#------------------------------------------------------------------------------ #$Date: 2019-10-11 11:54:38 +0300 (Fri, 11 Oct 2019) $ #$Revision: 219290 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234556.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_7234556 loop_ _publ_author_name 'Maciej Ptak' 'Miroslaw Maczka' 'Anna Gagor' 'Pawel Gluchowski' 'Lucyna Macalik' _publ_section_title ; Synthesis, structure and optical properties of two novel luminescent polar dysprosium metal-organic frameworks: [(CH3)2NH2][Dy(HCOO)4] and [N2H5][Dy(HCOO)4] ; _journal_name_full 'Journal of Materials Chemistry C' _journal_page_first 1019 _journal_page_last 1028 _journal_paper_doi 10.1039/C5TC04264J _journal_volume 4 _journal_year 2016 _chemical_formula_sum 'C6 H12 Dy N O8' _chemical_formula_weight 388.67 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.73830(10) _cell_length_b 18.1604(2) _cell_length_c 6.70720(10) _cell_measurement_reflns_used 14033 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 29.6260 _cell_measurement_theta_min 3.9840 _cell_volume 1064.37(2) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 297(2) _diffrn_measured_fraction_theta_full 0.968 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_device_type KM4CCD _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0101 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 22091 _diffrn_reflns_theta_full 27.86 _diffrn_reflns_theta_max 27.86 _diffrn_reflns_theta_min 3.99 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.56626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.425 _exptl_crystal_description 'rectangular prism' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.331 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.073 _refine_ls_abs_structure_details ; Flack x determined using 923 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.013(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 145 _refine_ls_number_reflns 2322 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.104 _refine_ls_R_factor_all 0.0131 _refine_ls_R_factor_gt 0.0122 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0111P)^2^+0.8200P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0273 _reflns_number_gt 2239 _reflns_number_total 2322 _reflns_threshold_expression >2sigma(I) _cod_data_source_file J-Mater-Chem-C-2016-4-1019.cif _cod_data_source_block nc _cod_database_code 7234556 _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_res_file ; nc.res created by SHELXL-2014/7 TITL nc in Pna2(1) CELL 0.71073 8.7383 18.1604 6.7072 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0002 0.0001 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H N O DY UNIT 24 48 4 32 4 L.S. 8 bond $h htab eqiv $1 x+1/2, -y+3/2, z eqiv $2 x+1/2, -y+3/2, z+1 htab N1 O5_$1 htab N1 O1_$2 htab N1 O6 htab N1 O8 BOND FMAP 2 PLAN 20 acta 56 shel 10 0.76 WGHT 0.011100 0.820000 FVAR 0.20386 MOLE 1 DY1 5 0.744151 0.605544 0.405909 11.00000 0.01081 0.01054 = 0.01175 -0.00114 -0.00053 -0.00007 O1 4 0.721468 0.654129 -0.262710 11.00000 0.04088 0.02772 = 0.01392 0.00432 -0.00303 0.00681 O3 4 0.854146 0.510338 0.223801 11.00000 0.02442 0.02777 = 0.02411 -0.00577 0.00272 0.00957 O4 4 0.654100 0.501681 0.593567 11.00000 0.02266 0.03066 = 0.02845 0.00935 0.00290 -0.01057 O5 4 0.603113 0.715882 0.408225 11.00000 0.02538 0.02141 = 0.02791 -0.00211 -0.00435 0.01144 C3 1 0.986720 0.753297 0.343134 11.00000 0.02459 0.02079 = 0.01950 0.00289 -0.00393 -0.00217 AFIX 43 H3 2 0.929462 0.777930 0.247152 11.00000 -1.20000 AFIX 0 C4 1 0.528877 0.478074 0.646723 11.00000 0.03540 0.03438 = 0.03118 -0.00053 0.00495 -0.00862 AFIX 43 H4 2 0.445969 0.501712 0.587882 11.00000 -1.20000 AFIX 0 C5 1 0.983975 0.495881 0.162531 11.00000 0.02343 0.01306 = 0.02881 0.00142 0.00724 -0.00395 AFIX 43 H5 2 1.055323 0.533767 0.170415 11.00000 -1.20000 AFIX 0 C6 1 0.738072 0.622188 -0.098206 11.00000 0.02920 0.02296 = 0.01684 -0.00301 0.00283 0.00178 AFIX 43 H6 2 0.739216 0.570987 -0.100391 11.00000 -1.20000 AFIX 0 O6 4 0.969820 0.562412 0.592535 11.00000 0.02215 0.01935 = 0.03018 0.00632 -0.00795 0.00348 O7 4 0.493855 0.429543 0.761996 11.00000 0.02486 0.02997 = 0.03110 0.00660 0.00754 -0.00846 O8 4 0.941738 0.691705 0.397832 11.00000 0.02623 0.02216 = 0.03478 0.00779 -0.00565 -0.01160 O9 4 0.752982 0.651758 0.065596 11.00000 0.04262 0.02918 = 0.01314 10.00410 -0.00012 -10.00810 mole 1 N1 3 1.172742 0.678138 0.726806 11.00000 0.03250 0.03198 = 0.03320 0.01113 -0.00807 -0.00744 AFIX 23 H1A 2 1.167948 0.722636 0.671557 11.00000 -1.20000 H1B 2 1.110041 0.648687 0.659162 11.00000 -1.20000 AFIX 0 C1 1 1.120265 0.682990 0.930709 11.00000 0.08484 0.06251 = 0.05110 -0.01378 0.02299 -0.03224 AFIX 137 H1C 2 1.131151 0.635885 0.994097 11.00000 -1.50000 H1D 2 1.014590 0.697428 0.932442 11.00000 -1.50000 H1E 2 1.180195 0.718881 1.001042 11.00000 -1.50000 AFIX 0 C2 1 1.327978 0.650411 0.708554 11.00000 0.05375 0.04592 = 0.15096 0.01854 0.04389 0.00249 AFIX 137 H2A 2 1.398422 0.686324 0.759621 11.00000 -1.50000 H2B 2 1.350391 0.641022 0.570760 11.00000 -1.50000 H2C 2 1.337747 0.605556 0.783214 11.00000 -1.50000 MOLE 2 AFIX 0 HKLF 4 REM nc in Pna2(1) REM R1 = 0.0122 for 2239 Fo > 4sig(Fo) and 0.0131 for all 2322 data REM 145 parameters refined using 1 restraints END ; _shelx_res_checksum 87127 _shelx_hkl_file ; 0 -3 0 0.11 0.23 0 3 0 0.29 0.28 0 -4 0 1171.99 14.04 0 -4 0 1156.79 14.02 0 -4 0 1186.49 13.82 0 4 0 1188.33 14.06 0 4 0 1193.54 14.06 0 4 0 1201.70 13.81 0 -5 0 0.64 0.42 0 -5 0 0.61 0.31 0 5 0 0.85 0.42 0 5 0 0.38 0.42 0 -5 0 0.60 0.42 0 5 0 0.74 0.37 0 6 0 72.53 2.08 0 -6 0 72.40 2.24 0 -6 0 72.86 2.11 0 -6 0 70.70 2.21 0 6 0 72.23 2.23 0 6 0 72.05 2.23 0 7 0 0.41 0.40 0 7 0 0.61 0.50 0 -7 0 0.28 0.36 0 -7 0 0.69 0.52 0 -7 0 0.17 0.51 0 7 0 0.81 0.51 0 -8 0 546.33 8.81 0 -8 0 545.66 8.81 0 -8 0 567.50 8.57 0 8 0 561.30 8.50 0 8 0 558.72 8.87 0 8 0 547.16 8.82 0 9 0 0.20 0.41 0 -9 0 -0.51 0.47 0 -9 0 0.44 0.56 0 9 0 0.43 0.59 0 9 0 0.23 0.50 0 -9 0 0.42 0.53 0 10 0 1345.35 18.30 0 10 0 1340.15 17.68 0 10 0 1345.80 18.29 0 -10 0 1380.23 17.85 0 -10 0 1332.17 18.24 0 -10 0 1344.57 18.27 0 11 0 0.94 0.53 0 -11 0 -0.04 0.45 0 11 0 -0.05 0.42 0 -11 0 -0.11 0.42 0 -11 0 0.35 0.45 0 11 0 0.64 0.45 0 -12 0 19.40 1.65 0 12 0 19.55 1.70 0 -12 0 19.20 1.54 0 12 0 23.84 1.84 0 -12 0 18.19 1.61 0 12 0 22.18 1.59 0 13 0 -0.34 0.67 0 13 0 0.11 0.51 0 -13 0 1.11 0.59 0 13 0 1.02 0.74 0 -13 0 0.30 0.57 0 -13 0 -0.67 0.72 0 -14 0 536.25 10.04 0 -14 0 526.64 10.50 0 14 0 519.76 9.80 0 14 0 516.26 10.44 0 -14 0 527.57 10.50 0 14 0 515.80 10.45 0 15 0 -0.64 0.77 0 -15 0 -0.90 0.79 0 -15 0 -0.22 0.57 0 15 0 -1.31 0.87 0 -15 0 1.14 0.95 0 15 0 0.76 0.68 0 -16 0 30.88 2.45 0 16 0 28.91 2.16 0 16 0 33.28 2.55 0 -16 0 34.49 2.61 0 16 0 36.27 2.67 0 -16 0 31.74 2.33 0 17 0 -0.39 0.57 0 -17 0 0.19 0.60 0 -17 0 0.52 0.60 0 17 0 -1.17 0.89 0 -17 0 0.22 0.62 0 17 0 0.20 0.58 0 18 0 484.16 10.50 0 18 0 486.18 11.33 0 18 0 484.04 11.32 0 -18 0 489.46 10.73 0 -19 0 0.74 0.75 0 19 0 0.15 0.87 0 19 0 -1.33 1.10 0 19 0 -0.32 0.71 0 20 0 361.65 9.36 0 20 0 368.44 10.20 0 20 0 364.28 10.15 0 21 0 0.20 0.76 0 22 0 99.55 4.91 -1 -3 0 4.76 0.46 -1 -3 0 5.45 0.55 -1 3 0 5.47 0.57 1 -3 0 5.90 0.60 1 3 0 5.50 0.57 -1 3 0 5.15 0.56 -1 3 0 5.68 0.56 1 -3 0 4.96 0.55 1 3 0 5.37 0.54 1 3 0 4.91 0.48 -1 -3 0 5.35 0.54 1 -4 0 556.57 7.62 -1 4 0 557.16 7.62 -1 4 0 557.00 7.62 1 4 0 555.18 7.32 1 -4 0 559.08 7.62 -1 -4 0 561.20 7.61 -1 4 0 543.56 7.56 1 4 0 543.15 7.59 -1 -4 0 543.88 7.29 1 4 0 546.51 7.60 1 -4 0 544.45 7.59 -1 -4 0 553.36 7.59 -1 -5 0 62.27 2.00 1 -5 0 61.69 2.01 -1 5 0 66.97 2.04 -1 5 0 69.28 2.04 -1 -5 0 65.13 1.83 1 -5 0 64.21 2.00 1 5 0 65.29 1.86 -1 -5 0 62.57 2.00 1 5 0 68.66 2.05 1 5 0 65.44 2.02 -1 5 0 63.91 2.00 1 -5 0 62.01 2.02 -1 -6 0 1233.78 15.77 -1 6 0 1296.45 15.87 -1 -6 0 1226.79 15.77 1 6 0 1252.51 15.32 -1 6 0 1252.02 15.62 1 -6 0 1252.62 15.82 -1 6 0 1284.78 15.84 1 -6 0 1256.06 15.67 1 6 0 1256.79 15.81 1 6 0 1263.24 15.81 1 -6 0 1228.62 15.79 -1 -6 0 1258.86 15.32 1 7 0 1.46 0.56 -1 -7 0 0.84 0.44 1 -7 0 0.68 0.46 -1 -7 0 1.38 0.49 1 7 0 1.60 0.58 -1 7 0 1.84 0.55 -1 7 0 0.86 0.43 1 7 0 1.08 0.41 -1 7 0 0.55 0.41 1 -7 0 1.96 0.62 -1 -7 0 0.82 0.35 1 -7 0 1.33 0.58 1 -8 0 1018.00 13.70 -1 -8 0 1019.74 13.36 -1 -8 0 994.92 13.84 -1 -8 0 1003.19 13.86 1 -8 0 997.46 13.87 1 8 0 1001.17 13.28 -1 8 0 976.35 13.82 -1 8 0 979.57 13.83 1 8 0 997.70 13.87 1 -8 0 997.87 13.86 1 8 0 1007.20 13.91 -1 8 0 1023.61 13.64 1 9 0 34.24 1.89 1 9 0 34.31 1.89 -1 -9 0 35.38 1.73 -1 9 0 34.93 1.82 -1 9 0 37.91 1.96 1 -9 0 37.11 1.89 -1 9 0 35.58 1.91 1 -9 0 35.27 1.91 -1 -9 0 38.35 1.98 -1 -9 0 38.85 1.99 1 9 0 35.46 1.74 1 -9 0 36.20 1.94 -1 10 0 309.69 6.66 -1 -10 0 326.14 6.31 1 10 0 309.31 6.17 1 -10 0 311.98 6.66 1 -10 0 308.94 6.63 -1 10 0 310.08 6.65 1 10 0 331.84 5.15 1 -10 0 323.69 6.53 1 10 0 314.99 6.69 1 10 0 318.56 6.72 -1 -10 0 320.33 6.68 -1 -10 0 319.47 6.68 -1 10 0 312.78 6.38 -1 -11 0 26.66 1.84 1 -11 0 26.71 1.82 1 -11 0 27.17 1.79 1 11 0 27.56 1.90 1 -11 0 26.90 1.85 -1 -11 0 28.46 1.74 -1 11 0 29.69 1.91 -1 11 0 29.37 1.92 1 11 0 26.82 1.68 1 11 0 26.49 1.86 -1 -11 0 28.16 1.87 1 11 0 28.07 1.21 -1 11 0 27.97 1.79 1 12 0 901.08 11.20 -1 12 0 886.54 14.23 1 -12 0 894.14 13.86 -1 -12 0 887.50 14.20 -1 -12 0 915.73 13.61 1 -12 0 906.29 14.27 1 12 0 881.69 13.42 1 12 0 906.76 11.23 1 -12 0 897.33 14.23 -1 12 0 893.09 14.26 1 12 0 905.92 14.21 -1 12 0 891.65 13.75 1 12 0 891.25 14.15 -1 -12 0 886.40 14.21 -1 13 0 10.85 1.39 -1 -13 0 11.00 1.25 1 13 0 10.70 1.35 -1 -13 0 11.62 1.37 1 13 0 11.34 0.75 1 -13 0 12.96 1.49 1 13 0 9.76 1.27 -1 -13 0 14.13 1.51 -1 13 0 11.74 1.33 1 -13 0 12.01 1.34 1 -13 0 9.13 1.27 1 13 0 12.32 1.29 -1 13 0 12.19 1.41 1 13 0 11.51 0.73 -1 14 0 30.87 2.26 1 14 0 31.66 2.26 1 14 0 30.58 1.14 1 14 0 31.74 1.16 -1 -14 0 30.25 2.26 1 14 0 31.63 2.28 1 14 0 33.43 2.14 -1 -14 0 31.02 2.28 -1 14 0 27.97 2.17 1 -14 0 31.69 2.29 -1 -14 0 31.88 2.10 -1 14 0 31.26 2.12 1 -14 0 33.00 2.23 1 -14 0 29.45 2.23 -1 -15 0 11.77 1.54 1 15 0 11.59 0.65 1 15 0 13.33 1.62 1 -15 0 11.48 1.41 1 -15 0 11.69 1.49 -1 15 0 10.86 1.50 1 15 0 13.51 1.47 1 -15 0 9.83 1.40 1 15 0 10.91 1.48 -1 15 0 12.56 1.50 -1 -15 0 12.43 1.60 -1 15 0 12.72 1.62 -1 -15 0 10.47 1.34 1 15 0 10.89 0.64 -1 -16 0 524.30 11.13 -1 16 0 521.76 10.53 -1 16 0 531.19 11.18 -1 -16 0 519.59 11.07 1 16 0 523.00 11.07 1 -16 0 526.45 10.72 -1 -16 0 518.11 10.38 1 16 0 520.09 11.05 1 -16 0 512.22 11.00 1 16 0 505.86 10.19 1 -16 0 529.73 11.15 1 16 0 493.29 6.32 -1 16 0 521.78 11.12 -1 17 0 9.19 1.36 1 17 0 9.83 1.57 -1 -17 0 7.91 1.37 -1 -17 0 8.22 1.29 1 17 0 9.11 1.37 1 -17 0 7.43 1.33 -1 17 0 8.39 1.41 -1 -17 0 7.83 1.36 1 -17 0 10.30 1.49 1 -17 0 9.90 1.56 -1 17 0 8.01 1.39 1 17 0 8.90 1.46 1 -18 0 239.12 7.24 1 18 0 253.05 7.84 1 18 0 239.13 6.94 -1 18 0 244.29 7.13 -1 18 0 243.20 7.61 1 18 0 251.74 7.81 -1 -18 0 254.13 7.27 -1 18 0 244.31 7.64 1 19 0 0.67 0.92 1 19 0 0.35 0.80 -1 19 0 -0.14 0.87 1 -19 0 -0.02 0.78 -1 19 0 -0.43 0.79 1 19 0 0.13 0.70 -1 -19 0 0.95 0.77 -1 20 0 269.91 8.00 1 20 0 273.53 8.70 1 20 0 268.64 7.87 -1 20 0 274.18 8.72 -1 20 0 265.17 8.59 1 20 0 269.32 8.66 -1 21 0 7.81 1.46 1 21 0 7.45 1.43 -1 22 0 334.10 9.59 1 22 0 335.21 9.44 -2 0 0 1786.03 20.30 2 0 0 1815.66 20.79 2 0 0 1832.01 20.90 2 0 0 1775.07 20.38 2 0 0 1838.26 21.14 2 0 0 1850.08 21.13 -2 0 0 1826.18 20.81 -2 0 0 1824.21 20.91 -2 -1 0 72.64 2.05 -2 -1 0 75.94 1.71 -2 1 0 73.19 2.08 -2 -1 0 77.58 2.16 2 -1 0 74.64 2.05 2 1 0 73.26 1.71 2 -1 0 77.20 1.96 -2 1 0 72.60 1.94 2 1 0 75.53 2.12 -2 1 0 77.67 1.94 -2 -1 0 75.09 2.07 2 1 0 74.99 2.05 2 -1 0 71.58 1.94 2 1 0 76.86 2.16 -2 -1 0 76.47 2.15 2 1 0 74.08 2.05 -2 2 0 15.64 0.98 -2 2 0 15.92 0.95 2 -2 0 16.86 1.05 2 2 0 14.08 0.75 -2 2 0 14.87 1.03 2 -2 0 14.39 0.97 -2 -2 0 16.25 1.05 -2 -2 0 15.88 1.02 2 2 0 16.76 0.99 2 2 0 14.13 1.01 2 2 0 17.57 1.10 -2 -2 0 16.16 1.05 -2 -2 0 13.89 0.98 2 -2 0 15.92 0.94 -2 3 0 12.96 0.99 -2 3 0 11.73 0.84 2 3 0 11.53 0.88 -2 -3 0 14.16 1.02 -2 -3 0 13.49 1.01 -2 -3 0 11.41 0.89 2 3 0 12.57 0.95 2 3 0 11.67 0.94 2 -3 0 10.98 0.92 2 -3 0 12.68 0.85 2 -3 0 10.75 0.90 -2 3 0 11.52 0.92 2 -3 0 12.29 0.92 2 -4 0 3323.87 37.71 -2 -4 0 3352.49 37.82 2 4 0 3470.55 37.87 -2 4 0 3399.13 37.86 -2 -4 0 3446.05 37.45 -2 -4 0 3331.71 37.81 -2 4 0 3300.93 37.94 2 -4 0 3431.84 37.43 -2 -4 0 3383.02 37.76 2 -4 0 3331.19 37.83 2 4 0 3487.69 37.88 2 -4 0 3307.38 37.80 -2 4 0 3404.04 37.86 2 -5 0 14.76 1.05 -2 -5 0 14.84 1.09 2 -5 0 13.98 1.07 2 5 0 13.40 1.06 -2 -5 0 14.74 1.09 -2 -5 0 13.20 0.93 -2 5 0 13.48 1.07 2 -5 0 15.33 1.00 -2 -5 0 14.14 1.06 -2 5 0 14.05 1.07 -2 5 0 15.20 1.21 -2 5 0 14.58 1.09 2 -5 0 13.74 1.05 2 5 0 13.58 1.05 -2 6 0 212.62 4.55 2 6 0 206.84 4.50 -2 6 0 204.07 4.49 2 -6 0 200.77 4.47 -2 -6 0 198.63 4.13 2 6 0 200.78 4.45 -2 -6 0 204.17 4.48 2 -6 0 209.39 4.50 -2 6 0 208.78 4.52 -2 -6 0 206.85 4.51 2 -6 0 196.30 4.43 2 -7 0 10.48 1.03 -2 -7 0 11.35 1.07 -2 7 0 11.48 1.05 2 -7 0 12.18 0.66 -2 7 0 11.77 1.10 -2 7 0 11.40 1.08 2 7 0 11.61 1.07 2 7 0 10.55 1.04 -2 -7 0 11.30 0.97 2 -7 0 12.79 1.14 -2 -7 0 12.36 1.07 2 7 0 10.37 0.94 -2 8 0 976.80 13.82 -2 8 0 956.86 13.75 2 -8 0 960.91 13.77 -2 -8 0 970.53 13.13 2 8 0 971.51 13.76 -2 -8 0 956.36 13.75 2 -8 0 961.87 10.91 2 8 0 946.77 13.10 -2 8 0 953.03 13.61 -2 -8 0 962.07 13.77 2 8 0 983.72 13.80 2 -8 0 942.93 10.89 2 -8 0 960.41 13.79 -2 9 0 13.47 1.24 2 9 0 16.34 1.35 2 -9 0 14.72 1.32 2 9 0 15.49 1.36 2 9 0 13.12 1.12 -2 -9 0 13.33 1.23 -2 -9 0 15.11 1.34 2 -9 0 12.66 1.21 -2 -9 0 14.47 1.14 -2 9 0 14.08 1.31 -2 9 0 14.40 1.30 -2 -10 0 884.74 13.68 2 10 0 902.42 13.73 2 -10 0 890.38 13.60 2 -10 0 904.94 13.74 -2 10 0 898.81 13.52 2 10 0 895.57 13.02 -2 -10 0 890.71 13.01 2 -10 0 891.11 13.69 -2 -10 0 894.20 13.73 -2 10 0 890.95 13.72 2 10 0 899.92 13.71 -2 10 0 906.59 13.79 2 11 0 3.97 0.78 -2 -11 0 4.84 0.99 -2 11 0 4.65 0.93 2 -11 0 3.97 0.87 -2 11 0 5.27 0.94 2 -11 0 3.96 0.87 2 11 0 3.46 0.90 -2 11 0 5.85 1.00 2 11 0 4.81 0.94 -2 -11 0 4.95 0.95 2 -11 0 4.38 0.87 -2 -11 0 4.04 0.78 2 12 0 11.76 1.34 2 -12 0 12.12 1.42 2 -12 0 11.43 1.32 2 12 0 9.25 1.12 -2 -12 0 13.70 1.48 -2 12 0 10.92 1.33 -2 12 0 12.16 1.40 2 -12 0 11.29 1.36 -2 -12 0 11.80 1.21 2 12 0 14.12 1.23 -2 -12 0 12.98 1.41 -2 12 0 10.38 1.22 2 12 0 12.72 1.43 -2 -13 0 0.09 0.63 2 -13 0 -0.01 0.71 2 13 0 0.23 0.68 2 13 0 1.73 0.63 2 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6 -12 0 84.88 3.98 -6 13 0 19.97 2.27 6 -13 0 21.53 1.61 -6 -13 0 18.85 2.18 -6 -13 0 20.06 2.04 6 13 0 18.60 2.17 6 -13 0 23.91 1.67 -6 13 0 20.40 2.28 6 13 0 19.62 2.24 6 -13 0 19.62 2.02 -6 -14 0 585.52 13.06 -6 14 0 555.18 13.08 6 14 0 587.00 13.31 6 14 0 584.37 13.31 -6 -14 0 576.88 12.27 6 -14 0 597.58 9.66 -6 14 0 585.97 13.41 6 -14 0 581.76 12.37 6 -14 0 593.42 9.63 -6 15 0 1.99 1.16 6 -15 0 2.15 0.82 -6 -15 0 2.60 1.15 6 15 0 1.46 0.81 6 15 0 3.71 1.44 6 -15 0 2.22 0.52 6 15 0 -0.13 0.74 -6 15 0 4.76 1.46 -6 -15 0 0.07 0.64 6 16 0 151.47 6.51 -6 -16 0 152.58 6.51 6 16 0 151.44 6.25 -6 16 0 146.14 6.60 -6 16 0 143.79 6.38 6 16 0 144.05 6.35 6 17 0 29.00 2.71 -6 17 0 26.40 2.89 -6 -17 0 29.23 2.92 6 18 0 216.47 7.42 -6 18 0 212.70 8.45 -6 -18 0 217.15 8.20 -6 19 0 -0.15 1.19 -6 -19 0 -0.67 1.02 7 0 0 -0.13 0.90 7 0 0 0.58 0.77 7 0 0 -0.11 0.64 7 0 0 0.22 0.58 -7 0 0 0.79 0.56 -7 0 0 0.87 0.69 -7 0 0 -0.15 0.77 7 0 0 0.12 0.86 7 -1 0 40.94 2.93 -7 -1 0 42.06 2.76 7 1 0 42.57 3.00 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391.28 9.72 7 8 0 400.56 9.96 7 9 0 48.31 3.29 7 -9 0 49.24 2.98 -7 -9 0 42.64 3.10 7 9 0 52.76 3.45 -7 -9 0 48.20 3.22 -7 9 0 50.35 3.46 -7 -9 0 46.93 3.28 7 -9 0 43.77 3.22 7 -9 0 42.45 3.16 7 9 0 48.08 2.49 -7 9 0 48.21 3.08 -7 -9 0 48.54 3.11 -7 -9 0 46.43 3.27 7 -10 0 152.01 5.53 -7 -10 0 147.64 5.99 7 10 0 147.61 5.94 -7 10 0 148.10 5.64 -7 10 0 146.78 6.07 -7 -10 0 146.09 5.87 -7 -10 0 144.84 5.55 7 10 0 143.36 4.59 7 -10 0 147.85 5.45 7 10 0 146.93 5.92 -7 -10 0 146.85 5.97 -7 -10 0 138.47 5.67 -7 -11 0 7.77 1.62 7 -11 0 10.15 1.56 7 11 0 9.13 1.53 -7 11 0 8.79 1.57 -7 -11 0 9.16 1.69 7 11 0 9.79 1.26 7 11 0 6.81 1.34 -7 -11 0 9.80 1.57 7 -11 0 8.70 1.41 -7 11 0 7.82 1.50 -7 -12 0 512.49 12.20 7 -12 0 525.22 11.57 7 12 0 533.94 12.58 -7 -12 0 531.84 11.73 7 -12 0 535.35 10.74 7 -12 0 536.22 10.68 -7 12 0 521.64 12.17 -7 12 0 505.99 12.53 7 12 0 535.26 12.60 7 12 0 509.90 10.27 -7 -12 0 526.39 12.56 7 13 0 12.78 1.53 7 -13 0 13.84 1.48 -7 -13 0 13.73 1.98 -7 -13 0 9.95 1.78 -7 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4.12 -8 3 0 60.29 3.10 8 -3 0 56.84 3.37 8 -3 0 56.36 3.71 -8 3 0 59.19 3.43 -8 3 0 53.86 3.50 8 3 0 55.03 3.64 -8 -3 0 58.67 3.56 -8 -3 0 55.07 3.48 8 3 0 59.55 2.86 8 -3 0 55.99 3.72 8 3 0 55.14 3.63 8 -4 0 449.12 10.23 -8 -4 0 430.80 10.47 -8 4 0 438.86 10.64 -8 -4 0 436.47 10.55 8 4 0 438.65 10.90 8 -4 0 428.21 11.00 8 4 0 447.71 8.78 -8 4 0 441.69 10.18 8 4 0 441.27 10.97 -8 4 0 447.50 9.50 8 -4 0 437.80 11.09 8 5 0 -0.29 0.58 8 -5 0 1.14 0.84 8 -5 0 -0.90 1.03 8 5 0 0.69 0.82 8 -5 0 -1.26 1.05 -8 5 0 -0.75 0.66 -8 5 0 0.14 0.72 8 -5 0 0.98 0.67 -8 -5 0 -1.04 1.06 -8 -5 0 -0.88 0.97 -8 -5 0 0.80 0.72 8 -5 0 -0.02 0.87 8 5 0 1.21 0.83 -8 5 0 -0.73 0.90 8 6 0 302.46 8.94 8 -6 0 307.55 9.08 -8 -6 0 307.09 9.03 -8 -6 0 304.65 8.68 -8 -6 0 298.62 8.90 8 6 0 299.03 6.90 -8 6 0 308.38 8.81 -8 6 0 309.56 7.96 8 -6 0 308.17 9.07 8 -6 0 307.52 8.25 8 6 0 304.04 8.94 -8 6 0 295.46 8.09 -8 -6 0 302.74 8.69 -8 7 0 44.88 2.92 8 -7 0 46.33 3.39 8 7 0 49.04 2.58 -8 -7 0 42.24 3.15 8 -7 0 45.21 3.39 -8 -7 0 43.49 3.20 -8 7 0 45.54 3.03 8 -7 0 44.55 3.01 -8 7 0 48.69 3.40 8 7 0 42.63 3.25 8 7 0 46.89 3.41 8 8 0 255.13 8.23 8 8 0 252.37 8.20 8 8 0 244.07 6.21 -8 -8 0 252.48 7.93 -8 8 0 255.02 7.49 -8 -8 0 243.13 7.84 8 -8 0 254.90 7.50 8 -9 0 3.01 1.43 -8 -9 0 0.01 0.78 -8 9 0 -0.81 0.86 -8 -9 0 0.57 0.92 8 -9 0 -1.33 0.88 -8 -9 0 0.98 0.96 8 9 0 -0.09 0.83 8 9 0 -0.65 1.06 -8 9 0 1.05 0.97 8 9 0 0.70 0.56 -8 10 0 402.58 10.18 8 -10 0 378.37 9.90 8 10 0 402.38 10.86 -8 10 0 391.12 10.93 -8 -10 0 382.92 10.35 8 10 0 372.44 8.33 -8 -10 0 387.58 10.51 8 -10 0 378.99 9.69 8 10 0 396.62 10.78 -8 -11 0 31.67 2.90 -8 -11 0 30.78 2.95 8 11 0 26.66 2.75 -8 11 0 26.89 2.79 8 -11 0 32.93 2.70 8 11 0 27.90 2.82 8 -11 0 31.38 2.62 -8 11 0 30.51 2.79 -8 12 0 -0.49 0.87 -8 -12 0 3.02 1.28 -8 -12 0 0.98 1.00 8 -12 0 0.81 0.73 8 -12 0 0.91 0.82 -8 13 0 16.30 2.26 8 -13 0 17.44 1.87 -8 -13 0 16.51 2.28 -8 14 0 287.35 9.46 -8 -14 0 304.85 9.77 -8 -15 0 7.17 1.79 -8 15 0 5.46 1.57 -8 -16 0 33.45 3.30 -8 16 0 43.35 3.81 -8 17 0 19.78 2.75 -9 0 0 0.71 0.74 -9 0 0 -0.82 0.95 -9 0 0 -0.77 0.94 9 0 0 0.49 0.61 9 0 0 -0.57 1.08 9 0 0 -0.08 0.90 -9 1 0 52.70 2.92 9 -1 0 51.79 3.02 9 1 0 53.81 2.96 9 -1 0 56.80 3.95 9 1 0 54.45 3.91 -9 -1 0 53.07 3.72 -9 1 0 56.33 3.64 -9 -1 0 55.27 3.64 9 -1 0 54.76 3.92 9 1 0 53.77 3.88 -9 1 0 56.11 3.84 -9 2 0 576.59 13.25 9 2 0 548.70 13.44 9 -2 0 571.76 13.64 -9 2 0 563.48 11.09 9 2 0 585.93 13.77 9 2 0 571.85 10.98 -9 2 0 564.67 12.61 -9 -2 0 575.97 12.92 -9 -2 0 562.51 13.10 9 -2 0 590.29 13.81 9 -2 0 572.91 12.70 -9 -3 0 35.63 3.01 -9 3 0 38.70 2.55 -9 3 0 40.72 3.05 9 3 0 34.67 3.15 9 -3 0 35.64 3.14 9 -3 0 37.61 3.25 -9 -3 0 37.85 3.06 9 3 0 36.82 3.21 -9 3 0 38.88 3.26 9 3 0 36.74 2.38 9 -3 0 40.34 3.02 9 4 0 145.00 4.76 -9 4 0 135.24 5.04 9 -4 0 145.27 5.81 -9 4 0 140.18 6.06 9 4 0 147.61 6.39 9 4 0 148.04 6.41 -9 4 0 141.94 5.73 -9 -4 0 131.77 5.87 -9 -4 0 136.59 5.89 9 -4 0 129.42 6.08 9 -4 0 139.57 6.31 9 5 0 52.36 2.78 -9 5 0 48.84 3.28 9 -5 0 51.69 3.79 9 -5 0 53.10 3.85 9 5 0 43.99 3.51 9 -5 0 45.81 3.24 9 5 0 52.39 3.85 -9 5 0 46.83 3.52 -9 -5 0 45.29 3.43 -9 5 0 46.40 2.98 -9 -5 0 46.97 3.46 9 6 0 278.98 9.10 -9 6 0 277.36 8.78 9 -6 0 275.26 9.14 -9 -6 0 271.61 8.62 -9 6 0 266.66 8.09 9 -6 0 280.37 8.31 9 -6 0 279.85 9.20 -9 6 0 268.19 7.63 9 6 0 279.78 9.10 -9 -6 0 264.29 8.59 9 7 0 10.69 1.89 9 7 0 9.43 1.66 -9 -7 0 15.20 2.12 9 -7 0 9.54 1.62 9 -7 0 9.66 1.84 -9 7 0 11.29 1.81 -9 7 0 9.19 1.50 9 -7 0 11.34 1.92 -9 7 0 13.93 1.91 -9 -7 0 8.47 1.50 -9 8 0 246.25 7.58 9 -8 0 239.53 7.69 -9 -8 0 241.66 8.30 9 8 0 249.76 8.69 -9 -8 0 253.56 8.47 9 8 0 246.39 8.63 9 -8 0 241.74 8.41 -9 -9 0 30.69 2.94 -9 -9 0 28.18 2.78 9 -9 0 34.17 3.08 -9 9 0 26.96 2.56 -9 10 0 27.92 2.66 9 -10 0 28.14 2.74 -9 -10 0 30.94 3.02 -9 -11 0 9.34 1.84 -9 11 0 8.13 1.71 9 -11 0 10.22 1.64 9 -12 0 280.41 8.45 -9 12 0 283.38 9.11 -9 -12 0 288.91 9.63 -9 13 0 20.67 2.46 -9 -13 0 25.32 2.86 -9 -14 0 4.93 1.44 -9 14 0 2.15 1.03 -9 15 0 23.97 2.81 -10 0 0 417.93 11.26 -10 0 0 438.28 11.93 -10 1 0 20.97 2.42 -10 -1 0 19.48 2.41 -10 1 0 23.13 2.69 -10 1 0 27.13 2.23 -10 -1 0 24.25 2.83 -10 2 0 39.78 3.43 -10 -2 0 38.18 3.24 -10 2 0 38.03 3.16 -10 -2 0 35.63 3.26 -10 2 0 45.21 2.87 -10 3 0 40.06 2.76 -10 3 0 43.45 3.35 -10 -3 0 47.48 3.73 -10 3 0 43.83 3.58 -10 -3 0 46.92 3.66 -10 -4 0 297.93 9.56 -10 4 0 299.39 8.05 -10 4 0 279.91 8.91 -10 4 0 293.34 9.60 -10 -4 0 308.30 9.75 -10 5 0 9.48 1.78 -10 5 0 9.62 1.44 -10 -5 0 9.99 1.78 -10 5 0 7.22 1.54 -10 -5 0 7.35 1.64 -10 6 0 84.38 4.70 -10 -6 0 86.97 5.03 -10 6 0 88.42 4.38 -10 6 0 92.93 5.21 -10 -6 0 96.44 5.38 -10 -7 0 55.79 4.09 -10 7 0 51.47 3.68 -10 7 0 57.62 3.57 -10 7 0 60.07 4.28 -10 8 0 118.96 5.37 -10 -8 0 115.49 5.96 -10 9 0 4.63 1.29 -10 -9 0 4.76 1.42 -10 -10 0 297.42 10.00 -10 10 0 287.63 9.02 -10 11 0 35.20 3.18 -10 -11 0 33.78 3.40 -10 12 0 3.04 1.27 -10 13 0 11.53 2.11 -10 14 0 232.82 8.83 -11 0 0 1.48 1.10 -11 1 0 23.41 2.86 -11 -1 0 26.69 3.12 -11 2 0 251.34 8.89 -11 -2 0 268.91 9.69 -11 2 0 259.48 9.56 -11 3 0 8.32 1.56 -11 3 0 9.02 1.89 -11 -3 0 7.45 1.79 -11 4 0 53.54 3.98 -11 -4 0 57.53 4.39 -11 4 0 54.42 4.24 -11 5 0 47.97 3.97 -11 -5 0 51.29 4.20 -11 6 0 150.54 7.16 -11 -6 0 149.90 7.19 -11 -7 0 -0.56 1.21 -11 7 0 2.01 1.34 0 -2 -1 0.90 0.22 0 2 1 0.54 0.20 0 2 1 1.22 0.24 0 2 -1 1.06 0.25 0 2 1 1.01 0.31 0 -2 -1 1.20 0.30 0 -2 -1 1.17 0.41 0 -2 1 1.06 0.25 0 2 -1 1.11 0.25 0 2 1 1.87 0.44 0 -2 -1 1.20 0.24 0 -2 1 1.08 0.25 0 -2 -1 1.03 0.31 0 3 1 1313.83 14.82 0 3 -1 1335.38 14.94 0 -3 -1 1291.58 14.77 0 3 -1 1317.68 14.16 0 -3 -1 1218.84 15.34 0 -3 1 1329.26 14.94 0 -3 1 1324.46 14.93 0 3 1 1174.63 15.43 0 -3 -1 1294.02 14.74 0 3 1 1323.97 15.28 0 -3 -1 1310.76 15.26 0 -3 -1 1287.89 14.77 0 3 -1 1335.87 14.94 0 3 1 1307.41 14.81 0 4 1 0.11 0.57 0 -4 -1 0.21 0.35 0 4 -1 0.39 0.38 0 -4 -1 0.17 0.29 0 -4 -1 0.30 0.30 0 4 -1 0.01 0.24 0 4 1 -0.07 0.34 0 4 1 0.12 0.42 0 -4 1 0.51 0.25 0 4 1 0.31 0.38 0 -4 -1 0.31 0.32 0 -4 -1 0.63 0.46 0 -4 1 0.29 0.37 0 4 -1 0.02 0.36 0 -4 1 0.43 0.38 0 -5 1 245.69 4.24 0 5 1 236.53 4.14 0 5 -1 212.25 3.44 0 -5 -1 215.30 3.44 0 5 1 235.02 4.13 0 5 -1 215.06 4.05 0 -5 -1 212.33 3.97 0 -5 -1 215.28 3.98 0 -5 1 233.81 3.59 0 -5 -1 219.72 3.44 0 5 1 234.89 4.35 0 -5 1 236.16 4.18 0 5 1 246.99 4.65 0 -5 -1 208.26 4.17 0 5 -1 215.46 4.05 0 -6 -1 0.58 0.43 0 6 1 0.58 0.48 0 -6 -1 0.61 0.41 0 -6 -1 0.41 0.25 0 -6 1 0.44 0.33 0 -6 -1 0.12 0.40 0 6 -1 0.19 0.27 0 -6 1 0.54 0.47 0 6 1 1.29 0.56 0 6 1 0.67 0.48 0 6 -1 0.32 0.43 0 -6 -1 -0.19 0.27 0 6 -1 0.09 0.45 0 -6 1 1.64 0.58 0 -7 -1 1869.30 21.19 0 -7 -1 1910.64 22.80 0 -7 1 1896.45 22.89 0 -7 1 1880.98 21.92 0 7 1 1906.16 23.03 0 -7 1 1897.30 22.88 0 7 -1 1924.21 22.96 0 7 -1 1921.54 22.96 0 7 -1 1884.18 21.84 0 -7 -1 1926.69 22.82 0 7 1 1896.08 22.79 0 7 1 1889.68 22.79 0 -7 -1 1899.14 23.06 0 -7 -1 1867.05 21.17 0 8 1 0.60 0.49 0 -8 -1 0.23 0.41 0 -8 -1 0.44 0.43 0 -8 -1 0.42 0.32 0 -8 1 0.40 0.48 0 8 1 -0.50 0.49 0 -8 1 1.54 0.59 0 8 -1 0.63 0.51 0 -8 1 0.62 0.38 0 8 1 0.42 0.52 0 -8 -1 0.09 0.42 0 8 -1 0.26 0.50 0 8 -1 0.37 0.33 0 9 1 334.41 6.47 0 9 -1 316.31 6.42 0 -9 -1 315.56 6.32 0 -9 -1 318.74 6.34 0 -9 1 328.72 6.51 0 9 1 340.53 6.52 0 -9 -1 312.76 6.41 0 -9 1 336.67 5.83 0 9 -1 322.04 5.67 0 -9 1 332.91 6.54 0 9 1 321.60 6.43 0 9 -1 316.16 6.42 0 10 1 0.04 0.45 0 -10 -1 0.89 0.61 0 10 -1 1.03 0.65 0 10 -1 -0.03 0.39 0 10 1 0.55 0.53 0 10 -1 0.32 0.54 0 -10 1 0.45 0.54 0 10 1 -0.08 0.42 0 -10 -1 -0.56 0.55 0 -10 1 1.07 0.65 0 -10 1 0.97 0.49 0 -10 -1 0.07 0.51 0 -11 1 1006.81 14.19 0 11 -1 1070.48 15.42 0 -11 -1 1039.51 15.26 0 11 1 1026.83 15.23 0 11 1 1011.74 15.18 0 -11 -1 1052.04 15.30 0 -11 -1 1041.00 15.29 0 11 1 975.31 14.97 0 -11 1 999.96 15.21 0 -11 1 1005.92 15.24 0 11 -1 1083.42 15.47 0 11 -1 1065.98 14.24 0 -12 1 1.10 0.58 0 12 1 0.73 0.61 0 -12 -1 -0.19 0.58 0 -12 1 0.02 0.54 0 -12 -1 0.15 0.58 0 12 -1 0.11 0.45 0 -12 1 0.11 0.61 0 12 -1 0.19 0.53 0 12 1 0.46 0.61 0 12 1 -0.31 0.56 0 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7 1.76 0.74 -2 -4 7 1.14 0.81 -2 4 7 1.92 1.12 2 -5 -7 5.21 1.30 -2 -5 7 6.39 1.15 2 -5 -7 3.03 0.91 -2 5 -7 7.71 1.66 -2 -5 -7 4.55 1.32 -2 -5 -7 4.06 0.99 -2 5 7 5.94 1.14 -2 -5 7 5.36 1.08 -2 5 7 7.21 1.66 -2 -6 7 8.56 1.40 2 -6 -7 10.24 1.52 -2 6 -7 8.50 1.60 -2 -6 -7 9.66 1.70 -2 6 7 7.25 1.29 -2 -6 7 8.78 1.41 -2 6 7 7.64 1.65 -2 7 7 478.80 10.89 -2 -7 7 503.82 10.90 2 -7 -7 466.10 10.68 -2 7 -7 479.11 11.72 -2 7 7 495.57 12.83 -2 -7 -7 497.33 12.24 -2 -7 7 471.36 10.75 -2 -8 7 1.69 0.75 -2 8 -7 2.98 1.20 -2 -8 -7 3.00 1.27 -2 8 7 2.66 1.01 -2 -8 7 3.19 1.08 -2 8 7 3.29 1.40 -2 9 7 35.03 2.88 -2 -9 7 40.25 2.93 2 9 7 41.20 2.77 -2 9 -7 38.60 3.11 -2 9 7 41.75 3.68 -2 -9 7 41.56 3.00 -2 -10 7 1.70 0.92 -2 10 -7 0.70 0.82 -2 10 7 2.84 1.02 2 -10 -7 0.67 0.96 -2 -10 7 2.52 0.97 2 10 7 3.02 0.89 -2 10 7 3.21 1.35 -2 -11 7 239.47 7.84 2 -11 -7 225.73 7.81 -2 11 7 244.51 9.47 -2 11 -7 227.20 7.73 2 -12 -7 1.57 1.03 -2 12 -7 1.39 0.87 -2 -12 7 4.29 1.46 -2 12 7 2.82 1.81 -2 -13 7 190.81 7.32 2 -13 -7 182.85 6.97 -2 13 7 190.62 8.74 -2 13 -7 184.53 6.91 -2 -14 7 0.86 0.84 -2 14 7 -2.49 1.74 3 0 -7 0.48 1.00 -3 0 7 0.80 0.93 -3 0 -7 0.68 1.12 -3 0 -7 1.07 0.72 -3 0 7 0.98 0.53 -3 0 7 -0.59 0.70 -3 -1 7 235.39 7.47 -3 1 7 236.15 5.82 -3 -1 7 234.46 7.10 -3 1 7 227.57 6.90 -3 1 -7 259.46 8.30 -3 -1 -7 243.50 8.13 -3 -1 -7 224.71 6.64 -3 1 -7 224.67 6.40 3 1 -7 230.09 7.65 3 -1 -7 225.27 7.70 3 2 -7 2.85 1.10 3 -2 -7 2.59 0.99 -3 -2 7 3.04 1.02 -3 2 -7 2.05 0.88 -3 -2 -7 1.71 0.93 -3 -2 -7 1.49 0.58 -3 2 -7 2.21 0.75 -3 2 7 4.69 0.94 -3 -2 7 3.40 0.93 -3 2 7 2.65 0.85 -3 3 7 32.31 2.24 -3 -3 7 30.56 2.60 -3 -3 7 30.35 2.50 -3 3 7 30.92 2.47 -3 3 -7 31.88 2.87 -3 -3 -7 30.10 2.86 -3 -3 -7 31.90 2.50 3 3 -7 32.85 2.84 -3 3 -7 31.51 2.15 -3 -4 7 1.50 0.88 -3 4 -7 1.76 1.17 -3 -4 -7 0.81 0.71 -3 4 7 2.09 0.77 -3 -4 7 1.83 0.89 -3 4 7 1.62 1.28 -3 -5 7 444.43 10.98 -3 -5 7 451.65 10.77 3 -5 -7 444.53 9.94 -3 5 7 493.18 13.03 -3 5 -7 450.33 11.48 -3 5 7 454.31 10.00 -3 -6 7 2.16 0.90 3 -6 -7 4.39 1.15 -3 6 -7 2.60 1.16 -3 6 7 2.23 0.94 -3 -6 7 2.41 0.99 -3 -7 7 3.76 1.14 3 -7 -7 3.46 1.11 -3 7 -7 2.85 1.24 -3 7 7 2.63 0.95 -3 -7 7 4.94 1.19 -3 7 7 2.43 1.25 -3 -8 7 4.11 1.24 -3 8 -7 6.34 1.45 -3 8 7 4.71 1.16 -3 -8 7 5.53 1.34 -3 8 7 4.90 1.70 -3 -9 7 321.40 9.37 -3 9 7 320.99 10.88 -3 9 -7 324.09 9.46 -3 9 7 314.66 9.09 -3 -9 7 318.47 9.48 -3 -10 7 2.12 0.98 -3 10 -7 1.89 1.02 -3 10 7 3.43 1.27 -3 -10 7 3.19 1.25 -3 10 7 4.52 1.68 -3 -11 7 113.21 5.58 -3 11 7 111.58 6.57 -3 11 -7 97.01 5.05 -3 -11 7 106.89 5.52 -3 12 -7 8.54 1.56 -3 -12 7 6.10 1.39 -3 12 7 3.71 1.35 -3 -13 7 143.30 6.59 -3 13 7 145.51 7.89 -3 -14 7 7.21 1.60 -3 -15 7 213.14 8.45 -4 0 7 16.38 2.14 -4 0 -7 11.95 1.52 -4 0 7 15.25 1.86 -4 -1 7 110.69 5.38 -4 1 7 107.65 5.32 -4 -1 7 102.01 4.91 -4 1 7 109.30 5.02 -4 -1 -7 100.16 4.60 -4 1 -7 105.58 4.55 -4 -2 7 5.15 1.50 -4 2 -7 5.16 1.15 -4 2 7 3.81 0.86 -4 -2 7 3.22 1.11 -4 2 7 2.89 1.02 -4 -3 7 388.20 10.65 -4 -3 7 388.67 10.32 -4 3 7 380.09 9.97 -4 3 7 404.83 11.92 -4 3 7 391.81 8.69 -4 3 -7 360.44 8.82 -4 -4 7 7.59 1.55 -4 4 7 5.78 1.16 -4 -4 7 5.85 1.41 -4 4 7 4.79 1.15 -4 4 7 7.05 1.66 -4 -5 7 5.53 1.29 -4 5 7 4.27 1.01 -4 -5 7 5.34 1.35 -4 5 7 3.76 1.51 -4 -6 7 5.40 1.43 -4 6 7 2.52 0.93 -4 -6 7 3.20 1.10 -4 6 7 3.37 1.41 -4 -7 7 306.67 9.41 -4 7 7 310.11 10.83 -4 7 7 303.11 8.59 -4 -7 7 321.89 9.93 -4 -8 7 0.97 0.94 -4 8 7 1.48 0.92 -4 -8 7 1.06 0.90 -4 8 7 2.78 1.41 -4 -9 7 54.12 3.90 -4 9 7 53.12 4.55 -4 9 7 42.54 3.28 -4 -9 7 52.75 3.97 -4 -10 7 8.78 1.70 -4 -10 7 9.44 1.81 -4 10 7 12.85 2.54 -4 -11 7 237.95 8.71 -4 -11 7 236.34 8.91 -4 -12 7 3.38 1.44 -4 -13 7 151.54 7.14 -4 -14 7 8.00 1.82 -5 0 7 3.03 1.46 -5 0 7 -0.36 0.95 -5 -1 7 210.87 8.09 -5 1 7 210.73 8.04 -5 -1 7 224.31 7.96 -5 1 7 231.28 8.00 -5 -2 7 8.23 1.73 -5 2 7 10.44 1.88 -5 -2 7 9.72 1.66 -5 2 7 7.53 1.52 -5 -3 7 49.21 3.85 -5 -3 7 47.03 3.67 -5 3 7 46.97 3.50 -5 3 7 57.21 4.54 -5 -4 7 8.98 1.90 -5 4 7 8.65 1.33 -5 -4 7 9.40 1.79 -5 4 7 8.85 1.74 -5 4 7 10.94 2.14 -5 -5 7 300.98 9.65 -5 5 7 303.76 9.42 -5 5 7 313.79 11.01 -5 5 7 293.40 8.18 -5 -5 7 291.84 9.82 -5 -6 7 6.25 1.57 -5 6 7 5.82 1.25 -5 -6 7 5.87 1.45 -5 6 7 8.76 2.15 -5 7 7 5.02 1.20 -5 -7 7 3.79 1.30 -5 7 7 5.03 1.74 -5 8 7 7.33 1.44 -5 -8 7 4.43 1.43 -5 8 7 8.01 2.09 -5 -9 7 288.41 9.94 -5 -10 7 0.68 1.21 -5 -11 7 100.08 5.85 -5 -12 7 18.25 2.50 -6 0 7 8.85 1.79 -6 -1 7 116.07 6.04 -6 1 7 119.01 6.12 -6 -2 7 9.45 1.86 -6 2 7 8.29 1.75 -6 -3 7 201.56 8.13 -6 3 7 187.16 7.72 -6 -4 7 17.27 2.57 -6 4 7 11.58 2.02 -6 -5 7 2.56 1.19 -6 5 7 2.08 1.10 -6 -6 7 7.82 1.81 -6 -7 7 288.97 10.18 -6 -8 7 4.68 1.46 -6 -9 7 26.87 3.16 -6 -10 7 5.81 1.67 -7 0 7 0.21 1.17 -7 -1 7 159.32 7.54 -7 1 7 157.16 7.49 -7 -2 7 10.54 2.01 -7 2 7 9.26 1.89 -7 -3 7 31.85 3.45 -7 3 7 30.75 3.28 -7 -4 7 7.96 2.10 -7 4 7 2.83 1.22 -7 -5 7 219.16 9.17 0 8 8 94.73 5.20 0 9 8 1.48 1.33 0 10 8 317.99 10.12 0 11 8 1.53 1.19 -1 7 8 1.65 1.40 -1 8 8 258.27 9.30 -1 9 8 1.12 1.16 -1 10 8 40.00 3.79 -1 11 8 -0.25 0.97 -1 12 8 266.01 10.06 -1 13 8 1.17 1.06 -2 6 8 222.82 7.19 -2 6 8 232.12 9.01 -2 7 8 4.02 0.97 -2 7 8 4.06 1.78 -2 8 8 103.93 5.07 -2 8 8 96.91 5.92 -2 9 8 2.34 1.35 -2 10 8 206.52 8.91 -2 11 8 2.80 1.49 -3 -2 8 316.12 9.23 -3 -3 8 3.78 1.26 -3 -4 8 103.41 5.06 -3 6 8 204.56 8.81 -3 7 8 4.38 1.86 -3 8 8 208.15 9.10 -4 0 8 333.72 9.47 -4 -1 8 0.78 0.83 -4 -1 8 0.80 0.97 -4 1 8 -0.10 0.93 -4 -2 8 43.93 3.54 -4 -2 8 50.02 3.52 -4 2 8 47.25 3.40 -4 -3 8 7.27 1.49 -4 -3 8 4.13 1.15 -4 -4 8 231.24 8.34 -4 -4 8 227.22 7.96 -4 -5 8 2.12 1.29 -5 0 8 -1.73 1.42 -5 -1 8 7.14 1.59 -5 1 8 6.91 1.55 -5 -2 8 246.46 8.78 -5 2 8 252.55 8.67 -5 -3 8 0.16 0.89 -5 3 8 -0.38 1.09 -5 -4 8 62.35 4.44 -5 -5 8 15.06 2.44 -5 -6 8 153.55 7.13 -5 -7 8 1.34 1.42 -6 0 8 307.24 10.34 -6 -1 8 1.90 0.99 -6 1 8 1.32 1.04 -6 -2 8 8.32 2.03 -6 2 8 5.18 1.36 -6 -3 8 9.71 2.06 -6 3 8 10.12 1.77 -6 -4 8 168.16 7.77 -6 4 8 163.52 7.37 -6 -5 8 -0.64 1.02 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 41722 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.744151(9) 0.605544(4) 0.40591(15) 0.01104(4) Uani 1 1 d . . . O1 O 0.7215(3) 0.6541(2) -0.2627(6) 0.0275(7) Uani 1 1 d . . . O3 O 0.8541(2) 0.51034(11) 0.2238(4) 0.0254(4) Uani 1 1 d . . . O4 O 0.6541(2) 0.50168(11) 0.5936(4) 0.0273(5) Uani 1 1 d . . . O5 O 0.60311(18) 0.71588(8) 0.4082(6) 0.0249(3) Uani 1 1 d . . . C3 C 0.9867(3) 0.75330(14) 0.3431(4) 0.0216(7) Uani 1 1 d . . . H3 H 0.9295 0.7779 0.2472 0.026 Uiso 1 1 calc R . . C4 C 0.5289(4) 0.47807(18) 0.6467(6) 0.0337(8) Uani 1 1 d . . . H4 H 0.4460 0.5017 0.5879 0.040 Uiso 1 1 calc R . . C5 C 0.9840(4) 0.4959(2) 0.1625(6) 0.0218(6) Uani 1 1 d . . . H5 H 1.0553 0.5338 0.1704 0.026 Uiso 1 1 calc R . . C6 C 0.7381(3) 0.62219(14) -0.0982(17) 0.0230(5) Uani 1 1 d . . . H6 H 0.7392 0.5710 -0.1004 0.028 Uiso 1 1 calc R . . O6 O 0.9698(2) 0.56241(10) 0.5925(3) 0.0239(4) Uani 1 1 d . . . O7 O 0.4939(2) 0.42954(11) 0.7620(3) 0.0286(5) Uani 1 1 d . . . O8 O 0.94174(19) 0.69171(9) 0.3978(7) 0.0277(4) Uani 1 1 d . . . O9 O 0.7530(2) 0.6518(3) 0.0656(7) 0.0283(9) Uani 1 1 d . . . N1 N 1.1727(3) 0.67814(15) 0.7268(4) 0.0325(6) Uani 1 1 d . . . H1A H 1.1679 0.7231 0.6709 0.039 Uiso 1 1 calc R . . H1B H 1.1093 0.6484 0.6584 0.039 Uiso 1 1 calc R . . C1 C 1.1203(5) 0.6830(2) 0.9307(7) 0.0662(13) Uani 1 1 d . . . H1C H 1.1312 0.6359 0.9941 0.099 Uiso 1 1 calc R . . H1D H 1.0146 0.6974 0.9325 0.099 Uiso 1 1 calc R . . 1E H 1.1802 0.7189 1.0010 0.099 Uiso 1 1 calc R . . C2 C 1.3280(6) 0.6504(2) 0.7086(11) 0.0836(18) Uani 1 1 d . . . H2A H 1.3984 0.6863 0.7596 0.125 Uiso 1 1 calc R . . H2B H 1.3504 0.6410 0.5708 0.125 Uiso 1 1 calc R . . H2C H 1.3377 0.6056 0.7833 0.125 Uiso 1 1 calc R . . 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 0.01081(5) 0.01055(5) 0.01175(6) -0.00114(12) -0.00053(13) -0.00007(3) O1 0.0409(13) 0.0277(17) 0.0139(15) 0.0043(9) -0.0030(14) 0.0068(14) O3 0.0244(10) 0.0278(11) 0.0241(11) -0.0058(9) 0.0027(8) 0.0096(8) O4 0.0227(10) 0.0307(12) 0.0285(12) 0.0094(9) 0.0029(8) -0.0106(9) O5 0.0254(8) 0.0214(8) 0.0279(9) -0.0021(16) -0.0043(17) 0.0114(7) C3 0.0246(14) 0.0208(15) 0.0195(16) 0.0029(10) -0.0039(10) -0.0022(12) C4 0.035(2) 0.034(2) 0.0312(19) -0.0005(16) 0.0050(15) -0.0086(14) C5 0.0234(17) 0.0131(12) 0.0288(15) 0.0014(10) 0.0072(12) -0.0039(12) C6 0.0292(12) 0.0230(11) 0.0168(13) -0.003(4) 0.003(2) 0.0018(9) O6 0.0222(10) 0.0193(10) 0.0302(11) 0.0063(8) -0.0080(8) 0.0035(8) O7 0.0249(10) 0.0300(12) 0.0311(12) 0.0066(9) 0.0075(9) -0.0085(9) O8 0.0262(8) 0.0222(9) 0.0348(11) 0.0078(16) -0.0056(17) -0.0116(7) O9 0.0426(18) 0.0292(19) 0.0131(15) 0.004 -0.0001(10) 0.000 N1 0.0324(15) 0.0320(15) 0.0331(15) 0.0111(12) -0.0080(12) -0.0074(11) C1 0.085(3) 0.062(2) 0.051(3) -0.014(2) 0.023(3) -0.032(2) C2 0.054(3) 0.046(3) 0.151(5) 0.019(3) 0.044(3) 0.002(2) 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O3 Dy1 O8 100.42(9) . . O3 Dy1 O5 148.59(13) . . O8 Dy1 O5 79.42(6) . . O3 Dy1 O7 87.08(8) . 2_664 O8 Dy1 O7 144.86(11) . 2_664 O5 Dy1 O7 76.87(7) . 2_664 O3 Dy1 O4 80.02(7) . . O8 Dy1 O4 141.50(12) . . O5 Dy1 O4 119.61(10) . . O7 Dy1 O4 73.49(7) 2_664 . O3 Dy1 O1 142.58(11) . 1_556 O8 Dy1 O1 80.55(14) . 1_556 O5 Dy1 O1 68.74(14) . 1_556 O7 Dy1 O1 113.70(9) 2_664 1_556 O4 Dy1 O1 77.07(13) . 1_556 O3 Dy1 O9 75.55(13) . . O8 Dy1 O9 73.93(14) . . O5 Dy1 O9 74.28(15) . . O7 Dy1 O9 74.90(9) 2_664 . O4 Dy1 O9 140.66(13) . . O1 Dy1 O9 138.13(6) 1_556 . O3 Dy1 O6 72.52(7) . . O8 Dy1 O6 68.43(8) . . O5 Dy1 O6 133.38(9) . . O7 Dy1 O6 145.14(6) 2_664 . O4 Dy1 O6 75.29(7) . . O1 Dy1 O6 73.28(9) 1_556 . O9 Dy1 O6 124.12(8) . . C6 O1 Dy1 129.4(4) . 1_554 C5 O3 Dy1 135.5(2) . . C4 O4 Dy1 135.9(2) . . C3 O5 Dy1 144.3(2) 3_465 . O8 C3 O5 124.2(3) . 3_565 O8 C3 H3 117.9 . . O5 C3 H3 117.9 3_565 . O7 C4 O4 131.6(3) . . O7 C4 H4 114.2 . . O4 C4 H4 114.2 . . O6 C5 O3 127.8(3) 2_764 . O6 C5 H5 116.1 2_764 . O3 C5 H5 116.1 . . O9 C6 O1 126.6(2) . . O9 C6 H6 116.7 . . O1 C6 H6 116.7 . . C5 O6 Dy1 137.1(2) 2_765 . C4 O7 Dy1 132.4(2) . 2_665 C3 O8 Dy1 147.8(2) . . C6 O9 Dy1 133.2(4) . . C1 N1 C2 113.4(4) . . C1 N1 H1A 108.9 . . C2 N1 H1A 108.9 . . C1 N1 H1B 108.9 . . C2 N1 H1B 108.9 . . H1A N1 H1B 107.7 . . N1 C1 H1C 109.5 . . N1 C1 H1D 109.5 . . H1C C1 H1D 109.5 . . N1 C2 H2A 109.5 . . N1 C2 H2B 109.5 . . H2A C2 H2B 109.5 . . N1 C2 H2C 109.5 . . H2A C2 H2C 109.5 . . H2B C2 H2C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Dy1 O3 2.325(2) . Dy1 O8 2.3307(15) . Dy1 O5 2.3525(15) . Dy1 O7 2.380(2) 2_664 Dy1 O4 2.400(2) . Dy1 O1 2.400(5) 1_556 Dy1 O9 2.433(5) . Dy1 O6 2.464(2) . O1 C6 1.255(11) . O1 Dy1 2.400(5) 1_554 O3 C5 1.235(4) . O4 C4 1.228(4) . O5 C3 1.240(3) 3_465 C3 O8 1.241(3) . C3 O5 1.240(3) 3_565 C3 H3 0.9300 . C4 O7 1.212(4) . C4 H4 0.9300 . C5 O6 1.226(4) 2_764 C5 H5 0.9300 . C6 O9 1.230(12) . C6 H6 0.9300 . O6 C5 1.226(4) 2_765 O7 Dy1 2.380(2) 2_665 N1 C1 1.445(5) . N1 C2 1.452(5) . N1 H1A 0.9000 . N1 H1B 0.9000 . C1 H1C 0.9600 . C1 H1D 0.9600 . 2 H2A 0.9600 . C2 H2B 0.9600 . C2 H2C 0.9600 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O5 0.90 2.16 2.939(4) 145.0 3_565 N1 H1A O1 0.90 2.32 3.076(5) 141.5 3_566 N1 H1B O6 0.90 2.03 2.893(3) 160.6 . N1 H1B O8 0.90 2.41 3.000(4) 123.2 .