#------------------------------------------------------------------------------ #$Date: 2021-10-06 18:34:01 +0300 (Wed, 06 Oct 2021) $ #$Revision: 269711 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/81/7708163.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_7708163 loop_ _publ_author_name 'Yang, Feng' 'Xu, Yuangang' 'Wang, Pengcheng' 'Lin, Qiuhan' 'Lu, Ming' _publ_section_title ; Novel metal-organic frameworks assembled from the combination of polynitro-pyrazole and 5-nitroamine-1,2,4-oxadiazole: synthesis, structure and thermal properties. ; _journal_issue 37 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12906 _journal_page_last 12912 _journal_paper_doi 10.1039/d1dt02093e _journal_volume 50 _journal_year 2021 _chemical_formula_moiety 'C6 H4 K N9 O7, H2 O' _chemical_formula_sum 'C6 H6 K N9 O8' _chemical_formula_weight 371.30 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-11-18 deposited with the CCDC. 2021-08-16 downloaded from the CCDC. ; _cell_angle_alpha 97.197(3) _cell_angle_beta 99.588(3) _cell_angle_gamma 90.474(3) _cell_formula_units_Z 2 _cell_length_a 7.1587(6) _cell_length_b 8.4966(7) _cell_length_c 11.1631(10) _cell_measurement_reflns_used 4561 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.51 _cell_measurement_theta_min 2.42 _cell_volume 663.94(10) _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-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_detector_area_resol_mean 10.42 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON 100' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_unetI/netI 0.0380 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 10026 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.522 _diffrn_reflns_theta_min 2.417 _diffrn_source.source 'Ius 2.0' _diffrn_source.type microfocus _exptl_absorpt_coefficient_mu 0.470 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6378 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.857 _exptl_crystal_description block _exptl_crystal_F_000 376 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.521 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 223 _refine_ls_number_reflns 3035 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0527 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+0.7319P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1199 _refine_ls_wR_factor_ref 0.1327 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2246 _reflns_number_total 3035 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02093e2.cif _cod_data_source_block YF_040_a _cod_depositor_comments 'Adding full bibliography for 7708161--7708163.cif.' _cod_database_code 7708163 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.904 _shelx_estimated_absorpt_t_max 0.933 _shelx_res_file ; TITL YF_040_a.res in P-1 YF_040_a.res created by SHELXL-2018/3 at 19:23:55 on 18-Nov-2020 CELL 0.71073 7.1587 8.4966 11.1631 97.197 99.588 90.474 ZERR 2.00 0.0006 0.0007 0.0010 0.003 0.003 0.003 LATT 1 SFAC C H N O K UNIT 12 12 18 16 2 L.S. 10 ACTA BOND $H FMAP 2 PLAN -5 omit 0 0 1 CONF EQIV $5 x, y-1, z HTAB C1 O6_$5 EQIV $6 -x+1, -y, -z+1 HTAB N9 N1_$6 HTAB N9 O7 EQIV $7 -x+2, -y+1, -z+1 HTAB N9 O8_$7 EQIV $4 x+1, y, z HTAB O8 O3_$4 EQIV $8 -x+2, -y+1, -z HTAB O8 O2_$8 HTAB O8 O3_$8 dfix 0.85 o8 h8a o8 h8b dfix 1.39 h8a h8b size 0.22 0.20 0.15 FREE K1 N4 TEMP 23.000 WGHT 0.049700 0.731900 FVAR 1.31027 K1 5 1.164312 0.233054 0.016688 11.00000 0.04769 0.04890 = 0.04020 0.00516 -0.00237 0.01813 C1 1 0.243404 0.085184 0.344912 11.00000 0.06662 0.02447 = 0.04028 0.00696 0.00807 0.00487 AFIX 23 H1A 2 0.139454 0.026672 0.290141 11.00000 -1.20000 H1B 2 0.257692 0.044097 0.423077 11.00000 -1.20000 AFIX 0 C2 1 0.420644 0.061607 0.292983 11.00000 0.05644 0.02204 = 0.03190 0.00086 -0.00491 0.00908 C3 1 0.618909 0.072982 0.177153 11.00000 0.04137 0.03111 = 0.04172 -0.00876 -0.00788 0.01008 C4 1 0.089008 0.465632 0.305627 11.00000 0.03345 0.03250 = 0.03709 0.00984 0.00841 0.00412 C5 1 0.185896 0.506029 0.426259 11.00000 0.03571 0.02593 = 0.03613 0.00545 0.01258 0.00328 C6 1 0.259345 0.361648 0.460154 11.00000 0.03633 0.03134 = 0.03297 0.00705 0.01152 0.00354 N1 3 0.556489 -0.021649 0.341684 11.00000 0.07397 0.03895 = 0.04840 0.00946 -0.00653 0.02163 N2 3 0.450937 0.123683 0.190967 11.00000 0.03888 0.03285 = 0.03235 0.00096 -0.00173 0.00904 N3 3 0.736485 0.081076 0.094199 11.00000 0.03867 0.05213 = 0.05649 -0.01503 0.00228 0.01016 N4 3 0.686547 0.174851 0.008919 11.00000 0.03930 0.05447 = 0.05562 -0.01598 0.01027 -0.01307 N5 3 0.199646 0.252881 0.361907 11.00000 0.04721 0.02633 = 0.03275 0.00674 0.00674 0.00677 N6 3 0.096519 0.315101 0.266353 11.00000 0.04161 0.03423 = 0.03474 0.00846 0.00514 0.00518 N7 3 -0.014558 0.560873 0.219074 11.00000 0.05312 0.04164 = 0.04274 0.01427 0.01240 0.01624 N8 3 0.212155 0.649960 0.505016 11.00000 0.04215 0.02870 = 0.05743 0.00352 0.00570 0.00016 N9 3 0.366137 0.328594 0.562055 11.00000 0.06071 0.03437 = 0.03640 0.00856 0.00162 0.00915 AFIX 93 H9A 2 0.401535 0.233085 0.568400 11.00000 -1.20000 H9B 2 0.400141 0.402623 0.621933 11.00000 -1.20000 AFIX 0 O1 4 0.693144 -0.015956 0.264410 11.00000 0.06049 0.04824 = 0.06248 0.00396 -0.00601 0.03011 O2 4 0.792405 0.175594 -0.069303 11.00000 0.05403 0.09418 = 0.07115 -0.02039 0.02756 -0.02084 O3 4 0.544585 0.257972 0.002769 11.00000 0.05254 0.06072 = 0.07108 0.01846 0.02290 0.00819 O4 4 -0.072098 0.498757 0.117051 11.00000 0.14012 0.05668 = 0.07725 0.01224 -0.05731 0.01144 O5 4 -0.036660 0.694250 0.247909 11.00000 0.27404 0.07207 = 0.05575 0.00303 -0.00857 0.09984 O6 4 0.146435 0.769291 0.470090 11.00000 0.14371 0.03011 = 0.12050 -0.00107 -0.05856 0.01661 O7 4 0.300286 0.647051 0.608825 11.00000 0.07270 0.04273 = 0.04410 -0.00282 0.00503 0.00032 O8 4 1.437436 0.520982 0.185795 11.00000 0.10641 0.06113 = 0.07303 0.01554 0.03675 0.01015 H8A 2 1.512160 0.454714 0.156465 11.00000 -1.50000 H8B 2 1.425125 0.596170 0.141821 11.00000 -1.50000 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM YF_040_a.res in P-1 REM wR2 = 0.1327, GooF = S = 1.026, Restrained GooF = 1.025 for all data REM R1 = 0.0527 for 2246 Fo > 4sig(Fo) and 0.0778 for all 3035 data REM 223 parameters refined using 3 restraints END WGHT 0.0470 0.7473 REM Highest difference peak 0.521, deepest hole -0.461, 1-sigma level 0.061 Q1 1 0.9267 0.3078 -0.2393 11.00000 0.05 0.52 Q2 1 1.0995 0.3539 -0.2569 11.00000 0.05 0.45 Q3 1 1.1628 0.4517 -0.1591 11.00000 0.05 0.45 Q4 1 0.2240 0.7445 0.4238 11.00000 0.05 0.43 Q5 1 0.0895 0.7470 0.4876 11.00000 0.05 0.40 ; _shelx_res_checksum 88477 _shelx_hkl_file ; -1 0 0 4.70 0.60 -1 0 0 3.10 0.60 -1 0 0 4.90 0.70 1 0 0 5.60 0.80 1 0 0 3.30 0.60 1 0 0 5.00 0.60 -2 0 0 1695.93 52.29 -2 0 0 1660.33 52.09 2 0 0 1708.53 52.49 2 0 0 1631.74 52.29 2 0 0 1683.93 51.89 -3 0 0 1401.36 45.80 -3 0 0 1391.26 44.30 -3 0 0 1323.37 45.00 3 0 0 1421.36 43.80 3 0 0 1376.96 44.40 3 0 0 1431.56 44.60 -4 0 0 2.70 1.80 -4 0 0 5.00 2.80 -4 0 0 3.20 1.80 4 0 0 3.90 2.20 4 0 0 3.00 1.90 -5 0 0 110.99 7.00 -5 0 0 100.99 9.10 -5 0 0 112.69 6.80 5 0 0 118.99 7.50 5 0 0 104.39 7.20 5 0 0 102.39 5.80 -6 0 0 -1.50 5.30 -6 0 0 3.20 3.70 6 0 0 4.20 2.90 6 0 0 1.10 3.50 -7 0 0 26.00 5.50 -7 0 0 23.30 4.00 7 0 0 31.70 7.40 -8 0 0 52.99 7.70 -8 0 0 57.89 12.10 8 0 0 51.19 8.40 -9 0 0 -23.40 15.60 9 0 0 11.70 9.20 9 -1 0 9.10 8.70 -9 1 0 7.70 17.00 8 -1 0 34.00 7.10 -8 1 0 11.70 5.80 -8 1 0 12.70 11.70 -7 1 0 74.59 7.80 -7 1 0 57.19 5.20 6 -1 0 2.60 3.60 -6 1 0 5.60 5.50 -6 1 0 3.90 2.20 -6 1 0 3.70 3.00 5 -1 0 201.58 9.80 5 -1 0 194.38 10.00 -5 1 0 199.18 9.00 -5 1 0 207.08 12.80 -5 1 0 206.28 10.00 4 -1 0 95.69 6.10 4 -1 0 100.49 4.50 4 -1 0 92.79 5.60 -4 1 0 103.09 6.00 -4 1 0 106.89 7.60 -4 1 0 95.29 5.30 3 -1 0 614.74 20.70 3 -1 0 595.84 19.40 3 -1 0 610.34 21.10 -3 1 0 619.54 20.80 -3 1 0 603.74 22.30 -3 1 0 607.84 19.80 2 -1 0 19.00 1.10 2 -1 0 19.60 2.30 2 -1 0 19.60 2.40 -2 1 0 17.50 2.00 -2 1 0 17.20 2.50 -2 1 0 19.70 1.30 1 -1 0 3563.34 108.69 1 -1 0 3532.75 108.99 -1 1 0 3592.94 108.79 -1 1 0 3498.35 109.19 0 -1 0 136.99 5.00 0 -1 0 130.29 5.50 0 1 0 161.18 5.60 0 1 0 145.39 5.00 0 1 0 160.28 5.10 -1 -1 0 7227.78 220.78 -2 -1 0 4783.32 148.69 2 1 0 4839.82 148.79 2 1 0 4913.41 148.59 -3 -1 0 693.53 23.90 -3 -1 0 673.23 23.30 -3 -1 0 677.63 22.80 3 1 0 702.23 22.90 3 1 0 679.93 23.60 3 1 0 662.93 23.40 -4 -1 0 258.07 10.90 -4 -1 0 243.88 11.80 -4 -1 0 240.18 10.10 4 1 0 242.58 10.90 4 1 0 236.38 10.20 4 1 0 246.08 9.90 -5 -1 0 126.29 7.20 -5 -1 0 110.99 7.80 -5 -1 0 134.79 10.00 5 1 0 130.49 8.40 5 1 0 122.49 7.50 5 1 0 113.69 6.80 -6 -1 0 12.60 6.20 -6 -1 0 9.60 4.10 6 1 0 12.10 4.80 6 1 0 15.30 3.50 -7 -1 0 22.10 9.20 -7 -1 0 32.80 6.50 7 1 0 33.20 5.50 -8 -1 0 17.60 11.30 -8 -1 0 15.30 7.60 8 1 0 40.50 8.30 -9 -1 0 15.10 16.60 9 1 0 22.60 10.40 9 -2 0 -3.40 8.10 -9 2 0 36.20 18.70 8 -2 0 6.60 6.00 -8 2 0 -0.70 12.30 -7 2 0 105.29 7.70 -7 2 0 121.69 15.90 6 -2 0 470.75 18.70 -6 2 0 432.36 15.10 -6 2 0 472.35 23.70 5 -2 0 7.60 3.00 5 -2 0 5.30 3.10 -5 2 0 2.60 1.20 -5 2 0 -0.40 4.20 -5 2 0 6.30 2.00 4 -2 0 137.49 7.10 4 -2 0 135.79 7.40 -4 2 0 141.69 9.40 -4 2 0 131.29 5.20 -4 2 0 127.89 7.50 -4 2 0 127.49 4.60 3 -2 0 1904.81 60.19 3 -2 0 1842.32 59.59 -3 2 0 1914.51 60.09 -3 2 0 1868.41 61.69 2 -2 0 561.94 18.80 2 -2 0 512.85 18.10 -2 2 0 537.55 19.40 1 -2 0 3018.20 88.29 1 -2 0 2839.22 86.69 1 -2 0 2836.72 87.79 1 -2 0 2595.74 88.49 -1 2 0 2827.32 88.19 -1 2 0 2880.51 86.59 0 -2 0 266.47 10.20 0 -2 0 257.37 9.10 0 -2 0 254.87 9.10 0 -2 0 264.27 9.20 0 2 0 271.57 10.10 0 2 0 253.17 9.00 -1 -2 0 474.45 16.10 -1 -2 0 496.85 17.70 1 2 0 491.55 18.10 1 2 0 529.05 16.30 1 2 0 509.75 16.80 -2 -2 0 2474.85 77.59 -2 -2 0 2561.94 77.79 -2 -2 0 2335.87 76.99 2 2 0 2493.25 78.39 2 2 0 2417.66 77.99 2 2 0 2540.35 76.69 -3 -2 0 1558.04 52.39 -3 -2 0 1649.13 52.99 -3 -2 0 1615.94 53.19 3 2 0 1651.43 53.89 3 2 0 1658.23 52.49 3 2 0 1728.23 52.39 -4 -2 0 1106.19 37.80 -4 -2 0 1122.19 38.20 -4 -2 0 1098.99 36.70 4 2 0 1091.29 38.20 4 2 0 1103.89 36.60 -5 -2 0 99.99 8.80 -5 -2 0 90.69 7.60 -5 -2 0 92.89 6.60 5 2 0 83.49 6.40 5 2 0 96.49 8.40 5 2 0 75.99 7.10 -6 -2 0 81.89 9.20 -6 -2 0 75.99 10.90 6 2 0 85.49 9.70 6 2 0 58.49 7.50 -7 -2 0 36.80 9.70 -7 -2 0 45.60 7.80 -8 -2 0 -5.20 11.10 8 2 0 16.50 9.20 8 -3 0 9.60 6.30 -8 3 0 -4.70 12.60 7 -3 0 12.50 5.40 -7 3 0 21.60 10.00 6 -3 0 355.06 15.60 -6 3 0 324.47 20.40 5 -3 0 261.67 11.60 5 -3 0 216.48 11.50 -5 3 0 248.58 15.30 -5 3 0 229.98 12.50 4 -3 0 117.79 7.40 4 -3 0 117.49 6.90 -4 3 0 122.59 8.20 -4 3 0 132.29 9.70 3 -3 0 2468.15 78.39 3 -3 0 2569.34 78.99 -3 3 0 2471.25 80.69 -3 3 0 2435.16 79.29 2 -3 0 1653.03 53.39 2 -3 0 1679.83 52.59 2 -3 0 1584.74 52.49 -2 3 0 1643.54 53.69 1 -3 0 2033.80 63.09 1 -3 0 1918.11 60.79 1 -3 0 1936.41 61.69 -1 3 0 1980.20 60.59 -1 3 0 1921.91 62.19 -1 3 0 1972.70 62.39 0 -3 0 36.20 2.80 0 -3 0 40.10 2.90 0 -3 0 44.10 4.90 0 3 0 40.50 2.70 0 3 0 44.40 4.20 -1 -3 0 17.20 3.50 -1 -3 0 14.90 2.20 -1 -3 0 17.10 1.70 1 3 0 12.70 1.80 1 3 0 11.70 1.90 1 3 0 11.70 2.90 -2 -3 0 89.39 4.60 -2 -3 0 89.69 5.80 2 3 0 83.89 6.70 2 3 0 84.89 5.20 2 3 0 87.09 4.60 -3 -3 0 77.29 5.60 -3 -3 0 83.59 5.10 3 3 0 80.79 5.30 3 3 0 81.89 5.10 3 3 0 73.59 6.90 -4 -3 0 26.20 4.10 -4 -3 0 25.00 4.00 -4 -3 0 19.40 3.00 4 3 0 23.40 3.40 4 3 0 30.80 5.90 4 3 0 22.90 3.20 -5 -3 0 679.13 26.00 -5 -3 0 722.43 28.00 -5 -3 0 755.42 28.60 5 3 0 718.13 26.30 5 3 0 751.92 29.30 -6 -3 0 3.60 4.90 -6 -3 0 -0.80 5.90 6 3 0 3.20 5.60 -7 -3 0 -18.80 8.00 7 3 0 12.30 8.00 -8 -3 0 111.39 13.00 -8 -3 0 105.79 16.90 8 3 0 131.29 18.40 8 -4 0 209.78 15.40 -8 4 0 198.98 25.50 7 -4 0 -1.90 5.60 -7 4 0 -5.30 9.50 6 -4 0 163.88 12.10 -6 4 0 119.59 21.70 5 -4 0 130.19 8.90 5 -4 0 142.59 8.90 -5 4 0 109.89 12.20 4 -4 0 278.77 12.30 4 -4 0 269.37 12.40 -4 4 0 288.17 15.40 -4 4 0 256.47 13.40 3 -4 0 655.43 25.50 3 -4 0 701.33 24.20 3 -4 0 649.83 24.00 -3 4 0 685.13 26.30 2 -4 0 11.90 1.60 2 -4 0 14.90 2.80 2 -4 0 11.30 1.20 2 -4 0 9.80 3.10 2 -4 0 7.40 3.20 -2 4 0 4.60 2.90 1 -4 0 1912.01 62.99 1 -4 0 1900.81 60.79 -1 4 0 1886.71 61.49 -1 4 0 1915.91 62.09 -1 4 0 1973.40 59.89 0 -4 0 2782.92 92.89 0 -4 0 3025.60 92.79 0 -4 0 3119.19 95.59 0 -4 0 2980.70 92.39 0 4 0 2956.00 92.69 0 4 0 3022.00 94.89 -1 -4 0 52.09 3.00 -1 -4 0 45.70 5.70 -1 -4 0 43.30 3.90 1 4 0 43.00 5.70 1 4 0 42.90 3.80 1 4 0 48.40 4.60 -2 -4 0 615.54 23.80 -2 -4 0 648.54 23.30 -2 -4 0 642.84 21.20 2 4 0 636.34 22.50 2 4 0 611.34 24.80 2 4 0 675.33 22.20 -3 -4 0 1273.47 44.90 -3 -4 0 1340.17 43.50 -3 -4 0 1371.26 45.60 3 4 0 1323.07 43.60 3 4 0 1384.36 47.70 -4 -4 0 201.68 10.60 -4 -4 0 231.28 11.00 -4 -4 0 211.18 11.70 4 4 0 198.38 10.40 4 4 0 226.48 14.10 4 4 0 197.78 10.00 -5 -4 0 12.30 4.80 -5 -4 0 7.60 4.60 5 4 0 13.40 4.50 5 4 0 20.70 7.40 -6 -4 0 146.79 12.90 -6 -4 0 145.89 13.80 6 4 0 139.09 15.00 -7 -4 0 6.90 8.00 -7 -4 0 7.30 9.50 7 4 0 10.90 8.70 -8 -4 0 11.40 13.80 -8 -4 0 -18.10 10.10 8 4 0 -0.70 11.70 8 -5 0 -1.00 7.40 -8 5 0 3.90 15.00 7 -5 0 344.47 18.50 -7 5 0 369.26 27.20 6 -5 0 327.37 16.20 -6 5 0 313.37 22.00 5 -5 0 108.49 9.80 -5 5 0 118.29 13.20 4 -5 0 79.29 7.10 4 -5 0 66.99 6.70 -4 5 0 85.49 9.50 3 -5 0 402.66 16.50 3 -5 0 392.16 18.40 3 -5 0 423.56 16.20 -3 5 0 388.16 18.40 2 -5 0 1.10 1.10 2 -5 0 2.70 3.10 2 -5 0 1.80 1.90 2 -5 0 3.90 4.30 2 -5 0 -1.00 2.30 -2 5 0 -3.40 3.00 1 -5 0 691.63 23.90 1 -5 0 683.83 23.70 1 -5 0 706.13 27.30 -1 5 0 683.73 25.30 -1 5 0 695.03 25.90 -1 5 0 715.03 23.40 0 -5 0 401.46 18.20 0 -5 0 393.06 14.20 0 -5 0 397.76 14.80 0 -5 0 392.96 15.30 0 5 0 412.06 14.90 0 5 0 399.86 17.40 -1 -5 0 772.52 30.50 -1 -5 0 796.52 26.10 -1 -5 0 863.01 28.00 -1 -5 0 787.22 28.50 1 5 0 836.62 30.90 1 5 0 828.12 27.90 -2 -5 0 1264.57 41.80 -2 -5 0 1214.28 38.80 -2 -5 0 1151.38 42.50 2 5 0 1208.08 40.50 2 5 0 1198.68 43.70 2 5 0 1239.68 40.80 -3 -5 0 197.18 10.90 -3 -5 0 174.48 10.80 -3 -5 0 188.18 8.60 3 5 0 174.48 9.80 3 5 0 189.38 13.10 3 5 0 175.28 9.60 -4 -5 0 32.30 5.50 -4 -5 0 55.89 6.50 4 5 0 35.60 8.30 4 5 0 34.10 5.00 -5 -5 0 44.70 7.20 -5 -5 0 49.50 7.80 5 5 0 40.70 6.70 5 5 0 34.20 9.00 -6 -5 0 26.20 8.90 -6 -5 0 18.40 7.40 6 5 0 33.30 13.10 -7 -5 0 13.80 10.80 -7 -5 0 -4.40 8.60 7 5 0 10.10 12.60 -8 -5 0 -9.50 12.20 -8 -5 0 7.50 14.90 8 5 0 -4.00 14.30 7 -6 0 -0.50 6.80 -7 6 0 -7.60 12.10 6 -6 0 85.39 10.60 -5 6 0 370.66 21.50 4 -6 0 117.39 9.40 4 -6 0 130.79 8.90 -4 6 0 136.69 12.30 3 -6 0 252.07 9.20 3 -6 0 260.17 12.80 3 -6 0 242.38 8.50 3 -6 0 250.77 11.50 -3 6 0 243.78 14.20 2 -6 0 22.80 4.60 2 -6 0 22.00 3.70 2 -6 0 5.30 6.60 2 -6 0 20.90 3.10 -2 6 0 13.60 4.40 1 -6 0 3.80 2.20 1 -6 0 -1.20 6.00 1 -6 0 6.30 2.80 -1 6 0 6.60 3.60 -1 6 0 8.80 2.40 0 -6 0 10.00 2.40 0 -6 0 7.10 2.50 0 -6 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6.80 -2 4 -12 33.40 13.20 -2 4 -12 4.80 6.60 2 -4 12 4.40 9.10 -3 4 -12 -6.00 14.50 -3 4 -12 3.90 7.20 6 3 -12 -13.00 7.40 -6 -3 12 -6.80 9.10 5 3 -12 3.70 6.20 -5 -3 12 2.50 8.00 4 3 -12 125.29 10.90 -4 -3 12 123.89 14.00 3 3 -12 74.29 9.30 -3 -3 12 74.29 10.50 2 3 -12 213.88 12.70 -2 -3 12 210.08 18.60 1 3 -12 17.80 5.60 -1 -3 12 -9.70 8.90 0 3 -12 39.40 6.30 0 -3 12 58.69 14.10 -1 3 -12 19.50 6.30 1 -3 12 11.70 5.90 1 -3 12 1.40 14.10 -2 3 -12 37.20 7.40 -2 3 -12 51.69 13.90 2 -3 12 28.50 7.90 -3 3 -12 46.20 8.80 -3 3 -12 33.50 14.60 3 -3 12 30.50 9.70 6 2 -12 -11.70 6.90 -6 -2 12 -17.70 7.80 5 2 -12 14.30 6.10 -5 -2 12 -0.50 7.30 4 2 -12 18.90 5.80 -4 -2 12 15.00 7.60 3 2 -12 -2.00 5.10 -3 -2 12 -14.30 7.10 2 2 -12 475.45 20.30 -2 -2 12 467.75 25.80 1 2 -12 272.57 14.80 -1 -2 12 286.07 22.40 0 2 -12 17.10 5.90 0 -2 12 24.40 6.20 0 -2 12 19.00 11.60 -1 2 -12 0.10 5.60 1 -2 12 -0.30 6.50 1 -2 12 12.20 13.50 -2 2 -12 21.50 12.10 -2 2 -12 19.80 6.70 2 -2 12 15.60 7.60 -3 2 -12 13.70 13.80 -3 2 -12 3.50 7.10 3 -2 12 -3.00 8.30 6 1 -12 1.70 7.20 -6 -1 12 -6.10 7.70 5 1 -12 12.60 6.50 -5 -1 12 16.20 7.40 4 1 -12 -7.40 5.90 -4 -1 12 0.20 6.60 3 1 -12 26.40 6.00 -3 -1 12 28.60 7.90 2 1 -12 31.30 6.00 -2 -1 12 19.90 8.80 1 1 -12 53.29 8.10 -1 -1 12 68.49 11.70 0 1 -12 320.37 16.70 0 -1 12 286.67 16.20 0 -1 12 300.87 24.00 -1 1 -12 53.59 7.80 1 -1 12 41.20 14.80 1 -1 12 65.59 9.20 -2 1 -12 17.20 6.70 -2 1 -12 5.30 12.20 2 -1 12 6.70 8.00 -3 1 -12 40.00 9.10 -3 1 -12 47.70 15.80 3 -1 12 46.10 11.30 6 0 -12 19.60 7.10 -6 0 12 -0.40 8.40 5 0 -12 2.50 6.40 -5 0 12 -1.50 7.10 4 0 -12 132.89 11.30 -4 0 12 111.09 12.40 3 0 -12 38.00 6.60 -3 0 12 35.40 7.80 2 0 -12 44.00 6.80 1 0 -12 57.09 8.20 0 0 -12 22.10 6.10 0 0 12 17.20 7.40 -1 0 -12 46.00 8.20 1 0 12 44.80 9.50 1 0 12 54.79 14.90 -2 0 -12 166.58 15.10 2 0 12 166.18 21.50 -3 0 -12 -6.70 8.10 -3 0 -12 -6.70 13.10 3 0 12 12.70 10.20 6 -1 -12 10.00 7.50 -6 1 12 23.30 8.70 5 -1 -12 91.09 11.50 -5 1 12 61.99 9.10 4 -1 -12 43.50 7.70 -4 1 12 52.29 8.30 3 -1 -12 276.77 15.70 2 -1 -12 40.10 6.90 -2 1 12 33.60 15.60 1 -1 -12 154.98 12.60 -1 1 12 132.19 13.10 -1 1 12 154.98 16.40 0 -1 -12 53.69 7.80 0 1 12 61.99 10.30 -1 -1 -12 9.00 6.80 1 1 12 16.80 9.30 -2 -1 -12 13.80 8.30 2 1 12 17.50 15.40 2 1 12 7.60 10.10 -3 -1 -12 69.69 11.90 -3 -1 -12 99.49 17.70 3 1 12 78.89 14.10 5 -2 -12 38.80 8.50 -5 2 12 27.40 8.40 4 -2 -12 5.90 6.60 -4 2 12 -1.10 7.00 3 -2 -12 10.40 6.70 -3 2 12 21.30 8.10 2 -2 -12 10.00 6.30 -2 2 12 -2.50 13.40 1 -2 -12 30.40 7.70 -1 2 12 28.40 8.80 -1 2 12 21.90 8.50 0 -2 -12 134.09 15.00 0 2 12 172.28 27.40 0 2 12 136.09 16.60 -1 -2 -12 55.69 9.20 1 2 12 104.29 20.10 2 2 12 32.90 17.00 2 2 12 32.00 12.10 -3 -2 -12 41.50 14.40 -3 -2 -12 41.90 12.40 3 2 12 23.20 13.70 5 -3 -12 1.80 7.60 -5 3 12 4.20 7.60 4 -3 -12 11.40 7.40 3 -3 -12 129.29 13.90 -3 3 12 87.99 11.30 2 -3 -12 26.60 7.60 -2 3 12 16.60 6.70 -2 3 12 29.40 16.20 1 -3 -12 17.20 7.10 -1 3 12 9.10 9.00 -1 3 12 9.10 7.00 0 -3 -12 25.20 8.40 0 3 12 36.30 9.60 0 3 12 35.30 11.00 -1 -3 -12 102.89 13.20 1 3 12 119.39 15.90 1 3 12 93.89 14.20 -2 -3 -12 -0.80 10.40 2 3 12 4.30 13.30 4 -4 -12 6.80 8.10 3 -4 -12 1.40 8.30 2 -4 -12 32.10 9.30 1 -4 -12 -1.10 8.70 -1 4 12 -1.10 22.60 0 -4 -12 35.10 9.70 0 4 12 4.10 12.60 -1 -4 -12 46.40 12.80 1 4 12 13.00 12.90 -1 5 12 0.10 13.20 1 6 -13 -1.90 6.80 -1 -6 13 8.10 19.50 3 5 -13 89.89 11.40 -3 -5 13 54.49 12.30 2 5 -13 -0.40 6.20 -2 -5 13 4.30 11.80 1 5 -13 37.80 7.20 -1 -5 13 34.00 14.00 0 5 -13 36.50 7.80 0 -5 13 33.20 16.10 -1 5 -13 17.90 7.60 1 -5 13 31.40 18.90 4 4 -13 -6.20 6.80 -4 -4 13 -6.60 8.60 3 4 -13 20.20 6.70 -3 -4 13 5.60 9.70 2 4 -13 49.70 7.10 -2 -4 13 72.49 13.60 1 4 -13 7.80 6.90 -1 -4 13 23.30 12.40 0 4 -13 17.30 6.60 0 -4 13 25.40 15.00 -1 4 -13 74.69 9.50 1 -4 13 53.59 19.70 5 3 -13 2.30 7.60 -5 -3 13 18.60 9.60 -4 -3 13 40.70 10.20 3 3 -13 4.90 6.20 -3 -3 13 7.40 9.70 2 3 -13 5.60 5.90 -2 -3 13 10.40 10.40 1 3 -13 22.00 7.00 -1 -3 13 30.30 12.60 0 3 -13 -0.30 6.50 0 -3 13 4.40 13.70 -1 3 -13 -5.90 6.50 1 -3 13 9.70 16.40 -2 3 -13 6.10 7.60 2 -3 13 4.10 19.20 5 2 -13 20.50 7.40 -5 -2 13 6.10 8.90 4 2 -13 7.60 6.30 -4 -2 13 18.10 8.90 3 2 -13 35.30 7.10 -3 -2 13 27.70 10.00 2 2 -13 -14.50 5.30 -2 -2 13 15.30 10.10 1 2 -13 6.20 5.80 -1 -2 13 10.90 11.60 0 2 -13 11.10 6.30 0 -2 13 26.70 13.60 -1 2 -13 59.89 9.40 1 -2 13 57.89 17.20 -2 2 -13 -1.30 7.50 2 -2 13 7.60 9.80 2 -2 13 11.90 17.80 5 1 -13 4.90 7.50 -5 -1 13 -1.80 8.70 4 1 -13 29.80 7.80 -4 -1 13 22.20 8.70 3 1 -13 -2.10 6.40 -3 -1 13 20.30 8.60 2 1 -13 1.20 5.60 -2 -1 13 6.50 9.60 1 1 -13 -2.70 6.10 -1 -1 13 0.80 10.60 0 1 -13 16.40 7.10 0 -1 13 11.00 12.90 -1 1 -13 -13.80 6.90 1 -1 13 17.00 14.50 1 -1 13 -25.80 14.70 -2 1 -13 46.90 8.90 2 -1 13 31.90 19.10 2 -1 13 46.20 11.30 5 0 -13 42.40 8.40 -5 0 13 55.49 10.10 4 0 -13 13.70 7.20 -4 0 13 9.10 7.70 3 0 -13 45.50 7.30 -3 0 13 45.30 9.30 2 0 -13 7.20 6.20 -2 0 13 -3.70 8.90 1 0 -13 7.10 6.20 -1 0 13 4.70 10.20 0 0 -13 -1.90 7.30 0 0 13 17.00 12.00 -1 0 -13 -3.60 7.40 1 0 13 25.40 10.60 1 0 13 5.50 14.90 -2 0 -13 63.69 11.10 2 0 13 57.49 12.70 2 0 13 84.59 20.60 5 -1 -13 -0.20 8.10 -5 1 13 2.00 8.60 4 -1 -13 -2.90 7.40 -4 1 13 -6.10 8.20 3 -1 -13 8.20 7.00 -3 1 13 14.20 8.10 2 -1 -13 80.49 9.40 -2 1 13 87.29 11.70 1 -1 -13 6.40 7.30 -1 1 13 -1.80 9.40 0 -1 -13 75.99 9.80 0 1 13 127.49 16.60 -1 -1 -13 10.30 9.00 1 1 13 24.60 15.00 1 1 13 14.70 12.60 -2 -1 -13 16.70 10.20 2 1 13 16.30 19.30 2 1 13 5.80 13.00 4 -2 -13 -0.40 8.00 -4 2 13 8.70 8.30 3 -2 -13 -3.40 7.50 -3 2 13 15.10 8.10 2 -2 -13 2.80 7.60 -2 2 13 2.60 9.10 1 -2 -13 27.50 8.60 0 -2 -13 9.20 9.30 0 2 13 18.10 12.70 -1 -2 -13 59.79 11.00 1 2 13 71.79 17.40 1 2 13 102.79 15.60 3 -3 -13 7.60 8.60 2 -3 -13 2.60 9.20 1 -3 -13 9.20 9.30 0 -3 -13 -5.90 9.60 2 4 -14 -5.50 7.90 -2 -4 14 7.70 13.00 1 4 -14 11.90 7.90 -1 -4 14 6.50 15.00 3 3 -14 3.00 7.90 -3 -3 14 -2.40 10.60 2 3 -14 10.70 7.60 -2 -3 14 22.60 13.00 1 3 -14 43.60 8.60 -1 -3 14 -14.00 13.40 0 3 -14 29.10 8.10 0 -3 14 45.60 18.20 3 2 -14 45.00 9.00 -3 -2 14 52.49 12.00 2 2 -14 6.20 7.10 -2 -2 14 2.60 11.30 1 2 -14 1.20 7.00 -1 -2 14 1.80 12.90 0 2 -14 -2.60 7.20 0 -2 14 -12.80 15.40 3 1 -14 -12.00 7.70 -3 -1 14 28.40 10.30 2 1 -14 29.60 8.10 -2 -1 14 21.20 11.60 1 1 -14 -12.80 7.00 -1 -1 14 -18.40 12.20 0 1 -14 3.60 8.10 0 -1 14 1.50 14.90 3 0 -14 20.10 8.70 -3 0 14 22.80 9.60 2 0 -14 16.80 8.00 -2 0 14 13.70 10.40 1 0 -14 15.90 7.90 -1 0 14 22.90 13.00 0 0 -14 20.30 8.60 0 0 14 25.00 15.00 2 -1 -14 -5.90 8.40 -2 1 14 -1.90 10.20 1 -1 -14 3.10 8.50 -1 1 14 -2.10 12.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 69455 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 K1 K 1.16431(9) 0.23305(8) 0.01669(6) 0.0467(2) Uani 1 1 d . . . . . C1 C 0.2434(5) 0.0852(3) 0.3449(3) 0.0436(7) Uani 1 1 d . . . . . H1A H 0.139454 0.026672 0.290141 0.052 Uiso 1 1 calc R U . . . H1B H 0.257692 0.044097 0.423077 0.052 Uiso 1 1 calc R U . . . C2 C 0.4206(4) 0.0616(3) 0.2930(2) 0.0384(6) Uani 1 1 d . . . . . C3 C 0.6189(4) 0.0730(3) 0.1772(3) 0.0409(7) Uani 1 1 d . . . . . C4 C 0.0890(4) 0.4656(3) 0.3056(2) 0.0336(6) Uani 1 1 d . . . . . C5 C 0.1859(4) 0.5060(3) 0.4263(2) 0.0317(5) Uani 1 1 d . . . . . C6 C 0.2593(4) 0.3616(3) 0.4602(2) 0.0326(6) Uani 1 1 d . . . . . N1 N 0.5565(4) -0.0216(3) 0.3417(2) 0.0553(7) Uani 1 1 d . . . . . N2 N 0.4509(3) 0.1237(3) 0.1910(2) 0.0358(5) Uani 1 1 d . . . . . N3 N 0.7365(4) 0.0811(3) 0.0942(3) 0.0516(7) Uani 1 1 d . . . . . N4 N 0.6865(4) 0.1749(3) 0.0089(3) 0.0516(7) Uani 1 1 d . . . . . N5 N 0.1996(3) 0.2529(2) 0.36191(19) 0.0351(5) Uani 1 1 d . . . . . N6 N 0.0965(3) 0.3151(3) 0.2664(2) 0.0366(5) Uani 1 1 d . . . . . N7 N -0.0146(4) 0.5609(3) 0.2191(2) 0.0445(6) Uani 1 1 d . . . . . N8 N 0.2122(3) 0.6500(3) 0.5050(2) 0.0433(6) Uani 1 1 d . . . . . N9 N 0.3661(4) 0.3286(3) 0.5621(2) 0.0442(6) Uani 1 1 d . . . . . H9A H 0.401535 0.233085 0.568400 0.053 Uiso 1 1 calc R U . . . H9B H 0.400141 0.402623 0.621933 0.053 Uiso 1 1 calc R U . . . O1 O 0.6931(3) -0.0160(3) 0.2644(2) 0.0591(6) Uani 1 1 d . . . . . O2 O 0.7924(3) 0.1756(3) -0.0693(2) 0.0740(8) Uani 1 1 d . . . . . O3 O 0.5446(3) 0.2580(3) 0.0028(2) 0.0591(6) Uani 1 1 d . . . . . O4 O -0.0721(5) 0.4988(3) 0.1171(3) 0.0997(12) Uani 1 1 d . . . . . O5 O -0.0367(7) 0.6942(4) 0.2479(3) 0.1381(19) Uani 1 1 d . . . . . O6 O 0.1464(5) 0.7693(3) 0.4701(3) 0.1083(13) Uani 1 1 d . . . . . O7 O 0.3003(3) 0.6471(3) 0.6088(2) 0.0545(6) Uani 1 1 d . . . . . O8 O 1.4374(5) 0.5210(3) 0.1858(3) 0.0771(8) Uani 1 1 d D . . . . H8A H 1.512(6) 0.455(4) 0.156(4) 0.116 Uiso 1 1 d D U . . . H8B H 1.425(7) 0.596(4) 0.142(4) 0.116 Uiso 1 1 d D U . . . 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 K1 0.0477(4) 0.0489(4) 0.0402(4) 0.0052(3) -0.0024(3) 0.0181(3) C1 0.0666(19) 0.0245(13) 0.0403(15) 0.0070(11) 0.0081(14) 0.0049(12) C2 0.0564(17) 0.0220(12) 0.0319(13) 0.0009(10) -0.0049(12) 0.0091(11) C3 0.0414(15) 0.0311(14) 0.0417(15) -0.0088(11) -0.0079(12) 0.0101(12) C4 0.0335(13) 0.0325(13) 0.0371(14) 0.0098(11) 0.0084(11) 0.0041(10) C5 0.0357(13) 0.0259(12) 0.0361(13) 0.0055(10) 0.0126(11) 0.0033(10) C6 0.0363(14) 0.0313(13) 0.0330(13) 0.0071(10) 0.0115(11) 0.0035(10) N1 0.0740(19) 0.0390(14) 0.0484(15) 0.0095(11) -0.0065(14) 0.0216(13) N2 0.0389(12) 0.0328(12) 0.0324(12) 0.0010(9) -0.0017(9) 0.0090(9) N3 0.0387(14) 0.0521(16) 0.0565(16) -0.0150(13) 0.0023(12) 0.0102(12) N4 0.0393(14) 0.0545(16) 0.0556(16) -0.0160(13) 0.0103(12) -0.0131(12) N5 0.0472(13) 0.0263(11) 0.0327(11) 0.0067(9) 0.0067(10) 0.0068(9) N6 0.0416(13) 0.0342(12) 0.0347(12) 0.0085(9) 0.0051(10) 0.0052(10) N7 0.0531(15) 0.0416(14) 0.0427(14) 0.0143(11) 0.0124(12) 0.0162(11) N8 0.0422(13) 0.0287(12) 0.0574(16) 0.0035(11) 0.0057(12) 0.0002(10) N9 0.0607(16) 0.0344(12) 0.0364(12) 0.0086(10) 0.0016(11) 0.0091(11) O1 0.0605(14) 0.0482(13) 0.0625(14) 0.0040(11) -0.0060(12) 0.0301(11) O2 0.0540(14) 0.094(2) 0.0712(17) -0.0204(14) 0.0276(13) -0.0208(13) O3 0.0525(13) 0.0607(14) 0.0711(16) 0.0185(12) 0.0229(12) 0.0082(11) O4 0.140(3) 0.0567(16) 0.077(2) 0.0122(14) -0.0573(19) 0.0114(17) O5 0.274(5) 0.072(2) 0.0558(17) 0.0030(15) -0.009(2) 0.100(3) O6 0.144(3) 0.0301(13) 0.121(3) -0.0011(14) -0.059(2) 0.0166(15) O7 0.0727(15) 0.0427(12) 0.0441(12) -0.0028(9) 0.0050(11) 0.0003(10) O8 0.106(2) 0.0611(17) 0.0730(18) 0.0155(14) 0.0367(16) 0.0102(15) 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' K K 0.2009 0.2494 '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 O2 K1 O3 156.20(8) . 1_655 ? O2 K1 N2 138.26(8) . 1_655 ? O3 K1 N2 57.44(7) 1_655 1_655 ? O2 K1 O4 78.62(10) . 2_665 ? O3 K1 O4 92.79(9) 1_655 2_665 ? N2 K1 O4 141.52(8) 1_655 2_665 ? O2 K1 N6 92.18(7) . 1_655 ? O3 K1 N6 111.62(7) 1_655 1_655 ? N2 K1 N6 67.71(6) 1_655 1_655 ? O4 K1 N6 108.81(8) 2_665 1_655 ? O2 K1 N3 92.08(8) . 2_755 ? O3 K1 N3 74.43(7) 1_655 2_755 ? N2 K1 N3 74.12(7) 1_655 2_755 ? O4 K1 N3 124.53(9) 2_665 2_755 ? N6 K1 N3 126.25(8) 1_655 2_755 ? O2 K1 O4 69.02(8) . 1_655 ? O3 K1 O4 125.55(9) 1_655 1_655 ? N2 K1 O4 115.39(7) 1_655 1_655 ? O4 K1 O4 59.83(13) 2_665 1_655 ? N6 K1 O4 51.40(7) 1_655 1_655 ? N3 K1 O4 160.01(9) 2_755 1_655 ? O2 K1 O5 65.73(12) . 2_665 ? O3 K1 O5 93.40(11) 1_655 2_665 ? N2 K1 O5 147.99(10) 1_655 2_665 ? O4 K1 O5 40.01(8) 2_665 2_665 ? N6 K1 O5 142.58(8) 1_655 2_665 ? N3 K1 O5 86.18(8) 2_755 2_665 ? O4 K1 O5 91.56(8) 1_655 2_665 ? O2 K1 O8 137.80(8) . . ? O3 K1 O8 59.10(7) 1_655 . ? N2 K1 O8 66.49(7) 1_655 . ? O4 K1 O8 77.61(8) 2_665 . ? N6 K1 O8 63.79(6) 1_655 . ? N3 K1 O8 130.10(7) 2_755 . ? O4 K1 O8 68.93(8) 1_655 . ? O5 K1 O8 112.12(10) 2_665 . ? O2 K1 N7 68.91(8) . 2_665 ? O3 K1 N7 95.59(7) 1_655 2_665 ? N2 K1 N7 152.47(7) 1_655 2_665 ? O4 K1 N7 20.25(7) 2_665 2_665 ? N6 K1 N7 125.35(6) 1_655 2_665 ? N3 K1 N7 105.95(7) 2_755 2_665 ? O4 K1 N7 74.08(7) 1_655 2_665 ? O5 K1 N7 20.01(7) 2_665 2_665 ? O8 K1 N7 96.19(7) . 2_665 ? O2 K1 K1 52.59(7) . 2_755 ? O3 K1 K1 124.30(6) 1_655 2_755 ? N2 K1 K1 90.05(5) 1_655 2_755 ? O4 K1 K1 128.35(6) 2_665 2_755 ? N6 K1 K1 90.79(5) 1_655 2_755 ? N3 K1 K1 52.31(6) 2_755 2_755 ? O4 K1 K1 108.56(7) 1_655 2_755 ? O5 K1 K1 97.67(9) 2_665 2_755 ? O8 K1 K1 150.05(5) . 2_755 ? N7 K1 K1 112.10(5) 2_665 2_755 ? N5 C1 C2 110.9(2) . . ? N5 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N5 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N1 C2 N2 115.4(3) . . ? N1 C2 C1 121.7(3) . . ? N2 C2 C1 122.8(2) . . ? N2 C3 O1 112.7(3) . . ? N2 C3 N3 136.4(3) . . ? O1 C3 N3 110.8(2) . . ? N6 C4 C5 112.8(2) . . ? N6 C4 N7 115.5(2) . . ? C5 C4 N7 131.6(2) . . ? N8 C5 C4 132.6(2) . . ? N8 C5 C6 123.2(2) . . ? C4 C5 C6 104.2(2) . . ? N9 C6 N5 123.9(2) . . ? N9 C6 C5 131.1(2) . . ? N5 C6 C5 105.0(2) . . ? C2 N1 O1 103.5(2) . . ? C3 N2 C2 102.6(2) . . ? C3 N2 K1 129.11(18) . 1_455 ? C2 N2 K1 125.00(18) . 1_455 ? N4 N3 C3 116.8(2) . . ? N4 N3 K1 110.62(18) . 2_755 ? C3 N3 K1 113.02(19) . 2_755 ? O3 N4 O2 119.9(3) . . ? O3 N4 N3 124.4(3) . . ? O2 N4 N3 115.7(3) . . ? C6 N5 N6 113.5(2) . . ? C6 N5 C1 128.1(2) . . ? N6 N5 C1 118.3(2) . . ? C4 N6 N5 104.5(2) . . ? C4 N6 K1 116.99(16) . 1_455 ? N5 N6 K1 121.65(15) . 1_455 ? O5 N7 O4 121.3(3) . . ? O5 N7 C4 120.4(3) . . ? O4 N7 C4 118.3(2) . . ? O5 N7 K1 65.67(18) . 2_665 ? O4 N7 K1 56.89(16) . 2_665 ? C4 N7 K1 166.14(17) . 2_665 ? O6 N8 O7 122.6(3) . . ? O6 N8 C5 119.8(3) . . ? O7 N8 C5 117.5(2) . . ? C6 N9 H9A 120.0 . . ? C6 N9 H9B 120.0 . . ? H9A N9 H9B 120.0 . . ? C3 O1 N1 105.9(2) . . ? N4 O2 K1 116.4(2) . . ? N4 O3 K1 139.4(2) . 1_455 ? N7 O4 K1 102.86(19) . 2_665 ? N7 O4 K1 116.3(2) . 1_455 ? K1 O4 K1 120.17(13) 2_665 1_455 ? N7 O5 K1 94.3(2) . 2_665 ? K1 O8 H8A 74(4) . . ? K1 O8 H8B 103(4) . . ? H8A O8 H8B 108(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 K1 O2 2.694(3) . ? K1 O3 2.760(2) 1_655 ? K1 N2 2.831(2) 1_655 ? K1 O4 2.899(3) 2_665 ? K1 N6 2.908(2) 1_655 ? K1 N3 2.942(3) 2_755 ? K1 O4 3.046(3) 1_655 ? K1 O5 3.084(3) 2_665 ? K1 O8 3.302(3) . ? K1 N7 3.375(2) 2_665 ? K1 K1 4.5323(15) 2_755 ? C1 N5 1.457(3) . ? C1 C2 1.485(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N1 1.294(3) . ? C2 N2 1.361(4) . ? C3 N2 1.307(3) . ? C3 O1 1.349(3) . ? C3 N3 1.358(4) . ? C4 N6 1.304(3) . ? C4 C5 1.408(4) . ? C4 N7 1.451(3) . ? C5 N8 1.406(3) . ? C5 C6 1.409(3) . ? C6 N9 1.323(3) . ? C6 N5 1.350(3) . ? N1 O1 1.412(4) . ? N3 N4 1.323(4) . ? N4 O3 1.240(3) . ? N4 O2 1.248(3) . ? N5 N6 1.359(3) . ? N7 O5 1.158(4) . ? N7 O4 1.198(4) . ? N8 O6 1.203(3) . ? N8 O7 1.227(3) . ? N9 H9A 0.8600 . ? N9 H9B 0.8600 . ? O8 H8A 0.853(19) . ? O8 H8B 0.850(19) . ? 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 _geom_hbond_publ_flag C1 H1B O6 0.97 2.60 3.297(4) 128.6 1_545 yes N9 H9A N1 0.86 2.16 2.965(3) 154.7 2_656 yes N9 H9B O7 0.86 2.22 2.751(3) 120.1 . yes N9 H9B O8 0.86 2.28 3.047(4) 149.0 2_766 yes O8 H8A O3 0.853(19) 2.28(3) 3.027(4) 146(5) 1_655 yes O8 H8B O2 0.850(19) 2.62(3) 3.353(4) 145(4) 2_765 yes O8 H8B O3 0.850(19) 2.19(3) 3.009(3) 161(4) 2_765 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 C1 C2 N1 129.5(3) . . . . ? N5 C1 C2 N2 -51.3(3) . . . . ? N6 C4 C5 N8 -178.7(3) . . . . ? N7 C4 C5 N8 1.7(5) . . . . ? N6 C4 C5 C6 0.5(3) . . . . ? N7 C4 C5 C6 -179.0(3) . . . . ? N8 C5 C6 N9 -2.5(4) . . . . ? C4 C5 C6 N9 178.1(3) . . . . ? N8 C5 C6 N5 178.4(2) . . . . ? C4 C5 C6 N5 -0.9(3) . . . . ? N2 C2 N1 O1 -0.2(3) . . . . ? C1 C2 N1 O1 179.1(2) . . . . ? O1 C3 N2 C2 -0.1(3) . . . . ? N3 C3 N2 C2 176.5(3) . . . . ? O1 C3 N2 K1 -159.88(17) . . . 1_455 ? N3 C3 N2 K1 16.7(5) . . . 1_455 ? N1 C2 N2 C3 0.2(3) . . . . ? C1 C2 N2 C3 -179.1(2) . . . . ? N1 C2 N2 K1 161.09(19) . . . 1_455 ? C1 C2 N2 K1 -18.2(3) . . . 1_455 ? N2 C3 N3 N4 8.3(5) . . . . ? O1 C3 N3 N4 -175.0(2) . . . . ? N2 C3 N3 K1 -121.7(3) . . . 2_755 ? O1 C3 N3 K1 55.0(3) . . . 2_755 ? C3 N3 N4 O3 2.3(4) . . . . ? K1 N3 N4 O3 133.5(2) 2_755 . . . ? C3 N3 N4 O2 -177.2(2) . . . . ? K1 N3 N4 O2 -46.1(3) 2_755 . . . ? N9 C6 N5 N6 -178.0(2) . . . . ? C5 C6 N5 N6 1.1(3) . . . . ? N9 C6 N5 C1 -2.7(4) . . . . ? C5 C6 N5 C1 176.5(3) . . . . ? C2 C1 N5 C6 -87.8(3) . . . . ? C2 C1 N5 N6 87.4(3) . . . . ? C5 C4 N6 N5 0.1(3) . . . . ? N7 C4 N6 N5 179.8(2) . . . . ? C5 C4 N6 K1 -137.57(18) . . . 1_455 ? N7 C4 N6 K1 42.1(3) . . . 1_455 ? C6 N5 N6 C4 -0.8(3) . . . . ? C1 N5 N6 C4 -176.7(2) . . . . ? C6 N5 N6 K1 134.41(18) . . . 1_455 ? C1 N5 N6 K1 -41.5(3) . . . 1_455 ? N6 C4 N7 O5 176.2(4) . . . . ? C5 C4 N7 O5 -4.2(5) . . . . ? N6 C4 N7 O4 -5.5(4) . . . . ? C5 C4 N7 O4 174.1(3) . . . . ? N6 C4 N7 K1 -71.3(8) . . . 2_665 ? C5 C4 N7 K1 108.3(7) . . . 2_665 ? C4 C5 N8 O6 -1.3(5) . . . . ? C6 C5 N8 O6 179.6(3) . . . . ? C4 C5 N8 O7 177.6(3) . . . . ? C6 C5 N8 O7 -1.5(4) . . . . ? N2 C3 O1 N1 0.0(3) . . . . ? N3 C3 O1 N1 -177.5(2) . . . . ? C2 N1 O1 C3 0.1(3) . . . . ? O3 N4 O2 K1 127.7(2) . . . . ? N3 N4 O2 K1 -52.8(3) . . . . ? O2 N4 O3 K1 133.3(3) . . . 1_455 ? N3 N4 O3 K1 -46.2(4) . . . 1_455 ? O5 N7 O4 K1 13.4(5) . . . 2_665 ? C4 N7 O4 K1 -164.88(19) . . . 2_665 ? O5 N7 O4 K1 146.9(4) . . . 1_455 ? C4 N7 O4 K1 -31.4(4) . . . 1_455 ? K1 N7 O4 K1 133.5(3) 2_665 . . 1_455 ? O4 N7 O5 K1 -12.3(4) . . . 2_665 ? C4 N7 O5 K1 165.9(2) . . . 2_665 ?