#------------------------------------------------------------------------------ #$Date: 2021-09-07 02:10:07 +0300 (Tue, 07 Sep 2021) $ #$Revision: 268987 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/82/7708224.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_7708224 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 'C18 Ho N3 O6' _chemical_formula_sum 'C18 Ho N3 O6' _chemical_formula_weight 519.14 _chemical_melting_point ? _chemical_name_common 'Holmium 2,2':6',2''-terpyridine-4'-carboxyli' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/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 125.173(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.943(3) _cell_length_b 9.4929(16) _cell_length_c 11.8703(19) _cell_measurement_reflns_used 9942 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 55.056 _cell_measurement_theta_min 5.112 _cell_volume 1652.7(5) _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 293(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.987 _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 0.0402 _diffrn_reflns_av_unetI/netI 0.0207 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 15216 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.577 _diffrn_reflns_theta_min 2.556 _exptl_absorpt_coefficient_mu 4.831 _exptl_absorpt_correction_T_max 0.679 _exptl_absorpt_correction_T_min 0.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SHELTXPREP _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.086 _exptl_crystal_description block _exptl_crystal_F_000 976 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.825 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.117 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 129 _refine_ls_number_reflns 1896 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.095 _refine_ls_R_factor_all 0.0198 _refine_ls_R_factor_gt 0.0189 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+3.5236P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.0546 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1848 _reflns_number_total 1896 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01618k2.cif _cod_data_source_block HoTPC2 _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 'C 2/c' _cod_database_code 7708224 _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 C2/c REM Old TITL SAVE in C2/c REM SHELXT solution in C2/c REM R1 0.079, Rweak 0.006, Alpha 0.028, Orientation as input REM Formula found by SHELXT: C20 N2 O5 Ho CELL 0.71073 17.9429 9.4929 11.8703 90.000 125.173 90.000 ZERR 4.000 0.0030 0.0016 0.0019 0.000 0.005 0.000 LATT 7 SYMM -X, Y, 1/2-Z SFAC C N O HO UNIT 72 12 24 4 L.S. 20 BOND $H ACTA LIST 6 FMAP 2 PLAN 20 WGHT 0.033600 3.523600 FVAR 0.28567 HO1 4 0.500000 -0.158241 0.750000 10.50000 0.02300 0.00661 = 0.02477 0.00000 0.01684 0.00000 N1 2 0.500000 0.577518 0.750000 10.50000 0.02045 0.00995 = 0.02112 0.00000 0.01378 0.00000 N2 2 0.590359 0.733529 0.677540 11.00000 0.02569 0.01204 = 0.03094 0.00167 0.01979 0.00010 O1 3 0.484267 0.063993 0.827426 11.00000 0.05260 0.01049 = 0.04085 -0.00053 0.03546 -0.00026 O2 3 0.396531 -0.226903 0.511918 11.00000 0.04017 0.03682 = 0.03648 -0.00890 0.01657 0.00488 O3 3 0.338593 -0.079693 0.582645 11.00000 0.04005 0.04730 = 0.04463 0.00244 0.02477 0.01491 C1 1 0.545094 0.505864 0.708653 11.00000 0.02126 0.01014 = 0.02065 0.00101 0.01174 0.00094 C2 1 0.500000 0.127603 0.750000 10.50000 0.03137 0.01235 = 0.02797 0.00000 0.01732 0.00000 C3 1 0.500000 0.286059 0.750000 10.50000 0.02626 0.00959 = 0.02473 0.00000 0.01497 0.00000 C4 1 0.595754 0.592796 0.669038 11.00000 0.02058 0.01154 = 0.02200 -0.00052 0.01269 -0.00069 C5 1 0.544677 0.358829 0.703642 11.00000 0.02743 0.01161 = 0.02702 -0.00034 0.01774 0.00033 C6 1 0.333481 -0.154890 0.492983 11.00000 0.03239 0.02861 = 0.03173 0.00168 0.01571 0.00376 C7 1 0.634448 0.817563 0.642343 11.00000 0.03716 0.01570 = 0.04436 0.00223 0.03021 -0.00335 C8 1 0.647451 0.532290 0.628401 11.00000 0.03153 0.02082 = 0.03266 0.00027 0.02329 0.00350 C9 1 0.695191 0.620013 0.596212 11.00000 0.03615 0.02657 = 0.04122 0.00308 0.02983 0.00492 C10 1 0.687687 0.764644 0.601718 11.00000 0.04143 0.02562 = 0.04623 0.00313 0.03528 -0.00185 HKLF 4 REM SAVE_a.res in C2/c REM R1 = 0.0189 for 1848 Fo > 4sig(Fo) and 0.0198 for all 1896 data REM 129 parameters refined using 0 restraints END WGHT 0.0288 3.7734 REM Highest difference peak 0.825, deepest hole -0.583, 1-sigma level 0.117 Q1 1 0.5677 0.3068 0.6637 11.00000 0.05 0.83 Q2 1 0.6462 0.4362 0.6200 11.00000 0.05 0.81 Q3 1 0.7216 0.8327 0.5856 11.00000 0.05 0.76 Q4 1 0.6272 0.9058 0.6448 11.00000 0.05 0.73 Q5 1 0.2688 -0.1442 0.3947 11.00000 0.05 0.70 Q6 1 0.7298 0.5783 0.5660 11.00000 0.05 0.68 Q7 1 0.4294 -0.1822 0.6213 11.00000 0.05 0.60 Q8 1 0.5715 0.5504 0.6984 11.00000 0.05 0.42 Q9 1 0.5313 0.3335 0.7321 11.00000 0.05 0.39 Q10 1 0.5401 -0.0640 0.8550 11.00000 0.05 0.39 Q11 1 0.4613 -0.0340 0.7733 11.00000 0.05 0.35 Q12 1 0.5359 0.7603 0.6319 11.00000 0.05 0.32 Q13 1 0.5291 0.4382 0.6745 11.00000 0.05 0.32 Q14 1 0.3767 -0.1616 0.5543 11.00000 0.05 0.32 Q15 1 0.6043 0.5471 0.6031 11.00000 0.05 0.32 Q16 1 0.5192 0.2134 0.7877 11.00000 0.05 0.32 Q17 1 0.4521 0.0998 0.8514 11.00000 0.05 0.31 Q18 1 0.5290 0.8458 0.5738 11.00000 0.05 0.31 Q19 1 0.4325 -0.3353 0.6173 11.00000 0.05 0.30 Q20 1 0.7617 0.8534 0.6575 11.00000 0.05 0.30 ; _shelx_res_checksum 24044 _shelx_hkl_file ; -4 0 0 2133.79 96.49 4 0 0 2099.29 96.49 -4 0 0 2015.60 96.09 -4 0 0 2061.09 95.09 4 0 0 2177.68 95.19 4 0 0 2172.18 96.39 6 0 0 6780.02 303.27 -6 0 0 6012.60 302.57 -6 0 0 7055.29 301.67 6 0 0 7024.80 301.67 6 0 0 7013.90 303.77 -6 0 0 6637.84 303.47 8 0 0 2785.82 128.69 -8 0 0 2834.72 128.79 -8 0 0 2759.72 131.29 -8 0 0 2535.35 130.09 8 0 0 3112.79 131.79 8 0 0 2947.41 130.99 10 0 0 2467.35 120.29 -10 0 0 2471.95 120.39 10 0 0 3047.99 124.79 -10 0 0 2648.64 122.59 10 0 0 2774.12 123.09 -10 0 0 2347.17 123.19 12 0 0 2019.40 97.59 -12 0 0 1877.61 95.99 12 0 0 2122.09 97.09 -12 0 0 2061.79 98.29 12 0 0 1948.51 93.89 -12 0 0 2001.70 94.29 14 0 0 751.72 40.70 -14 0 0 688.73 41.70 -14 0 0 711.03 38.50 16 0 0 462.85 28.30 -16 0 0 439.16 30.90 16 0 0 434.96 29.10 18 0 0 460.45 29.00 18 0 0 407.76 29.50 -1 -1 0 868.71 38.80 1 -1 0 792.12 38.70 -1 -1 0 841.12 38.50 1 -1 0 920.71 38.70 -1 -1 0 875.51 38.70 -1 1 0 827.22 38.60 1 1 0 914.21 38.70 1 1 0 852.91 38.50 1 1 0 841.42 38.70 -1 1 0 866.91 38.30 -1 1 0 794.92 38.60 1 1 0 826.02 38.80 -3 -1 0 864.21 42.40 3 -1 0 980.60 42.90 3 -1 0 934.61 42.50 -3 -1 0 928.61 43.20 -3 -1 0 944.91 42.70 -3 1 0 921.41 43.00 3 1 0 1014.30 42.60 3 1 0 900.81 43.10 -3 1 0 834.42 42.50 -3 1 0 884.81 42.30 3 1 0 939.01 42.60 5 -1 0 2113.89 89.79 5 -1 0 1917.21 89.29 5 -1 0 1904.41 88.79 -5 -1 0 1802.12 89.79 -5 -1 0 1784.92 88.99 -5 1 0 1990.00 88.09 -5 1 0 1874.11 89.19 -5 1 0 2004.10 89.89 5 1 0 2102.09 88.59 -7 -1 0 1882.31 95.09 -7 -1 0 1960.20 95.99 7 -1 0 2025.70 95.89 7 -1 0 2043.50 95.59 7 -1 0 2068.39 94.89 -7 -1 0 2033.40 94.19 -7 1 0 1981.10 95.99 7 1 0 2222.18 94.39 -7 1 0 2008.70 93.59 7 1 0 2105.89 95.59 -7 1 0 2235.68 96.09 -9 -1 0 686.33 37.30 -9 -1 0 731.83 35.20 9 -1 0 707.23 36.70 -9 -1 0 647.94 36.10 9 -1 0 691.23 35.70 9 -1 0 640.74 36.70 9 1 0 678.63 34.70 -9 1 0 643.44 36.80 -9 1 0 715.13 34.40 9 1 0 716.43 37.70 9 1 0 677.53 36.50 -9 1 0 776.42 37.20 11 -1 0 735.13 37.90 -11 -1 0 602.14 34.50 11 -1 0 622.74 36.30 -11 -1 0 716.63 37.00 11 -1 0 633.24 35.40 -11 -1 0 652.13 37.40 11 1 0 732.63 38.50 11 1 0 638.84 36.20 -11 1 0 718.53 36.90 11 1 0 613.84 34.10 -11 1 0 710.23 34.40 -11 1 0 640.94 37.40 13 -1 0 566.94 32.30 -13 -1 0 471.45 31.40 13 -1 0 538.15 30.80 -13 -1 0 590.64 33.80 -13 -1 0 525.15 30.10 13 1 0 538.85 36.80 -13 1 0 547.55 29.40 -13 1 0 529.15 33.20 -13 1 0 569.84 32.40 13 1 0 510.35 29.20 13 1 0 481.85 30.90 -15 -1 0 179.18 17.00 15 -1 0 185.28 16.60 15 -1 0 183.28 15.60 -15 1 0 208.78 15.60 15 1 0 199.18 16.60 15 1 0 173.88 14.10 -17 -1 0 184.08 19.70 17 -1 0 180.08 16.60 17 -1 0 210.08 18.80 17 1 0 226.68 18.40 19 -1 0 59.99 11.50 19 -1 0 56.49 12.30 19 1 0 48.80 10.10 19 1 0 47.30 9.70 0 -2 0 1452.45 62.69 0 2 0 1375.96 62.09 0 2 0 1351.16 62.49 0 2 0 1333.97 62.49 0 2 0 1343.97 62.49 -2 -2 0 259.97 13.70 2 -2 0 275.27 13.60 -2 -2 0 249.18 13.20 -2 -2 0 270.07 13.90 2 -2 0 269.37 13.70 2 2 0 283.27 13.40 2 2 0 260.67 13.90 2 2 0 265.07 13.50 -2 2 0 244.78 12.80 -2 2 0 249.88 13.50 -2 2 0 261.67 13.30 2 2 0 278.47 13.70 -4 -2 0 32.70 3.30 -4 -2 0 33.10 3.70 -4 -2 0 31.40 3.40 4 -2 0 31.10 3.20 4 -2 0 33.30 3.50 4 -2 0 41.60 3.80 4 2 0 34.20 3.20 -4 2 0 31.30 3.30 4 2 0 33.10 3.40 -4 2 0 28.30 3.00 4 2 0 36.40 3.80 4 2 0 38.20 3.90 6 -2 0 18.60 3.10 -6 -2 0 18.60 3.60 -6 -2 0 14.30 3.20 6 -2 0 10.40 2.70 6 -2 0 19.70 3.70 -6 -2 0 16.00 3.20 6 2 0 21.40 4.00 -6 2 0 9.80 2.40 6 2 0 11.60 2.50 6 2 0 11.10 3.20 -6 2 0 14.70 2.50 6 2 0 17.60 3.00 -8 -2 0 321.87 19.70 -8 -2 0 309.97 18.80 -8 -2 0 306.07 18.10 8 -2 0 294.87 18.80 8 -2 0 280.57 17.90 8 -2 0 319.47 19.30 8 2 0 300.97 18.30 -8 2 0 339.17 17.20 8 2 0 324.47 19.80 8 2 0 351.96 18.10 -8 2 0 325.47 18.90 10 -2 0 1086.49 53.69 -10 -2 0 1030.70 52.89 10 -2 0 901.21 51.29 -10 -2 0 980.20 53.19 10 -2 0 985.10 52.89 -10 -2 0 1057.09 51.89 10 2 0 1141.19 54.59 10 2 0 952.30 52.09 -10 2 0 1141.39 53.59 10 2 0 1161.18 51.69 -10 2 0 1061.29 50.29 12 -2 0 270.37 19.80 -12 -2 0 310.17 20.90 12 -2 0 265.17 20.50 -12 -2 0 291.07 18.90 12 -2 0 268.37 18.50 -12 -2 0 249.78 19.40 12 2 0 261.77 19.00 12 2 0 279.77 17.70 12 2 0 286.67 21.00 -12 2 0 286.27 17.00 -12 2 0 263.07 19.40 -14 -2 0 101.89 12.50 14 -2 0 85.19 12.40 14 -2 0 72.59 10.30 14 2 0 73.49 9.10 -14 2 0 72.69 9.40 14 2 0 84.09 11.30 16 -2 0 144.19 14.60 -16 -2 0 146.19 16.50 16 -2 0 126.49 15.10 16 2 0 147.09 13.30 -16 2 0 131.59 13.80 16 2 0 137.99 14.70 18 -2 0 41.20 10.80 18 -2 0 26.50 8.80 -18 -2 0 42.20 11.80 18 2 0 59.69 11.10 18 2 0 35.60 8.40 -1 -3 0 5806.82 248.18 -1 -3 0 5504.45 248.28 -1 3 0 5133.89 247.58 1 3 0 5718.23 248.28 3 -3 0 1356.46 66.59 3 -3 0 1322.67 66.79 -3 -3 0 1495.45 66.79 -3 -3 0 1517.95 66.49 -3 -3 0 1374.66 66.79 -3 -3 0 1475.25 67.19 -3 3 0 1508.55 66.39 3 3 0 1451.15 67.29 -3 3 0 1408.46 66.59 -3 3 0 1482.05 65.59 3 3 0 1475.65 66.39 3 3 0 1407.26 66.69 -5 -3 0 2741.03 124.89 5 -3 0 2739.63 124.99 -5 -3 0 2634.64 125.09 5 -3 0 2641.34 124.59 -5 -3 0 2717.53 125.09 5 -3 0 2683.13 125.09 5 3 0 3035.00 124.79 -5 3 0 2711.23 124.09 5 3 0 2615.94 124.79 -5 3 0 2710.33 124.59 5 3 0 2816.62 125.89 5 3 0 2807.22 124.79 -7 -3 0 3719.33 165.38 7 -3 0 3520.15 164.08 -7 -3 0 3539.85 164.68 7 -3 0 3505.85 164.78 7 -3 0 3435.76 164.68 -7 -3 0 3733.73 164.48 7 3 0 3761.42 163.98 7 3 0 3517.15 163.98 -7 3 0 3656.93 164.18 7 3 0 3546.15 165.48 7 3 0 3742.13 165.48 9 -3 0 1390.06 72.89 -9 -3 0 1582.04 73.59 9 -3 0 1523.35 74.29 -9 -3 0 1539.75 74.19 -9 -3 0 1532.65 74.79 9 -3 0 1513.85 74.39 9 3 0 1383.06 72.79 9 3 0 1641.84 75.39 -9 3 0 1561.14 73.59 9 3 0 1577.14 75.39 9 3 0 1608.74 72.79 -9 3 0 1520.65 71.19 11 -3 0 1098.09 53.99 11 -3 0 1045.40 52.09 -11 -3 0 987.00 53.19 -11 -3 0 930.11 52.39 -11 -3 0 1018.60 51.99 11 -3 0 1012.20 53.39 11 3 0 1047.20 54.49 -11 3 0 1085.29 49.70 11 3 0 948.91 50.59 -11 3 0 1023.50 52.59 11 3 0 1024.10 53.49 11 3 0 1028.80 52.19 13 -3 0 1090.49 55.39 -13 -3 0 1027.80 54.79 13 -3 0 949.51 52.59 -13 3 0 1066.89 50.19 13 3 0 1061.39 51.99 13 3 0 883.31 52.69 13 3 0 1026.20 55.79 -15 -3 0 653.73 38.40 15 -3 0 627.94 36.20 15 -3 0 594.64 37.80 15 3 0 542.85 35.60 -15 3 0 653.63 33.50 15 3 0 570.84 34.10 17 -3 0 461.35 30.70 17 -3 0 477.45 33.20 -17 -3 0 460.55 32.50 17 3 0 435.96 30.40 17 3 0 483.95 29.20 0 -4 0 1514.55 67.69 0 -4 0 1438.06 67.69 0 -4 0 1560.14 68.89 0 4 0 1434.06 68.59 0 4 0 1443.36 68.39 0 4 0 1446.36 67.49 0 4 0 1417.46 68.39 2 -4 0 1040.10 49.80 -2 -4 0 1041.70 51.49 -2 -4 0 1102.39 51.49 2 -4 0 1055.89 51.19 2 -4 0 1060.29 51.39 -2 -4 0 1092.29 50.39 2 4 0 1116.29 51.69 -2 4 0 1011.00 49.80 2 4 0 1124.39 50.49 -2 4 0 1118.69 50.89 2 4 0 1090.49 51.29 -2 4 0 1030.80 50.99 2 4 0 1054.79 50.59 4 -4 0 2380.16 108.59 -4 -4 0 2196.58 108.59 -4 -4 0 2333.27 107.79 -4 -4 0 2446.46 108.89 -4 -4 0 2386.06 108.39 4 -4 0 2418.66 108.99 4 4 0 2307.87 107.69 -4 4 0 2411.26 107.69 -4 4 0 2302.37 108.09 4 4 0 2490.85 108.09 4 4 0 2334.67 109.19 4 4 0 2309.67 108.29 -4 4 0 2313.37 106.79 -6 -4 0 2156.88 101.39 -6 -4 0 2295.17 101.89 6 -4 0 2135.39 101.69 6 -4 0 2132.99 101.09 6 -4 0 2285.47 101.49 -6 -4 0 2148.58 101.19 6 4 0 2148.98 100.89 -6 4 0 2118.59 99.09 6 4 0 2243.88 102.49 -6 4 0 2106.79 100.69 6 4 0 2149.88 100.99 -6 4 0 2218.08 100.19 8 -4 0 858.61 42.50 -8 -4 0 831.22 42.30 -8 -4 0 875.31 42.20 8 -4 0 756.92 41.20 8 -4 0 827.42 42.50 -8 -4 0 764.82 42.00 8 4 0 779.92 41.10 8 4 0 823.32 43.40 8 4 0 876.31 42.80 -8 4 0 793.82 41.20 -8 4 0 801.42 40.30 8 4 0 803.12 41.00 10 -4 0 681.53 35.90 10 -4 0 602.64 34.80 -10 -4 0 632.64 34.50 -10 -4 0 574.24 34.50 10 -4 0 621.84 34.20 -10 -4 0 621.94 35.20 10 4 0 659.93 35.90 -10 4 0 669.53 31.70 10 4 0 582.64 32.90 -10 4 0 652.03 34.30 10 4 0 587.54 33.40 10 4 0 612.74 36.20 -12 -4 0 595.54 34.10 12 -4 0 547.85 32.50 12 -4 0 534.25 33.80 12 4 0 528.65 31.20 -12 4 0 654.73 30.30 12 4 0 553.54 34.70 12 4 0 522.05 32.10 -12 4 0 574.54 33.40 14 -4 0 408.76 27.80 14 -4 0 356.46 25.10 -14 -4 0 390.36 26.90 -14 4 0 375.96 22.20 14 4 0 371.96 25.50 14 4 0 381.26 24.20 16 -4 0 282.17 24.10 -16 -4 0 272.47 23.10 16 -4 0 268.27 21.50 16 4 0 244.38 21.20 -16 4 0 256.37 19.00 16 4 0 277.67 20.10 18 -4 0 235.18 23.10 18 -4 0 189.78 19.60 -18 -4 0 183.18 20.80 18 4 0 177.88 17.40 18 4 0 201.98 20.10 -1 -5 0 114.79 9.30 -1 -5 0 111.59 8.40 1 -5 0 115.49 8.10 -1 -5 0 116.79 8.30 1 -5 0 118.69 9.30 1 5 0 134.59 9.60 -1 5 0 123.19 9.20 -1 5 0 120.99 9.10 -1 5 0 115.19 9.20 -1 5 0 125.09 8.30 1 5 0 112.89 8.30 1 5 0 133.09 9.60 1 5 0 128.69 9.50 -3 -5 0 3.60 1.90 3 -5 0 4.80 2.40 -3 -5 0 3.70 2.30 -3 -5 0 0.80 2.20 3 -5 0 6.80 2.70 -3 -5 0 6.20 2.70 3 5 0 0.60 2.30 -3 5 0 5.90 2.30 3 5 0 6.50 2.50 -3 5 0 3.10 1.60 3 5 0 5.70 2.20 3 5 0 4.40 2.20 -3 5 0 3.40 2.30 5 -5 0 19.50 4.40 5 -5 0 26.00 5.00 -5 -5 0 20.50 4.40 -5 -5 0 33.60 5.70 -5 -5 0 33.50 4.80 -5 -5 0 27.20 5.00 5 5 0 19.90 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13.90 15 -1 -14 110.89 12.70 15 -1 -14 124.79 15.50 15 1 -14 136.49 11.90 15 1 -14 114.09 13.50 15 1 -14 170.68 15.40 13 -1 -14 173.88 15.40 13 -1 -14 169.98 13.30 13 -1 -14 201.68 17.90 13 1 -14 172.68 11.50 13 1 -14 171.28 16.40 13 1 -14 173.58 16.20 13 1 -14 136.09 11.20 11 -1 -14 73.39 7.90 11 -1 -14 70.19 12.00 11 -1 -14 74.49 11.20 11 1 -14 86.19 12.10 11 1 -14 99.49 13.20 9 -1 -14 39.10 10.40 9 -1 -14 27.50 5.70 -9 -1 14 36.20 5.20 9 1 -14 27.40 8.70 9 1 -14 36.30 9.00 9 1 -14 33.80 5.60 -9 1 14 25.80 5.40 7 -1 -14 42.00 10.80 7 -1 -14 68.59 9.50 7 1 -14 61.09 8.80 7 1 -14 42.70 11.10 5 -1 -14 99.69 17.00 5 -1 -14 95.29 13.60 5 1 -14 128.99 18.10 5 1 -14 89.29 13.30 18 -2 -14 66.79 11.60 18 -2 -14 84.29 9.90 18 -2 -14 84.49 13.80 18 2 -14 97.69 11.60 18 2 -14 84.49 11.00 18 2 -14 117.79 13.40 16 -2 -14 51.19 13.20 16 -2 -14 69.29 10.80 16 -2 -14 71.09 9.40 16 -2 -14 68.99 12.10 16 2 -14 77.89 9.30 16 2 -14 83.09 12.10 16 2 -14 72.49 10.30 14 -2 -14 86.59 10.50 14 -2 -14 74.29 12.70 14 -2 -14 70.79 10.20 14 2 -14 78.39 8.40 14 2 -14 64.99 10.40 14 2 -14 75.69 9.20 14 2 -14 68.69 11.00 12 -2 -14 179.98 13.90 12 -2 -14 163.38 15.30 12 -2 -14 163.28 17.40 12 2 -14 187.98 17.50 12 2 -14 154.98 15.70 10 -2 -14 87.79 13.50 10 -2 -14 97.59 9.10 10 -2 -14 84.09 8.40 10 2 -14 80.79 12.60 10 2 -14 90.39 13.80 10 2 -14 86.79 7.50 8 -2 -14 19.60 8.20 -8 -2 14 8.80 6.10 8 -2 -14 1.50 5.20 8 2 -14 4.40 7.20 8 2 -14 -3.40 4.70 -8 2 14 5.70 5.90 8 2 -14 5.50 7.60 6 -2 -14 48.40 11.10 6 -2 -14 39.60 9.00 6 2 -14 36.60 11.00 6 2 -14 30.10 8.60 17 -3 -14 656.03 38.00 17 -3 -14 684.63 33.10 17 -3 -14 625.54 41.10 17 3 -14 615.14 34.30 17 3 -14 615.54 37.70 17 3 -14 580.64 33.70 15 -3 -14 641.54 33.20 15 -3 -14 576.74 38.40 15 -3 -14 632.54 35.50 15 3 -14 594.34 36.50 15 3 -14 546.35 32.50 15 3 -14 590.44 31.00 13 -3 -14 496.25 29.50 13 -3 -14 476.05 33.00 13 -3 -14 464.85 28.60 13 3 -14 506.75 29.80 13 3 -14 488.25 32.10 11 -3 -14 524.25 29.40 11 -3 -14 501.25 35.10 11 3 -14 529.35 25.10 11 3 -14 535.95 32.10 11 3 -14 466.65 24.80 11 3 -14 583.34 34.80 9 -3 -14 434.96 23.90 9 -3 -14 414.96 24.80 9 -3 -14 365.86 29.70 -9 -3 14 377.96 28.70 9 3 -14 487.35 29.80 9 3 -14 433.06 30.20 9 3 -14 410.66 23.90 7 -3 -14 265.27 25.30 7 -3 -14 287.67 21.50 7 3 -14 305.27 25.00 7 3 -14 287.27 21.00 7 3 -14 311.77 25.80 16 -4 -14 203.88 13.50 16 -4 -14 181.38 18.00 16 -4 -14 159.58 19.60 16 4 -14 175.88 14.00 16 4 -14 177.08 18.60 14 -4 -14 221.88 21.80 14 -4 -14 247.08 19.40 14 -4 -14 227.88 16.70 14 4 -14 210.68 16.20 14 4 -14 208.18 20.00 14 4 -14 222.68 13.50 12 -4 -14 149.39 14.50 12 -4 -14 126.79 18.00 12 4 -14 114.29 15.80 12 4 -14 138.29 14.40 10 -4 -14 184.48 15.70 10 -4 -14 167.98 19.80 10 4 -14 180.28 17.60 10 4 -14 152.98 12.80 10 4 -14 177.08 19.00 10 4 -14 161.68 12.10 8 -4 -14 263.57 19.70 8 -4 -14 230.98 23.80 8 -4 -14 225.38 17.10 8 4 -14 273.37 22.60 8 4 -14 200.38 22.40 8 4 -14 243.48 18.50 13 -5 -14 13.90 9.40 13 -5 -14 8.10 8.10 13 5 -14 1.40 8.40 11 -5 -14 31.30 11.00 11 -5 -14 16.20 8.30 11 5 -14 36.40 5.80 11 5 -14 31.50 6.60 11 5 -14 16.90 8.30 16 0 -15 7.90 6.30 16 0 -15 -0.10 7.30 16 0 -15 4.70 7.10 14 0 -15 -6.50 7.00 14 0 -15 0.40 5.00 14 0 -15 0.40 7.00 12 0 -15 4.80 7.20 12 0 -15 4.10 7.10 10 0 -15 20.80 8.40 10 0 -15 -3.10 8.20 10 0 -15 0.80 3.80 17 -1 -15 302.67 24.90 17 -1 -15 295.37 22.00 17 -1 -15 311.77 21.80 17 1 -15 297.07 22.90 17 1 -15 334.97 23.40 17 1 -15 305.37 20.70 15 -1 -15 312.17 25.00 15 -1 -15 334.47 21.30 15 -1 -15 309.77 22.80 15 1 -15 303.47 23.30 15 1 -15 316.97 19.20 15 1 -15 335.67 24.00 13 -1 -15 201.98 13.90 13 -1 -15 163.88 17.00 13 -1 -15 196.78 19.90 13 1 -15 165.68 18.50 13 1 -15 207.28 18.60 11 -1 -15 246.18 22.90 11 -1 -15 246.18 21.00 11 1 -15 232.98 21.00 11 1 -15 245.28 21.30 9 -1 -15 216.18 22.90 9 -1 -15 286.17 17.90 9 1 -15 263.07 23.70 9 1 -15 244.98 22.40 9 1 -15 286.77 17.50 16 -2 -15 408.26 30.10 16 -2 -15 384.16 25.10 16 -2 -15 422.76 26.70 16 2 -15 397.46 27.90 16 2 -15 421.56 23.50 16 2 -15 377.06 26.40 14 -2 -15 263.67 18.70 14 -2 -15 260.27 23.20 14 -2 -15 238.88 19.60 14 2 -15 249.78 21.30 14 2 -15 228.28 20.40 12 -2 -15 374.96 25.50 12 -2 -15 387.66 21.90 12 -2 -15 337.17 28.00 12 2 -15 320.27 26.30 12 2 -15 382.76 26.80 10 -2 -15 308.17 19.00 10 -2 -15 336.67 27.50 10 2 -15 326.47 18.20 10 2 -15 317.97 26.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 73165 loop_ _space_group_symop_operation_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' '-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_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 0.5000 -0.15824(2) 0.7500 0.01635(8) Uani 1 2 d S T P . . N1 N 0.5000 0.5775(3) 0.7500 0.0161(6) Uani 1 2 d S T P . . N2 N 0.59036(17) 0.7335(2) 0.6775(3) 0.0209(5) Uani 1 1 d . . . . . O1 O 0.48427(17) 0.0640(2) 0.8274(2) 0.0297(5) Uani 1 1 d . . . . . O2 O 0.39653(18) -0.2269(3) 0.5119(3) 0.0410(6) Uani 1 1 d . . . . . O3 O 0.33859(19) -0.0797(3) 0.5826(3) 0.0438(6) Uani 1 1 d . . . . . C1 C 0.54509(18) 0.5059(3) 0.7087(3) 0.0175(5) Uani 1 1 d . . . . . C2 C 0.5000 0.1276(5) 0.7500 0.0238(8) Uani 1 2 d S T P . . C3 C 0.5000 0.2861(4) 0.7500 0.0200(7) Uani 1 2 d S T P . . C4 C 0.59575(18) 0.5928(3) 0.6690(3) 0.0178(5) Uani 1 1 d . . . . . C5 C 0.5447(2) 0.3588(3) 0.7036(3) 0.0208(6) Uani 1 1 d . . . . . C6 C 0.3335(3) -0.1549(3) 0.4930(4) 0.0325(8) Uani 1 1 d . . . . . C7 C 0.6344(2) 0.8176(3) 0.6423(4) 0.0285(7) Uani 1 1 d . . . . . C8 C 0.6475(2) 0.5323(3) 0.6284(3) 0.0256(6) Uani 1 1 d . . . . . C9 C 0.6952(2) 0.6200(4) 0.5962(4) 0.0303(7) Uani 1 1 d . . . . . C10 C 0.6877(2) 0.7646(4) 0.6017(4) 0.0320(7) 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 0.02300(11) 0.00661(10) 0.02477(11) 0.000 0.01684(9) 0.000 N1 0.0205(15) 0.0099(14) 0.0211(15) 0.000 0.0138(13) 0.000 N2 0.0257(12) 0.0120(11) 0.0309(13) 0.0017(9) 0.0198(11) 0.0001(9) O1 0.0526(14) 0.0105(9) 0.0408(13) -0.0005(8) 0.0355(12) -0.0003(9) O2 0.0402(14) 0.0368(14) 0.0365(13) -0.0089(11) 0.0166(11) 0.0049(11) O3 0.0401(14) 0.0473(16) 0.0446(14) 0.0024(12) 0.0248(12) 0.0149(12) C1 0.0213(12) 0.0101(12) 0.0206(12) 0.0010(9) 0.0117(11) 0.0009(9) C2 0.031(2) 0.0123(17) 0.028(2) 0.000 0.0173(18) 0.000 C3 0.0263(19) 0.0096(18) 0.0247(19) 0.000 0.0150(16) 0.000 C4 0.0206(12) 0.0115(12) 0.0220(13) -0.0005(10) 0.0127(11) -0.0007(10) C5 0.0274(15) 0.0116(12) 0.0270(15) -0.0003(10) 0.0177(13) 0.0003(10) C6 0.0324(18) 0.0286(18) 0.0317(18) 0.0017(12) 0.0157(15) 0.0038(12) C7 0.0372(17) 0.0157(13) 0.0444(19) 0.0022(13) 0.0302(16) -0.0034(12) C8 0.0315(15) 0.0208(14) 0.0327(15) 0.0003(12) 0.0233(13) 0.0035(12) C9 0.0361(17) 0.0266(15) 0.0412(18) 0.0031(14) 0.0298(15) 0.0049(14) C10 0.0414(18) 0.0256(16) 0.0462(19) 0.0031(14) 0.0353(16) -0.0018(13) 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 O1 Ho1 O1 55.33(10) 2_656 . ? O1 Ho1 O2 88.26(9) 2_656 . ? O1 Ho1 O2 120.62(9) . . ? O1 Ho1 O2 120.62(9) 2_656 2_656 ? O1 Ho1 O2 88.25(9) . 2_656 ? O2 Ho1 O2 148.63(13) . 2_656 ? O1 Ho1 N2 138.99(8) 2_656 2_646 ? O1 Ho1 N2 89.23(8) . 2_646 ? O2 Ho1 N2 94.56(9) . 2_646 ? O2 Ho1 N2 72.20(9) 2_656 2_646 ? O1 Ho1 N2 89.23(8) 2_656 1_545 ? O1 Ho1 N2 138.99(8) . 1_545 ? O2 Ho1 N2 72.20(9) . 1_545 ? O2 Ho1 N2 94.56(9) 2_656 1_545 ? N2 Ho1 N2 130.54(11) 2_646 1_545 ? O1 Ho1 N1 152.33(5) 2_656 1_545 ? O1 Ho1 N1 152.33(5) . 1_545 ? O2 Ho1 N1 74.32(7) . 1_545 ? O2 Ho1 N1 74.32(7) 2_656 1_545 ? N2 Ho1 N1 65.27(5) 2_646 1_545 ? N2 Ho1 N1 65.27(5) 1_545 1_545 ? O1 Ho1 O3 76.70(9) 2_656 . ? O1 Ho1 O3 72.67(9) . . ? O2 Ho1 O3 52.59(9) . . ? O2 Ho1 O3 140.23(9) 2_656 . ? N2 Ho1 O3 72.96(9) 2_646 . ? N2 Ho1 O3 122.84(9) 1_545 . ? N1 Ho1 O3 107.34(7) 1_545 . ? O1 Ho1 O3 72.67(9) 2_656 2_656 ? O1 Ho1 O3 76.70(9) . 2_656 ? O2 Ho1 O3 140.23(9) . 2_656 ? O2 Ho1 O3 52.59(9) 2_656 2_656 ? N2 Ho1 O3 122.84(9) 2_646 2_656 ? N2 Ho1 O3 72.96(9) 1_545 2_656 ? N1 Ho1 O3 107.34(7) 1_545 2_656 ? O3 Ho1 O3 145.33(14) . 2_656 ? O1 Ho1 C2 27.67(5) 2_656 . ? O1 Ho1 C2 27.67(5) . . ? O2 Ho1 C2 105.68(7) . . ? O2 Ho1 C2 105.68(7) 2_656 . ? N2 Ho1 C2 114.73(5) 2_646 . ? N2 Ho1 C2 114.73(5) 1_545 . ? N1 Ho1 C2 180.0 1_545 . ? O3 Ho1 C2 72.66(7) . . ? O3 Ho1 C2 72.66(7) 2_656 . ? O1 Ho1 C6 81.83(9) 2_656 . ? O1 Ho1 C6 97.00(9) . . ? O2 Ho1 C6 26.10(10) . . ? O2 Ho1 C6 154.71(10) 2_656 . ? N2 Ho1 C6 83.12(10) 2_646 . ? N2 Ho1 C6 97.43(10) 1_545 . ? N1 Ho1 C6 90.66(6) 1_545 . ? O3 Ho1 C6 26.48(10) . . ? O3 Ho1 C6 152.65(10) 2_656 . ? C2 Ho1 C6 89.34(6) . . ? O1 Ho1 C6 97.00(9) 2_656 2_656 ? O1 Ho1 C6 81.83(9) . 2_656 ? O2 Ho1 C6 154.71(10) . 2_656 ? O2 Ho1 C6 26.10(10) 2_656 2_656 ? N2 Ho1 C6 97.44(10) 2_646 2_656 ? N2 Ho1 C6 83.12(10) 1_545 2_656 ? N1 Ho1 C6 90.66(6) 1_545 2_656 ? O3 Ho1 C6 152.65(10) . 2_656 ? O3 Ho1 C6 26.48(10) 2_656 2_656 ? C2 Ho1 C6 89.34(6) . 2_656 ? C6 Ho1 C6 178.69(13) . 2_656 ? C1 N1 C1 119.4(3) . 2_656 ? C1 N1 Ho1 120.32(16) . 1_565 ? C1 N1 Ho1 120.32(16) 2_656 1_565 ? C4 N2 C7 118.9(2) . . ? C4 N2 Ho1 122.10(17) . 1_565 ? C7 N2 Ho1 119.0(2) . 1_565 ? C2 O1 Ho1 91.0(2) . . ? C6 O2 Ho1 94.0(2) . . ? C6 O3 Ho1 89.4(2) . . ? N1 C1 C5 122.0(3) . . ? N1 C1 C4 116.0(2) . . ? C5 C1 C4 121.9(3) . . ? O1 C2 O1 122.7(4) 2_656 . ? O1 C2 C3 118.6(2) 2_656 . ? O1 C2 C3 118.6(2) . . ? O1 C2 Ho1 61.4(2) 2_656 . ? O1 C2 Ho1 61.4(2) . . ? C3 C2 Ho1 180.0 . . ? C5 C3 C5 120.4(4) . 2_656 ? C5 C3 C2 119.81(18) . . ? C5 C3 C2 119.81(18) 2_656 . ? N2 C4 C8 121.7(3) . . ? N2 C4 C1 116.2(2) . . ? C8 C4 C1 122.0(3) . . ? C3 C5 C1 118.0(3) . . ? O2 C6 O3 124.0(4) . . ? O2 C6 Ho1 59.87(19) . . ? O3 C6 Ho1 64.1(2) . . ? N2 C7 C10 122.5(3) . . ? C4 C8 C9 119.0(3) . . ? C8 C9 C10 119.1(3) . . ? C7 C10 C9 118.7(3) . . ? 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 O1 2.382(2) 2_656 ? Ho1 O1 2.382(2) . ? Ho1 O2 2.411(3) . ? Ho1 O2 2.411(3) 2_656 ? Ho1 N2 2.456(2) 2_646 ? Ho1 N2 2.456(2) 1_545 ? Ho1 N1 2.508(3) 1_545 ? Ho1 O3 2.502(3) . ? Ho1 O3 2.502(3) 2_656 ? Ho1 C2 2.713(4) . ? Ho1 C6 2.781(4) . ? Ho1 C6 2.781(4) 2_656 ? N1 C1 1.348(3) . ? N1 C1 1.348(3) 2_656 ? N1 Ho1 2.508(3) 1_565 ? N2 C4 1.347(4) . ? N2 C7 1.348(4) . ? N2 Ho1 2.456(2) 1_565 ? O1 C2 1.260(3) . ? O2 C6 1.227(5) . ? O3 C6 1.240(5) . ? C1 C5 1.397(4) . ? C1 C4 1.490(4) . ? C2 O1 1.260(3) 2_656 ? C2 C3 1.504(5) . ? C3 C5 1.390(4) . ? C3 C5 1.390(4) 2_656 ? C4 C8 1.392(4) . ? C7 C10 1.389(5) . ? C8 C9 1.397(5) . ? C9 C10 1.385(4) . ?