.8(3) . . ? C36 N16 C16 107.5(3) . . ? C26 N16 C46 109.9(4) . . ? C36 N16 C46 109.0(3) . . ? C16 N16 C46 108.9(3) . . ? N16 C16 H16A 109.5 . . ? N16 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N16 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N16 C26 H26A 109.5 . . ? N16 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N16 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N16 C36 H36A 109.5 . . ? N16 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N16 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N16 C46 H46A 109.5 . . ? N16 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N16 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N17 C27 C37 178.3(5) . . ? C27 C37 H37A 109.5 . . ? C27 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C27 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.519 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.327 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.114