#------------------------------------------------------------------------------ #$Date: 2025-02-12 01:09:41 +0200 (Wed, 12 Feb 2025) $ #$Revision: 297686 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573890.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_1573890 loop_ _publ_author_name 'Yan, Han' 'Calado, Claudia M. S.' 'Wang, Hao' 'Murugesu, Muralee' 'Sun, Wen-Bin' _publ_section_title ; A novel Ln3+/Al3+ metallacrown multifunctional material for latent fingerprint detection, luminescent thermometers and luminescent sensors ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC08549C _journal_year 2025 _chemical_formula_moiety '2(C56 H46 Al4 Dy N4 Na O29), 8(C3 H7 N O), 0.25(H8 O4)' _chemical_formula_sum 'C136 H150 Al8 Dy2 N16 Na2 O67' _chemical_formula_weight 3667.53 _space_group_crystal_system tetragonal _space_group_IT_number 104 _space_group_name_Hall 'P 4 -2n' _space_group_name_H-M_alt 'P 4 n c' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2024-01-09 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-08-13 deposited with the CCDC. 2025-01-30 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 1 _cell_length_a 17.1664(7) _cell_length_b 17.1664(7) _cell_length_c 15.3325(17) _cell_measurement_reflns_used 5494 _cell_measurement_temperature 293 _cell_measurement_theta_max 26.6450 _cell_measurement_theta_min 3.7250 _cell_volume 4518.3(6) _computing_cell_refinement 'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 293 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1954 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -46.00 47.00 1.00 8.18 -- 17.07 -82.00 71.00 93 2 \w -21.00 21.00 1.00 8.18 -- -16.76 -99.00 -60.00 42 3 \w 62.00 89.00 1.00 8.18 -- 17.07 178.00 90.00 27 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0138992000 _diffrn_orient_matrix_UB_12 -0.0306576000 _diffrn_orient_matrix_UB_13 -0.0268359000 _diffrn_orient_matrix_UB_21 -0.0148094000 _diffrn_orient_matrix_UB_22 -0.0277215000 _diffrn_orient_matrix_UB_23 0.0299871000 _diffrn_orient_matrix_UB_31 -0.0360321000 _diffrn_orient_matrix_UB_32 -0.0004224000 _diffrn_orient_matrix_UB_33 -0.0227057000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_unetI/netI 0.0381 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 13411 _diffrn_reflns_point_group_measured_fraction_full 0.975 _diffrn_reflns_point_group_measured_fraction_max 0.971 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.977 _diffrn_reflns_theta_min 3.563 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.952 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_correction_T_min 0.910 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.348 _exptl_crystal_description block _exptl_crystal_F_000 1872 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.008 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.109 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack -0.06(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 243 _refine_ls_number_reflns 4327 _refine_ls_number_restraints 251 _refine_ls_restrained_S_all 1.196 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0526 _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^)+(0.0807P)^2^+7.1477P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1416 _refine_ls_wR_factor_ref 0.1531 _reflns_Friedel_coverage 0.874 _reflns_Friedel_fraction_full 0.954 _reflns_Friedel_fraction_max 0.944 _reflns_number_gt 3335 _reflns_number_total 4327 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc08549c2.cif _cod_data_source_block 754_auto _cod_database_code 1573890 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.911 _shelx_estimated_absorpt_t_min 0.911 _olex2_refinement_description ; 1. Twinned data refinement Scales: 1.06(3) -0.06(3) 2. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups, All O(H,H) groups 3. Restrained distances C7-O7 1.22 with sigma of 0.02 C7-N2 1.36 with sigma of 0.02 N2-C15 1.45 with sigma of 0.02 N2-C2 1.46 with sigma of 0.02 O9-O2_$1 2.5 with sigma of 0.02 C7-C15 2.46 with sigma of 0.04 C7-C2 2.45 with sigma of 0.04 N2-C15 \\sim N2-C2 with sigma of 0.02 4. Restrained planarity C7, O7, N2, C15, C2 with sigma of 0.1 5. Uiso/Uaniso restraints and constraints C15 \\sim C2 \\sim C7 \\sim O7 \\sim N2 \\sim C5 \\sim O8 \\sim C4 \\sim C17 \\sim C9 \\sim C11 \\sim C3 \\sim C13 \\sim O5 \\sim N1 \\sim O6: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A C2 \\sim C7 \\sim O7 \\sim N2 \\sim C15: within 3A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3A Uanis(C17) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C2) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06 6. Rigid body (RIGU) restrains C5, C17, C13, C11, C9, C3 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002 C7, O7, N2, C15, C2 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 7. Others Fixed Sof: H2B(0.25) H2A(0.25) O9(0.125) H9A(0.125) H9B(0.125) 8.a Riding coordinates: C15(H15C,H15A,H15B), C2(H2C,H2D,H2E), O2(H2B,H2A), O9(H9A,H9B) 8.b Secondary CH2 refined with riding coordinates: O3(H3A,H3B) 8.c Aromatic/amide H refined with riding coordinates: C6(H6), C10(H10A), C12(H12), C16(H16), C17(H17), C9(H9), C5(H5), C13(H13), C7(H7) 8.d Fitted hexagon refined as free rotating group: C6(C8,C10,C12,C14,C16), C17(C9,C5,C11,C3,C13) 8.e Idealised tetrahedral OH refined as rotating group: O10(H10) ; _shelx_res_file ; TITL 754_auto_a.res in P4nc 754_auto.res created by SHELXL-2018/3 at 10:06:06 on 09-Jan-2024 REM Old TITL 754_auto_e.res in P4/mnc REM SHELXT solution in P4nc: R1 0.136, Rweak 0.002, Alpha 0.021 REM 0.612 for 274 systematic absences, Orientation as input REM Flack x = -0.245 ( 0.021 ) from 1453 Parsons' quotients REM Formula found by SHELXT: C41 O20 N16 Al29 I CELL 0.71073 17.1664 17.1664 15.3325 90 90 90 ZERR 1 0.0007 0.0007 0.0017 0 0 0 LATT -1 SYMM -X,-Y,+Z SYMM -Y,+X,+Z SYMM +Y,-X,+Z SYMM 0.5+X,0.5-Y,0.5+Z SYMM 0.5-X,0.5+Y,0.5+Z SYMM 0.5-Y,0.5-X,0.5+Z SYMM 0.5+Y,0.5+X,0.5+Z SFAC C H Al Dy N Na O UNIT 136 150 8 2 16 2 67 EQIV $1 +X,+Y,-1+Z RIGU 0.0001 0.0002 C5 C17 C13 C11 C9 C3 ISOR 0.01 0.02 C17 C9 C5 C11 C13 DFIX 1.22 C7 O7 DFIX 1.36 C7 N2 DANG 2.46 C7 C15 DANG 2.45 C7 C2 DFIX 1.45 N2 C15 DFIX 1.46 N2 C2 SADI N2 C15 N2 C2 FLAT C7 O7 N2 C15 C2 RIGU C7 O7 N2 C15 C2 DFIX 2.5 O9 O2_$1 SIMU 0.005 0.01 2 C15 C2 C7 O7 N2 C5 O8 C4 C17 C9 C11 C3 C13 O5 N1 O6 SIMU 0.01 0.02 3 C2 C7 O7 N2 C15 ISOR 0.03 0.06 C2 C7 O7 N2 C15 L.S. 20 PLAN 99 SIZE 0.1 0.1 0.1 TEMP 19.85 CONF list 4 MORE -1 BOND $H fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 0 52 OMIT 0 4 0 OMIT 3 3 0 REM REM REM WGHT 0.080700 7.147700 BASF -0.05954 FVAR 0.27038 DY1 4 0.500000 0.500000 0.517201 10.25000 0.01980 0.01980 = 0.05935 0.00000 0.00000 0.00000 AL1 3 0.319575 0.447645 0.638787 11.00000 0.02644 0.02816 = 0.09337 0.01191 0.00520 -0.00170 O1 7 0.288258 0.434112 0.522626 11.00000 0.03201 0.04458 = 0.09293 0.00836 -0.00949 -0.00490 NA1 6 0.500000 0.500000 0.741148 10.25000 0.07021 0.07021 = 0.05873 0.00000 0.00000 0.00000 O4 7 0.382395 0.492016 0.444426 11.00000 0.03408 0.04591 = 0.07473 0.00608 -0.01625 -0.00755 O6 7 0.424961 0.426027 0.616432 11.00000 0.02289 0.02089 = 0.06414 0.00388 0.00275 0.00332 O8 7 0.314346 0.341462 0.661706 11.00000 0.03265 0.03653 = 0.11508 0.02396 0.00818 -0.00714 C1 1 0.317931 0.452715 0.453443 11.00000 0.03178 0.03078 = 0.09842 0.00849 -0.01744 0.00518 O10 7 0.166217 0.363381 0.146245 11.00000 0.11305 0.05142 = 0.13091 0.00138 -0.04911 -0.02275 AFIX 147 H10 2 0.124589 0.342580 0.158317 11.00000 -1.50000 AFIX 0 N1 5 0.443204 0.345209 0.632110 11.00000 0.02222 0.03240 = 0.07850 0.00488 -0.00026 -0.00173 C4 1 0.381304 0.308491 0.655368 11.00000 0.03476 0.03744 = 0.10901 0.01963 0.00254 -0.00320 AFIX 66 C6 1 0.274891 0.419190 0.213942 11.00000 0.09190 0.05866 = 0.08591 -0.01247 -0.02315 -0.01788 AFIX 43 H6 2 0.297283 0.429300 0.159882 11.00000 -1.20000 AFIX 65 C8 1 0.203434 0.381358 0.218830 11.00000 0.07943 0.03492 = 0.08183 -0.00002 -0.02709 -0.01229 C10 1 0.169966 0.366247 0.299629 11.00000 0.07202 0.05478 = 0.11712 0.00601 -0.03355 -0.02449 AFIX 43 H10A 2 0.122157 0.340935 0.302899 11.00000 -1.20000 AFIX 65 C12 1 0.207956 0.388967 0.375540 11.00000 0.05408 0.04784 = 0.09141 0.00207 -0.00947 -0.00960 AFIX 43 H12 2 0.185564 0.378857 0.429599 11.00000 -1.20000 AFIX 65 C14 1 0.279414 0.426799 0.370652 11.00000 0.04277 0.03709 = 0.09145 0.00369 -0.01852 -0.00680 C16 1 0.312882 0.441910 0.289854 11.00000 0.05609 0.04508 = 0.11076 0.01019 -0.02512 -0.01365 AFIX 43 H16 2 0.360692 0.467222 0.286584 11.00000 -1.20000 AFIX 66 C17 1 0.321626 0.104569 0.705034 11.00000 0.07302 0.05556 = 0.18766 0.03423 0.00629 -0.00692 AFIX 43 H17 2 0.275318 0.077552 0.713752 11.00000 -1.20000 AFIX 65 C9 1 0.392262 0.064999 0.706266 11.00000 0.07437 0.05582 = 0.19499 0.03582 0.00775 -0.00561 AFIX 43 H9 2 0.393214 0.011506 0.715809 11.00000 -1.20000 AFIX 65 C5 1 0.461475 0.105379 0.693235 11.00000 0.07263 0.05270 = 0.17929 0.03450 0.00619 -0.00338 AFIX 43 H5 2 0.508735 0.078903 0.694059 11.00000 -1.20000 AFIX 65 C11 1 0.460053 0.185329 0.678972 11.00000 0.06649 0.05196 = 0.14823 0.02942 -0.00146 -0.00444 C3 1 0.389418 0.224901 0.677740 11.00000 0.06546 0.05181 = 0.14170 0.02903 -0.00196 -0.00541 C13 1 0.320204 0.184522 0.690771 11.00000 0.06738 0.05526 = 0.16979 0.03144 0.00124 -0.00749 AFIX 43 H13 2 0.272944 0.210998 0.689946 11.00000 -1.20000 AFIX 0 O5 7 0.529695 0.221171 0.670361 11.00000 0.04705 0.02927 = 0.14025 0.02749 -0.01320 -0.00013 O3 7 0.539927 0.354978 0.770213 11.00000 0.07425 0.07211 = 0.09340 0.01579 -0.01837 -0.00176 AFIX 23 H3A 2 0.588420 0.351013 0.802382 11.00000 -1.50000 H3B 2 0.499383 0.326154 0.800219 11.00000 -1.50000 AFIX 0 C7 1 0.210814 0.156716 0.380455 11.00000 0.31110 0.29988 = 0.24901 0.00796 -0.09968 -0.07218 AFIX 43 H7 2 0.190426 0.205963 0.369591 11.00000 -1.20000 AFIX 0 O7 7 0.168814 0.100337 0.363543 11.00000 0.30077 0.28446 = 0.22224 0.01095 -0.10478 -0.07405 N2 5 0.286149 0.153165 0.414415 11.00000 0.31382 0.30438 = 0.25615 0.00861 -0.09789 -0.07197 C15 1 0.331823 0.223330 0.436692 11.00000 0.31511 0.30483 = 0.26127 -0.00775 -0.10465 -0.07541 AFIX 3 H15C 2 0.386983 0.218360 0.427932 11.00000 -1.50000 H15A 2 0.321763 0.237650 0.496152 11.00000 -1.50000 H15B 2 0.311673 0.262810 0.398522 11.00000 -1.50000 AFIX 0 C2 1 0.315442 0.071058 0.421986 11.00000 0.31952 0.30925 = 0.26551 0.00871 -0.08703 -0.06329 AFIX 3 H2C 2 0.303942 0.041278 0.370586 11.00000 -1.50000 H2D 2 0.287012 0.050198 0.470576 11.00000 -1.50000 H2E 2 0.370282 0.068438 0.433916 11.00000 -1.50000 AFIX 0 O2 7 0.500000 0.500000 0.893736 10.25000 0.16949 0.16949 = 0.06335 0.00000 0.00000 0.00000 PART -1 AFIX 3 H2B 2 0.539150 0.500000 0.927666 10.25000 -1.50000 H2A 2 0.460850 0.500000 0.927666 10.25000 -1.50000 AFIX 0 PART 0 O9 7 0.500000 0.500000 0.055668 10.12500 0.20263 0.20263 = 0.14816 0.00000 0.00000 0.00000 PART -1 AFIX 3 H9A 2 0.540430 0.500000 0.087638 10.12500 -1.50000 H9B 2 0.459570 0.500000 0.087638 10.12500 -1.50000 AFIX 0 HKLF 4 REM 754_auto_a.res in P4nc REM wR2 = 0.1531, GooF = S = 1.115, Restrained GooF = 1.196 for all data REM R1 = 0.0526 for 3335 Fo > 4sig(Fo) and 0.0749 for all 4327 data REM 243 parameters refined using 251 restraints END WGHT 0.0807 7.1546 REM Highest difference peak 1.008, deepest hole -0.701, 1-sigma level 0.109 Q1 1 0.5017 0.4737 0.4588 11.00000 0.05 0.73 Q2 1 0.5035 0.4773 0.5759 11.00000 0.05 0.65 Q3 1 0.2707 0.0026 0.3750 11.00000 0.05 0.61 Q4 1 0.4024 0.0827 0.7688 11.00000 0.05 0.58 Q5 1 0.3952 0.0548 0.6357 11.00000 0.05 0.56 Q6 1 0.5000 0.5000 0.0244 10.25000 0.05 0.53 Q7 1 0.2334 0.2346 0.5157 11.00000 0.05 0.53 Q8 1 0.4575 0.0947 0.6350 11.00000 0.05 0.52 Q9 1 0.3187 0.1329 0.7887 11.00000 0.05 0.48 Q10 1 0.2572 0.2138 0.4429 11.00000 0.05 0.46 Q11 1 0.4556 0.1146 0.7418 11.00000 0.05 0.45 Q12 1 0.3858 0.2186 0.6460 11.00000 0.05 0.45 Q13 1 0.2695 -0.0026 0.6605 11.00000 0.05 0.43 Q14 1 0.3213 0.1044 0.6376 11.00000 0.05 0.41 Q15 1 0.3621 -0.0044 0.5184 11.00000 0.05 0.41 Q16 1 0.1393 0.1793 0.3920 11.00000 0.05 0.40 Q17 1 0.3174 0.1771 0.6357 11.00000 0.05 0.39 Q18 1 0.3342 0.1845 0.7460 11.00000 0.05 0.39 Q19 1 0.3865 0.0398 0.8009 11.00000 0.05 0.38 Q20 1 0.3291 0.3990 0.1763 11.00000 0.05 0.36 Q21 1 0.3776 0.2225 0.3570 11.00000 0.05 0.36 Q22 1 0.3132 0.4350 0.5777 11.00000 0.05 0.35 Q23 1 0.3013 0.3871 0.3831 11.00000 0.05 0.35 Q24 1 0.3801 0.1921 0.7774 11.00000 0.05 0.35 Q25 1 0.3816 0.0238 0.4579 11.00000 0.05 0.35 Q26 1 0.3750 0.2389 0.3407 11.00000 0.05 0.34 Q27 1 0.4353 0.2860 0.5213 11.00000 0.05 0.32 Q28 1 0.4648 0.1847 0.7014 11.00000 0.05 0.32 Q29 1 0.5371 0.1963 0.6911 11.00000 0.05 0.31 Q30 1 0.1264 0.3210 0.2627 11.00000 0.05 0.31 Q31 1 0.1842 0.3567 0.2787 11.00000 0.05 0.31 Q32 1 0.5000 0.5000 0.3951 10.25000 0.05 0.31 Q33 1 0.4662 0.1792 0.6421 11.00000 0.05 0.30 Q34 1 0.1718 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164.91 11.75 -13 -5 -8 150.53 11.37 -5 -13 -7 9.70 4.91 -13 -5 -7 7.47 4.62 -5 -13 -6 500.18 20.27 -13 -5 -6 499.21 20.19 -5 -13 -5 47.06 6.67 -13 -5 -5 45.81 7.10 -5 -13 -4 437.90 18.57 -13 -5 -4 420.20 18.26 13 -5 -4 408.86 10.63 -13 -5 -3 -5.68 5.04 -5 -13 -3 -2.12 4.84 13 -5 -3 -0.72 2.18 -13 -5 -2 78.66 8.08 -5 -13 -2 75.55 7.86 13 -5 -2 74.04 5.04 -13 -5 -1 -3.10 5.06 13 -5 -1 4.53 2.83 -5 -13 -1 4.75 4.22 13 -5 0 324.68 11.93 -5 -13 0 323.15 15.98 -13 -5 0 338.39 15.89 -13 -5 1 -3.21 5.01 -5 -13 1 -2.19 5.15 13 -5 1 5.71 3.23 13 -5 2 103.50 7.65 -13 -5 2 103.28 9.09 -5 -13 2 98.75 9.04 -13 -5 3 3.43 4.19 -5 -13 3 -3.68 4.62 13 -5 3 -5.03 4.07 -5 -13 4 416.19 17.88 13 -5 4 394.91 15.81 -13 -5 4 408.51 17.73 -13 -5 5 45.45 6.99 -5 -13 5 48.00 7.11 13 -5 5 27.53 5.08 -5 -13 6 535.67 20.88 13 -5 6 527.08 19.92 -13 -5 6 508.93 20.04 -13 -5 7 2.04 4.56 13 -5 7 2.86 4.82 -5 -13 7 0.71 4.39 -5 -13 8 169.76 11.83 13 -5 8 157.35 12.17 -13 -5 8 166.01 11.53 -5 -13 9 -0.72 4.61 -13 -5 9 0.41 4.12 13 -5 9 2.36 5.00 -5 -13 10 57.85 7.52 13 5 10 53.44 8.54 13 -5 10 52.93 8.19 -13 -5 10 64.33 7.72 -5 -13 11 3.57 3.94 13 5 11 10.87 6.77 13 -5 11 12.86 6.68 -13 -5 11 2.00 4.06 -5 -13 12 62.06 7.91 -13 -5 12 68.24 8.09 13 -5 12 53.07 10.00 13 5 12 56.26 9.67 13 -5 13 5.63 6.30 5 13 13 6.09 5.12 13 5 13 8.58 7.12 13 -5 14 34.30 9.52 13 5 14 18.05 7.99 5 13 14 17.01 6.12 5 13 15 2.94 6.05 -6 -13 -14 -3.00 6.41 -6 -13 -13 48.17 9.42 -13 -6 -12 0.78 3.97 -6 -13 -12 3.98 4.67 -6 -13 -12 2.89 5.39 -13 -6 -11 54.01 7.58 -6 -13 -11 52.95 7.65 -13 -6 -10 13.33 5.09 -6 -13 -10 4.93 4.24 -13 -6 -9 107.29 10.14 -6 -13 -9 100.22 9.56 -13 -6 -8 -3.56 5.26 -6 -13 -8 -2.44 4.57 -6 -13 -7 122.79 10.79 -13 -6 -7 117.43 10.34 -13 -6 -6 11.68 5.58 -6 -13 -6 14.13 5.50 -13 -6 -5 650.02 23.40 -6 -13 -5 632.29 23.41 -13 -6 -4 12.81 4.79 -6 -13 -4 19.23 5.72 13 -6 -4 13.30 1.90 -13 -6 -3 275.40 14.74 13 -6 -3 262.54 7.97 -6 -13 -3 276.44 14.89 -13 -6 -2 -0.15 4.76 -6 -13 -2 10.59 4.55 13 -6 -2 4.90 2.41 -13 -6 -1 91.62 8.38 13 -6 -1 82.24 5.21 -6 -13 -1 79.66 8.14 -6 13 0 27.09 4.07 -13 -6 0 13.75 3.81 13 -6 0 19.36 3.16 -6 -13 0 20.01 4.93 13 -6 1 88.26 6.30 -13 -6 1 103.03 9.02 -6 -13 1 112.27 9.69 -6 -13 2 14.07 4.65 -6 -13 2 8.41 2.03 13 -6 2 -0.73 4.10 -13 -6 2 5.20 4.27 -13 -6 3 246.06 13.80 13 -6 3 255.75 11.83 -6 -13 3 255.13 7.37 -6 -13 3 267.54 14.47 -13 -6 4 11.89 4.96 -6 -13 4 16.03 5.69 13 -6 4 11.39 4.13 13 -6 5 625.70 21.07 -6 -13 5 635.42 23.05 -13 -6 5 633.76 22.86 -6 -13 6 11.36 4.94 -13 -6 6 7.94 4.39 13 -6 6 14.90 5.74 -6 -13 7 152.34 11.37 13 -6 7 135.05 10.64 -13 -6 7 143.06 10.98 -6 -13 8 2.05 4.28 -13 -6 8 6.23 4.15 13 -6 8 -3.83 5.23 -13 -6 9 101.68 9.47 13 -6 9 105.28 10.88 -6 -13 9 100.25 9.60 -13 -6 10 10.93 4.54 -6 -13 10 5.08 4.47 13 -6 10 7.11 5.36 -13 -6 11 50.98 7.37 -6 -13 11 58.98 7.83 13 6 11 30.38 7.84 13 -6 11 58.83 9.40 -6 -13 12 -0.68 4.12 -13 -6 12 1.52 4.24 13 -6 12 8.26 6.72 13 6 12 1.40 5.72 13 -6 13 58.71 10.53 13 6 13 41.14 8.99 6 13 13 30.31 7.35 13 6 14 0.34 6.34 6 13 14 6.22 6.14 13 -6 14 15.85 8.19 6 13 15 17.01 7.00 -7 -13 -14 29.40 8.37 -7 -13 -13 -5.53 6.19 -7 -13 -12 36.15 8.29 -7 -13 -12 21.33 5.81 -13 -7 -11 1.80 4.32 -7 -13 -11 -0.20 4.92 -7 -13 -11 -3.35 6.16 -7 -13 -10 84.73 9.15 -13 -7 -10 74.32 9.06 -7 -13 -10 77.20 9.91 -7 -13 -9 4.47 4.61 -7 -13 -9 9.60 4.71 -13 -7 -9 2.35 4.44 -13 -7 -8 101.69 9.86 -7 -13 -8 91.71 9.57 -13 -7 -7 3.49 4.61 -7 -13 -7 4.26 4.29 -13 -7 -6 94.37 9.12 -7 -13 -6 101.21 9.71 -7 -13 -5 23.21 6.30 -13 -7 -5 25.69 6.09 -7 -13 -4 506.79 20.83 -13 -7 -4 479.47 20.23 -7 -13 -3 0.53 4.59 -13 -7 -3 3.81 4.31 -13 -7 -2 348.18 17.13 13 -7 -2 343.13 9.60 -7 -13 -2 350.06 17.25 -7 -13 -1 27.75 6.28 13 -7 -1 26.73 3.73 -7 -13 -1 25.94 4.05 -13 -7 -1 21.26 5.41 -7 -13 0 10.16 4.43 13 -7 0 11.99 3.20 -7 -13 0 5.76 2.37 -13 -7 0 4.14 4.28 -7 -13 1 28.22 5.98 -13 -7 1 26.50 5.91 -7 -13 1 27.41 3.58 13 -7 1 28.90 4.55 -13 -7 2 306.62 15.97 13 -7 2 323.52 12.59 -7 -13 2 319.91 16.47 -7 -13 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4.95 -8 -13 -8 -1.01 4.21 -13 -8 -8 0.74 4.63 -13 -8 -7 168.02 12.41 -8 -13 -7 158.01 11.89 -8 -13 -7 166.90 12.58 -8 -13 -6 -2.64 4.88 -8 -13 -6 5.53 4.55 -13 -8 -6 4.95 4.59 -13 -8 -5 139.70 11.37 -8 -13 -5 140.17 10.09 -8 -13 -5 133.26 10.94 -8 -13 -4 -3.14 5.28 -8 -13 -4 -5.64 4.00 -13 -8 -4 -3.15 5.09 -13 -8 -3 269.88 15.51 -8 -13 -3 308.70 13.39 -8 -13 -3 274.86 15.68 -8 -13 -2 7.93 4.81 -8 -13 -2 7.71 3.36 -13 -8 -2 11.48 4.93 -13 -8 -1 263.55 15.17 -8 -13 -1 232.93 10.57 -8 -13 -1 245.44 14.81 13 -8 0 10.43 3.57 -8 -13 0 0.47 4.11 -8 -13 0 4.24 2.51 -13 -8 0 0.14 4.35 -8 -13 1 209.66 8.62 -13 -8 1 212.36 13.78 13 -8 1 201.78 9.58 -8 -13 1 204.87 13.33 -8 -13 2 10.85 4.53 -13 -8 2 12.64 5.28 13 -8 2 15.27 4.38 -13 -8 3 308.18 16.29 13 -8 3 280.75 12.58 -8 -13 3 290.19 15.74 -8 -13 4 -6.99 5.45 -13 -8 4 -2.61 5.17 13 -8 4 2.82 4.17 -13 -8 5 138.57 11.01 13 -8 5 123.56 9.47 -8 -13 5 132.52 10.77 -8 -13 6 1.01 4.44 -13 -8 6 1.86 4.39 13 -8 6 8.81 4.67 -13 -8 7 164.04 12.00 13 -8 7 172.67 11.99 -8 -13 7 150.85 12.13 -8 -13 8 1.41 4.57 -13 -8 8 1.98 4.64 13 -8 8 2.80 5.10 13 -8 9 103.23 10.48 -13 -8 9 69.96 8.71 -8 -13 9 95.06 9.95 13 -8 10 9.61 6.26 -13 -8 10 0.44 4.72 -8 -13 10 0.70 4.34 13 -8 11 30.07 7.68 -13 -8 11 24.94 5.73 -8 -13 11 26.07 6.32 13 -8 12 7.53 6.58 -13 -8 12 -0.44 4.44 -8 -13 12 -7.23 5.78 8 13 13 13.27 6.46 13 8 13 18.12 7.27 8 13 14 -1.80 6.39 8 13 15 9.87 7.21 -13 -9 -13 1.74 5.72 -9 -13 -13 2.00 6.18 -13 -9 -12 17.91 6.47 -9 -13 -12 19.00 7.32 -13 -9 -11 -10.91 5.88 -9 -13 -11 -3.26 5.25 -13 -9 -11 -13.24 6.97 -9 -13 -11 -2.64 5.35 -13 -9 -10 46.14 7.84 -9 -13 -10 50.72 7.98 -9 -13 -10 44.42 8.37 -9 -13 -9 1.30 4.52 -13 -9 -9 1.61 4.82 -9 -13 -9 -2.17 5.56 -13 -9 -8 124.14 11.19 -9 -13 -8 112.52 10.85 -9 -13 -8 124.18 11.29 -9 -13 -7 8.40 5.02 -13 -9 -7 4.69 5.08 -9 -13 -7 -6.11 4.97 -13 -9 -6 186.91 13.42 -9 -13 -6 192.97 12.45 -9 -13 -6 186.06 13.50 -9 -13 -5 17.53 4.63 -13 -9 -5 14.19 5.72 -9 -13 -5 14.71 5.37 -13 -9 -4 188.75 13.52 -9 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84.25 10.92 -13 -12 -9 97.45 11.18 -12 -13 -8 -1.39 5.66 -13 -12 -8 4.28 5.28 -12 -13 -8 2.10 4.66 -13 -12 -8 1.07 5.19 -13 -12 -7 113.70 10.83 -12 -13 -7 97.11 10.03 -13 -12 -7 106.93 11.03 -12 -13 -7 125.68 12.19 -12 -13 -6 5.75 5.13 -12 -13 -6 -2.54 4.56 -13 -12 -6 5.25 5.47 -12 -13 -5 76.65 7.90 -12 -13 -5 88.21 10.21 -13 -12 -5 84.85 10.39 -12 -13 -4 3.05 3.66 -12 -13 -4 4.00 4.84 -13 -12 -4 -4.03 5.61 -12 -13 -3 84.05 10.12 -13 -12 -3 92.00 10.31 -12 -13 -2 -3.50 5.43 -13 -12 -2 2.08 4.95 -13 -12 -1 173.39 13.79 -12 -13 -1 167.50 13.64 -12 -13 0 0.45 4.68 -13 -12 0 -5.89 5.68 -13 -12 1 179.85 14.06 -12 -13 1 181.48 14.00 -12 -13 2 -0.73 5.25 -13 -12 2 3.43 5.38 -12 -13 3 130.25 11.87 -13 -12 3 122.91 11.48 -12 -13 4 3.50 4.75 -13 -12 4 11.05 5.21 -12 -13 5 78.90 9.44 -13 -12 5 94.75 10.16 -12 -13 6 -2.94 5.12 -13 -12 6 -2.51 5.33 -12 -13 7 83.70 10.06 -13 -12 7 91.90 10.54 -12 -13 8 -5.62 5.65 -13 -12 8 -1.06 4.82 -12 -13 9 109.10 11.58 -13 -12 9 99.85 11.49 -13 -12 10 0.15 5.49 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73.59 10.00 -6 -14 11 1.80 4.23 -14 -6 11 -8.21 5.31 14 6 11 -4.85 6.14 14 -6 11 11.59 7.03 -6 -14 12 28.48 6.52 -14 -6 12 26.76 5.70 14 -6 12 23.58 7.86 14 6 12 16.04 6.68 14 -6 13 1.18 6.59 6 14 13 -2.74 6.78 14 6 13 -3.49 6.61 6 14 14 18.32 7.35 -7 -14 -13 21.41 6.75 -7 -14 -12 -12.69 7.54 -14 -7 -11 30.40 6.70 -7 -14 -11 23.23 6.22 -7 -14 -11 14.59 5.55 -14 -7 -10 -4.35 5.38 -7 -14 -10 -0.26 4.88 -7 -14 -10 -6.32 6.46 -14 -7 -9 84.72 9.72 -7 -14 -9 91.09 9.72 -7 -14 -9 68.62 9.17 -14 -7 -8 0.51 4.84 -7 -14 -8 -11.16 5.74 -14 -7 -7 74.16 8.87 -7 -14 -7 68.37 8.67 -14 -7 -6 11.54 5.29 -7 -14 -6 12.79 5.35 -14 -7 -5 187.87 12.97 -7 -14 -5 174.29 12.97 -7 -14 -4 -4.98 5.39 -14 -7 -4 -3.89 5.06 -14 -7 -3 220.61 13.77 -7 -14 -3 215.89 14.29 -14 -7 -2 6.08 4.34 14 -7 -2 10.31 2.62 -7 -14 -2 7.03 4.82 -14 -7 -1 82.49 8.51 -7 -14 -1 81.91 6.39 14 -7 -1 87.33 5.56 -7 -14 -1 84.72 8.86 -7 -14 0 -5.54 5.06 -14 -7 0 -3.56 4.59 -7 -14 0 -2.43 2.89 14 -7 0 -1.07 2.62 -14 -7 1 86.13 8.94 -7 -14 1 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4.68 -8 -14 -9 -3.19 5.11 -8 -14 -9 -5.25 6.28 -14 -8 -8 84.83 9.53 -8 -14 -8 77.90 9.53 -8 -14 -8 84.05 9.47 -14 -8 -7 -5.91 5.17 -8 -14 -7 -1.48 4.66 -8 -14 -7 -4.59 5.62 -14 -8 -6 176.78 13.29 -8 -14 -6 176.92 11.97 -8 -14 -6 182.10 13.61 -8 -14 -5 -1.33 5.04 -8 -14 -5 -3.77 4.44 -14 -8 -5 9.21 4.87 -14 -8 -4 144.53 11.96 -8 -14 -4 134.91 9.61 -8 -14 -4 139.81 11.55 -8 -14 -3 5.32 4.72 -8 -14 -3 10.15 3.18 -14 -8 -3 10.07 4.59 -14 -8 -2 128.52 11.00 -8 -14 -2 133.15 8.62 -8 -14 -2 124.04 11.07 -8 -14 -1 16.14 5.33 -8 -14 -1 11.54 3.03 -14 -8 -1 14.30 5.97 -8 -14 0 352.09 12.67 -14 -8 0 364.01 18.09 -8 -14 0 359.15 18.27 14 -8 0 333.71 11.92 -8 -14 1 14.18 5.29 14 -8 1 13.13 3.87 -8 -14 1 11.04 2.74 -14 -8 1 8.95 4.82 -14 -8 2 135.70 11.44 14 -8 2 135.06 8.63 -8 -14 2 140.61 11.46 -14 -8 3 10.83 5.11 -8 -14 3 4.43 4.38 14 -8 3 9.25 3.68 -14 -8 4 102.74 10.33 14 -8 4 110.49 8.70 -8 -14 4 116.37 10.53 -14 -8 5 3.71 4.48 -8 -14 5 2.20 4.56 14 -8 5 16.17 4.85 -14 -8 6 206.39 13.94 14 -8 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308.28 14.33 -15 -4 4 20.00 5.89 15 -4 4 15.54 4.95 -4 -15 4 21.34 6.18 -4 -15 5 259.56 15.68 15 -4 5 249.09 13.81 -15 -4 5 243.30 14.73 -4 -15 6 148.40 12.21 15 -4 6 125.31 10.60 -15 -4 6 121.26 10.48 -4 -15 7 167.78 12.67 -15 -4 7 170.40 12.42 15 -4 7 147.62 11.94 15 -4 8 -0.78 5.77 -15 -4 8 4.12 4.92 -4 -15 8 2.07 4.48 15 -4 9 84.66 10.02 -15 -4 9 83.60 9.30 -4 -15 9 74.30 9.44 15 -4 10 6.08 5.95 -4 -15 10 11.68 5.23 15 4 10 -2.09 6.71 -4 -15 11 52.58 7.92 15 -4 11 48.30 9.03 15 4 11 39.73 8.73 4 -15 11 55.62 8.07 -4 -15 12 6.13 5.45 15 4 12 17.02 7.65 15 -4 12 11.39 7.15 4 -15 12 6.18 5.04 15 4 13 39.95 9.98 15 -4 13 43.69 10.02 -15 -5 -11 12.49 5.65 -5 -15 -11 9.71 5.34 -15 -5 -10 71.80 8.95 -5 -15 -10 51.86 7.78 -15 -5 -9 5.42 4.97 -5 -15 -9 7.56 4.93 -15 -5 -8 140.29 11.84 -5 -15 -8 147.06 12.20 -15 -5 -7 18.58 5.97 -5 -15 -7 18.57 6.65 -15 -5 -6 235.21 14.75 -5 -15 -6 231.59 14.95 -15 -5 -5 49.34 7.47 -5 -15 -5 51.63 8.27 -5 -15 -4 217.78 14.22 -15 -5 -4 206.96 13.76 -15 -5 -3 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38.31 7.38 15 -5 12 55.93 10.28 15 -5 13 14.32 8.37 5 15 13 2.72 5.34 -6 -15 -13 33.24 8.46 -15 -6 -11 41.57 7.44 -6 -15 -11 36.50 7.64 -15 -6 -10 -2.39 4.66 -6 -15 -10 -1.48 5.25 -15 -6 -9 100.73 10.30 -6 -15 -9 84.42 9.79 -6 -15 -8 4.36 4.76 -15 -6 -8 3.54 5.02 -6 -15 -7 89.84 10.06 -15 -6 -7 101.21 10.29 -15 -6 -6 -1.04 5.43 -6 -15 -6 -4.07 5.11 -6 -15 -5 213.70 14.52 -15 -6 -5 201.98 13.85 -15 -6 -4 5.74 4.58 -6 -15 -4 11.39 5.65 -6 -15 -3 136.02 11.47 -15 -6 -3 142.39 11.66 -6 -15 -2 -3.98 5.30 -15 -6 -2 -0.20 4.75 15 -6 -2 -2.60 2.70 -15 -6 -1 187.63 13.19 15 -6 -1 173.22 8.67 -6 -15 -1 190.10 13.45 -6 -15 0 -0.51 4.28 -15 -6 0 -0.61 4.58 15 -6 0 -1.54 3.51 -15 -6 1 184.53 13.02 15 -6 1 184.77 9.76 -6 -15 1 183.15 13.24 -6 -15 2 -2.91 4.53 -15 -6 2 -5.22 4.51 15 -6 2 -1.57 4.06 -15 -6 3 143.13 11.61 15 -6 3 134.24 9.33 -6 -15 3 136.04 11.56 -6 -15 4 7.15 4.95 -15 -6 4 2.33 5.08 15 -6 4 9.50 4.15 15 -6 5 211.16 12.66 -6 -15 5 210.52 14.23 -15 -6 5 200.33 13.87 15 -6 6 -1.66 5.15 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17.20 6.26 -8 -15 -10 -9.08 5.88 -15 -8 -10 -8.32 6.24 -8 -15 -10 -10.30 6.84 -8 -15 -9 40.71 7.17 -15 -8 -9 39.35 7.42 -8 -15 -9 45.86 7.99 -8 -15 -8 -15.58 6.87 -8 -15 -8 -7.44 5.36 -15 -8 -8 -13.70 6.83 -8 -15 -7 101.32 10.73 -15 -8 -7 117.56 11.36 -8 -15 -7 99.70 9.96 -15 -8 -6 5.80 5.11 -8 -15 -6 0.80 4.63 -8 -15 -6 2.47 5.30 -15 -8 -5 134.39 12.00 -8 -15 -5 158.09 11.21 -8 -15 -5 156.54 12.78 -15 -8 -4 8.96 5.70 -8 -15 -4 1.70 3.41 -8 -15 -4 4.30 4.97 -15 -8 -3 149.19 12.44 -8 -15 -3 140.22 9.56 -8 -15 -3 149.61 12.56 -15 -8 -2 9.88 5.49 -8 -15 -2 4.81 3.22 -8 -15 -2 6.08 5.20 -15 -8 -1 190.97 13.67 -8 -15 -1 188.77 9.87 -8 -15 -1 210.79 14.64 -8 -15 0 -1.69 2.74 -8 -15 0 -5.94 5.75 -15 -8 0 -5.50 5.44 -8 -15 1 220.06 14.82 -15 -8 1 203.52 14.01 15 -8 1 197.80 9.90 15 -8 2 10.18 3.67 -8 -15 2 1.85 4.71 -15 -8 2 0.21 4.51 -8 -15 3 116.06 11.10 -15 -8 3 127.56 11.36 15 -8 3 119.92 8.85 15 -8 4 6.25 3.84 -8 -15 4 5.14 5.38 -15 -8 4 4.04 4.78 -15 -8 5 123.93 11.37 15 -8 5 127.57 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1.83 3.07 -15 -9 -3 5.60 5.04 -15 -9 -2 168.39 13.38 -9 -15 -2 162.64 13.35 -9 -15 -2 162.55 9.99 -9 -15 -1 21.49 6.11 -9 -15 -1 27.09 4.51 -15 -9 -1 14.84 5.41 -9 -15 0 294.35 17.18 -15 -9 0 297.02 17.44 -15 -9 1 19.73 5.58 -9 -15 1 33.08 6.85 -9 -15 2 169.17 13.38 -15 -9 2 178.39 13.55 15 -9 2 161.18 9.56 -9 -15 3 1.17 4.90 -15 -9 3 2.78 5.09 15 -9 3 7.42 4.23 -9 -15 4 117.09 11.28 -15 -9 4 118.27 11.19 15 -9 4 127.14 9.69 -9 -15 5 9.56 5.03 -15 -9 5 9.83 5.60 15 -9 5 21.74 6.17 -9 -15 6 142.97 12.81 -15 -9 6 159.72 12.84 15 -9 6 146.05 11.32 -9 -15 7 9.01 5.36 15 -9 7 9.30 5.35 -15 -9 7 0.79 4.89 -9 -15 8 102.02 11.04 -15 -9 8 102.44 11.07 15 -9 8 101.87 10.75 -15 -9 9 -6.24 5.97 15 -9 9 0.92 5.15 -9 -15 9 -8.40 5.99 -15 -9 10 19.68 5.95 -9 -15 10 21.77 6.07 -9 -15 11 2.47 5.15 -15 -9 11 1.54 4.72 -10 -15 -11 47.93 9.17 -10 -15 -11 36.57 7.60 -15 -10 -11 40.48 8.61 -10 -15 -10 0.61 5.07 -10 -15 -10 8.92 6.19 -15 -10 -10 9.63 5.47 -10 -15 -9 54.18 9.02 -10 -15 -9 70.84 9.47 -15 -10 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8.06 -15 -11 6 58.64 8.72 -11 -15 7 -0.73 5.88 -15 -11 7 -0.34 5.56 -11 -15 8 57.91 9.00 -15 -11 8 61.80 9.05 -11 -15 9 -3.06 5.79 -15 -11 9 7.74 5.77 -15 -11 10 29.20 7.39 -11 -15 10 37.41 8.01 -15 -11 11 1.40 5.98 -11 -15 11 1.28 5.11 -12 -15 -11 22.10 7.63 -15 -12 -11 41.55 8.72 -15 -12 -10 -0.31 5.62 -12 -15 -10 -0.62 6.29 -12 -15 -10 -1.59 5.36 -15 -12 -9 75.95 10.81 -12 -15 -9 63.22 10.39 -12 -15 -9 65.65 9.53 -15 -12 -8 -1.62 5.60 -12 -15 -8 13.07 6.38 -12 -15 -8 0.93 4.66 -12 -15 -7 59.83 9.29 -15 -12 -7 71.57 10.46 -12 -15 -7 71.95 8.97 -12 -15 -6 20.93 6.86 -15 -12 -6 27.99 7.21 -12 -15 -6 24.81 6.00 -12 -15 -5 57.70 8.93 -15 -12 -5 61.64 9.40 -12 -15 -5 49.13 6.85 -12 -15 -4 14.90 5.35 -15 -12 -4 16.30 6.69 -12 -15 -4 15.83 4.34 -12 -15 -3 103.65 11.90 -15 -12 -3 81.88 10.83 -12 -15 -2 37.86 8.21 -15 -12 -2 37.02 8.09 -12 -15 -1 148.47 13.48 -15 -12 -1 151.81 13.99 -12 -15 0 58.96 9.37 -15 -12 0 56.14 8.93 -12 -15 1 181.50 14.77 -15 -12 1 150.54 13.78 -12 -15 2 37.14 7.82 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7.56 0 -16 7 -5.92 4.72 16 0 7 -3.52 5.58 0 -16 8 147.65 12.14 16 0 8 149.97 12.85 0 -16 9 2.97 5.69 16 0 9 -6.72 5.33 0 -16 10 142.26 12.17 16 0 10 156.63 14.11 16 0 11 8.44 6.87 0 -16 11 -15.86 5.79 16 0 12 18.14 6.81 0 -16 12 14.04 5.72 1 -16 -11 34.11 7.04 -1 -16 -11 32.92 7.05 1 -16 -10 -2.02 4.81 -1 -16 -10 0.23 5.04 -1 -16 -9 131.90 11.76 1 -16 -9 137.65 12.03 1 -16 -8 0.78 4.74 -1 -16 -8 0.97 4.77 -1 -16 -7 76.98 9.44 1 -16 -7 73.32 9.36 -1 -16 -6 11.51 5.20 1 -16 -6 1.96 4.90 1 -16 -5 130.18 11.55 -1 -16 -5 128.71 11.32 -1 -16 -4 11.11 5.17 1 -16 -4 10.97 5.42 1 -16 -3 107.21 10.28 -1 -16 -3 116.96 10.96 -16 -1 -2 14.19 6.10 1 -16 -2 17.34 5.98 -1 -16 -2 10.08 5.28 -1 -16 -1 439.83 20.22 -16 -1 -1 436.12 20.19 1 -16 -1 431.86 19.90 -16 -1 0 19.56 6.70 -1 -16 0 20.92 6.76 1 -16 0 21.87 6.75 -1 -16 1 475.49 20.96 -16 -1 1 451.66 20.47 1 -16 1 431.71 19.93 -16 -1 2 14.73 6.00 1 -16 2 12.30 5.60 -1 -16 2 14.27 5.30 1 -16 3 120.34 10.89 -1 -16 3 118.49 10.90 1 -16 4 8.21 4.62 -1 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48.32 7.53 16 3 9 38.99 7.51 16 -3 9 40.87 7.94 3 -16 10 1.10 5.15 -3 -16 10 9.95 5.50 16 3 10 4.34 6.19 16 -3 10 5.73 6.24 3 -16 11 46.51 8.18 -3 -16 11 65.91 8.95 16 3 11 58.66 10.05 16 -3 11 44.61 9.07 16 3 12 6.38 6.42 16 -3 12 9.60 6.93 3 -16 12 5.43 5.19 -3 -16 12 4.12 5.26 4 -16 -11 14.83 6.23 -4 -16 -11 18.23 6.35 -16 -4 -10 64.20 9.33 -4 -16 -10 71.19 9.80 4 -16 -10 58.24 9.04 -4 -16 -9 1.91 5.00 -16 -4 -9 10.28 5.63 -4 -16 -8 90.71 10.31 -16 -4 -8 83.66 9.79 -4 -16 -7 -3.62 5.75 -16 -4 -7 6.74 5.54 -4 -16 -6 136.24 12.32 -16 -4 -6 142.75 12.24 -4 -16 -5 57.67 8.97 -16 -4 -5 57.94 8.62 -16 -4 -4 250.43 15.62 -4 -16 -4 267.10 16.59 -16 -4 -3 31.56 7.25 -4 -16 -3 29.32 7.04 -16 -4 -2 250.78 15.29 -4 -16 -2 228.54 15.23 -16 -4 -1 19.48 6.06 16 -4 -1 23.44 4.54 -4 -16 -1 21.19 5.63 -16 -4 0 189.26 13.40 16 -4 0 191.74 10.80 -4 -16 0 199.54 13.86 -16 -4 1 28.55 6.61 16 -4 1 23.41 4.96 -4 -16 1 16.29 5.31 -16 -4 2 220.44 14.30 -4 -16 2 223.55 14.80 16 -4 2 209.46 11.97 -16 -4 3 26.63 6.59 16 -4 3 25.85 6.00 -4 -16 3 21.64 6.52 -4 -16 4 286.12 16.92 -16 -4 4 251.59 15.52 16 -4 4 256.52 14.13 16 -4 5 52.12 7.33 -16 -4 5 48.25 7.81 -4 -16 5 62.92 8.92 -4 -16 6 167.12 13.43 16 -4 6 141.64 11.38 -16 -4 6 147.05 12.11 16 -4 7 9.28 4.94 -4 -16 7 -9.27 5.84 -16 -4 7 -2.18 4.65 16 -4 8 67.09 9.30 -4 -16 8 78.87 9.52 -16 -4 8 92.12 10.14 16 -4 9 6.14 5.34 -4 -16 9 6.43 5.02 16 4 9 -5.85 6.73 -16 -4 9 12.69 5.73 4 -16 10 49.75 8.21 -16 -4 10 71.44 9.18 16 -4 10 56.34 9.49 -4 -16 10 69.52 9.09 16 4 10 47.72 9.53 16 -4 11 10.57 6.65 4 -16 11 15.22 6.06 16 4 11 5.83 6.68 -4 -16 11 9.16 5.58 16 -4 12 40.62 9.36 -4 -16 12 45.13 8.08 4 -16 12 49.83 8.82 16 4 12 39.86 9.31 -5 -16 -11 54.42 8.67 -16 -5 -11 41.60 7.96 -5 -16 -10 -7.53 5.93 -16 -5 -10 10.05 5.90 -5 -16 -9 105.41 11.28 -16 -5 -9 112.90 11.18 -5 -16 -8 3.57 5.02 -16 -5 -8 8.84 5.44 -16 -5 -7 121.23 11.35 -5 -16 -7 122.22 11.94 -16 -5 -6 14.26 5.66 -5 -16 -6 21.08 6.60 -16 -5 -5 173.09 13.55 -5 -16 -5 174.22 13.90 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52.09 9.47 5 -16 12 22.57 7.34 -5 -16 12 2.26 4.99 16 -5 12 7.52 7.64 -6 -16 -11 0.99 4.70 -16 -6 -11 6.95 5.67 -6 -16 -10 59.02 8.83 -16 -6 -10 53.73 8.38 -6 -16 -9 1.86 5.05 -16 -6 -9 -6.64 5.48 -6 -16 -8 137.39 12.48 -16 -6 -8 123.83 11.71 -16 -6 -7 0.60 5.05 -6 -16 -7 7.46 5.89 -16 -6 -6 123.30 11.54 -6 -16 -6 119.24 11.83 -6 -16 -5 -7.37 5.15 -16 -6 -5 -2.01 5.62 -16 -6 -4 135.77 11.75 -6 -16 -4 153.35 12.67 -6 -16 -3 6.23 5.51 -16 -6 -3 -9.87 6.40 -16 -6 -2 152.16 12.25 -6 -16 -2 166.11 13.10 -6 -16 -1 -2.12 4.50 -16 -6 -1 -1.26 5.08 -16 -6 0 355.24 18.47 16 -6 0 341.73 13.25 -6 -16 0 329.50 18.29 -6 -16 1 8.59 5.60 -16 -6 1 -2.84 4.77 16 -6 1 -2.62 3.90 -16 -6 2 182.13 13.33 16 -6 2 163.19 10.21 -6 -16 2 193.85 14.04 -6 -16 3 -1.28 4.69 -16 -6 3 -4.03 4.89 16 -6 3 -4.07 4.52 -16 -6 4 134.18 11.65 16 -6 4 143.41 10.26 -6 -16 4 143.22 12.31 -6 -16 5 -2.60 4.83 16 -6 5 -3.11 4.88 -16 -6 5 1.38 4.85 -6 -16 6 108.38 10.97 16 -6 6 107.15 10.06 -16 -6 6 137.31 11.91 -6 -16 7 7.84 5.11 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107.50 12.68 -19 -8 4 0.00 5.64 -8 -19 4 -2.74 6.00 -19 -8 5 60.28 9.50 -8 -19 5 62.59 10.42 -19 -8 6 -2.21 5.17 -8 -19 6 -0.60 4.80 -19 -8 7 21.64 6.72 -8 -19 7 23.50 7.24 -8 -19 8 -7.83 6.92 19 -8 8 -1.68 5.58 19 -8 9 47.38 9.16 -9 -19 -9 0.53 5.62 -9 -19 -8 35.79 7.81 -9 -19 -7 -9.54 7.03 -19 -9 -7 -1.42 6.91 -9 -19 -6 23.14 7.73 -19 -9 -6 29.99 7.32 -9 -19 -5 3.43 6.11 -19 -9 -5 -8.38 7.00 -9 -19 -4 116.24 13.20 -19 -9 -4 111.71 12.74 -19 -9 -3 -2.24 6.19 -9 -19 -3 -4.04 5.92 -19 -9 -2 80.21 11.28 -9 -19 -2 77.22 10.80 -19 -9 -1 -1.26 6.60 -9 -19 -1 -14.37 7.77 -19 -9 0 73.21 10.53 -9 -19 0 66.45 10.19 -19 -9 1 -9.45 7.84 -9 -19 1 -4.96 6.50 -19 -9 2 95.58 11.69 -9 -19 2 86.86 11.92 -19 -9 3 -3.23 6.06 -9 -19 3 -1.86 6.20 -19 -9 4 103.62 12.14 -9 -19 4 102.18 12.48 -19 -9 5 0.05 5.45 -9 -19 5 -0.07 5.42 -19 -10 -3 54.53 9.87 -10 -19 -3 56.93 10.05 -19 -10 -2 1.81 6.03 -10 -19 -2 -9.41 7.02 -19 -10 -1 107.97 12.71 -10 -19 -1 105.82 12.51 -19 -10 0 0.50 6.62 -10 -19 0 -1.08 6.40 -19 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139.03 14.01 -3 -20 -3 140.91 14.01 3 -20 -2 12.82 7.35 -3 -20 -2 4.06 6.06 3 -20 -1 54.72 9.46 -20 -3 -1 62.83 9.31 -3 -20 -1 42.96 8.45 3 -20 0 3.75 5.39 -20 -3 0 -0.59 5.71 -3 -20 0 -0.35 6.34 -3 -20 1 39.33 8.16 3 -20 1 38.46 8.21 -3 -20 2 -13.06 7.96 20 -3 2 1.83 4.46 3 -20 2 0.45 5.61 -3 -20 3 134.01 13.45 3 -20 3 149.68 14.04 20 -3 3 122.49 11.38 20 -3 4 10.55 6.24 3 -20 4 12.49 7.67 -3 -20 4 8.04 7.23 20 -3 5 194.15 14.82 3 -20 5 215.07 17.15 -3 -20 5 174.49 15.73 20 -3 6 19.80 6.88 -3 -20 6 2.40 5.70 3 -20 6 7.98 6.32 20 -3 7 68.56 10.18 -3 -20 7 45.79 9.00 3 -20 7 42.30 8.40 20 3 7 59.58 10.24 -3 -20 8 -4.29 6.15 3 -20 8 -5.83 6.17 20 -3 8 -8.13 8.53 -3 -20 9 26.39 7.77 3 -20 9 37.16 8.44 20 -3 9 19.59 7.21 -3 -20 10 -12.85 7.58 3 -20 10 -10.33 6.83 -4 -20 -10 47.42 9.44 4 -20 -10 52.95 10.23 -4 -20 -9 -16.73 7.76 4 -20 -9 5.31 6.48 -4 -20 -8 50.84 10.18 4 -20 -8 51.37 9.86 -4 -20 -7 1.38 5.54 4 -20 -7 2.61 6.41 -4 -20 -6 71.10 10.57 4 -20 -6 52.79 9.68 4 -20 -5 9.23 6.53 -4 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-4.36 6.90 0 -21 1 81.35 11.22 0 -21 2 -6.39 6.88 0 -21 3 44.98 8.45 0 -21 4 -18.71 8.59 21 0 4 -8.11 6.81 0 -21 5 77.60 11.12 21 0 5 70.60 10.24 21 0 6 -7.22 6.93 21 0 7 58.04 10.33 1 -21 -7 -8.48 6.72 -1 -21 -7 -3.47 7.01 1 -21 -6 57.36 10.08 -1 -21 -6 59.22 10.06 1 -21 -5 -3.35 6.90 -1 -21 -5 -8.29 7.61 1 -21 -4 90.69 12.21 -1 -21 -4 76.80 10.95 -1 -21 -3 0.47 6.26 1 -21 -3 1.71 6.32 -1 -21 -2 52.86 9.36 1 -21 -2 60.67 9.58 -1 -21 -1 10.22 6.11 1 -21 -1 13.82 6.63 -1 -21 0 108.34 12.59 1 -21 0 112.66 12.98 -1 -21 1 14.18 6.41 1 -21 1 12.71 6.91 -1 -21 2 61.47 10.18 1 -21 2 71.45 11.06 21 -1 2 38.66 7.42 1 -21 3 -5.43 6.86 -1 -21 3 9.72 6.44 21 -1 3 -2.96 6.14 1 -21 4 80.43 11.11 -1 -21 4 81.44 11.30 21 -1 4 94.85 11.41 1 -21 5 -1.01 6.71 -1 -21 5 -7.72 7.59 21 1 5 4.39 6.11 21 -1 5 4.39 5.91 21 -1 6 63.26 10.37 21 1 6 64.68 10.62 21 1 7 0.09 6.47 21 -1 7 0.88 6.04 -2 -21 -7 75.36 11.47 2 -21 -7 93.14 12.25 -2 -21 -6 11.91 6.71 2 -21 -6 7.40 6.77 -2 -21 -5 100.43 12.52 2 -21 -5 88.13 12.21 -2 -21 -4 -4.34 6.76 2 -21 -4 5.78 6.22 2 -21 -3 56.46 9.30 -2 -21 -3 61.53 10.39 2 -21 -2 3.16 6.03 -2 -21 -2 5.95 6.61 2 -21 -1 67.48 10.39 -2 -21 -1 77.47 10.72 2 -21 0 15.01 7.17 -2 -21 0 6.50 6.00 2 -21 1 78.99 11.61 -2 -21 1 60.84 10.36 2 -21 2 5.56 6.58 -2 -21 2 6.02 6.09 2 -21 3 73.00 10.86 -2 -21 3 77.38 10.54 21 -2 3 63.34 9.24 2 -21 4 2.80 6.60 -2 -21 4 9.89 6.96 21 -2 4 6.78 5.55 2 -21 5 83.82 11.76 -2 -21 5 83.30 11.75 21 -2 5 88.49 11.09 21 2 6 9.90 7.38 21 -2 6 13.63 7.14 21 -2 7 87.72 11.96 -3 -21 -6 54.72 10.43 3 -21 -6 70.58 11.14 -3 -21 -5 5.06 6.62 3 -21 -5 12.43 7.58 -3 -21 -4 126.79 13.93 3 -21 -4 110.33 13.31 -3 -21 -3 3.66 6.99 3 -21 -3 14.62 7.51 -3 -21 -2 93.80 12.13 3 -21 -2 82.28 12.05 -3 -21 -1 3.94 6.52 3 -21 -1 11.64 7.72 -3 -21 0 30.28 7.49 3 -21 0 40.54 8.91 -3 -21 1 -0.24 7.28 3 -21 1 8.15 6.31 -3 -21 2 76.00 11.39 3 -21 2 80.49 11.82 -3 -21 3 -3.42 6.74 3 -21 3 11.82 7.45 3 -21 4 137.04 14.32 -3 -21 4 112.75 13.21 21 -3 4 119.68 12.26 21 -3 5 17.84 7.22 21 -3 6 88.42 11.17 21 -3 7 0.88 6.07 -4 -21 -4 15.05 7.16 4 -21 -4 28.70 8.75 -4 -21 -3 110.91 13.57 -21 -4 -3 118.86 13.52 4 -21 -3 140.45 14.78 -4 -21 -2 -3.97 6.70 -21 -4 -2 2.71 6.17 4 -21 -2 4.94 7.23 -4 -21 -1 65.73 10.44 -21 -4 -1 59.73 9.54 4 -21 -1 61.40 10.04 -4 -21 0 -3.80 7.86 -21 -4 0 10.21 6.38 4 -21 0 12.01 6.84 -4 -21 1 47.11 9.64 -21 -4 1 58.24 9.72 4 -21 1 55.86 9.65 -4 -21 2 -1.24 6.25 4 -21 2 9.04 6.62 -21 -4 2 9.48 6.53 21 -4 6 -6.69 6.89 21 -4 7 32.15 8.17 21 -4 8 -10.27 7.53 21 -5 8 45.71 9.67 22 0 3 -1.75 5.88 22 0 4 23.61 7.55 22 0 5 -11.20 6.83 22 1 4 -7.21 7.87 22 -1 4 -5.32 6.09 22 1 5 44.33 9.45 22 -1 5 47.76 9.12 22 -1 6 5.90 7.18 22 -2 5 14.22 7.09 22 -2 6 93.31 12.10 0 0 0 0.00 0.00 TITL 754_auto in P4nc REM P4nc (#104 in standard setting) CELL 0.71073 17.166430 17.166430 15.332523 90.0000 90.0000 90.0000 ZERR 20.00 0.000733 0.000733 0.001710 0.0000 0.0000 0.0000 LATT -1 SYMM -x,-y, z SYMM -y, x, z SYMM y,-x, z SYMM x+1/2,-y+1/2, z+1/2 SYMM -x+1/2, y+1/2, z+1/2 SYMM -y+1/2,-x+1/2, z+1/2 SYMM y+1/2, x+1/2, z+1/2 SFAC C H N O UNIT 220.00 200.00 20.00 20.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 67385 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.085 _oxdiff_exptl_absorpt_empirical_full_min 0.925 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+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 0.500000 0.500000 0.51720(9) 0.0330(2) Uani 1 4 d S T P . . Al1 Al 0.31958(17) 0.44765(16) 0.6388(3) 0.0493(8) Uani 1 1 d . . . . . O1 O 0.2883(4) 0.4341(4) 0.5226(7) 0.0565(18) Uani 1 1 d . . . . . Na1 Na 0.500000 0.500000 0.7411(7) 0.066(3) Uani 1 4 d S T P . . O4 O 0.3824(5) 0.4920(4) 0.4444(5) 0.0516(19) Uani 1 1 d . . . . . O6 O 0.4250(3) 0.4260(3) 0.6164(5) 0.0360(13) Uani 1 1 d . U . . . O8 O 0.3143(4) 0.3415(4) 0.6617(7) 0.0614(19) Uani 1 1 d . U . . . C1 C 0.3179(6) 0.4527(6) 0.4534(10) 0.054(3) Uani 1 1 d . . . . . O10 O 0.1662(7) 0.3634(6) 0.1462(8) 0.098(4) Uani 1 1 d . . . . . H10 H 0.124589 0.342580 0.158317 0.148 Uiso 1 1 calc R U . . . N1 N 0.4432(4) 0.3452(4) 0.6321(6) 0.0444(16) Uani 1 1 d . U . . . C4 C 0.3813(6) 0.3085(6) 0.6554(9) 0.060(2) Uani 1 1 d . U . . . C6 C 0.2749(5) 0.4192(5) 0.2139(5) 0.079(4) Uani 1 1 d G . . . . H6 H 0.297283 0.429300 0.159882 0.095 Uiso 1 1 calc R U . . . C8 C 0.2034(5) 0.3814(5) 0.2188(5) 0.065(4) Uani 1 1 d G . . . . C10 C 0.1700(4) 0.3662(5) 0.2996(6) 0.081(4) Uani 1 1 d G . . . . H10A H 0.122157 0.340935 0.302899 0.098 Uiso 1 1 calc R U . . . C12 C 0.2080(4) 0.3890(5) 0.3755(5) 0.064(3) Uani 1 1 d G . . . . H12 H 0.185564 0.378857 0.429599 0.077 Uiso 1 1 calc R U . . . C14 C 0.2794(4) 0.4268(4) 0.3707(5) 0.057(3) Uani 1 1 d G . . . . C16 C 0.3129(4) 0.4419(5) 0.2899(6) 0.071(4) Uani 1 1 d G . . . . H16 H 0.360692 0.467222 0.286584 0.085 Uiso 1 1 calc R U . . . C17 C 0.3216(5) 0.1046(5) 0.7050(10) 0.105(2) Uani 1 1 d G U . . . H17 H 0.275318 0.077552 0.713752 0.126 Uiso 1 1 calc R U . . . C9 C 0.3923(6) 0.0650(4) 0.7063(10) 0.108(2) Uani 1 1 d G U . . . H9 H 0.393214 0.011506 0.715809 0.130 Uiso 1 1 calc R U . . . C5 C 0.4615(5) 0.1054(5) 0.6932(9) 0.102(2) Uani 1 1 d G U . . . H5 H 0.508735 0.078903 0.694059 0.122 Uiso 1 1 calc R U . . . C11 C 0.4601(4) 0.1853(5) 0.6790(9) 0.089(2) Uani 1 1 d G U . . . C3 C 0.3894(5) 0.2249(4) 0.6777(9) 0.086(2) Uani 1 1 d G U . . . C13 C 0.3202(4) 0.1845(5) 0.6908(9) 0.097(2) Uani 1 1 d G U . . . H13 H 0.272944 0.210998 0.689946 0.117 Uiso 1 1 calc R U . . . O5 O 0.5297(5) 0.2212(4) 0.6704(7) 0.072(2) Uani 1 1 d . U . . . O3 O 0.5399(6) 0.3550(6) 0.7702(7) 0.080(3) Uani 1 1 d . . . . . H3A H 0.588420 0.351013 0.802382 0.120 Uiso 1 1 calc R U . . . H3B H 0.499383 0.326154 0.800219 0.120 Uiso 1 1 calc R U . . . C7 C 0.211(2) 0.157(3) 0.380(2) 0.287(9) Uani 1 1 d D U . . . H7 H 0.190426 0.205963 0.369591 0.344 Uiso 1 1 calc R U . . . O7 O 0.169(2) 0.100(2) 0.3635(18) 0.269(9) Uani 1 1 d D U . . . N2 N 0.286(2) 0.153(2) 0.414(2) 0.291(9) Uani 1 1 d D U . . . C15 C 0.332(2) 0.223(3) 0.437(3) 0.294(10) Uani 1 1 d D U . . . H15C H 0.386983 0.218360 0.427932 0.441 Uiso 1 1 d R U . . . H15A H 0.321763 0.237650 0.496152 0.441 Uiso 1 1 d R U . . . H15B H 0.311673 0.262810 0.398522 0.441 Uiso 1 1 d R U . . . C2 C 0.315(2) 0.071(2) 0.422(3) 0.298(10) Uani 1 1 d D U . . . H2C H 0.303942 0.041278 0.370586 0.447 Uiso 1 1 d R U . . . H2D H 0.287012 0.050198 0.470576 0.447 Uiso 1 1 d R U . . . H2E H 0.370282 0.068438 0.433916 0.447 Uiso 1 1 d R U . . . O2 O 0.500000 0.500000 0.8937(16) 0.134(13) Uani 1 4 d S T P . . H2B H 0.539150 0.500000 0.927666 0.201 Uiso 0.25 1 d R U P A -1 H2A H 0.460850 0.500000 0.927666 0.201 Uiso 0.25 1 d R U P A -1 O9 O 0.500000 0.500000 0.056(2) 0.18(4) Uani 0.5 4 d DS T P . . H9A H 0.540430 0.500000 0.087638 0.277 Uiso 0.125 1 d R U P B -1 H9B H 0.459570 0.500000 0.087638 0.277 Uiso 0.125 1 d 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 0.0198(2) 0.0198(2) 0.0593(4) 0.000 0.000 0.000 Al1 0.0264(14) 0.0282(14) 0.093(2) 0.0119(17) 0.0052(17) -0.0017(11) O1 0.032(3) 0.045(4) 0.093(6) 0.008(5) -0.009(5) -0.005(3) Na1 0.070(4) 0.070(4) 0.059(5) 0.000 0.000 0.000 O4 0.034(4) 0.046(4) 0.075(5) 0.006(3) -0.016(3) -0.008(3) O6 0.023(3) 0.021(3) 0.064(4) 0.004(3) 0.003(3) 0.003(2) O8 0.033(3) 0.037(3) 0.115(5) 0.024(4) 0.008(4) -0.007(3) C1 0.032(6) 0.031(5) 0.098(10) 0.008(6) -0.017(6) 0.005(4) O10 0.113(9) 0.051(5) 0.131(8) 0.001(6) -0.049(7) -0.023(5) N1 0.022(3) 0.032(3) 0.079(4) 0.005(4) 0.000(3) -0.002(3) C4 0.035(3) 0.037(3) 0.109(5) 0.020(4) 0.003(4) -0.003(3) C6 0.092(11) 0.059(8) 0.086(9) -0.012(7) -0.023(8) -0.018(7) C8 0.079(9) 0.035(6) 0.082(9) 0.000(6) -0.027(7) -0.012(6) C10 0.072(9) 0.055(8) 0.117(12) 0.006(8) -0.034(9) -0.024(7) C12 0.054(7) 0.048(7) 0.091(9) 0.002(6) -0.009(7) -0.010(5) C14 0.043(6) 0.037(6) 0.091(8) 0.004(6) -0.019(6) -0.007(5) C16 0.056(8) 0.045(7) 0.111(11) 0.010(7) -0.025(8) -0.014(6) C17 0.073(3) 0.056(3) 0.188(6) 0.034(4) 0.006(4) -0.007(2) C9 0.074(3) 0.056(3) 0.195(6) 0.036(4) 0.008(4) -0.006(2) C5 0.073(3) 0.053(3) 0.179(6) 0.035(3) 0.006(4) -0.003(2) C11 0.066(3) 0.052(3) 0.148(5) 0.029(3) -0.001(4) -0.004(2) C3 0.065(3) 0.052(3) 0.142(5) 0.029(3) -0.002(4) -0.005(2) C13 0.067(3) 0.055(3) 0.170(6) 0.031(4) 0.001(4) -0.007(2) O5 0.047(4) 0.029(3) 0.140(6) 0.027(4) -0.013(4) 0.000(3) O3 0.074(7) 0.072(6) 0.093(7) 0.016(5) -0.018(6) -0.002(5) C7 0.311(19) 0.30(2) 0.249(14) 0.008(15) -0.100(14) -0.072(15) O7 0.301(19) 0.28(2) 0.222(15) 0.011(16) -0.105(14) -0.074(16) N2 0.314(18) 0.30(2) 0.256(14) 0.009(15) -0.098(14) -0.072(15) C15 0.32(2) 0.30(2) 0.261(17) -0.008(18) -0.105(16) -0.075(17) C2 0.32(2) 0.31(2) 0.266(16) 0.009(18) -0.087(16) -0.063(17) O2 0.17(2) 0.17(2) 0.063(14) 0.000 0.000 0.000 O9 0.20(6) 0.20(6) 0.15(6) 0.000 0.000 0.000 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' Al Al 0.0645 0.0514 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 O4 Dy1 Na1 118.9(2) 2_665 . ? O4 Dy1 Na1 118.9(2) 4_565 . ? O4 Dy1 Na1 118.9(2) . . ? O4 Dy1 Na1 118.9(2) 3_655 . ? O4 Dy1 O4 76.51(19) 3_655 2_665 ? O4 Dy1 O4 76.52(19) 2_665 4_565 ? O4 Dy1 O4 76.52(19) 4_565 . ? O4 Dy1 O4 76.51(19) 3_655 . ? O4 Dy1 O4 122.3(4) 2_665 . ? O4 Dy1 O4 122.3(4) 3_655 4_565 ? O4 Dy1 O6 138.4(2) . 3_655 ? O4 Dy1 O6 82.8(3) 2_665 3_655 ? O4 Dy1 O6 138.4(2) 4_565 . ? O4 Dy1 O6 82.8(3) . 4_565 ? O4 Dy1 O6 82.8(3) 4_565 2_665 ? O4 Dy1 O6 145.0(2) 3_655 4_565 ? O4 Dy1 O6 82.7(3) 3_655 . ? O4 Dy1 O6 78.6(2) 2_665 2_665 ? O4 Dy1 O6 145.0(2) 2_665 . ? O4 Dy1 O6 145.0(2) 4_565 3_655 ? O4 Dy1 O6 138.4(2) 2_665 4_565 ? O4 Dy1 O6 138.4(2) 3_655 2_665 ? O4 Dy1 O6 145.0(2) . 2_665 ? O4 Dy1 O6 78.6(2) 3_655 3_655 ? O4 Dy1 O6 78.6(2) . . ? O4 Dy1 O6 78.6(2) 4_565 4_565 ? O6 Dy1 Na1 49.93(16) 4_565 . ? O6 Dy1 Na1 49.93(16) . . ? O6 Dy1 Na1 49.93(17) 2_665 . ? O6 Dy1 Na1 49.93(16) 3_655 . ? O6 Dy1 O6 99.9(3) . 2_665 ? O6 Dy1 O6 65.52(18) . 4_565 ? O6 Dy1 O6 65.52(18) 2_665 4_565 ? O6 Dy1 O6 65.52(18) 2_665 3_655 ? O6 Dy1 O6 65.52(18) . 3_655 ? O6 Dy1 O6 99.9(3) 4_565 3_655 ? O1 Al1 Na1 134.0(3) . . ? O1 Al1 O6 94.5(4) . . ? O1 Al1 N1 97.8(4) . 4_565 ? O1 Al1 O3 178.7(4) . 4_565 ? O6 Al1 Na1 45.4(2) . . ? O6 Al1 N1 87.9(3) . 4_565 ? O6 Al1 O3 85.2(4) . 4_565 ? O8 Al1 O1 92.5(4) . . ? O8 Al1 Na1 101.8(3) . . ? O8 Al1 O6 83.5(3) . . ? O8 Al1 N1 167.0(4) . 4_565 ? O8 Al1 O3 86.1(4) . 4_565 ? N1 Al1 Na1 65.3(3) 4_565 . ? N1 Al1 O3 83.5(4) 4_565 4_565 ? O5 Al1 O1 90.8(4) 4_565 . ? O5 Al1 Na1 129.7(4) 4_565 . ? O5 Al1 O6 174.7(5) 4_565 . ? O5 Al1 O8 96.6(4) 4_565 . ? O5 Al1 N1 91.1(4) 4_565 4_565 ? O5 Al1 O3 89.5(5) 4_565 4_565 ? O3 Al1 Na1 46.4(3) 4_565 . ? C1 O1 Al1 132.4(7) . . ? Dy1 Na1 Al1 64.05(16) . 3_655 ? Dy1 Na1 Al1 64.05(16) . 2_665 ? Al1 Na1 Al1 78.96(13) 3_655 2_665 ? O6 Na1 Dy1 43.4(2) 4_565 . ? O6 Na1 Dy1 43.4(2) 2_665 . ? O6 Na1 Dy1 43.4(2) . . ? O6 Na1 Dy1 43.4(2) 3_655 . ? O6 Na1 Al1 103.0(3) . 2_665 ? O6 Na1 Al1 30.52(14) 3_655 3_655 ? O6 Na1 Al1 88.6(2) 2_665 3_655 ? O6 Na1 Al1 88.6(2) 4_565 2_665 ? O6 Na1 Al1 52.28(15) . 3_655 ? O6 Na1 Al1 103.0(3) 4_565 3_655 ? O6 Na1 Al1 52.28(15) 3_655 2_665 ? O6 Na1 Al1 30.52(14) 2_665 2_665 ? O6 Na1 O6 86.8(4) 4_565 3_655 ? O6 Na1 O6 86.8(4) 2_665 . ? O6 Na1 O6 58.1(2) 4_565 . ? O6 Na1 O6 58.1(2) 3_655 . ? O6 Na1 O6 58.1(2) 4_565 2_665 ? O6 Na1 O6 58.1(2) 3_655 2_665 ? O3 Na1 Dy1 99.8(3) 4_565 . ? O3 Na1 Dy1 99.8(3) 2_665 . ? O3 Na1 Dy1 99.8(3) 3_655 . ? O3 Na1 Dy1 99.8(3) . . ? O3 Na1 Al1 35.7(2) 3_655 2_665 ? O3 Na1 Al1 163.8(4) 4_565 2_665 ? O3 Na1 Al1 95.0(3) 4_565 3_655 ? O3 Na1 Al1 163.8(4) 2_665 3_655 ? O3 Na1 Al1 93.6(2) 3_655 3_655 ? O3 Na1 Al1 95.0(3) . 2_665 ? O3 Na1 Al1 93.6(2) 2_665 2_665 ? O3 Na1 Al1 35.7(2) . 3_655 ? O3 Na1 O6 78.1(3) . . ? O3 Na1 O6 135.6(4) 3_655 . ? O3 Na1 O6 78.1(3) 2_665 2_665 ? O3 Na1 O6 62.1(3) 4_565 . ? O3 Na1 O6 62.1(3) 2_665 4_565 ? O3 Na1 O6 117.0(3) 2_665 . ? O3 Na1 O6 62.1(3) . 3_655 ? O3 Na1 O6 135.6(4) 2_665 3_655 ? O3 Na1 O6 78.1(3) 3_655 3_655 ? O3 Na1 O6 117.0(3) 3_655 4_565 ? O3 Na1 O6 117.0(3) 4_565 3_655 ? O3 Na1 O6 135.6(4) . 4_565 ? O3 Na1 O6 117.0(3) . 2_665 ? O3 Na1 O6 62.1(3) 3_655 2_665 ? O3 Na1 O6 78.1(3) 4_565 4_565 ? O3 Na1 O6 135.6(4) 4_565 2_665 ? O3 Na1 O3 88.34(11) . 3_655 ? O3 Na1 O3 88.34(11) 3_655 2_665 ? O3 Na1 O3 88.34(11) 4_565 2_665 ? O3 Na1 O3 88.34(11) . 4_565 ? O3 Na1 O3 160.4(7) . 2_665 ? O3 Na1 O3 160.4(7) 3_655 4_565 ? O2 Na1 Dy1 180.0 . . ? O2 Na1 Al1 115.95(16) . 2_665 ? O2 Na1 Al1 115.95(16) . 3_655 ? O2 Na1 O6 136.6(2) . . ? O2 Na1 O6 136.6(2) . 2_665 ? O2 Na1 O6 136.6(2) . 4_565 ? O2 Na1 O6 136.6(2) . 3_655 ? O2 Na1 O3 80.2(3) . 2_665 ? O2 Na1 O3 80.2(3) . 4_565 ? O2 Na1 O3 80.2(3) . . ? O2 Na1 O3 80.2(3) . 3_655 ? C1 O4 Dy1 136.2(7) . . ? Dy1 O6 Na1 86.7(2) . . ? Al1 O6 Dy1 122.4(3) . . ? Al1 O6 Na1 104.1(3) . . ? N1 O6 Dy1 120.4(5) . . ? N1 O6 Al1 111.6(5) . . ? N1 O6 Na1 103.7(5) . . ? C4 O8 Al1 112.0(6) . . ? O1 C1 O4 125.6(11) . . ? O1 C1 C14 118.3(9) . . ? O4 C1 C14 116.0(11) . . ? C8 O10 H10 109.5 . . ? O6 N1 Al1 116.1(5) . 3_655 ? C4 N1 Al1 132.6(7) . 3_655 ? C4 N1 O6 109.8(8) . . ? O8 C4 N1 123.0(9) . . ? O8 C4 C3 119.5(9) . . ? N1 C4 C3 117.5(9) . . ? C8 C6 H6 120.0 . . ? C8 C6 C16 120.0 . . ? C16 C6 H6 120.0 . . ? O10 C8 C6 119.4(8) . . ? O10 C8 C10 120.5(8) . . ? C6 C8 C10 120.0 . . ? C8 C10 H10A 120.0 . . ? C12 C10 C8 120.0 . . ? C12 C10 H10A 120.0 . . ? C10 C12 H12 120.0 . . ? C14 C12 C10 120.0 . . ? C14 C12 H12 120.0 . . ? C12 C14 C1 118.8(7) . . ? C16 C14 C1 121.1(7) . . ? C16 C14 C12 120.0 . . ? C6 C16 H16 120.0 . . ? C14 C16 C6 120.0 . . ? C14 C16 H16 120.0 . . ? C9 C17 H17 120.0 . . ? C9 C17 C13 120.0 . . ? C13 C17 H17 120.0 . . ? C17 C9 H9 120.0 . . ? C5 C9 C17 120.0 . . ? C5 C9 H9 120.0 . . ? C9 C5 H5 120.0 . . ? C11 C5 C9 120.0 . . ? C11 C5 H5 120.0 . . ? C5 C11 C3 120.0 . . ? O5 C11 C5 116.7(7) . . ? O5 C11 C3 123.2(7) . . ? C11 C3 C4 123.9(7) . . ? C11 C3 C13 120.0 . . ? C13 C3 C4 115.8(7) . . ? C17 C13 H13 120.0 . . ? C3 C13 C17 120.0 . . ? C3 C13 H13 120.0 . . ? C11 O5 Al1 130.2(7) . 3_655 ? Al1 O3 Na1 97.9(4) 3_655 . ? Al1 O3 H3A 112.2 3_655 . ? Al1 O3 H3B 112.2 3_655 . ? Na1 O3 H3A 112.2 . . ? Na1 O3 H3B 112.2 . . ? H3A O3 H3B 109.8 . . ? O7 C7 H7 117.1 . . ? O7 C7 N2 126(4) . . ? N2 C7 H7 117.1 . . ? C7 N2 C15 123(3) . . ? C7 N2 C2 112(3) . . ? C15 N2 C2 125(4) . . ? N2 C15 H15C 114.7 . . ? N2 C15 H15A 109.4 . . ? N2 C15 H15B 104.1 . . ? H15C C15 H15A 109.5 . . ? H15C C15 H15B 109.4 . . ? H15A C15 H15B 109.5 . . ? N2 C2 H2C 111.6 . . ? N2 C2 H2D 103.9 . . ? N2 C2 H2E 112.8 . . ? H2C C2 H2D 109.5 . . ? H2C C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? Na1 O2 H2B 127.7 . . ? Na1 O2 H2A 127.7 . . ? H2B O2 H2A 104.5 . . ? H9A O9 H9B 109.5 . . ? 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 Na1 3.434(10) . ? Dy1 O4 2.311(7) 3_655 ? Dy1 O4 2.311(7) 2_665 ? Dy1 O4 2.311(7) 4_565 ? Dy1 O4 2.311(7) . ? Dy1 O6 2.364(6) 4_565 ? Dy1 O6 2.364(6) 3_655 ? Dy1 O6 2.364(6) 2_665 ? Dy1 O6 2.364(6) . ? Al1 O1 1.875(11) . ? Al1 Na1 3.587(5) . ? Al1 O6 1.878(6) . ? Al1 O8 1.859(8) . ? Al1 N1 1.927(8) 4_565 ? Al1 O5 1.800(8) 4_565 ? Al1 O3 2.116(11) 4_565 ? O1 C1 1.219(15) . ? Na1 O6 2.632(10) 2_665 ? Na1 O6 2.632(10) 4_565 ? Na1 O6 2.632(10) 3_655 ? Na1 O6 2.632(10) . ? Na1 O3 2.620(10) 4_565 ? Na1 O3 2.620(10) 3_655 ? Na1 O3 2.620(10) 2_665 ? Na1 O3 2.620(10) . ? Na1 O2 2.34(3) . ? O4 C1 1.303(13) . ? O6 N1 1.442(9) . ? O8 C4 1.285(13) . ? C1 C14 1.499(14) . ? O10 H10 0.8200 . ? O10 C8 1.320(11) . ? N1 C4 1.286(13) . ? C4 C3 1.482(12) . ? C6 H6 0.9300 . ? C6 C8 1.3900 . ? C6 C16 1.3900 . ? C8 C10 1.3900 . ? C10 H10A 0.9300 . ? C10 C12 1.3900 . ? C12 H12 0.9300 . ? C12 C14 1.3900 . ? C14 C16 1.3900 . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C17 C9 1.3900 . ? C17 C13 1.3900 . ? C9 H9 0.9300 . ? C9 C5 1.3900 . ? C5 H5 0.9300 . ? C5 C11 1.3900 . ? C11 C3 1.3900 . ? C11 O5 1.351(10) . ? C3 C13 1.3900 . ? C13 H13 0.9300 . ? O3 H3A 0.9700 . ? O3 H3B 0.9700 . ? C7 H7 0.9300 . ? C7 O7 1.23(2) . ? C7 N2 1.40(2) . ? N2 C15 1.48(2) . ? N2 C2 1.50(2) . ? C15 H15C 0.9602 . ? C15 H15A 0.9599 . ? C15 H15B 0.9599 . ? C2 H2C 0.9599 . ? C2 H2D 0.9599 . ? C2 H2E 0.9601 . ? O2 H2B 0.8499 . ? O2 H2A 0.8499 . ? O9 H9A 0.8497 . ? O9 H9B 0.8497 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Dy1 O4 C1 O1 35.3(17) . . . . ? Dy1 O4 C1 C14 -142.8(8) . . . . ? Dy1 O6 N1 Al1 39.8(8) . . . 3_655 ? Dy1 O6 N1 C4 -152.7(8) . . . . ? Al1 O1 C1 O4 -2.8(16) . . . . ? Al1 O1 C1 C14 175.2(6) . . . . ? Al1 O6 N1 Al1 -165.9(5) . . . 3_655 ? Al1 O6 N1 C4 1.7(11) . . . . ? Al1 O8 C4 N1 -2.8(16) . . . . ? Al1 O8 C4 C3 175.6(10) . . . . ? Al1 N1 C4 O8 165.5(9) 3_655 . . . ? Al1 N1 C4 C3 -12.9(19) 3_655 . . . ? O1 Al1 O6 Dy1 59.2(4) . . . . ? O1 Al1 O6 Na1 154.3(3) . . . . ? O1 Al1 O6 N1 -94.5(6) . . . . ? O1 Al1 O8 C4 97.0(9) . . . . ? O1 C1 C14 C12 5.8(11) . . . . ? O1 C1 C14 C16 -175.9(7) . . . . ? Na1 Al1 O1 C1 -14.8(10) . . . . ? Na1 Al1 O6 Dy1 -95.1(4) . . . . ? Na1 Al1 O6 N1 111.2(7) . . . . ? Na1 Al1 O8 C4 -39.0(9) . . . . ? Na1 O6 N1 Al1 -54.4(7) . . . 3_655 ? Na1 O6 N1 C4 113.1(9) . . . . ? O4 C1 C14 C12 -176.0(7) . . . . ? O4 C1 C14 C16 2.2(11) . . . . ? O6 Al1 O1 C1 -40.2(9) . . . . ? O6 Al1 O8 C4 2.8(9) . . . . ? O6 N1 C4 O8 0.7(17) . . . . ? O6 N1 C4 C3 -177.6(10) . . . . ? O8 Al1 O1 C1 -123.9(9) . . . . ? O8 Al1 O6 Dy1 151.3(5) . . . . ? O8 Al1 O6 Na1 -113.7(4) . . . . ? O8 Al1 O6 N1 -2.4(7) . . . . ? O8 C4 C3 C11 -175.3(10) . . . . ? O8 C4 C3 C13 10.2(16) . . . . ? C1 C14 C16 C6 -178.2(8) . . . . ? O10 C8 C10 C12 -176.8(9) . . . . ? N1 Al1 O1 C1 48.2(9) 4_565 . . . ? N1 Al1 O6 Dy1 -38.4(5) 4_565 . . . ? N1 Al1 O6 Na1 56.6(4) 4_565 . . . ? N1 Al1 O6 N1 167.9(8) 4_565 . . . ? N1 Al1 O8 C4 -46(2) 4_565 . . . ? N1 C4 C3 C11 3.2(18) . . . . ? N1 C4 C3 C13 -171.4(10) . . . . ? C4 C3 C13 C17 174.8(12) . . . . ? C6 C8 C10 C12 0.0 . . . . ? C8 C6 C16 C14 0.0 . . . . ? C8 C10 C12 C14 0.0 . . . . ? C10 C12 C14 C1 178.2(8) . . . . ? C10 C12 C14 C16 0.0 . . . . ? C12 C14 C16 C6 0.0 . . . . ? C16 C6 C8 O10 176.8(9) . . . . ? C16 C6 C8 C10 0.0 . . . . ? C17 C9 C5 C11 0.0 . . . . ? C9 C17 C13 C3 0.0 . . . . ? C9 C5 C11 C3 0.0 . . . . ? C9 C5 C11 O5 177.4(11) . . . . ? C5 C11 C3 C4 -174.4(13) . . . . ? C5 C11 C3 C13 0.0 . . . . ? C5 C11 O5 Al1 171.6(8) . . . 3_655 ? C11 C3 C13 C17 0.0 . . . . ? C3 C11 O5 Al1 -11.1(16) . . . 3_655 ? C13 C17 C9 C5 0.0 . . . . ? O5 Al1 O1 C1 139.4(9) 4_565 . . . ? O5 Al1 O8 C4 -171.9(9) 4_565 . . . ? O5 C11 C3 C4 8.4(14) . . . . ? O5 C11 C3 C13 -177.2(12) . . . . ? O3 Al1 O6 Dy1 -122.1(4) 4_565 . . . ? O3 Al1 O6 Na1 -27.0(4) 4_565 . . . ? O3 Al1 O6 N1 84.2(6) 4_565 . . . ? O3 Al1 O8 C4 -82.8(9) 4_565 . . . ? O7 C7 N2 C15 -177(3) . . . . ? O7 C7 N2 C2 5(4) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 1.06(3) 2 -0.06(3)