#------------------------------------------------------------------------------ #$Date: 2021-09-07 02:10:07 +0300 (Tue, 07 Sep 2021) $ #$Revision: 268987 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/82/7708225.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_7708225 loop_ _publ_author_name 'Qian, Junfeng' 'Lu, Huangjie' 'Zheng, Zhaofa' 'Xu, Miaomiao' 'Qian, Yuan' 'Zhang, Zhi-Hui' 'Wang, Jian-Qiang' 'He, Mingyang' 'Lin, Jian' _publ_section_title ; Achieving Colour Tuneable and White-Light Luminescence in a Large Family of Dual-Emission Lanthanide Coordination Polymers ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT01618K _journal_year 2021 _chemical_formula_moiety 'C33 Ho N6 O7' _chemical_formula_sum 'C33 Ho N6 O7' _chemical_formula_weight 757.32 _chemical_melting_point ? _chemical_name_common 'Holmium 2,2':6',2''-terpyridine-4'-carboxyli' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _audit_creation_method SHELXL-2014 _audit_update_record ; 2021-07-16 deposited with the CCDC. 2021-09-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.468(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.8861(7) _cell_length_b 36.999(2) _cell_length_c 9.4549(7) _cell_measurement_reflns_used 9984 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 54.373 _cell_measurement_theta_min 4.625 _cell_volume 2981.0(4) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '0.5 wide w/ exposures' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_av_unetI/netI 0.0560 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 40582 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.516 _diffrn_reflns_theta_min 2.202 _exptl_absorpt_coefficient_mu 2.714 _exptl_absorpt_correction_T_max 0.897 _exptl_absorpt_correction_T_min 0.796 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SHELTXPREP _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.687 _exptl_crystal_description block _exptl_crystal_F_000 1452 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.062 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.136 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 424 _refine_ls_number_reflns 6854 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.008 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0380 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+6.9833P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0883 _refine_ls_wR_factor_ref 0.1001 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5212 _reflns_number_total 6854 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01618k2.cif _cod_data_source_block HoTPC1 _cod_depositor_comments ; The following automatic conversions were performed: data item '_chemical_melting_point' value 'N/a' was changed to '?' -- the value is undefined or not given. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7708225 _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. ; _shelxl_version_number 2014-3 _shelx_res_file ; TITL SAVE_a.res in P2(1)/c REM Old TITL SAVE in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.084, Rweak 0.004, Alpha 0.032, Orientation as input REM Formula found by SHELXT: C35 N3 O8 Ho CELL 0.71073 8.8861 36.9991 9.4549 90.000 106.468 90.000 ZERR 4.000 0.0007 0.0023 0.0007 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C N O HO UNIT 132 24 28 4 TEMP 0 L.S. 20 ACTA BOND $H LIST 6 FMAP 2 PLAN 20 WGHT 0.044800 6.983300 FVAR 0.26642 HO1 4 0.158517 0.570311 0.180662 11.00000 0.02215 0.02366 = 0.01458 -0.00177 0.00538 0.00086 O1 3 0.142193 0.532101 0.955770 11.00000 0.04273 0.02844 = 0.01756 0.00214 0.01073 0.00334 O2 3 0.061678 0.588476 0.926223 11.00000 0.04858 0.02931 = 0.01852 -0.00157 0.00824 0.00683 O3 3 0.315785 0.606334 0.385091 11.00000 0.04232 0.02787 = 0.03107 -0.00192 0.00585 -0.00354 O4 3 -0.083575 0.538836 0.110090 11.00000 0.02768 0.03640 = 0.03664 -0.00837 0.00982 -0.00348 O5 3 0.234528 0.633463 0.170319 11.00000 0.04782 0.03308 = 0.02458 -0.00520 0.00016 -0.00816 O6 3 0.405547 0.564914 0.159178 11.00000 0.03160 0.06397 = 0.06528 -0.01010 0.02584 0.00092 O7 3 0.633768 0.553045 0.131849 11.00000 0.05057 0.13466 = 0.12460 0.02275 0.04981 0.02694 N1 2 0.251238 0.511544 0.305806 11.00000 0.02913 0.03183 = 0.01770 -0.00286 0.00883 0.00500 N2 2 0.089419 0.558465 0.420097 11.00000 0.02477 0.02411 = 0.01843 -0.00099 0.00628 0.00264 N3 2 -0.049019 0.609320 0.229884 11.00000 0.03096 0.02983 = 0.02397 0.00434 0.01121 0.00749 N4 2 0.511460 0.733257 0.501388 11.00000 0.03552 0.03380 = 0.03445 -0.00537 0.00567 -0.00513 N5 2 0.235699 0.770063 0.182113 11.00000 0.04531 0.04587 = 0.04368 0.00682 0.00729 0.00193 N6 2 0.801415 0.674299 0.721983 11.00000 0.04046 0.04563 = 0.03044 -0.00141 0.00752 -0.00056 C1 1 0.321595 0.487220 0.238752 11.00000 0.03172 0.03623 = 0.03237 -0.00995 0.00404 0.00960 C2 1 0.165278 0.532321 0.511696 11.00000 0.02164 0.02380 = 0.02172 -0.00229 0.00568 -0.00284 C3 1 0.390744 0.455789 0.308256 11.00000 0.03733 0.04025 = 0.03419 -0.00643 0.00557 0.01054 C4 1 0.095303 0.559167 0.874795 11.00000 0.03102 0.02960 = 0.01694 -0.00328 0.00577 -0.00339 C5 1 0.086699 0.557582 0.713398 11.00000 0.02966 0.03200 = 0.01566 -0.00467 0.00523 -0.00813 C6 1 0.246746 0.505003 0.445058 11.00000 0.02742 0.03042 = 0.02122 -0.00411 0.00594 -0.00094 C7 1 0.003255 0.584271 0.618184 11.00000 0.02578 0.02943 = 0.02051 -0.00408 0.00692 -0.00362 C8 1 0.008500 0.583921 0.471701 11.00000 0.02610 0.02761 = 0.01903 -0.00191 0.00633 0.00169 C9 1 0.166813 0.530943 0.660209 11.00000 0.02849 0.02925 = 0.02012 -0.00003 0.00470 -0.00023 C10 1 0.389289 0.449188 0.454229 11.00000 0.04278 0.03238 = 0.04143 0.00056 0.00904 0.00992 C11 1 0.324314 0.701413 0.306938 11.00000 0.03323 0.03520 = 0.03505 -0.00070 0.00612 -0.00590 C12 1 0.381574 0.668748 0.373537 11.00000 0.02965 0.03324 = 0.02798 -0.00676 0.00814 -0.00589 C13 1 0.503806 0.668078 0.504260 11.00000 0.02497 0.03270 = 0.03082 -0.00454 0.00893 -0.00244 C14 1 -0.074069 0.611015 0.363725 11.00000 0.03275 0.02216 = 0.02217 -0.00089 0.00906 0.00458 C15 1 0.315598 0.474097 0.523615 11.00000 0.03348 0.02594 = 0.03452 0.00026 0.00566 0.00498 C16 1 -0.249554 0.661518 0.285571 11.00000 0.06699 0.04922 = 0.05612 0.01898 0.03528 0.02690 C17 1 0.568637 0.701109 0.561068 11.00000 0.03189 0.03330 = 0.02578 -0.00575 0.00685 -0.00254 C18 1 0.306421 0.634136 0.304222 11.00000 0.02572 0.03197 = 0.03312 -0.00827 0.00911 -0.00507 C19 1 0.334122 0.769558 0.317252 11.00000 0.03444 0.03514 = 0.04306 0.00376 0.01134 0.00168 C20 1 0.738755 0.735130 0.774231 11.00000 0.05123 0.04936 = 0.04592 -0.01281 0.00171 -0.01016 C21 1 -0.125027 0.632580 0.123300 11.00000 0.05195 0.04731 = 0.03436 0.01725 0.01772 0.01851 C22 1 -0.173144 0.636889 0.396189 11.00000 0.05233 0.04216 = 0.03852 0.00807 0.02346 0.01811 C23 1 0.974856 0.707545 0.919264 11.00000 0.04800 0.08334 = 0.04023 0.00383 -0.00074 -0.01332 C24 1 -0.225151 0.658949 0.148122 11.00000 0.05888 0.06028 = 0.04693 0.03055 0.02916 0.03392 C25 1 0.392479 0.733333 0.378355 11.00000 0.03372 0.03459 = 0.03532 0.00391 0.00763 -0.00193 C26 1 0.188016 0.802869 0.122420 11.00000 0.05217 0.05215 = 0.05650 0.01393 0.02096 0.00975 C27 1 0.386282 0.800650 0.402760 11.00000 0.05307 0.02773 = 0.07039 -0.00696 0.01007 0.00212 C28 1 0.933716 0.676649 0.834336 11.00000 0.04064 0.07793 = 0.02897 0.01080 0.00714 -0.00712 C29 1 0.873627 0.736930 0.892859 11.00000 0.05893 0.06938 = 0.05037 -0.01564 -0.00401 -0.01891 C30 1 0.710242 0.703693 0.692087 11.00000 0.03632 0.03526 = 0.02899 -0.00535 0.00867 -0.00372 C31 1 0.337229 0.834025 0.339362 11.00000 0.05921 0.03880 = 0.08381 -0.00118 0.01348 0.00156 C32 1 0.238475 0.834832 0.195693 11.00000 0.05881 0.05046 = 0.08401 0.01921 0.03055 0.01041 C33 1 0.508314 0.567533 0.099986 11.00000 0.04234 0.08252 = 0.07277 0.01437 0.02915 0.01732 HKLF 4 REM SAVE_a.res in P2(1)/c REM R1 = 0.0380 for 5212 Fo > 4sig(Fo) and 0.0622 for all 6854 data REM 424 parameters refined using 0 restraints END WGHT 0.0346 7.2293 REM Highest difference peak 1.062, deepest hole -0.750, 1-sigma level 0.136 Q1 1 0.4740 0.4297 0.5424 11.00000 0.05 1.06 Q2 1 0.2189 0.5105 0.7297 11.00000 0.05 0.84 Q3 1 0.2322 0.6987 0.2281 11.00000 0.05 0.84 Q4 1 -0.1623 0.6436 0.5125 11.00000 0.05 0.81 Q5 1 0.4538 0.4354 0.2773 11.00000 0.05 0.81 Q6 1 0.3186 0.4718 0.6337 11.00000 0.05 0.73 Q7 1 0.4742 0.5824 -0.0135 11.00000 0.05 0.73 Q8 1 0.5260 0.6447 0.5390 11.00000 0.05 0.72 Q9 1 -0.0415 0.6072 0.6457 11.00000 0.05 0.71 Q10 1 -0.1060 0.6307 0.0229 11.00000 0.05 0.71 Q11 1 0.4429 0.8004 0.4936 11.00000 0.05 0.70 Q12 1 0.3201 0.4963 0.1242 11.00000 0.05 0.69 Q13 1 0.3630 0.8561 0.3979 11.00000 0.05 0.68 Q14 1 0.9956 0.6535 0.8450 11.00000 0.05 0.67 Q15 1 0.1077 0.8028 0.0180 11.00000 0.05 0.66 Q16 1 -0.1086 0.5182 0.0732 11.00000 0.05 0.66 Q17 1 0.6651 0.7511 0.7607 11.00000 0.05 0.65 Q18 1 0.3158 0.5675 0.1965 11.00000 0.05 0.62 Q19 1 -0.3043 0.6716 0.0538 11.00000 0.05 0.60 Q20 1 0.4000 0.4216 0.4790 11.00000 0.05 0.60 ; _shelx_res_checksum 98096 _shelx_hkl_file ; 1 0 0 2600.14 110.99 -1 0 0 2646.34 110.99 2 0 0 2383.36 105.39 -2 0 0 2267.37 104.79 -3 0 0 1856.41 89.19 3 0 0 1713.53 87.99 -4 0 0 1315.27 77.69 -4 0 0 1513.75 63.29 4 0 0 1396.56 78.39 -5 0 0 49.90 7.20 -5 0 0 65.59 18.00 5 0 0 44.50 13.20 -6 0 0 1153.18 50.49 6 0 0 1109.59 73.59 -6 0 0 1092.99 74.79 6 0 0 1013.90 72.39 -7 0 0 298.27 38.20 7 0 0 247.58 38.40 7 0 0 304.37 37.10 8 0 0 15.90 14.60 9 0 0 566.44 61.09 10 0 0 194.58 42.40 11 0 0 8.90 25.70 -1 -1 0 1392.36 61.49 1 -1 0 1435.46 62.69 1 1 0 1493.65 61.89 -1 1 0 1273.27 58.49 -1 1 0 1428.16 62.69 2 -1 0 37.20 8.10 -2 -1 0 26.40 6.50 2 1 0 30.40 7.30 -2 1 0 39.50 8.60 -3 -1 0 13.80 6.10 3 -1 0 -2.30 3.70 3 1 0 9.80 5.40 -3 1 0 9.70 6.40 -3 1 0 10.20 3.10 4 -1 0 155.48 19.80 -4 -1 0 158.78 10.60 -4 -1 0 129.19 20.70 -4 1 0 113.09 19.80 4 1 0 160.48 23.50 -4 1 0 168.48 12.00 5 -1 0 750.92 56.89 5 -1 0 869.71 58.29 -5 -1 0 883.31 59.39 -5 -1 0 917.11 40.10 -5 1 0 845.42 59.39 -5 1 0 848.22 41.90 5 1 0 855.21 58.49 -6 -1 0 -15.80 12.80 6 -1 0 9.00 9.30 6 -1 0 -0.50 12.20 -6 -1 0 3.50 3.00 6 1 0 5.60 9.70 -6 1 0 -4.00 11.00 6 1 0 3.10 13.10 -6 1 0 -3.20 3.90 -7 -1 0 22.50 17.70 7 -1 0 62.49 23.10 7 -1 0 24.40 15.40 7 1 0 53.99 22.60 -7 1 0 51.39 22.00 7 1 0 33.70 16.80 -7 1 0 51.49 6.90 8 -1 0 104.39 28.40 8 1 0 81.69 24.40 9 -1 0 4.60 17.50 9 1 0 -11.00 16.40 10 -1 0 -5.10 21.10 10 1 0 -4.30 21.00 11 -1 0 51.19 29.10 11 1 0 79.49 34.20 1 -2 0 2747.82 108.19 -1 -2 0 2534.35 106.09 -1 -2 0 2514.55 109.09 1 -2 0 2547.95 109.59 1 -2 0 2570.54 111.29 1 2 0 2591.04 106.09 -1 2 0 2691.53 108.09 -1 2 0 2480.45 110.89 1 2 0 2644.24 109.19 -1 2 0 2724.93 109.99 -2 -2 0 8.90 4.00 2 -2 0 14.10 5.70 2 -2 0 9.00 4.30 -2 2 0 12.90 3.70 2 2 0 11.70 4.50 -2 2 0 5.60 4.20 3 -2 0 957.40 57.09 3 -2 0 1022.20 56.19 -3 -2 0 1026.10 56.09 3 2 0 1008.00 55.99 -3 2 0 947.51 56.89 -3 2 0 1099.69 47.80 4 -2 0 1475.75 83.09 -4 -2 0 1425.56 80.79 4 -2 0 1591.44 82.39 -4 2 0 1500.65 68.49 -4 2 0 1450.65 83.09 4 2 0 1659.63 83.49 5 -2 0 21.80 10.00 -5 -2 0 13.20 3.50 5 -2 0 8.20 8.00 -5 -2 0 15.30 11.70 -5 2 0 9.30 9.30 5 2 0 19.90 9.50 -5 2 0 5.30 4.40 6 -2 0 390.36 39.70 6 -2 0 431.56 40.60 -6 -2 0 443.86 41.10 6 2 0 304.67 35.30 -6 2 0 417.76 24.30 -6 2 0 395.46 42.00 7 -2 0 332.67 39.70 7 -2 0 261.47 40.10 -7 -2 0 322.97 46.60 7 2 0 301.17 37.20 -7 2 0 325.77 40.80 7 2 0 332.17 40.30 -7 2 0 301.27 19.30 8 -2 0 -9.70 12.70 8 2 0 5.80 15.70 9 -2 0 224.98 44.00 9 2 0 148.09 34.00 10 -2 0 106.09 33.40 10 2 0 82.19 32.70 11 -2 0 -16.20 27.10 11 2 0 -11.30 26.00 1 -3 0 3720.73 161.48 -1 -3 0 3819.82 160.58 -1 -3 0 3864.41 159.18 1 -3 0 4028.50 164.08 1 -3 0 4062.99 161.38 1 3 0 4012.30 160.68 1 3 0 3989.80 159.08 -1 3 0 3834.82 161.08 -1 3 0 3902.91 161.78 -1 3 0 3818.32 163.78 2 -3 0 6431.66 279.37 2 -3 0 6881.11 282.97 -2 -3 0 7025.00 279.57 -2 -3 0 6636.44 271.47 -2 3 0 6629.34 274.87 -2 3 0 6690.93 282.37 2 3 0 6745.62 279.17 -3 -3 0 64.59 5.40 3 -3 0 48.40 10.90 3 -3 0 31.40 9.10 -3 -3 0 60.79 11.70 3 3 0 48.50 11.00 -3 3 0 63.59 13.40 -3 3 0 61.19 7.40 -4 -3 0 1087.19 48.90 4 -3 0 1138.99 65.19 4 -3 0 1099.59 66.79 -4 -3 0 1002.20 63.39 4 3 0 1219.48 66.09 -4 3 0 1240.98 54.49 -4 3 0 1042.90 66.79 -5 -3 0 1083.29 69.59 5 -3 0 914.11 68.19 -5 -3 0 1172.38 49.50 -5 -3 0 1312.27 50.09 5 -3 0 1173.38 70.79 -5 3 0 1139.49 73.09 -5 3 0 1122.19 55.59 5 3 0 1075.99 69.09 -6 -3 0 502.45 45.70 6 -3 0 467.05 44.70 6 -3 0 480.45 46.10 6 3 0 513.65 45.20 -6 3 0 551.44 30.70 -6 3 0 593.54 52.19 7 -3 0 472.45 48.10 7 -3 0 507.45 48.20 -7 -3 0 447.36 48.80 7 3 0 456.95 48.60 7 3 0 437.56 45.40 -7 3 0 496.25 53.09 -7 3 0 466.15 27.40 8 -3 0 882.81 73.49 8 3 0 839.32 70.59 -8 3 0 941.01 42.70 9 -3 0 85.49 28.20 9 3 0 56.89 25.40 10 -3 0 80.79 30.60 10 3 0 43.10 28.00 11 -3 0 182.88 52.79 11 3 0 248.48 51.99 0 -4 0 7.90 1.60 0 -4 0 12.70 3.00 0 -4 0 8.20 1.90 0 4 0 11.90 1.90 0 4 0 6.30 2.20 0 4 0 8.00 2.00 -1 -4 0 990.10 44.50 1 -4 0 1031.40 46.50 1 -4 0 989.20 45.90 -1 -4 0 981.10 44.10 1 -4 0 1071.79 48.60 -1 4 0 1011.10 46.00 -1 4 0 973.10 46.30 1 4 0 982.80 44.30 1 4 0 1005.30 44.20 -1 4 0 1049.99 48.60 -2 -4 0 111.39 7.80 2 -4 0 125.79 13.80 2 -4 0 92.39 10.80 -2 -4 0 106.99 10.80 -2 4 0 103.69 13.10 -2 4 0 101.29 9.60 2 4 0 112.29 11.00 -3 -4 0 13.70 6.30 -3 -4 0 22.00 3.80 3 -4 0 33.20 8.40 3 -4 0 21.50 7.60 -3 4 0 14.90 8.10 -3 4 0 26.30 6.10 3 4 0 19.10 6.60 4 -4 0 19.90 8.20 -4 -4 0 13.30 2.90 4 -4 0 13.10 7.80 -4 -4 0 -10.30 5.70 -4 4 0 5.90 4.40 -4 4 0 12.50 8.50 4 4 0 5.70 6.70 -5 -4 0 0.10 9.20 5 -4 0 23.40 11.30 5 -4 0 26.50 11.20 -5 4 0 38.70 14.00 5 4 0 22.40 10.80 -5 4 0 14.40 6.90 -6 -4 0 71.49 19.70 6 -4 0 68.59 18.90 6 -4 0 94.79 22.80 -6 4 0 70.79 11.90 -6 4 0 93.79 25.00 6 4 0 46.00 17.10 7 -4 0 3.00 11.60 -7 -4 0 -6.90 16.80 7 -4 0 11.50 17.30 -7 4 0 0.80 17.70 -7 4 0 -6.90 6.10 7 4 0 24.20 14.30 8 -4 0 14.30 15.10 -8 4 0 24.60 7.50 8 4 0 19.40 16.30 9 -4 0 -9.50 14.10 9 4 0 27.40 19.00 9 4 0 -61.09 22.00 10 -4 0 4.20 22.70 10 4 0 17.40 18.00 11 -4 0 33.80 36.80 11 4 0 15.60 27.50 0 -5 0 6.10 2.30 0 -5 0 4.90 1.70 0 -5 0 3.00 1.20 0 5 0 1.50 1.50 0 5 0 6.20 1.80 -1 -5 0 2921.71 119.49 1 -5 0 2851.81 124.69 1 -5 0 2976.50 123.69 1 -5 0 2959.90 122.29 -1 -5 0 2840.22 121.39 -1 5 0 2779.92 124.49 -1 5 0 2991.10 122.29 1 5 0 2868.61 121.29 1 5 0 2908.91 119.39 -2 -5 0 9393.66 388.16 2 -5 0 9999.00 392.66 2 -5 0 9964.00 399.06 -2 -5 0 9344.87 392.66 2 -5 0 9457.65 394.46 -2 5 0 9601.64 394.76 -2 5 0 9648.13 398.66 2 5 0 9706.33 388.26 2 5 0 9932.51 393.16 -2 5 0 8906.81 391.56 3 -5 0 247.28 21.40 -3 -5 0 219.18 13.40 3 -5 0 214.78 21.90 -3 -5 0 245.58 20.60 -3 5 0 243.08 17.40 -3 5 0 214.58 22.50 3 5 0 224.98 19.80 4 -5 0 1709.83 89.49 -4 -5 0 1659.63 84.59 -4 -5 0 1438.76 67.89 4 -5 0 1591.34 84.69 -4 5 0 1639.14 75.49 4 5 0 1750.72 85.69 -4 5 0 1462.45 87.09 5 -5 0 966.30 65.49 5 -5 0 919.31 61.69 -5 -5 0 920.01 61.49 -5 -5 0 971.60 41.90 -5 5 0 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7 -24 0 1.70 18.00 7 24 0 0.30 12.00 7 24 0 13.70 12.50 7 24 0 65.79 25.30 -7 24 0 15.80 22.90 8 -24 0 32.10 23.00 8 24 0 2.80 20.70 8 24 0 32.10 15.90 8 24 0 26.20 17.50 9 -24 0 8.70 25.70 9 24 0 25.30 20.00 9 24 0 77.29 30.90 0 -25 0 9.30 9.60 0 -25 0 2.90 7.40 0 -25 0 11.60 5.80 0 -25 0 6.60 6.00 0 25 0 3.40 11.90 0 25 0 12.00 7.90 -1 -25 0 1449.76 59.69 1 -25 0 1232.88 82.99 -1 -25 0 1363.26 59.69 1 -25 0 1484.15 74.79 1 -25 0 1377.16 73.69 1 -25 0 1392.66 72.39 -1 -25 0 1334.07 83.49 -1 25 0 1369.26 75.09 -1 25 0 1414.76 85.39 1 25 0 1539.05 85.09 1 25 0 1369.46 77.09 2 -25 0 991.40 59.89 -2 -25 0 946.41 65.59 2 -25 0 883.51 56.49 2 -25 0 1117.99 64.19 2 -25 0 953.20 68.09 2 25 0 1050.79 66.59 -2 25 0 1149.78 72.29 2 25 0 1011.30 63.79 -2 25 0 956.50 58.59 3 -25 0 67.89 18.50 3 -25 0 75.29 20.10 3 -25 0 50.49 15.50 -3 -25 0 86.69 21.40 3 -25 0 81.29 20.20 -3 25 0 57.59 20.10 -3 25 0 73.59 17.30 -3 25 0 57.19 19.50 3 25 0 72.49 18.10 3 25 0 37.00 15.00 4 -25 0 1174.58 81.39 4 -25 0 1307.77 74.39 4 -25 0 1157.78 79.49 -4 -25 0 1307.77 76.69 4 -25 0 1400.46 85.19 4 25 0 1221.68 74.19 -4 25 0 1161.98 80.29 -4 25 0 1220.78 73.89 -4 25 0 1268.17 82.49 4 25 0 1157.18 79.29 5 -25 0 1985.70 117.79 -5 -25 0 1915.01 101.99 5 -25 0 1942.91 105.39 5 25 0 1798.52 112.79 -5 25 0 1926.51 117.09 5 25 0 1963.20 84.69 -5 25 0 1916.11 112.79 -5 25 0 1723.43 103.49 5 25 0 1916.21 84.59 5 25 0 1882.71 101.89 6 -25 0 19.80 20.40 6 -25 0 36.10 20.50 -6 -25 0 40.50 16.20 -6 -25 0 45.30 15.70 6 25 0 74.39 13.80 6 25 0 45.90 21.20 -6 25 0 51.19 30.10 6 25 0 65.79 13.60 -6 25 0 93.19 29.50 -7 -25 0 293.47 36.30 7 -25 0 278.07 45.70 -7 -25 0 324.37 31.00 7 -25 0 343.37 55.49 7 25 0 327.27 31.30 7 25 0 305.97 30.30 7 25 0 259.57 47.10 8 -25 0 581.84 68.39 8 25 0 592.14 47.40 8 25 0 494.85 44.90 8 25 0 531.95 61.29 9 -25 0 10.20 32.60 9 25 0 62.19 22.80 9 25 0 -17.30 22.60 0 -26 0 278.17 21.40 0 -26 0 300.37 33.40 0 -26 0 269.37 20.60 0 -26 0 260.87 26.00 0 26 0 330.97 34.20 0 26 0 279.27 27.10 1 -26 0 61.59 18.60 1 -26 0 69.79 14.10 1 -26 0 78.19 15.00 -1 -26 0 70.69 6.00 1 -26 0 86.09 14.70 -1 -26 0 45.70 15.70 1 26 0 44.00 16.90 1 26 0 60.59 14.90 -1 26 0 95.09 22.70 -1 26 0 52.29 13.20 -2 -26 0 13.60 12.00 2 -26 0 47.00 16.40 2 -26 0 20.20 10.90 2 -26 0 33.40 12.80 2 -26 0 -4.70 9.80 2 26 0 22.40 13.20 2 26 0 25.70 12.10 -2 26 0 38.80 15.90 -2 26 0 20.80 10.40 3 -26 0 303.47 34.20 3 -26 0 363.16 31.10 -3 -26 0 310.07 32.70 3 -26 0 296.07 33.20 3 -26 0 263.37 40.50 -3 26 0 318.27 29.70 3 26 0 311.07 33.30 3 26 0 293.07 33.50 -3 26 0 353.56 38.30 -4 -26 0 39.80 15.50 4 -26 0 54.79 16.30 4 -26 0 69.79 21.70 4 -26 0 25.80 17.50 4 -26 0 47.60 18.50 4 26 0 37.00 17.00 -4 26 0 12.20 16.80 -4 26 0 4.20 19.20 -4 26 0 60.39 15.90 4 26 0 49.20 17.50 5 -26 0 28.20 17.90 -5 -26 0 57.89 17.70 5 -26 0 46.90 22.00 5 26 0 101.99 25.60 -5 26 0 84.29 19.60 -5 26 0 71.09 25.30 -5 26 0 37.90 22.10 5 26 0 83.09 20.10 6 -26 0 161.18 35.40 -6 -26 0 116.99 22.80 6 -26 0 128.59 27.50 6 26 0 135.99 31.20 -6 26 0 162.88 40.20 6 26 0 136.29 17.50 6 26 0 138.99 17.20 -7 -26 0 103.29 20.60 7 -26 0 80.89 30.30 7 -26 0 57.69 26.50 7 26 0 38.80 20.90 7 26 0 134.89 21.10 7 26 0 84.39 17.00 8 -26 0 -42.00 21.60 8 26 0 -11.00 14.90 8 26 0 -8.50 12.90 8 26 0 -7.60 20.70 9 -26 0 58.89 34.50 9 26 0 59.49 27.10 9 26 0 62.09 22.40 0 -27 0 33.10 10.80 0 -27 0 12.90 6.50 0 -27 0 19.80 11.20 0 -27 0 9.10 6.10 0 27 0 12.50 12.40 0 27 0 23.70 10.20 1 -27 0 387.46 32.20 -1 -27 0 403.76 40.40 1 -27 0 387.16 30.20 1 -27 0 365.76 39.20 1 -27 0 448.96 32.60 1 27 0 424.96 39.50 -1 27 0 455.85 43.30 -1 27 0 376.46 32.10 1 27 0 319.67 31.70 -2 -27 0 300.97 33.90 2 -27 0 350.46 29.90 2 -27 0 292.47 30.00 2 -27 0 262.47 39.70 2 -27 0 337.27 31.80 2 27 0 306.27 34.80 -2 27 0 320.67 29.30 -2 27 0 325.57 38.20 2 27 0 361.16 33.70 3 -27 0 70.99 20.90 -3 -27 0 83.19 21.30 3 -27 0 44.00 16.20 3 -27 0 55.19 15.20 3 -27 0 32.70 16.20 -3 27 0 75.89 16.10 3 27 0 50.39 16.90 -3 27 0 53.19 23.80 3 27 0 44.80 16.90 4 -27 0 270.27 39.40 -4 -27 0 252.47 30.60 4 -27 0 331.27 32.10 4 -27 0 210.28 34.20 4 -27 0 223.78 37.70 -4 27 0 234.28 27.70 -4 27 0 227.78 37.40 4 27 0 256.77 35.10 4 27 0 301.17 35.30 -4 27 0 278.37 41.80 5 -27 0 355.46 44.50 -5 -27 0 376.76 37.80 5 -27 0 451.05 42.00 5 27 0 433.86 40.20 -5 27 0 379.36 57.19 5 27 0 418.26 46.00 -5 27 0 374.86 45.60 -5 27 0 397.86 39.20 6 -27 0 39.20 27.80 -6 -27 0 100.29 22.50 6 -27 0 62.39 23.90 -6 27 0 105.89 33.60 6 27 0 76.09 12.40 6 27 0 121.49 13.70 6 27 0 72.59 24.30 7 -27 0 55.09 27.60 -7 -27 0 9.60 14.10 7 -27 0 47.20 30.00 7 27 0 49.00 22.50 7 27 0 45.20 13.50 7 27 0 41.70 13.40 8 -27 0 131.39 42.00 8 27 0 145.29 24.80 8 27 0 170.98 39.80 8 27 0 173.28 26.60 9 -27 0 -35.80 32.50 9 27 0 38.10 18.90 9 27 0 -18.00 28.30 0 -28 0 581.84 35.40 0 -28 0 557.34 50.99 0 -28 0 613.84 35.50 0 -28 0 595.64 41.80 0 28 0 643.54 44.60 0 28 0 610.04 51.39 -1 -28 0 580.54 51.49 1 -28 0 674.03 43.30 1 -28 0 649.74 43.90 1 -28 0 680.23 55.49 1 -28 0 667.03 42.60 1 28 0 600.24 45.80 -1 28 0 588.34 43.80 1 28 0 700.23 53.79 -1 28 0 681.73 55.39 2 -28 0 148.79 22.30 2 -28 0 196.38 24.10 -2 -28 0 183.18 31.60 2 -28 0 146.49 23.60 2 -28 0 202.48 34.30 2 28 0 175.18 30.90 -2 28 0 164.28 24.30 2 28 0 134.79 23.90 -2 28 0 166.88 31.10 3 -28 0 1359.86 90.39 3 -28 0 1325.97 76.49 3 -28 0 1359.26 82.29 -3 -28 0 1340.77 84.69 3 -28 0 1445.76 85.79 -3 28 0 1328.77 77.59 -3 28 0 1378.96 90.09 3 28 0 1386.16 84.69 3 28 0 1380.16 84.39 4 -28 0 430.46 46.60 -4 -28 0 528.05 45.10 4 -28 0 503.95 48.40 4 -28 0 497.95 40.60 4 28 0 550.24 46.60 -4 28 0 475.15 49.30 -4 28 0 506.05 49.00 4 28 0 462.35 46.50 -4 28 0 434.06 40.10 5 -28 0 44.30 18.10 5 -28 0 43.40 21.10 -5 -28 0 43.50 16.70 5 28 0 93.99 24.80 5 28 0 34.60 18.60 -5 28 0 41.60 17.60 -5 28 0 49.50 24.00 -6 -28 0 685.23 51.49 6 -28 0 697.53 67.49 6 -28 0 595.54 54.19 -6 28 0 644.44 66.39 6 28 0 575.04 60.09 6 28 0 664.03 51.99 -7 -28 0 309.77 34.70 7 -28 0 380.46 58.99 7 28 0 342.17 28.30 7 28 0 383.46 56.59 7 28 0 372.06 28.90 8 -28 0 38.30 33.90 8 28 0 38.80 28.50 8 28 0 29.60 16.50 8 28 0 51.69 18.40 9 28 0 292.87 36.20 0 -29 0 20.50 14.10 0 -29 0 6.90 6.90 0 -29 0 15.90 10.40 0 -29 0 14.60 7.10 0 29 0 15.20 10.30 0 29 0 13.10 14.10 1 -29 0 28.20 11.20 1 -29 0 13.70 9.10 1 -29 0 19.20 13.30 1 -29 0 11.50 9.30 -1 -29 0 11.90 11.40 -1 29 0 13.50 13.90 1 29 0 17.30 9.50 -1 29 0 23.50 10.00 1 29 0 -8.90 12.70 2 -29 0 21.90 12.80 2 -29 0 29.40 12.50 -2 -29 0 -8.60 10.70 2 -29 0 13.60 10.30 2 -29 0 29.70 12.70 -2 29 0 9.00 8.90 -2 29 0 2.50 16.80 2 29 0 3.00 12.90 2 29 0 35.90 14.30 3 -29 0 185.98 33.30 3 -29 0 169.28 30.20 3 -29 0 176.68 25.40 -3 -29 0 133.59 28.30 3 -29 0 166.48 28.90 -3 29 0 171.48 26.60 3 29 0 145.99 28.20 -3 29 0 164.38 33.30 3 29 0 187.68 30.70 4 -29 0 122.29 27.50 4 -29 0 137.19 24.50 -4 -29 0 92.09 22.50 -4 29 0 102.39 22.10 4 29 0 137.49 27.80 4 29 0 103.39 25.30 -5 -29 0 6.40 15.10 5 -29 0 21.90 16.80 5 -29 0 39.40 18.90 -5 29 0 28.00 19.20 5 29 0 52.99 18.70 -5 29 0 -6.00 12.40 5 29 0 23.30 17.20 -6 -29 0 62.99 17.70 6 -29 0 26.60 23.70 6 -29 0 43.90 24.10 6 29 0 70.59 21.70 -6 29 0 42.40 28.10 6 29 0 34.00 25.40 -7 -29 0 7.90 15.40 7 -29 0 -32.30 22.60 7 29 0 27.20 10.30 7 29 0 17.40 9.60 7 29 0 36.50 21.50 8 -29 0 -2.50 27.20 8 29 0 36.40 15.30 8 29 0 2.50 13.70 8 29 0 -20.10 20.80 0 -30 0 2557.84 111.69 0 -30 0 2413.16 120.69 0 -30 0 2469.45 111.09 0 -30 0 2441.26 136.59 0 30 0 2330.07 122.69 0 30 0 2551.24 136.69 1 -30 0 31.80 16.10 -1 -30 0 67.99 21.60 1 -30 0 38.80 12.40 1 -30 0 62.29 13.70 1 -30 0 29.80 11.20 -1 30 0 45.10 13.80 1 30 0 30.90 13.00 -1 30 0 14.40 14.90 1 30 0 33.50 16.90 2 -30 0 372.96 42.50 2 -30 0 396.16 36.00 -2 -30 0 417.46 43.50 2 -30 0 434.26 37.70 2 -30 0 423.66 35.40 -2 30 0 393.46 34.60 2 30 0 411.16 38.10 -2 30 0 361.76 49.60 2 30 0 411.66 41.70 -3 -30 0 1120.39 74.69 3 -30 0 1027.10 76.59 3 -30 0 981.00 68.69 3 -30 0 1047.40 70.59 3 -30 0 1001.40 62.79 3 30 0 1023.20 71.39 -3 30 0 1040.60 65.09 3 30 0 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41.40 5 16 -11 99.59 39.90 4 -16 -11 189.88 45.90 -4 -16 11 136.29 38.30 4 16 -11 192.28 47.40 4 16 -11 186.68 48.00 -3 -16 11 -4.10 22.60 3 -16 -11 -1.60 17.90 3 -16 -11 39.80 30.80 3 16 -11 29.50 27.90 3 16 -11 7.40 27.50 2 -16 -11 268.47 51.09 -2 -16 11 226.48 48.30 2 16 -11 275.77 52.79 2 16 -11 235.68 52.49 -1 -16 11 184.28 44.30 1 -16 -11 156.88 45.70 1 16 -11 179.38 48.50 1 16 -11 165.48 44.70 0 -16 11 14.50 25.10 0 -16 -11 44.80 31.00 0 16 -11 18.40 27.70 0 16 -11 -12.70 29.30 -5 -17 11 6.90 29.00 5 -17 -11 5.80 26.80 5 -17 -11 -12.80 15.60 5 17 -11 -31.70 28.40 5 17 -11 -58.99 23.30 4 -17 -11 123.89 38.90 -4 -17 11 152.58 40.90 4 17 -11 113.89 38.50 4 17 -11 114.19 38.10 3 -17 -11 103.99 38.60 -3 -17 11 92.49 36.70 3 17 -11 123.89 41.60 3 17 -11 122.19 42.20 -2 -17 11 96.29 31.90 2 -17 -11 149.19 40.10 2 17 -11 101.09 40.70 2 17 -11 45.70 29.00 1 -17 -11 33.10 32.10 -1 -17 11 -4.10 29.80 1 17 -11 5.90 28.70 1 17 -11 20.50 26.50 0 -17 -11 46.70 35.50 0 -17 11 77.09 33.70 0 17 -11 82.19 36.80 0 17 -11 72.49 36.00 -5 -18 11 459.25 74.99 5 -18 -11 422.16 68.59 5 18 -11 539.35 66.89 5 18 -11 478.55 71.29 -4 -18 11 272.97 58.39 4 -18 -11 340.87 60.09 4 18 -11 292.47 57.39 4 18 -11 359.16 60.19 3 -18 -11 -35.90 30.10 -3 -18 11 4.10 26.90 3 18 -11 -10.70 23.30 3 18 -11 -2.30 24.60 2 -18 -11 309.57 58.89 -2 -18 11 412.46 63.49 2 18 -11 347.87 63.19 2 18 -11 359.76 61.09 1 -18 -11 327.37 59.09 -1 -18 11 437.76 63.99 1 18 -11 352.66 65.39 1 18 -11 312.17 57.89 5 -19 -11 78.49 37.70 -5 -19 11 75.89 35.70 5 19 -11 53.99 39.30 5 19 -11 21.80 33.60 4 -19 -11 -0.10 31.20 -4 -19 11 -14.60 24.10 4 19 -11 15.80 30.10 4 19 -11 -5.80 26.60 -3 -19 11 24.70 26.60 3 -19 -11 48.40 34.90 3 19 -11 39.80 28.40 3 19 -11 14.70 28.00 2 -19 -11 27.10 30.90 -2 -19 11 -2.40 24.50 2 19 -11 -27.70 25.10 2 19 -11 18.70 29.20 -1 -19 11 45.80 31.30 1 -19 -11 54.69 35.70 1 19 -11 -15.30 30.40 1 19 -11 -7.20 31.50 4 -20 -11 172.08 46.30 -4 -20 11 187.78 43.10 4 20 -11 229.58 51.19 4 20 -11 165.58 46.90 3 -20 -11 1.90 32.10 -3 -20 11 -14.30 22.30 3 20 -11 7.70 26.40 3 20 -11 12.60 31.70 2 -20 -11 136.19 40.20 -2 -20 11 163.18 44.50 2 20 -11 127.19 40.70 2 20 -11 129.89 39.00 3 -21 -11 430.16 63.99 -3 -21 11 346.87 61.39 3 21 -11 316.57 66.29 3 21 -11 346.27 63.19 2 -21 -11 55.19 37.30 2 21 -11 110.59 43.50 5 0 -12 149.99 38.50 5 0 -12 220.28 52.39 4 0 -12 460.45 69.69 4 0 -12 461.05 56.59 3 0 -12 90.39 35.30 3 0 -12 79.49 32.20 2 0 -12 261.97 48.60 2 0 -12 328.97 60.89 1 0 -12 352.86 58.89 1 0 -12 322.47 59.69 5 -1 -12 9.10 25.90 5 -1 -12 11.60 28.90 5 1 -12 -2.00 29.90 5 1 -12 21.20 26.30 4 -1 -12 40.40 24.80 4 -1 -12 -1.30 27.40 4 1 -12 -8.60 26.20 4 1 -12 23.50 28.40 3 -1 -12 117.39 41.70 3 -1 -12 -8.20 26.10 3 1 -12 19.40 30.90 3 1 -12 48.90 30.60 2 -1 -12 22.80 27.30 2 -1 -12 68.19 35.70 2 1 -12 38.90 35.40 2 1 -12 93.99 32.50 1 -1 -12 -35.30 26.50 1 -1 -12 12.00 33.10 1 1 -12 9.80 31.50 1 1 -12 12.10 30.30 5 -2 -12 125.89 35.50 5 -2 -12 132.29 42.50 5 2 -12 78.69 34.00 5 2 -12 68.59 40.90 4 -2 -12 174.58 39.80 4 -2 -12 142.09 45.40 4 2 -12 133.09 43.40 4 2 -12 181.58 41.60 3 -2 -12 66.09 33.70 3 -2 -12 32.80 27.10 3 2 -12 14.20 27.20 3 2 -12 33.80 32.50 2 -2 -12 23.00 26.30 2 -2 -12 53.29 37.20 2 2 -12 47.10 33.10 2 2 -12 27.30 28.40 -1 -2 12 138.99 40.50 1 -2 -12 147.89 42.30 1 -2 -12 150.28 37.60 1 2 -12 152.28 41.60 1 2 -12 134.99 45.60 5 -3 -12 267.07 43.30 5 -3 -12 204.98 50.09 5 3 -12 113.49 44.90 5 3 -12 153.28 38.00 4 -3 -12 31.50 30.60 4 -3 -12 8.00 26.90 4 3 -12 27.80 28.50 4 3 -12 -0.10 25.80 3 -3 -12 477.05 73.39 3 -3 -12 521.35 58.39 3 3 -12 823.02 85.39 3 3 -12 472.05 64.49 2 -3 -12 221.68 50.49 2 -3 -12 173.48 40.40 2 3 -12 235.58 48.30 2 3 -12 303.17 56.39 1 -3 -12 27.90 26.70 -1 -3 12 3.60 25.70 1 -3 -12 -38.60 29.60 1 3 -12 13.30 28.40 1 3 -12 -13.60 26.90 5 -4 -12 30.20 27.70 5 -4 -12 15.50 28.80 5 4 -12 -16.50 28.60 5 4 -12 36.80 33.60 4 -4 -12 11.60 24.40 4 -4 -12 -17.60 28.00 4 4 -12 -6.10 25.60 4 4 -12 -32.80 30.70 3 -4 -12 -34.00 23.20 3 -4 -12 -14.50 31.00 3 4 -12 2.10 26.60 3 4 -12 -40.50 29.90 2 -4 -12 -29.60 30.60 2 -4 -12 -4.60 24.10 -2 -4 12 11.30 25.20 2 4 -12 3.80 28.40 2 4 -12 45.60 29.50 1 -4 -12 18.00 29.40 1 4 -12 67.39 35.40 5 -5 -12 194.38 39.60 5 -5 -12 213.38 49.70 5 5 -12 63.19 43.00 5 5 -12 161.28 41.90 4 -5 -12 45.90 35.10 4 -5 -12 33.20 23.20 4 5 -12 -12.20 25.30 4 5 -12 -2.60 28.70 3 -5 -12 440.16 67.39 3 -5 -12 322.77 48.40 3 5 -12 387.36 60.29 3 5 -12 306.27 61.29 2 -5 -12 174.58 43.80 2 -5 -12 155.38 35.70 -2 -5 12 170.18 45.80 2 5 -12 227.48 50.29 2 5 -12 124.89 38.00 5 -6 -12 182.98 49.70 5 -6 -12 154.88 37.20 5 6 -12 125.69 38.20 5 6 -12 117.29 42.60 4 -6 -12 220.38 52.49 4 -6 -12 265.07 45.40 4 6 -12 353.06 64.59 4 6 -12 283.57 52.59 3 -6 -12 76.19 31.00 -3 -6 12 76.29 33.40 3 -6 -12 91.09 35.80 3 6 -12 53.49 33.50 3 6 -12 25.20 34.10 2 -6 -12 66.79 30.90 -2 -6 12 123.49 36.70 2 -6 -12 172.58 44.00 2 6 -12 6.20 34.70 2 6 -12 69.59 32.50 4 -7 -12 -0.30 23.40 4 -7 -12 2.60 33.20 -4 -7 12 57.49 27.90 4 7 -12 29.10 28.30 4 7 -12 12.50 27.30 3 -7 -12 -5.80 26.20 -3 -7 12 -7.20 27.20 3 -7 -12 -4.00 27.00 3 7 -12 23.60 30.30 3 7 -12 -29.70 28.10 2 -7 -12 -34.10 28.60 2 -7 -12 7.40 26.40 -2 -7 12 27.40 28.30 2 7 -12 44.90 31.80 2 7 -12 -19.80 28.80 4 -8 -12 339.77 46.20 -4 -8 12 406.66 63.69 4 -8 -12 360.66 61.89 4 8 -12 311.27 59.59 4 8 -12 339.57 55.49 3 -8 -12 57.89 28.40 3 -8 -12 62.69 35.20 -3 -8 12 16.00 25.20 3 8 -12 -5.50 31.20 3 8 -12 22.90 31.40 2 -8 -12 97.99 38.80 -2 -8 12 119.19 36.40 2 -8 -12 95.39 33.00 2 8 -12 138.49 44.30 2 8 -12 153.98 42.10 4 -9 -12 51.59 25.90 4 -9 -12 28.90 32.10 -4 -9 12 1.40 25.70 4 9 -12 -46.80 23.60 4 9 -12 22.60 27.40 -3 -9 12 144.99 42.40 3 -9 -12 117.19 43.70 3 -9 -12 168.08 36.90 3 9 -12 230.68 51.79 3 9 -12 224.98 52.49 3 -10 -12 7.90 26.50 -3 -10 12 21.50 29.70 3 -10 -12 -46.50 28.30 3 10 -12 4.00 30.10 3 10 -12 -25.10 29.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 46731 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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_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 Ho1 Ho 0.15852(3) 0.57031(2) 0.18066(2) 0.02010(8) Uani 1 1 d . . . . . O1 O 0.1422(4) 0.53210(9) 0.9558(4) 0.0291(8) Uani 1 1 d . . . . . O2 O 0.0617(5) 0.58848(9) 0.9262(4) 0.0324(8) Uani 1 1 d . . . . . O3 O 0.3158(5) 0.60633(9) 0.3851(4) 0.0347(9) Uani 1 1 d . . . . . O4 O -0.0836(4) 0.53884(10) 0.1101(4) 0.0334(8) Uani 1 1 d . . . . . O5 O 0.2345(5) 0.63346(10) 0.1703(4) 0.0372(9) Uani 1 1 d . . . . . O6 O 0.4055(5) 0.56491(12) 0.1592(5) 0.0511(11) Uani 1 1 d . . . . . O7 O 0.6338(7) 0.5530(2) 0.1318(8) 0.098(2) Uani 1 1 d . . . . . N1 N 0.2512(5) 0.51154(11) 0.3058(4) 0.0258(9) Uani 1 1 d . . . . . N2 N 0.0894(5) 0.55847(10) 0.4201(4) 0.0224(8) Uani 1 1 d . . . . . N3 N -0.0490(5) 0.60932(11) 0.2299(4) 0.0275(9) Uani 1 1 d . . . . . N4 N 0.5115(6) 0.73326(12) 0.5014(5) 0.0355(11) Uani 1 1 d . . . . . N5 N 0.2357(6) 0.77006(14) 0.1821(6) 0.0460(13) Uani 1 1 d . . . . . N6 N 0.8014(6) 0.67430(13) 0.7220(5) 0.0394(11) Uani 1 1 d . . . . . C1 C 0.3216(6) 0.48722(15) 0.2388(6) 0.0345(13) Uani 1 1 d . . . . . C2 C 0.1653(6) 0.53232(12) 0.5117(5) 0.0225(10) Uani 1 1 d . . . . . C3 C 0.3907(7) 0.45579(16) 0.3083(6) 0.0382(13) Uani 1 1 d . . . . . C4 C 0.0953(6) 0.55917(13) 0.8748(5) 0.0261(11) Uani 1 1 d . . . . . C5 C 0.0867(6) 0.55758(14) 0.7134(5) 0.0260(11) Uani 1 1 d . . . . . C6 C 0.2467(6) 0.50500(13) 0.4451(5) 0.0266(11) Uani 1 1 d . . . . . C7 C 0.0033(6) 0.58427(13) 0.6182(5) 0.0252(10) Uani 1 1 d . . . . . C8 C 0.0085(6) 0.58392(13) 0.4717(5) 0.0243(10) Uani 1 1 d . . . . . C9 C 0.1668(6) 0.53094(14) 0.6602(5) 0.0264(11) Uani 1 1 d . . . . . C10 C 0.3893(7) 0.44919(15) 0.4542(7) 0.0395(14) Uani 1 1 d . . . . . C11 C 0.3243(6) 0.70141(15) 0.3069(6) 0.0352(13) Uani 1 1 d . . . . . C12 C 0.3816(6) 0.66875(14) 0.3735(6) 0.0303(12) Uani 1 1 d . . . . . C13 C 0.5038(6) 0.66808(14) 0.5043(6) 0.0293(11) Uani 1 1 d . . . . . C14 C -0.0741(6) 0.61102(13) 0.3637(5) 0.0254(11) Uani 1 1 d . . . . . C15 C 0.3156(6) 0.47410(13) 0.5236(6) 0.0321(12) Uani 1 1 d . . . . . C16 C -0.2496(9) 0.66152(18) 0.2856(8) 0.0538(18) Uani 1 1 d . . . . . C17 C 0.5686(6) 0.70111(14) 0.5611(6) 0.0306(12) Uani 1 1 d . . . . . C18 C 0.3064(6) 0.63414(14) 0.3042(6) 0.0301(12) Uani 1 1 d . . . . . C19 C 0.3341(7) 0.76956(15) 0.3173(6) 0.0375(13) Uani 1 1 d . . . . . C20 C 0.7388(8) 0.73513(17) 0.7742(7) 0.0513(17) Uani 1 1 d . . . . . C21 C -0.1250(8) 0.63258(16) 0.1233(6) 0.0434(15) Uani 1 1 d . . . . . C22 C -0.1731(8) 0.63689(16) 0.3962(7) 0.0422(15) Uani 1 1 d . . . . . C23 C 0.9749(9) 0.7075(2) 0.9193(7) 0.0599(19) Uani 1 1 d . . . . . C24 C -0.2252(8) 0.65895(18) 0.1481(7) 0.0525(18) Uani 1 1 d . . . . . C25 C 0.3925(7) 0.73333(15) 0.3784(6) 0.0350(13) Uani 1 1 d . . . . . C26 C 0.1880(8) 0.80287(18) 0.1224(8) 0.0525(17) Uani 1 1 d . . . . . C27 C 0.3863(8) 0.80065(16) 0.4028(8) 0.0519(17) Uani 1 1 d . . . . . C28 C 0.9337(8) 0.6766(2) 0.8343(7) 0.0497(17) Uani 1 1 d . . . . . C29 C 0.8736(9) 0.7369(2) 0.8929(8) 0.064(2) Uani 1 1 d . . . . . C30 C 0.7102(7) 0.70369(15) 0.6921(6) 0.0336(12) Uani 1 1 d . . . . . C31 C 0.3372(9) 0.83402(18) 0.3394(9) 0.062(2) Uani 1 1 d . . . . . C32 C 0.2385(9) 0.83483(19) 0.1957(9) 0.062(2) Uani 1 1 d . . . . . C33 C 0.5083(9) 0.5675(2) 0.1000(9) 0.063(2) Uani 1 1 d . . . . . 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 Ho1 0.02215(13) 0.02366(12) 0.01458(11) -0.00177(9) 0.00538(8) 0.00086(9) O1 0.043(2) 0.0284(18) 0.0176(17) 0.0021(14) 0.0107(16) 0.0033(16) O2 0.049(2) 0.0293(19) 0.0185(17) -0.0016(15) 0.0082(16) 0.0068(17) O3 0.042(2) 0.0279(19) 0.031(2) -0.0019(16) 0.0058(17) -0.0035(16) O4 0.028(2) 0.036(2) 0.037(2) -0.0084(16) 0.0098(17) -0.0035(16) O5 0.048(3) 0.033(2) 0.0246(19) -0.0052(15) 0.0002(17) -0.0082(17) O6 0.032(2) 0.064(3) 0.065(3) -0.010(2) 0.026(2) 0.001(2) O7 0.051(4) 0.135(6) 0.125(5) 0.023(5) 0.050(4) 0.027(4) N1 0.029(2) 0.032(2) 0.018(2) -0.0029(17) 0.0088(17) 0.0050(18) N2 0.025(2) 0.024(2) 0.0184(19) -0.0010(16) 0.0063(17) 0.0026(16) N3 0.031(2) 0.030(2) 0.024(2) 0.0043(17) 0.0112(18) 0.0075(18) N4 0.036(3) 0.034(2) 0.034(3) -0.005(2) 0.006(2) -0.005(2) N5 0.045(3) 0.046(3) 0.044(3) 0.007(2) 0.007(2) 0.002(2) N6 0.040(3) 0.046(3) 0.030(3) -0.001(2) 0.008(2) -0.001(2) C1 0.032(3) 0.036(3) 0.032(3) -0.010(2) 0.004(2) 0.010(2) C2 0.022(3) 0.024(2) 0.022(2) -0.0023(19) 0.006(2) -0.0028(19) C3 0.037(3) 0.040(3) 0.034(3) -0.006(2) 0.006(3) 0.011(3) C4 0.031(3) 0.030(3) 0.017(2) -0.003(2) 0.006(2) -0.003(2) C5 0.030(3) 0.032(3) 0.016(2) -0.0047(19) 0.005(2) -0.008(2) C6 0.027(3) 0.030(3) 0.021(2) -0.004(2) 0.006(2) -0.001(2) C7 0.026(3) 0.029(3) 0.021(2) -0.004(2) 0.007(2) -0.004(2) C8 0.026(3) 0.028(2) 0.019(2) -0.0019(19) 0.006(2) 0.002(2) C9 0.028(3) 0.029(3) 0.020(2) 0.0000(19) 0.005(2) 0.000(2) C10 0.043(4) 0.032(3) 0.041(3) 0.001(2) 0.009(3) 0.010(3) C11 0.033(3) 0.035(3) 0.035(3) -0.001(2) 0.006(2) -0.006(2) C12 0.030(3) 0.033(3) 0.028(3) -0.007(2) 0.008(2) -0.006(2) C13 0.025(3) 0.033(3) 0.031(3) -0.005(2) 0.009(2) -0.002(2) C14 0.033(3) 0.022(2) 0.022(2) -0.0009(19) 0.009(2) 0.005(2) C15 0.033(3) 0.026(3) 0.035(3) 0.000(2) 0.006(2) 0.005(2) C16 0.067(5) 0.049(4) 0.056(4) 0.019(3) 0.035(4) 0.027(3) C17 0.032(3) 0.033(3) 0.026(3) -0.006(2) 0.007(2) -0.003(2) C18 0.026(3) 0.032(3) 0.033(3) -0.008(2) 0.009(2) -0.005(2) C19 0.034(3) 0.035(3) 0.043(3) 0.004(3) 0.011(3) 0.002(2) C20 0.051(4) 0.049(4) 0.046(4) -0.013(3) 0.002(3) -0.010(3) C21 0.052(4) 0.047(3) 0.034(3) 0.017(3) 0.018(3) 0.019(3) C22 0.052(4) 0.042(3) 0.039(3) 0.008(3) 0.023(3) 0.018(3) C23 0.048(4) 0.083(5) 0.040(4) 0.004(4) -0.001(3) -0.013(4) C24 0.059(4) 0.060(4) 0.047(4) 0.031(3) 0.029(3) 0.034(3) C25 0.034(3) 0.035(3) 0.035(3) 0.004(2) 0.008(3) -0.002(2) C26 0.052(4) 0.052(4) 0.057(4) 0.014(3) 0.021(3) 0.010(3) C27 0.053(4) 0.028(3) 0.070(5) -0.007(3) 0.010(4) 0.002(3) C28 0.041(4) 0.078(5) 0.029(3) 0.011(3) 0.007(3) -0.007(3) C29 0.059(5) 0.069(5) 0.050(4) -0.016(4) -0.004(4) -0.019(4) C30 0.036(3) 0.035(3) 0.029(3) -0.005(2) 0.009(2) -0.004(2) C31 0.059(5) 0.039(4) 0.084(6) -0.001(4) 0.013(4) 0.002(3) C32 0.059(5) 0.050(4) 0.084(6) 0.019(4) 0.031(4) 0.010(4) C33 0.042(4) 0.083(5) 0.073(5) 0.014(4) 0.029(4) 0.017(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Ho Ho -0.2175 4.6783 '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 O6 Ho1 O4 139.05(14) . . ? O6 Ho1 O2 90.91(15) . 1_554 ? O4 Ho1 O2 79.47(13) . 1_554 ? O6 Ho1 O3 76.54(15) . . ? O4 Ho1 O3 139.74(13) . . ? O2 Ho1 O3 127.00(12) 1_554 . ? O6 Ho1 O5 78.18(15) . . ? O4 Ho1 O5 134.29(13) . . ? O2 Ho1 O5 73.60(12) 1_554 . ? O3 Ho1 O5 53.51(12) . . ? O6 Ho1 N1 76.62(15) . . ? O4 Ho1 N1 81.78(13) . . ? O2 Ho1 N1 133.74(12) 1_554 . ? O3 Ho1 N1 93.57(12) . . ? O5 Ho1 N1 142.48(13) . . ? O6 Ho1 N3 148.74(15) . . ? O4 Ho1 N3 71.08(13) . . ? O2 Ho1 N3 87.19(13) 1_554 . ? O3 Ho1 N3 79.81(14) . . ? O5 Ho1 N3 71.36(14) . . ? N1 Ho1 N3 125.33(13) . . ? O6 Ho1 N2 123.20(15) . . ? O4 Ho1 N2 74.77(13) . . ? O2 Ho1 N2 145.88(13) 1_554 . ? O3 Ho1 N2 67.50(13) . . ? O5 Ho1 N2 109.85(12) . . ? N1 Ho1 N2 63.88(13) . . ? N3 Ho1 N2 63.58(13) . . ? O6 Ho1 O1 72.62(14) . 1_554 ? O4 Ho1 O1 69.92(12) . 1_554 ? O2 Ho1 O1 52.84(11) 1_554 1_554 ? O3 Ho1 O1 149.12(13) . 1_554 ? O5 Ho1 O1 116.93(12) . 1_554 ? N1 Ho1 O1 81.03(11) . 1_554 ? N3 Ho1 O1 127.90(13) . 1_554 ? N2 Ho1 O1 133.01(12) . 1_554 ? O6 Ho1 C18 76.08(15) . . ? O4 Ho1 C18 144.63(14) . . ? O2 Ho1 C18 100.04(14) 1_554 . ? O3 Ho1 C18 27.03(14) . . ? O5 Ho1 C18 26.47(13) . . ? N1 Ho1 C18 118.98(15) . . ? N3 Ho1 C18 73.56(15) . . ? N2 Ho1 C18 88.69(14) . . ? O1 Ho1 C18 137.24(14) 1_554 . ? O6 Ho1 C4 79.14(16) . 1_554 ? O4 Ho1 C4 74.81(14) . 1_554 ? O2 Ho1 C4 26.44(13) 1_554 1_554 ? O3 Ho1 C4 142.90(14) . 1_554 ? O5 Ho1 C4 94.35(13) . 1_554 ? N1 Ho1 C4 107.56(13) . 1_554 ? N3 Ho1 C4 109.54(14) . 1_554 ? N2 Ho1 C4 149.30(14) . 1_554 ? O1 Ho1 C4 26.53(12) 1_554 1_554 ? C18 Ho1 C4 119.12(15) . 1_554 ? C4 O1 Ho1 89.8(3) . 1_556 ? C4 O2 Ho1 95.1(3) . 1_556 ? C18 O3 Ho1 92.3(3) . . ? C18 O5 Ho1 92.7(3) . . ? C33 O6 Ho1 156.3(5) . . ? C1 N1 C6 118.9(4) . . ? C1 N1 Ho1 119.4(3) . . ? C6 N1 Ho1 121.4(3) . . ? C2 N2 C8 119.2(4) . . ? C2 N2 Ho1 119.5(3) . . ? C8 N2 Ho1 119.1(3) . . ? C21 N3 C14 119.3(4) . . ? C21 N3 Ho1 118.1(3) . . ? C14 N3 Ho1 122.1(3) . . ? C17 N4 C25 118.5(5) . . ? C19 N5 C26 117.1(6) . . ? C30 N6 C28 117.1(5) . . ? N1 C1 C3 122.4(5) . . ? N2 C2 C9 122.1(4) . . ? N2 C2 C6 115.6(4) . . ? C9 C2 C6 122.2(4) . . ? C10 C3 C1 118.9(5) . . ? O2 C4 O1 121.7(4) . . ? O2 C4 C5 118.4(4) . . ? O1 C4 C5 119.9(4) . . ? O2 C4 Ho1 58.5(2) . 1_556 ? O1 C4 Ho1 63.7(2) . 1_556 ? C5 C4 Ho1 169.6(4) . 1_556 ? C7 C5 C9 120.0(4) . . ? C7 C5 C4 119.3(5) . . ? C9 C5 C4 120.6(5) . . ? N1 C6 C15 122.2(5) . . ? N1 C6 C2 116.4(4) . . ? C15 C6 C2 121.4(4) . . ? C5 C7 C8 118.1(5) . . ? N2 C8 C7 122.2(4) . . ? N2 C8 C14 115.8(4) . . ? C7 C8 C14 122.1(4) . . ? C5 C9 C2 118.4(4) . . ? C15 C10 C3 118.9(5) . . ? C25 C11 C12 117.3(5) . . ? C11 C12 C13 120.6(5) . . ? C11 C12 C18 118.8(5) . . ? C13 C12 C18 120.5(5) . . ? C12 C13 C17 117.3(5) . . ? N3 C14 C22 121.5(5) . . ? N3 C14 C8 116.0(4) . . ? C22 C14 C8 122.6(5) . . ? C6 C15 C10 118.7(5) . . ? C24 C16 C22 118.9(5) . . ? N4 C17 C13 123.1(5) . . ? N4 C17 C30 114.7(4) . . ? C13 C17 C30 122.3(5) . . ? O5 C18 O3 121.5(5) . . ? O5 C18 C12 119.7(5) . . ? O3 C18 C12 118.8(5) . . ? O5 C18 Ho1 60.9(3) . . ? O3 C18 Ho1 60.6(3) . . ? C12 C18 Ho1 177.9(4) . . ? N5 C19 C27 124.1(6) . . ? N5 C19 C25 116.5(5) . . ? C27 C19 C25 119.3(5) . . ? C29 C20 C30 118.2(6) . . ? N3 C21 C24 122.1(5) . . ? C14 C22 C16 118.9(5) . . ? C29 C23 C28 119.4(6) . . ? C16 C24 C21 119.2(5) . . ? N4 C25 C11 122.9(5) . . ? N4 C25 C19 116.3(5) . . ? C11 C25 C19 120.8(5) . . ? N5 C26 C32 122.7(7) . . ? C19 C27 C31 117.9(6) . . ? N6 C28 C23 122.6(7) . . ? C23 C29 C20 118.3(6) . . ? N6 C30 C20 124.2(5) . . ? N6 C30 C17 116.1(5) . . ? C20 C30 C17 119.7(5) . . ? C27 C31 C32 118.3(7) . . ? C26 C32 C31 119.8(6) . . ? O7 C33 O6 128.5(8) . . ? 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 Ho1 O6 2.270(4) . ? Ho1 O4 2.370(4) . ? Ho1 O2 2.410(3) 1_554 ? Ho1 O3 2.436(4) . ? Ho1 O5 2.442(4) . ? Ho1 N1 2.501(4) . ? Ho1 N3 2.487(4) . ? Ho1 N2 2.546(4) . ? Ho1 O1 2.523(3) 1_554 ? Ho1 C18 2.793(5) . ? Ho1 C4 2.816(5) 1_554 ? O1 C4 1.258(6) . ? O1 Ho1 2.523(3) 1_556 ? O2 C4 1.259(6) . ? O2 Ho1 2.410(3) 1_556 ? O3 C18 1.270(6) . ? O5 C18 1.246(6) . ? O6 C33 1.203(8) . ? O7 C33 1.196(8) . ? N1 C1 1.352(6) . ? N1 C6 1.350(6) . ? N2 C2 1.345(6) . ? N2 C8 1.357(6) . ? N3 C21 1.351(7) . ? N3 C14 1.347(6) . ? N4 C17 1.352(7) . ? N4 C25 1.332(7) . ? N5 C19 1.328(7) . ? N5 C26 1.355(8) . ? N6 C30 1.338(7) . ? N6 C28 1.345(8) . ? C1 C3 1.390(8) . ? C2 C9 1.401(6) . ? C2 C6 1.484(7) . ? C3 C10 1.405(8) . ? C4 C5 1.507(6) . ? C4 Ho1 2.816(5) 1_556 ? C5 C7 1.399(7) . ? C5 C9 1.391(7) . ? C6 C15 1.406(7) . ? C7 C8 1.399(7) . ? C8 C14 1.470(7) . ? C10 C15 1.397(8) . ? C11 C25 1.409(8) . ? C11 C12 1.391(8) . ? C12 C13 1.395(7) . ? C12 C18 1.506(7) . ? C13 C17 1.392(7) . ? C14 C22 1.392(7) . ? C16 C24 1.380(9) . ? C16 C22 1.408(8) . ? C17 C30 1.498(7) . ? C19 C27 1.407(8) . ? C19 C25 1.493(8) . ? C20 C29 1.392(9) . ? C20 C30 1.382(8) . ? C21 C24 1.385(8) . ? C23 C29 1.388(11) . ? C23 C28 1.385(10) . ? C26 C32 1.380(10) . ? C27 C31 1.388(9) . ? C31 C32 1.393(10) . ?