#------------------------------------------------------------------------------ #$Date: 2023-11-10 04:00:10 +0200 (Fri, 10 Nov 2023) $ #$Revision: 287506 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247691.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_7247691 loop_ _publ_author_name 'Atceken, Nurunnisa' 'Hemingway, Jack' 'Bull, Craig L.' 'Liu, Xiaojiao' 'Michalchuk, Adam A.L.' 'Konar, Sumit' 'Morrison, Carole' 'Pulham, Colin R.' _publ_section_title ; High-pressure Structural Studies and Pressure-induced Sensitisation of 3,4,5-trinitro-1H-pyrazole ; _journal_name_full 'Physical Chemistry Chemical Physics' _journal_paper_doi 10.1039/D3CP04526A _journal_year 2023 _chemical_formula_moiety '3(C3 H N5 O6)' _chemical_formula_sum 'C9 H3 N15 O18' _chemical_formula_weight 609.26 _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' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _audit_block_doi 10.5517/ccdc.csd.cc29gp4m _audit_creation_date 2021-12-16 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _audit_update_record ; 2021-12-16 deposited with the CCDC. 2023-11-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.018(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.6452(10) _cell_length_b 7.9546(7) _cell_length_c 16.7946(9) _cell_measurement_reflns_used 2710 _cell_measurement_temperature 298.4 _cell_measurement_theta_max 23.80 _cell_measurement_theta_min 2.78 _cell_volume 1955.3(2) _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 298.4 _diffrn_measured_fraction_theta_full 0.551 _diffrn_measured_fraction_theta_max 0.509 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_unetI/netI 0.0529 _diffrn_reflns_Laue_measured_fraction_full 0.551 _diffrn_reflns_Laue_measured_fraction_max 0.509 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 10399 _diffrn_reflns_point_group_measured_fraction_full 0.551 _diffrn_reflns_point_group_measured_fraction_max 0.509 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.369 _diffrn_reflns_theta_min 2.427 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.201 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6801 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.070 _exptl_crystal_description block _exptl_crystal_F_000 1224 _refine_diff_density_max 0.186 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 391 _refine_ls_number_reflns 2028 _refine_ls_number_restraints 306 _refine_ls_restrained_S_all 0.993 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0458 _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^)+(0.0822P)^2^+1.1680P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1243 _refine_ls_wR_factor_ref 0.1430 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1445 _reflns_number_total 2028 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3cp04526a2.cif _cod_data_source_block 2tnp_p05 _cod_database_code 7247691 _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. ; _olex2_refinement_description ; 1. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 ; _shelx_res_file ; TITL 2tnp_p05_a.res in P2(1)/c 2tnp_p05.res created by SHELXL-2018/3 at 15:49:54 on 16-Dec-2021 REM Old TITL 2TNP_P05 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.204, Rweak 0.008, Alpha 0.113 REM 0.462 for 99 systematic absences, Orientation as input REM Formula found by SHELXT: C32 N O9 CELL 0.71073 14.6452 7.9546 16.7946 90 92.018 90 ZERR 4 0.001 0.0007 0.0009 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 36 12 60 72 RIGU L.S. 10 PLAN 5 TEMP 25.25 CONF list 4 MORE -1 BOND $H fmap 2 53 acta OMIT -8 6 1 OMIT -7 1 1 OMIT 7 0 2 OMIT 1 2 7 REM REM REM WGHT 0.082200 1.168000 FVAR 0.69548 O001 4 0.519395 0.500795 0.811268 11.00000 0.03792 0.04740 = 0.03060 -0.00665 0.00496 0.01864 O002 4 0.685766 0.593441 0.652235 11.00000 0.05445 0.03400 = 0.04167 0.01131 0.00711 -0.01373 O003 4 0.659925 0.423198 0.833371 11.00000 0.02698 0.05416 = 0.02933 -0.00928 -0.00596 -0.00002 O004 4 0.981577 0.451918 0.173314 11.00000 0.03391 0.07283 = 0.03288 0.01375 0.00249 -0.01441 O005 4 0.837129 0.601286 0.354934 11.00000 0.06031 0.03343 = 0.04586 -0.01008 0.01529 0.01441 O006 4 0.560844 0.129983 0.478330 11.00000 0.04782 0.05410 = 0.03106 -0.01977 0.00455 0.00254 N007 3 0.758241 0.938616 0.463918 11.00000 0.02573 0.02037 = 0.01928 -0.00087 0.00065 -0.00016 O008 4 0.455207 0.315057 0.496313 11.00000 0.03243 0.07591 = 0.03243 -0.00875 -0.00556 0.01340 O009 4 0.923912 0.103198 0.508981 11.00000 0.03674 0.07353 = 0.04183 0.03360 0.00210 -0.00638 N00A 3 0.724693 0.942251 0.536536 11.00000 0.02638 0.02657 = 0.01748 -0.00048 0.00272 0.00014 N00B 3 0.687972 0.741916 0.635920 11.00000 0.02794 0.03724 = 0.02201 0.00246 0.00768 -0.00434 O00C 4 0.695177 0.412536 0.483414 11.00000 0.04948 0.03580 = 0.05385 -0.00355 0.00225 -0.01402 O00D 4 1.122546 0.283714 0.339548 11.00000 0.01906 0.08261 = 0.05238 0.00900 0.00261 0.00750 N00E 3 0.637681 0.204188 0.623156 11.00000 0.02370 0.02465 = 0.02289 -0.00266 0.00510 0.00578 O00F 4 0.835893 0.406125 0.155059 11.00000 0.03376 0.07882 = 0.03360 0.02132 -0.00851 -0.00635 N00G 3 0.815772 0.744966 0.366657 11.00000 0.03060 0.02633 = 0.02919 -0.00239 0.00767 0.00291 O00H 4 1.032394 0.283108 0.494060 11.00000 0.03555 0.07702 = 0.03505 0.00961 -0.01020 -0.01211 O00I 4 1.074972 0.539015 0.322363 11.00000 0.06249 0.04498 = 0.05643 0.01679 -0.01829 -0.03030 O00J 4 0.823880 0.862738 0.321314 11.00000 0.07638 0.04005 = 0.03505 0.00727 0.02592 0.00288 O00K 4 0.833212 0.435542 0.529519 11.00000 0.06138 0.03542 = 0.06657 -0.00316 -0.02205 0.01728 N00L 3 0.828678 0.262869 0.299331 11.00000 0.01905 0.02949 = 0.02156 -0.00021 0.00036 -0.00161 O00M 4 0.439470 0.601463 0.654690 11.00000 0.08004 0.04061 = 0.04997 -0.00981 -0.01156 0.03154 N00N 3 0.840766 0.210248 0.374328 11.00000 0.02415 0.02444 = 0.02392 0.00589 -0.00034 -0.00305 N00O 3 0.436040 0.450121 0.655274 11.00000 0.03146 0.04271 = 0.02085 -0.00506 -0.00233 0.01154 N00P 3 0.658067 0.251069 0.698578 11.00000 0.02427 0.03082 = 0.02039 -0.00117 0.00340 0.00403 N00Q 3 0.589040 0.429042 0.793229 11.00000 0.02434 0.02629 = 0.02350 -0.00099 0.00252 0.00277 O00R 4 0.664387 0.855713 0.678538 11.00000 0.09642 0.04626 = 0.03511 -0.00169 0.03166 0.01353 O00S 4 0.367911 0.364326 0.655213 11.00000 0.02451 0.09937 = 0.05100 0.00464 -0.00066 -0.00505 N00T 3 1.062224 0.390635 0.331021 11.00000 0.02315 0.04906 = 0.02306 0.00583 0.00315 -0.00879 N00U 3 0.963820 0.207511 0.471697 11.00000 0.02353 0.04102 = 0.02555 0.00688 0.00175 0.00095 N00V 3 0.522001 0.233025 0.517657 11.00000 0.02566 0.03561 = 0.02711 -0.00479 -0.00136 -0.00191 N00W 3 0.761312 0.493463 0.505311 11.00000 0.03835 0.02334 = 0.02675 0.00091 0.00275 0.00103 N00X 3 0.907452 0.402112 0.194089 11.00000 0.02653 0.04039 = 0.02626 0.00610 -0.00089 -0.00372 C00Y 1 0.721818 0.785094 0.559189 11.00000 0.02013 0.02167 = 0.02113 -0.00015 -0.00249 -0.00250 C00Z 1 0.777842 0.782067 0.441979 11.00000 0.01852 0.01785 = 0.02481 -0.00125 0.00092 0.00220 C010 1 0.587228 0.346697 0.717322 11.00000 0.02134 0.01827 = 0.01740 0.00013 0.00286 -0.00299 C011 1 0.558066 0.267293 0.596831 11.00000 0.02068 0.02702 = 0.02011 0.00026 0.00141 -0.00222 C012 1 0.926944 0.249985 0.393377 11.00000 0.02120 0.02139 = 0.02388 0.00133 0.00142 0.00300 C013 1 0.522307 0.360274 0.656370 11.00000 0.01781 0.01970 = 0.02654 0.00026 0.00176 -0.00028 C014 1 0.970233 0.329616 0.332170 11.00000 0.01422 0.03194 = 0.02228 0.00044 0.00291 0.00214 C015 1 0.904405 0.334695 0.272417 11.00000 0.02378 0.02494 = 0.02309 0.00243 0.00393 0.00253 C016 1 0.754336 0.674266 0.502502 11.00000 0.01792 0.02225 = 0.02748 -0.00062 -0.00052 -0.00089 H00E 2 0.672905 0.127743 0.597663 11.00000 0.03084 H00L 2 0.769296 0.273902 0.272680 11.00000 0.09962 H007 2 0.775663 1.040472 0.432212 11.00000 0.05969 HKLF 4 REM 2tnp_p05_a.res in P2(1)/c REM wR2 = 0.1430, GooF = S = 1.066, Restrained GooF = 0.993 for all data REM R1 = 0.0458 for 1445 Fo > 4sig(Fo) and 0.0761 for all 2028 data REM 391 parameters refined using 306 restraints END WGHT 0.0822 1.1680 REM Highest difference peak 0.186, deepest hole -0.209, 1-sigma level 0.050 Q1 1 0.5433 0.3323 0.7024 11.00000 0.05 0.19 Q2 1 0.9037 0.8541 0.3024 11.00000 0.05 0.18 Q3 1 0.4916 0.6547 0.6783 11.00000 0.05 0.18 Q4 1 0.9015 -0.0462 0.4381 11.00000 0.05 0.17 Q5 1 0.9415 0.3347 0.3028 11.00000 0.05 0.17 ; _shelx_res_checksum 99760 _shelx_hkl_file ; 2 0 0 379.06 23.30 -3 0 0 355.06 22.00 3 0 0 329.07 22.00 -4 0 0 69.79 7.50 4 0 0 70.29 7.60 5 0 0 281.87 19.70 -5 0 0 232.78 19.00 -1 -1 0 220.78 12.80 -1 -1 0 198.98 13.40 -1 -1 0 215.58 12.80 -1 -1 0 215.88 13.00 1 1 0 214.78 13.00 1 1 0 205.78 12.80 1 1 0 209.18 13.50 1 1 0 208.78 12.80 -2 -1 0 2.50 0.90 -2 -1 0 3.60 1.00 -2 -1 0 3.00 1.60 -2 -1 0 -0.10 1.90 -2 -1 0 5.80 1.00 -2 -1 0 4.10 1.80 -2 -1 0 -0.50 1.90 2 1 0 2.20 0.90 2 1 0 3.00 1.80 2 1 0 3.10 2.30 2 1 0 5.80 2.10 2 1 0 1.60 1.50 2 1 0 3.80 1.10 2 1 0 3.50 0.90 -4 -1 0 215.08 14.70 -4 -1 0 204.68 12.80 -4 -1 0 203.78 15.30 -4 -1 0 204.98 13.00 -4 -1 0 199.68 13.70 4 1 0 212.38 12.90 4 1 0 208.88 16.30 4 1 0 214.88 13.20 4 1 0 199.28 14.00 4 1 0 202.58 12.90 -5 -1 0 159.68 10.30 -5 -1 0 160.28 11.50 -5 -1 0 122.39 12.60 -5 -1 0 136.39 12.20 5 1 0 150.78 13.70 5 1 0 152.38 11.80 5 1 0 159.38 10.30 5 1 0 154.18 10.40 -6 -1 0 18.00 6.90 -6 -1 0 8.10 2.70 -6 -1 0 21.20 7.80 -6 -1 0 12.80 2.70 -6 -1 0 11.70 3.10 6 1 0 5.50 7.20 6 1 0 11.30 5.30 6 1 0 9.70 2.80 6 1 0 5.20 2.70 -7 -1 0 829.12 50.49 -7 -1 0 791.72 46.20 -7 -1 0 774.02 49.30 7 1 0 844.12 50.79 7 1 0 761.62 46.50 7 1 0 711.83 46.40 7 1 0 698.43 47.80 -8 -1 0 34.60 5.20 -8 -1 0 36.40 10.40 -8 -1 0 26.20 12.00 -8 -1 0 27.90 4.80 8 1 0 38.50 4.90 8 1 0 18.30 12.20 8 1 0 23.50 7.50 8 1 0 32.30 8.30 8 1 0 34.60 5.00 -9 -1 0 35.50 5.90 -9 -1 0 33.60 5.20 -9 -1 0 45.00 5.80 -9 -1 0 28.90 13.50 -9 -1 0 40.50 12.00 9 1 0 38.60 5.80 9 1 0 30.80 9.10 9 1 0 43.40 5.80 9 1 0 37.90 14.50 -10 -1 0 263.87 26.00 -10 -1 0 277.77 19.70 -10 -1 0 279.37 18.90 -10 -1 0 294.37 19.30 10 1 0 284.47 19.60 10 1 0 254.67 19.10 -11 -1 0 470.75 40.90 -2 -2 0 32.20 3.20 -2 -2 0 35.80 5.40 -2 -2 0 28.00 3.10 -2 -2 0 32.40 4.10 2 2 0 32.30 4.20 2 2 0 22.90 5.30 -3 -2 0 18.70 3.80 -3 -2 0 19.20 4.30 -3 -2 0 24.70 2.80 -3 -2 0 22.00 2.70 -3 -2 0 22.60 5.10 -3 -2 0 22.00 2.90 3 2 0 20.30 4.80 3 2 0 19.40 3.20 3 2 0 29.40 3.00 3 2 0 17.70 4.40 3 2 0 18.80 2.70 3 2 0 24.30 3.00 3 2 0 21.60 3.90 3 2 0 11.40 5.00 -4 -2 0 582.24 34.10 -4 -2 0 594.64 35.80 -4 -2 0 577.24 35.20 4 2 0 605.64 36.50 4 2 0 525.65 34.00 4 2 0 572.84 35.10 4 2 0 548.55 34.30 4 2 0 589.44 36.30 4 2 0 540.35 34.10 -5 -2 0 93.99 10.60 -5 -2 0 101.99 8.00 -5 -2 0 109.49 8.30 -5 -2 0 104.79 9.80 -5 -2 0 88.99 10.60 -5 -2 0 111.79 8.20 5 2 0 98.59 10.90 5 2 0 100.39 10.00 5 2 0 104.19 8.20 5 2 0 109.09 9.40 5 2 0 101.39 8.60 5 2 0 91.79 11.20 5 2 0 114.09 7.90 5 2 0 90.79 10.40 5 2 0 99.49 7.70 -6 -2 0 1422.16 83.49 -6 -2 0 1463.75 83.59 -6 -2 0 1442.16 83.49 -6 -2 0 1364.56 84.69 -6 -2 0 1305.97 85.09 6 2 0 1432.86 83.29 6 2 0 1400.56 84.79 6 2 0 1402.56 83.39 6 2 0 1417.36 83.59 6 2 0 1420.86 83.49 6 2 0 1272.27 85.89 6 2 0 1440.76 83.39 6 2 0 1468.95 86.39 -7 -2 0 35.70 11.40 -7 -2 0 52.29 6.10 -7 -2 0 49.30 8.60 -7 -2 0 58.49 6.40 7 2 0 51.49 6.30 7 2 0 55.09 5.60 7 2 0 45.70 11.20 7 2 0 55.09 5.70 7 2 0 67.29 9.00 7 2 0 56.59 5.50 7 2 0 59.69 10.40 7 2 0 54.89 6.00 -8 -2 0 65.69 13.70 -8 -2 0 70.79 7.30 8 2 0 62.49 10.00 8 2 0 66.79 6.60 8 2 0 43.80 11.60 8 2 0 70.99 6.40 8 2 0 63.69 7.20 8 2 0 60.99 7.00 8 2 0 58.99 15.10 -9 -2 0 -0.30 5.30 -9 -2 0 17.90 14.50 9 2 0 -10.50 11.00 9 2 0 -5.10 13.20 9 2 0 6.70 9.10 9 2 0 5.30 4.60 9 2 0 12.10 4.70 -10 -2 0 162.98 13.60 -10 -2 0 185.68 22.70 10 2 0 179.78 13.40 10 2 0 147.89 19.20 10 2 0 171.48 13.80 -11 -2 0 45.50 19.90 11 2 0 28.10 15.40 11 2 0 41.00 7.10 -12 -2 0 625.94 39.90 -12 -2 0 623.14 51.99 12 2 0 586.74 38.80 12 2 0 614.94 47.50 12 2 0 615.94 38.40 -13 -2 0 138.39 13.20 -13 -2 0 140.49 26.60 13 2 0 110.99 11.60 13 2 0 113.99 21.70 13 2 0 143.39 12.20 -14 -2 0 118.09 27.00 14 2 0 81.49 22.20 -3 -3 0 653.53 39.30 -3 -3 0 666.43 40.30 -3 -3 0 689.33 42.00 -3 -3 0 633.34 39.40 3 3 0 658.53 41.10 3 3 0 611.84 39.40 -4 -3 0 3.30 3.40 -4 -3 0 3.30 7.80 -4 -3 0 3.00 3.70 -4 -3 0 3.10 3.10 -4 -3 0 -0.40 6.20 -4 -3 0 3.40 5.70 4 3 0 1.20 3.80 4 3 0 11.30 3.70 4 3 0 2.60 5.60 4 3 0 11.50 4.50 4 3 0 -4.00 6.50 4 3 0 16.50 3.80 4 3 0 4.50 6.80 4 3 0 17.40 8.60 -5 -3 0 454.55 30.80 -5 -3 0 429.36 28.00 -5 -3 0 430.26 27.80 5 3 0 390.66 29.70 5 3 0 545.25 29.00 5 3 0 502.85 28.10 5 3 0 479.75 28.20 5 3 0 323.17 33.90 5 3 0 398.16 31.60 -6 -3 0 183.58 13.30 -6 -3 0 176.48 16.50 -6 -3 0 159.28 14.80 6 3 0 196.98 18.40 6 3 0 179.88 16.70 6 3 0 164.18 13.20 6 3 0 178.98 13.20 6 3 0 180.28 13.30 6 3 0 182.08 17.50 6 3 0 174.98 14.10 6 3 0 198.88 16.30 -7 -3 0 30.60 8.50 -7 -3 0 22.70 8.70 -7 -3 0 32.90 5.10 -7 -3 0 18.50 5.10 -7 -3 0 22.60 10.60 7 3 0 23.50 11.30 7 3 0 24.30 4.80 7 3 0 23.40 13.30 7 3 0 26.80 5.20 7 3 0 33.60 5.50 7 3 0 19.50 11.10 7 3 0 29.00 5.10 7 3 0 22.40 5.70 -8 -3 0 15.50 10.30 -8 -3 0 22.50 9.80 -8 -3 0 12.80 5.70 -8 -3 0 22.10 12.50 8 3 0 14.30 5.70 8 3 0 20.20 13.50 8 3 0 15.80 5.20 8 3 0 23.40 5.10 8 3 0 18.50 9.30 8 3 0 21.40 13.20 8 3 0 10.40 5.70 8 3 0 26.90 12.70 -9 -3 0 868.51 53.69 -9 -3 0 893.01 56.09 -9 -3 0 874.61 59.59 -9 -3 0 884.61 61.79 9 3 0 903.61 59.19 9 3 0 891.21 54.19 9 3 0 854.61 60.79 9 3 0 876.41 53.49 9 3 0 863.61 53.29 -10 -3 0 424.86 35.50 -10 -3 0 429.56 28.50 -10 -3 0 460.25 39.30 10 3 0 441.06 27.90 10 3 0 416.46 36.00 10 3 0 433.16 40.30 10 3 0 418.26 29.00 10 3 0 436.06 27.90 10 3 0 391.96 28.60 -11 -3 0 347.67 22.20 -11 -3 0 256.17 35.70 11 3 0 261.77 21.20 11 3 0 269.67 31.30 11 3 0 286.97 20.90 11 3 0 339.97 49.50 -12 -3 0 -1.90 7.70 -12 -3 0 -12.90 20.50 -12 -3 0 33.60 20.30 12 3 0 10.10 20.40 12 3 0 11.90 7.00 12 3 0 7.00 6.80 12 3 0 6.90 17.30 -13 -3 0 53.09 23.50 -13 -3 0 54.59 23.00 -13 -3 0 71.29 10.60 13 3 0 96.69 25.50 13 3 0 52.29 20.20 13 3 0 69.29 9.40 -14 -3 0 -5.30 8.40 -14 -3 0 19.80 23.80 -14 -3 0 6.20 22.80 14 3 0 3.50 7.50 14 3 0 1.00 24.10 14 3 0 -8.00 7.50 14 3 0 -16.30 19.70 -15 -3 0 32.70 25.80 -15 -3 0 8.10 25.40 15 3 0 13.00 26.90 15 3 0 18.30 22.70 -16 -3 0 36.50 27.70 -16 -3 0 22.60 27.00 16 3 0 16.60 23.80 16 3 0 -34.60 26.80 -4 -4 0 1360.66 80.59 -4 -4 0 1358.26 78.59 4 4 0 1141.09 78.99 -5 -4 0 3.20 8.60 -5 -4 0 2.50 4.50 -5 -4 0 1.40 10.60 -5 -4 0 6.90 5.10 -5 -4 0 3.30 8.00 -5 -4 0 1.30 4.70 5 4 0 5.70 7.90 5 4 0 7.00 5.10 5 4 0 -8.90 8.60 5 4 0 -13.40 12.00 5 4 0 -5.30 5.90 5 4 0 -3.10 9.00 -6 -4 0 78.49 8.30 -6 -4 0 96.29 12.70 -6 -4 0 85.59 11.50 -6 -4 0 74.89 7.80 6 4 0 78.89 11.00 6 4 0 71.29 8.70 6 4 0 59.29 14.70 6 4 0 94.99 14.30 -7 -4 0 118.09 14.50 -7 -4 0 128.59 10.70 7 4 0 118.99 13.60 7 4 0 138.19 18.60 7 4 0 112.49 10.20 7 4 0 106.99 10.90 7 4 0 102.99 10.20 7 4 0 103.79 17.50 7 4 0 114.19 10.50 7 4 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63.59 11.20 -5 -4 9 116.59 16.80 -5 -4 9 95.59 13.90 5 4 -9 100.59 14.50 5 4 -9 133.89 13.20 -4 -4 9 -2.80 8.30 -4 -4 9 -11.00 8.40 -4 -4 9 -0.80 8.10 4 4 -9 -2.00 8.00 4 4 -9 0.70 7.40 4 4 -9 3.30 7.50 -3 -4 9 319.07 24.20 -3 -4 9 308.17 24.50 -3 -4 9 281.27 24.00 3 4 -9 295.97 22.70 3 4 -9 299.97 23.20 3 4 -9 292.77 24.00 -2 -4 9 34.50 9.10 2 4 -9 33.60 8.90 2 4 -9 41.80 8.40 -1 -4 9 333.97 25.40 1 4 -9 349.27 24.30 1 4 -9 308.47 24.40 0 -4 9 3.40 7.30 0 4 -9 10.70 7.30 0 4 -9 -13.70 6.20 1 -4 9 479.55 34.50 -1 4 -9 545.55 34.30 2 -4 9 179.98 15.70 3 -4 9 91.09 11.00 -9 -4 -9 358.66 32.20 9 4 9 288.27 38.40 9 4 9 390.86 36.60 -10 -4 -9 45.40 18.60 10 4 9 20.50 27.70 10 4 9 39.30 23.00 -11 -4 -9 198.88 26.10 -11 -4 -9 184.98 24.00 11 4 9 223.78 31.20 11 4 9 148.39 32.20 -12 -4 -9 32.40 19.50 12 4 9 6.20 30.90 -13 -4 -9 18.80 20.20 13 4 9 33.40 30.60 -14 -5 9 16.90 15.70 14 5 -9 1.00 13.30 -13 -5 9 32.80 16.10 13 5 -9 19.50 13.30 13 5 -9 -8.00 24.80 -12 -5 9 -29.70 14.10 12 5 -9 -24.00 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6 -9 38.60 15.90 -9 -6 9 19.10 14.70 9 6 -9 29.20 12.80 9 6 -9 5.90 13.70 -8 -6 9 118.99 16.50 8 6 -9 59.59 14.80 8 6 -9 98.19 15.10 -7 -6 9 231.28 22.60 7 6 -9 252.77 22.50 7 6 -9 225.48 21.50 -6 -6 9 -9.50 11.40 -6 -6 9 1.10 11.90 6 6 -9 12.30 11.10 6 6 -9 13.50 11.70 6 6 -9 18.30 12.20 -5 -6 9 -15.60 10.80 -5 -6 9 10.50 11.90 5 6 -9 4.90 10.00 5 6 -9 3.90 11.10 5 6 -9 -4.90 11.40 -4 -6 9 55.09 12.90 -4 -6 9 41.80 8.40 4 6 -9 38.80 12.40 4 6 -9 16.80 10.60 4 6 -9 23.50 11.20 -3 -6 9 43.00 7.80 -3 -6 9 38.20 8.10 -3 -6 9 41.40 12.10 3 6 -9 45.10 11.20 3 6 -9 40.80 11.20 3 6 -9 40.80 10.40 3 6 -9 26.60 10.90 10 7 -9 7.60 15.50 10 7 -9 -13.40 17.10 -9 -7 9 5.10 15.10 9 7 -9 9.90 12.90 9 7 -9 -8.40 14.30 -8 -7 9 -8.70 13.60 8 7 -9 31.60 13.50 8 7 -9 -1.50 14.30 -7 -7 9 4.20 15.80 -7 -7 9 6.10 14.90 7 7 -9 20.60 14.60 7 7 -9 -8.30 12.40 7 7 -9 -22.50 15.10 0 0 -10 3.00 4.70 0 0 -10 -3.00 4.40 0 0 10 0.80 4.70 0 0 10 5.80 4.80 0 0 10 -0.30 5.60 1 0 10 109.19 9.20 1 0 10 100.89 9.90 -1 0 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-10 39.40 6.40 0 1 -10 37.80 5.10 0 1 -10 43.60 7.00 1 -1 10 3626.84 215.38 1 -1 10 3620.74 214.58 1 -1 10 3603.74 215.68 -1 1 -10 3791.02 215.18 -1 1 -10 3605.84 214.78 -1 1 -10 3684.33 214.38 -1 1 -10 3748.43 215.38 -1 1 -10 3516.05 214.98 -1 1 -10 3663.23 214.18 2 -1 10 -0.10 5.50 2 -1 10 6.00 6.60 2 -1 10 5.30 7.30 -2 1 -10 -2.60 5.00 -2 1 -10 4.90 5.30 -2 1 -10 3.30 4.40 -2 1 -10 -1.00 4.60 -2 1 -10 -1.60 4.40 -3 -1 -10 2.10 10.60 -3 -1 -10 -4.10 7.80 3 -1 10 -4.00 8.50 3 -1 10 1.30 5.70 3 -1 10 2.00 8.50 3 -1 10 -5.80 5.50 -3 -1 -10 2.90 4.30 -3 -1 -10 -5.60 8.40 3 1 10 -1.80 4.80 3 1 10 -2.60 9.00 3 1 10 3.70 4.30 -3 1 -10 5.30 5.70 3 1 10 9.20 9.70 -3 1 -10 -1.30 4.50 -3 1 -10 -6.70 4.30 -3 1 -10 4.60 5.50 4 -1 10 274.67 25.80 -4 -1 -10 342.97 25.40 -4 -1 -10 358.96 26.40 4 -1 10 360.06 27.40 4 -1 10 318.67 23.40 -4 1 -10 339.97 21.90 4 1 10 301.47 21.80 4 1 10 357.26 28.50 -4 1 -10 334.07 21.50 -4 1 -10 334.57 21.60 4 1 10 299.07 22.70 -4 1 -10 340.47 22.30 -5 -1 -10 296.87 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30.60 -9 -1 -10 374.96 29.30 9 -1 10 366.36 33.10 -9 1 -10 354.16 32.70 -9 1 -10 368.16 31.60 9 1 10 355.46 36.60 -10 -1 -10 59.89 20.10 10 -1 10 66.39 17.00 -10 1 -10 30.70 19.90 10 1 10 47.00 21.70 11 -1 10 93.79 20.80 -11 -1 -10 118.09 23.90 11 1 10 119.69 26.30 -11 1 -10 103.99 24.50 12 -1 10 12.30 18.00 -12 -1 -10 -2.00 20.50 12 1 10 -32.10 21.00 -12 1 -10 27.10 22.10 -13 -1 -10 -5.00 24.00 13 1 10 16.90 25.70 -14 -1 -10 20.60 28.90 14 1 10 9.30 27.50 -15 -1 -10 63.29 28.40 15 1 10 32.20 29.10 -7 -2 10 54.69 11.00 7 2 -10 71.59 11.30 -6 -2 10 11.30 9.90 -6 -2 10 11.00 8.40 -6 -2 10 10.60 9.70 6 2 -10 6.10 6.00 6 2 -10 1.30 8.10 6 2 -10 17.20 6.80 -5 -2 10 -0.60 7.60 -5 -2 10 1.30 6.80 -5 -2 10 -2.10 8.20 5 2 -10 4.30 5.60 5 2 -10 -11.70 7.10 -4 -2 10 313.37 21.10 -4 -2 10 329.47 25.10 -4 -2 10 318.17 21.90 4 2 -10 317.57 23.90 4 2 -10 319.77 20.40 -3 -2 10 -4.80 7.60 3 2 -10 -8.70 5.90 3 2 -10 -14.30 5.90 3 2 -10 -0.30 6.60 3 2 -10 -10.10 6.70 -2 -2 10 509.35 38.00 2 2 -10 594.64 37.30 2 2 -10 594.54 36.80 2 2 -10 603.84 37.20 2 2 -10 583.54 37.60 -1 -2 10 2.00 7.20 1 2 -10 1.00 6.10 1 2 -10 2.40 5.50 1 2 -10 -5.00 5.40 0 -2 10 391.56 26.30 0 -2 10 379.16 27.00 0 -2 10 350.46 25.60 0 2 -10 387.66 25.50 0 2 -10 368.76 25.10 0 2 -10 386.56 25.00 1 -2 10 275.07 20.30 1 -2 10 300.57 20.00 -1 2 -10 282.07 20.10 -1 2 -10 261.07 19.50 -1 2 -10 289.37 19.50 -1 2 -10 214.78 18.70 2 -2 10 16.70 6.60 2 -2 10 16.80 6.70 2 -2 10 16.30 7.00 -2 2 -10 19.20 6.30 -2 2 -10 18.10 5.80 -2 2 -10 23.30 6.30 -2 2 -10 26.50 5.90 -2 2 -10 22.30 5.90 3 -2 10 37.80 7.30 3 -2 10 44.50 6.60 3 -2 10 30.20 8.60 3 -2 10 43.10 7.30 -3 2 -10 44.30 6.70 -3 2 -10 40.60 6.80 -3 2 -10 30.90 6.80 -3 2 -10 32.30 7.00 -3 2 -10 44.80 7.20 4 -2 10 86.19 9.80 4 -2 10 102.99 10.00 4 -2 10 98.89 12.60 4 -2 10 94.99 9.80 -4 2 -10 99.39 9.60 -4 2 -10 86.19 9.20 -4 2 -10 97.79 9.20 -4 2 -10 87.89 9.60 -4 2 -10 102.69 12.20 -4 2 -10 98.39 9.80 5 -2 10 488.65 31.60 -5 -2 -10 505.25 36.10 -5 -2 -10 434.86 36.60 5 -2 10 503.85 33.30 5 -2 10 499.85 32.20 5 -2 10 509.85 35.10 -5 2 -10 454.15 34.20 -5 2 -10 479.65 31.90 5 2 10 513.85 39.60 -5 2 -10 505.35 35.40 -5 2 -10 483.05 31.10 6 -2 10 489.15 34.50 -6 -2 -10 526.75 37.60 6 -2 10 494.15 33.00 6 2 10 454.25 43.20 -6 2 -10 468.45 36.80 -6 2 -10 493.65 31.90 7 -2 10 45.50 7.30 -7 -2 -10 39.10 15.70 7 -2 10 47.80 12.90 7 -2 10 31.20 10.50 7 2 10 38.30 18.90 7 2 10 19.70 29.70 -7 2 -10 31.20 7.00 -7 2 -10 19.50 14.60 -7 2 -10 33.90 6.60 8 -2 10 549.85 38.60 8 -2 10 495.95 32.40 -8 -2 -10 482.25 39.00 8 -2 10 461.75 36.00 -8 -2 -10 519.45 38.50 8 2 10 489.75 42.50 -8 2 -10 515.85 32.00 8 2 10 511.35 46.20 -8 2 -10 504.55 32.60 -8 2 -10 474.95 42.40 9 -2 10 0.70 14.00 -9 -2 -10 4.60 15.30 -9 -2 -10 1.00 14.40 9 -2 10 1.90 6.30 9 2 10 17.90 18.60 -9 2 -10 2.40 6.90 -9 2 -10 -16.80 18.10 9 2 10 -6.30 19.20 -9 2 -10 -5.00 7.10 -10 -2 -10 213.38 22.60 10 2 10 190.38 29.20 -11 -2 -10 331.67 29.00 11 2 10 342.47 38.10 12 2 10 -1.00 23.90 13 2 10 27.00 43.50 14 2 10 71.09 30.30 -10 -3 10 103.69 18.60 -10 -3 10 103.29 15.70 10 3 -10 66.19 13.70 10 3 -10 103.59 16.70 10 3 -10 96.79 13.90 -9 -3 10 23.40 12.10 -9 -3 10 6.20 13.90 9 3 -10 -5.90 12.10 9 3 -10 8.00 9.90 9 3 -10 15.30 11.60 9 3 -10 22.40 10.40 -8 -3 10 19.60 16.00 -8 -3 10 -9.30 11.10 8 3 -10 4.70 10.70 8 3 -10 6.80 9.80 8 3 -10 14.10 9.20 -7 -3 10 850.21 54.19 -7 -3 10 842.62 53.69 -7 -3 10 876.21 55.79 7 3 -10 853.21 53.29 7 3 -10 805.92 53.49 7 3 -10 866.11 55.09 7 3 -10 776.92 54.19 7 3 -10 863.11 52.39 -6 -3 10 10.50 8.30 -6 -3 10 17.50 11.30 6 3 -10 15.50 9.90 6 3 -10 3.90 6.70 6 3 -10 7.20 8.60 -5 -3 10 272.87 24.90 5 3 -10 294.97 23.90 5 3 -10 299.37 19.70 5 3 -10 287.37 21.90 5 3 -10 302.77 22.40 4 3 -10 126.39 12.90 -3 -3 10 235.48 20.30 -3 -3 10 217.98 19.10 -3 -3 10 247.18 20.80 3 3 -10 243.28 19.00 3 3 -10 252.27 20.10 3 3 -10 255.67 20.10 -2 -3 10 140.69 14.20 -2 -3 10 112.99 12.60 -2 -3 10 100.29 12.50 2 3 -10 113.09 12.20 2 3 -10 116.89 11.60 2 3 -10 124.79 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222.08 21.40 3 -4 16 -15.70 12.30 -3 4 -16 -2.50 11.40 -3 4 -16 16.90 11.40 4 -4 16 75.59 14.50 -4 4 -16 63.79 14.10 5 -4 16 42.20 13.30 -5 4 -16 33.60 13.50 5 5 -16 -1.70 13.20 5 5 -16 14.10 15.10 4 5 -16 14.40 13.30 4 5 -16 11.60 14.50 3 5 -16 23.20 12.70 3 5 -16 37.00 14.50 2 5 -16 30.20 13.50 2 5 -16 34.50 16.10 1 5 -16 9.50 23.90 0 -5 16 30.50 15.90 0 5 -16 6.10 12.50 0 5 -16 18.50 13.00 1 -5 16 269.47 25.50 -1 5 -16 290.47 25.40 -1 5 -16 282.37 25.00 2 -5 16 8.50 13.40 -2 5 -16 11.50 13.10 3 -5 16 114.79 16.90 -3 5 -16 109.39 16.80 -1 -6 16 60.99 19.20 1 6 -16 41.10 15.60 1 6 -16 51.29 15.80 0 -6 16 97.89 18.50 0 6 -16 67.79 16.80 0 6 -16 65.39 15.40 1 -6 16 3.50 14.10 -1 6 -16 33.50 14.60 4 0 17 -0.40 8.90 -4 0 -17 -4.90 8.00 -5 0 -17 6.50 12.10 1 -1 17 25.20 12.70 1 -1 17 22.10 11.20 -1 1 -17 9.50 9.50 -1 1 -17 7.20 9.90 2 -1 17 5.70 12.70 2 -1 17 -8.90 10.30 -2 1 -17 -1.50 9.10 -2 1 -17 17.60 9.60 3 -1 17 -3.70 10.30 -3 1 -17 9.00 8.70 -4 1 -17 32.50 9.50 -5 1 -17 6.70 8.60 -5 1 -17 16.90 9.40 -8 -1 -17 86.59 18.10 -2 -2 17 2.40 13.00 -2 -2 17 2.00 12.30 2 2 -17 13.10 10.50 2 2 -17 -9.10 10.90 -1 -2 17 283.97 25.10 -1 -2 17 304.67 26.40 1 2 -17 281.37 24.00 1 2 -17 312.57 24.10 0 -2 17 37.60 12.70 0 -2 17 24.30 14.50 0 2 -17 42.90 11.60 0 2 -17 20.90 10.70 1 -2 17 25.00 12.30 -1 2 -17 51.49 11.50 2 -2 17 1.00 11.30 -2 2 -17 11.10 11.40 -2 2 -17 6.10 9.70 -3 2 -17 48.70 12.70 -3 2 -17 39.70 12.00 -4 2 -17 40.10 10.80 -4 2 -17 6.70 11.20 -5 2 -17 155.88 15.60 -5 -3 17 -6.20 13.40 -5 -3 17 4.80 16.40 5 3 -17 8.10 13.20 5 3 -17 1.60 12.60 -4 -3 17 58.99 16.80 -4 -3 17 42.70 15.20 4 3 -17 36.70 14.60 4 3 -17 46.00 13.80 4 3 -17 17.50 12.60 -3 -3 17 40.20 14.60 -3 -3 17 52.69 16.70 3 3 -17 25.00 13.90 3 3 -17 4.10 12.10 3 3 -17 23.00 12.10 -2 -3 17 190.48 20.70 2 3 -17 181.98 19.60 2 3 -17 151.38 18.70 -1 -3 17 96.69 17.20 1 3 -17 126.49 16.50 1 3 -17 101.99 15.20 0 -3 17 33.10 13.50 0 3 -17 6.60 12.70 0 3 -17 3.80 11.20 -1 3 -17 27.50 12.70 -1 3 -17 28.60 12.40 -2 3 -17 448.86 32.90 -2 3 -17 383.66 33.30 -3 3 -17 4.60 11.50 -3 3 -17 9.90 11.00 -4 3 -17 60.79 12.50 -4 3 -17 75.69 13.60 -5 3 -17 11.90 11.80 -6 3 -17 24.50 11.80 -6 -4 17 2.40 17.40 6 4 -17 7.20 16.10 6 4 -17 -15.50 14.60 -5 -4 17 -2.30 15.90 5 4 -17 -10.50 13.00 5 4 -17 24.40 15.10 -4 -4 17 4.40 15.20 4 4 -17 54.79 14.20 4 4 -17 44.00 15.20 -3 -4 17 14.10 14.80 3 4 -17 17.70 13.00 3 4 -17 28.80 15.00 2 4 -17 -5.60 13.70 2 4 -17 -12.50 16.60 1 4 -17 91.79 15.00 1 4 -17 35.00 15.00 0 4 -17 14.80 12.10 0 4 -17 -15.50 12.70 -1 4 -17 4.90 12.70 -1 4 -17 10.70 12.90 -2 4 -17 54.69 14.30 -2 4 -17 72.59 14.10 -3 4 -17 125.39 16.30 -3 4 -17 120.99 16.40 -4 4 -17 221.78 21.20 -5 4 -17 88.49 14.60 3 5 -17 10.30 14.90 3 5 -17 -2.70 12.80 2 5 -17 4.10 14.30 2 5 -17 11.90 13.00 1 5 -17 4.40 14.00 1 5 -17 7.60 13.20 0 5 -17 -9.50 12.70 -1 5 -17 102.49 16.70 -1 5 -17 84.59 16.70 2 -5 17 83.99 19.00 -2 5 -17 147.69 27.50 -3 5 -17 9.20 15.00 2 -1 18 19.20 14.00 2 -1 18 -3.00 10.90 -2 1 -18 -0.90 9.90 -2 1 -18 -13.80 9.70 -4 1 -18 24.50 9.60 -1 -2 18 30.90 13.50 -1 -2 18 18.50 14.90 1 2 -18 6.80 11.90 1 2 -18 0.80 10.60 0 -2 18 5.90 12.60 0 -2 18 27.40 15.70 0 2 -18 24.50 12.00 0 2 -18 15.20 11.80 1 -2 18 17.00 13.00 -1 2 -18 9.60 10.90 2 -2 18 14.30 12.50 -2 2 -18 3.70 10.50 -3 2 -18 68.79 12.40 -4 2 -18 247.18 21.10 -4 -3 18 12.20 15.00 -4 -3 18 -26.70 15.00 4 3 -18 10.60 13.60 4 3 -18 9.20 12.20 -3 -3 18 2.20 18.40 -3 -3 18 29.60 29.10 -2 -3 18 -16.40 13.30 2 3 -18 10.10 12.30 2 3 -18 14.20 14.20 -1 -3 18 112.69 17.70 1 3 -18 105.29 17.40 1 3 -18 104.29 15.70 0 -3 18 8.60 13.80 0 3 -18 10.80 13.40 0 3 -18 25.30 12.30 -1 3 -18 40.00 13.00 -1 3 -18 11.30 13.30 -2 3 -18 28.40 13.40 -2 3 -18 6.50 12.10 -3 3 -18 291.57 24.00 -3 3 -18 281.77 24.80 -4 3 -18 4.40 12.20 -4 3 -18 15.30 11.60 -5 3 -18 23.20 12.70 -4 -4 18 18.10 16.70 4 4 -18 21.60 14.80 4 4 -18 3.60 15.00 -3 -4 18 22.10 15.80 3 4 -18 -18.50 12.80 3 4 -18 -12.20 14.80 2 4 -18 0.80 12.80 2 4 -18 6.60 14.00 1 4 -18 19.20 13.20 1 4 -18 -0.20 16.30 -1 4 -18 57.59 14.90 -1 4 -18 62.09 15.90 -2 4 -18 2.20 13.10 -2 4 -18 -13.20 11.90 -3 4 -18 10.80 12.70 -3 4 -18 23.20 13.40 -4 4 -18 -13.80 11.80 -5 4 -18 10.30 12.40 1 5 -18 -7.50 16.90 1 5 -18 29.30 14.80 0 5 -18 55.09 16.40 0 5 -18 56.49 15.00 -1 5 -18 32.50 15.00 -1 5 -18 27.20 14.20 0 -2 19 79.89 15.50 0 2 -19 41.40 13.50 1 -2 19 -3.30 12.70 -1 2 -19 2.50 11.00 -2 2 -19 29.70 11.80 -3 2 -19 28.80 11.40 -4 2 -19 6.90 10.70 -3 -3 19 -1.80 14.50 3 3 -19 0.90 12.90 -2 -3 19 20.90 15.50 2 3 -19 19.80 13.50 -1 -3 19 23.20 16.40 0 3 -19 235.68 23.20 0 3 -19 180.28 20.40 -1 3 -19 8.50 14.20 -1 3 -19 13.40 12.30 -2 3 -19 117.49 17.60 -2 3 -19 104.49 16.20 -3 3 -19 0.70 13.40 -3 3 -19 10.40 11.90 -4 3 -19 223.98 21.10 -4 3 -19 209.58 22.00 2 4 -19 41.10 15.10 2 4 -19 69.59 19.30 1 4 -19 86.89 16.60 1 4 -19 115.29 18.50 0 4 -19 37.90 16.20 0 4 -19 34.60 14.60 -1 4 -19 116.19 17.30 -1 -3 20 14.90 15.30 1 3 -20 32.60 13.70 0 3 -20 -20.20 12.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 2222 _olex2_submission_special_instructions 'No special instructions were received' 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 O001 O 0.5194(2) 0.5008(5) 0.81127(16) 0.0386(9) Uani 1 1 d . . . . . O002 O 0.6858(2) 0.5934(5) 0.65224(17) 0.0432(10) Uani 1 1 d . . . . . O003 O 0.65993(19) 0.4232(4) 0.83337(16) 0.0370(9) Uani 1 1 d . . . . . O004 O 0.9816(2) 0.4519(5) 0.17331(17) 0.0465(10) Uani 1 1 d . . . . . O005 O 0.8371(2) 0.6013(5) 0.35493(18) 0.0462(10) Uani 1 1 d . . . . . O006 O 0.5608(2) 0.1300(5) 0.47833(17) 0.0443(10) Uani 1 1 d . . . . . N007 N 0.7582(2) 0.9386(5) 0.4639(2) 0.0218(9) Uani 1 1 d . . . . . O008 O 0.4552(2) 0.3151(5) 0.49631(16) 0.0471(10) Uani 1 1 d . . . . . O009 O 0.9239(2) 0.1032(5) 0.50898(19) 0.0507(11) Uani 1 1 d . . . . . N00A N 0.7247(2) 0.9423(5) 0.53654(18) 0.0234(8) Uani 1 1 d . . . . . N00B N 0.6880(2) 0.7419(6) 0.6359(2) 0.0289(9) Uani 1 1 d . . . . . O00C O 0.6952(2) 0.4125(5) 0.48341(18) 0.0464(9) Uani 1 1 d . . . . . O00D O 1.1225(2) 0.2837(5) 0.33955(18) 0.0513(11) Uani 1 1 d . . . . . N00E N 0.6377(2) 0.2042(5) 0.62316(19) 0.0236(9) Uani 1 1 d . . . . . O00F O 0.8359(2) 0.4061(5) 0.15506(17) 0.0490(10) Uani 1 1 d . . . . . N00G N 0.8158(2) 0.7450(5) 0.3667(2) 0.0286(10) Uani 1 1 d . . . . . O00H O 1.0324(2) 0.2831(5) 0.49406(17) 0.0495(10) Uani 1 1 d . . . . . O00I O 1.0750(2) 0.5390(5) 0.3224(2) 0.0551(12) Uani 1 1 d . . . . . O00J O 0.8239(2) 0.8627(5) 0.32131(18) 0.0499(10) Uani 1 1 d . . . . . O00K O 0.8332(2) 0.4355(5) 0.5295(2) 0.0550(11) Uani 1 1 d . . . . . N00L N 0.8287(2) 0.2629(5) 0.29933(18) 0.0234(9) Uani 1 1 d . . . . . O00M O 0.4395(2) 0.6015(6) 0.65469(19) 0.0572(12) Uani 1 1 d . . . . . N00N N 0.8408(2) 0.2102(5) 0.37433(18) 0.0242(9) Uani 1 1 d . . . . . N00O N 0.4360(2) 0.4501(6) 0.65527(19) 0.0318(10) Uani 1 1 d . . . . . N00P N 0.6581(2) 0.2511(5) 0.69858(18) 0.0251(9) Uani 1 1 d . . . . . N00Q N 0.5890(2) 0.4290(5) 0.79323(18) 0.0247(9) Uani 1 1 d . . . . . O00R O 0.6644(3) 0.8557(6) 0.67854(19) 0.0586(12) Uani 1 1 d . . . . . O00S O 0.3679(2) 0.3643(5) 0.65521(19) 0.0583(11) Uani 1 1 d . . . . . N00T N 1.0622(2) 0.3906(6) 0.33102(19) 0.0317(10) Uani 1 1 d . . . . . N00U N 0.9638(2) 0.2075(5) 0.47170(19) 0.0300(10) Uani 1 1 d . . . . . N00V N 0.5220(2) 0.2330(5) 0.5177(2) 0.0295(9) Uani 1 1 d . . . . . N00W N 0.7613(2) 0.4935(5) 0.50531(17) 0.0294(9) Uani 1 1 d . . . . . N00X N 0.9075(2) 0.4021(5) 0.19409(19) 0.0311(10) Uani 1 1 d . . . . . C00Y C 0.7218(3) 0.7851(6) 0.5592(2) 0.0211(10) Uani 1 1 d . . . . . C00Z C 0.7778(3) 0.7821(6) 0.4420(2) 0.0204(10) Uani 1 1 d . . . . . C010 C 0.5872(2) 0.3467(5) 0.7173(2) 0.0190(9) Uani 1 1 d . . . . . C011 C 0.5581(3) 0.2673(6) 0.5968(2) 0.0226(10) Uani 1 1 d . . . . . C012 C 0.9269(3) 0.2500(6) 0.3934(2) 0.0221(10) Uani 1 1 d . . . . . C013 C 0.5223(2) 0.3603(5) 0.6564(2) 0.0213(10) Uani 1 1 d . . . . . C014 C 0.9702(2) 0.3296(6) 0.3322(2) 0.0228(10) Uani 1 1 d . . . . . C015 C 0.9044(3) 0.3347(6) 0.2724(2) 0.0239(10) Uani 1 1 d . . . . . C016 C 0.7543(2) 0.6743(6) 0.5025(2) 0.0226(10) Uani 1 1 d . . . . . H00E H 0.673(3) 0.128(6) 0.598(2) 0.031(12) Uiso 1 1 d . . . . . H00L H 0.769(4) 0.274(8) 0.273(3) 0.10(2) Uiso 1 1 d . . . . . H007 H 0.776(3) 1.040(8) 0.432(3) 0.060(16) Uiso 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 O001 0.038(2) 0.047(3) 0.0306(17) -0.0067(14) 0.0050(15) 0.0186(15) O002 0.054(2) 0.034(3) 0.0417(19) 0.0113(16) 0.0071(18) -0.0137(16) O003 0.0270(19) 0.054(3) 0.0293(16) -0.0093(13) -0.0060(15) 0.0000(13) O004 0.034(2) 0.073(4) 0.0329(18) 0.0137(16) 0.0025(16) -0.0144(16) O005 0.060(2) 0.033(3) 0.046(2) -0.0101(17) 0.0153(17) 0.0144(17) O006 0.048(2) 0.054(4) 0.0311(19) -0.0198(16) 0.0046(18) 0.0025(15) N007 0.026(2) 0.020(3) 0.0193(17) -0.0009(15) 0.0007(15) -0.0002(14) O008 0.032(2) 0.076(4) 0.0324(18) -0.0088(15) -0.0056(16) 0.0134(16) O009 0.037(2) 0.074(4) 0.042(2) 0.0336(18) 0.0021(17) -0.0064(16) N00A 0.026(2) 0.027(3) 0.0175(17) -0.0005(15) 0.0027(15) 0.0001(14) N00B 0.028(2) 0.037(4) 0.0220(19) 0.0025(17) 0.0077(17) -0.0043(16) O00C 0.049(2) 0.036(3) 0.054(2) -0.0036(16) 0.0023(18) -0.0140(16) O00D 0.019(2) 0.083(4) 0.052(2) 0.0090(18) 0.0026(17) 0.0075(16) N00E 0.024(2) 0.025(4) 0.0229(19) -0.0027(14) 0.0051(17) 0.0058(14) O00F 0.034(2) 0.079(4) 0.0336(18) 0.0213(15) -0.0085(16) -0.0064(16) N00G 0.031(2) 0.026(4) 0.029(2) -0.0024(17) 0.0077(17) 0.0029(16) O00H 0.036(2) 0.077(4) 0.0350(18) 0.0096(16) -0.0102(16) -0.0121(17) O00I 0.062(3) 0.045(4) 0.056(2) 0.0168(19) -0.0183(19) -0.030(2) O00J 0.076(3) 0.040(4) 0.0350(19) 0.0073(16) 0.0259(18) 0.0029(18) O00K 0.061(3) 0.035(4) 0.067(2) -0.0032(17) -0.022(2) 0.0173(17) N00L 0.019(2) 0.029(3) 0.0216(18) -0.0002(14) 0.0004(16) -0.0016(14) O00M 0.080(3) 0.041(4) 0.050(2) -0.010(2) -0.012(2) 0.032(2) N00N 0.024(2) 0.024(3) 0.0239(18) 0.0059(14) -0.0003(15) -0.0030(14) N00O 0.031(2) 0.043(4) 0.0209(19) -0.0051(18) -0.0023(18) 0.0115(18) N00P 0.024(2) 0.031(3) 0.0204(18) -0.0012(14) 0.0034(16) 0.0040(14) N00Q 0.024(2) 0.026(3) 0.0235(18) -0.0010(14) 0.0025(16) 0.0028(14) O00R 0.096(3) 0.046(4) 0.035(2) -0.0017(17) 0.032(2) 0.0135(19) O00S 0.025(2) 0.099(4) 0.051(2) 0.0046(19) -0.0007(18) -0.0051(18) N00T 0.023(2) 0.049(4) 0.0231(19) 0.0058(18) 0.0031(17) -0.0088(18) N00U 0.024(2) 0.041(4) 0.0256(19) 0.0069(16) 0.0017(17) 0.0010(16) N00V 0.026(2) 0.036(4) 0.027(2) -0.0048(16) -0.0014(17) -0.0019(15) N00W 0.038(3) 0.023(3) 0.027(2) 0.0009(16) 0.0027(18) 0.0010(16) N00X 0.027(2) 0.040(4) 0.0263(19) 0.0061(16) -0.0009(17) -0.0037(16) C00Y 0.020(2) 0.022(4) 0.021(2) -0.0002(17) -0.0025(18) -0.0025(16) C00Z 0.019(2) 0.018(4) 0.025(2) -0.0013(17) 0.0009(18) 0.0022(16) C010 0.021(3) 0.018(4) 0.0174(19) 0.0001(16) 0.0029(18) -0.0030(16) C011 0.021(2) 0.027(4) 0.020(2) 0.0003(17) 0.0014(18) -0.0022(16) C012 0.021(2) 0.021(4) 0.024(2) 0.0013(17) 0.0014(18) 0.0030(16) C013 0.018(2) 0.020(4) 0.027(2) 0.0003(17) 0.0018(18) -0.0003(15) C014 0.014(2) 0.032(4) 0.022(2) 0.0004(17) 0.0029(18) 0.0021(15) C015 0.024(3) 0.025(4) 0.023(2) 0.0024(18) 0.0039(19) 0.0025(16) C016 0.018(3) 0.022(3) 0.027(2) -0.0006(17) -0.001(2) -0.0009(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' 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 N00A N007 C00Z 111.3(3) . . ? N00A N007 H007 125(3) . . ? C00Z N007 H007 123(4) . . ? C00Y N00A N007 105.2(3) . . ? O002 N00B C00Y 116.6(4) . . ? O00R N00B O002 125.7(5) . . ? O00R N00B C00Y 117.7(5) . . ? N00P N00E H00E 121(2) . . ? C011 N00E N00P 111.8(3) . . ? C011 N00E H00E 127(2) . . ? O005 N00G O00J 126.7(5) . . ? O005 N00G C00Z 116.9(4) . . ? O00J N00G C00Z 116.4(4) . . ? N00N N00L C015 111.6(3) . . ? N00N N00L H00L 124(3) . . ? C015 N00L H00L 123(3) . . ? C012 N00N N00L 104.2(3) . . ? O00M N00O O00S 126.8(4) . . ? O00M N00O C013 117.1(4) . . ? O00S N00O C013 116.1(5) . . ? C010 N00P N00E 103.4(3) . . ? O001 N00Q O003 125.8(3) . . ? O001 N00Q C010 116.5(3) . . ? O003 N00Q C010 117.6(3) . . ? O00D N00T C014 115.8(4) . . ? O00I N00T O00D 125.3(4) . . ? O00I N00T C014 118.9(4) . . ? O009 N00U O00H 126.2(3) . . ? O009 N00U C012 117.5(4) . . ? O00H N00U C012 116.3(3) . . ? O006 N00V O008 126.2(3) . . ? O006 N00V C011 118.0(4) . . ? O008 N00V C011 115.8(3) . . ? O00C N00W C016 117.8(4) . . ? O00K N00W O00C 125.4(5) . . ? O00K N00W C016 116.8(4) . . ? O004 N00X C015 116.4(3) . . ? O00F N00X O004 126.6(3) . . ? O00F N00X C015 117.0(3) . . ? N00A C00Y N00B 120.3(4) . . ? N00A C00Y C016 113.0(4) . . ? C016 C00Y N00B 126.7(5) . . ? N007 C00Z N00G 122.1(4) . . ? N007 C00Z C016 108.3(4) . . ? C016 C00Z N00G 129.6(4) . . ? N00P C010 N00Q 118.7(3) . . ? N00P C010 C013 113.1(3) . . ? C013 C010 N00Q 128.1(4) . . ? N00E C011 N00V 121.6(4) . . ? N00E C011 C013 108.4(3) . . ? C013 C011 N00V 130.0(4) . . ? N00N C012 N00U 119.0(3) . . ? N00N C012 C014 112.8(3) . . ? C014 C012 N00U 128.2(3) . . ? C010 C013 N00O 128.8(4) . . ? C011 C013 N00O 127.9(3) . . ? C011 C013 C010 103.3(3) . . ? C012 C014 N00T 128.5(3) . . ? C015 C014 N00T 128.2(4) . . ? C015 C014 C012 103.3(3) . . ? N00L C015 N00X 121.7(3) . . ? N00L C015 C014 108.1(3) . . ? C014 C015 N00X 130.2(4) . . ? C00Y C016 N00W 129.3(4) . . ? C00Z C016 N00W 128.6(4) . . ? C00Z C016 C00Y 102.1(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O001 N00Q 1.216(4) . ? O002 N00B 1.213(5) . ? O003 N00Q 1.219(4) . ? O004 N00X 1.218(4) . ? O005 N00G 1.203(5) . ? O006 N00V 1.208(4) . ? N007 N00A 1.331(5) . ? N007 C00Z 1.333(6) . ? N007 H007 1.01(5) . ? O008 N00V 1.219(4) . ? O009 N00U 1.203(5) . ? N00A C00Y 1.308(6) . ? N00B O00R 1.212(5) . ? N00B C00Y 1.439(6) . ? O00C N00W 1.209(5) . ? O00D N00T 1.231(5) . ? N00E N00P 1.344(4) . ? N00E C011 1.331(5) . ? N00E H00E 0.91(4) . ? O00F N00X 1.217(4) . ? N00G O00J 1.216(5) . ? N00G C00Z 1.430(5) . ? O00H N00U 1.218(4) . ? O00I N00T 1.205(5) . ? O00K N00W 1.207(4) . ? N00L N00N 1.333(4) . ? N00L C015 1.340(5) . ? N00L H00L 0.97(5) . ? O00M N00O 1.205(5) . ? N00N C012 1.329(5) . ? N00O O00S 1.209(5) . ? N00O C013 1.451(5) . ? N00P C010 1.333(5) . ? N00Q C010 1.433(5) . ? N00T C014 1.433(5) . ? N00U C012 1.444(5) . ? N00V C011 1.439(5) . ? N00W C016 1.442(6) . ? N00X C015 1.423(5) . ? C00Y C016 1.394(6) . ? C00Z C016 1.383(6) . ? C010 C013 1.377(5) . ? C011 C013 1.363(5) . ? C012 C014 1.380(5) . ? C014 C015 1.367(5) . ? 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 O001 N00Q C010 N00P -172.7(4) . . . . ? O001 N00Q C010 C013 11.5(7) . . . . ? O002 N00B C00Y N00A 178.7(3) . . . . ? O002 N00B C00Y C016 -1.6(6) . . . . ? O003 N00Q C010 N00P 8.2(6) . . . . ? O003 N00Q C010 C013 -167.5(4) . . . . ? O004 N00X C015 N00L -174.1(4) . . . . ? O004 N00X C015 C014 6.6(7) . . . . ? O005 N00G C00Z N007 174.8(4) . . . . ? O005 N00G C00Z C016 -6.0(6) . . . . ? O006 N00V C011 N00E 8.1(8) . . . . ? O006 N00V C011 C013 -171.1(5) . . . . ? N007 N00A C00Y N00B -179.6(3) . . . . ? N007 N00A C00Y C016 0.7(4) . . . . ? N007 C00Z C016 N00W 178.7(3) . . . . ? N007 C00Z C016 C00Y -0.8(4) . . . . ? O008 N00V C011 N00E -170.4(5) . . . . ? O008 N00V C011 C013 10.3(8) . . . . ? O009 N00U C012 N00N 18.0(7) . . . . ? O009 N00U C012 C014 -161.9(5) . . . . ? N00A N007 C00Z N00G -179.3(3) . . . . ? N00A N007 C00Z C016 1.3(4) . . . . ? N00A C00Y C016 N00W -179.5(3) . . . . ? N00A C00Y C016 C00Z 0.1(4) . . . . ? N00B C00Y C016 N00W 0.8(6) . . . . ? N00B C00Y C016 C00Z -179.6(4) . . . . ? O00C N00W C016 C00Y 86.6(5) . . . . ? O00C N00W C016 C00Z -92.8(5) . . . . ? O00D N00T C014 C012 62.2(6) . . . . ? O00D N00T C014 C015 -117.0(5) . . . . ? N00E N00P C010 N00Q -175.8(4) . . . . ? N00E N00P C010 C013 0.6(5) . . . . ? N00E C011 C013 N00O -178.9(4) . . . . ? N00E C011 C013 C010 0.6(5) . . . . ? O00F N00X C015 N00L 6.7(6) . . . . ? O00F N00X C015 C014 -172.5(5) . . . . ? N00G C00Z C016 N00W -0.6(7) . . . . ? N00G C00Z C016 C00Y 179.9(4) . . . . ? O00H N00U C012 N00N -161.2(4) . . . . ? O00H N00U C012 C014 19.0(7) . . . . ? O00I N00T C014 C012 -117.5(5) . . . . ? O00I N00T C014 C015 63.3(6) . . . . ? O00J N00G C00Z N007 -4.6(5) . . . . ? O00J N00G C00Z C016 174.7(4) . . . . ? O00K N00W C016 C00Y -93.3(5) . . . . ? O00K N00W C016 C00Z 87.2(5) . . . . ? N00L N00N C012 N00U -179.0(4) . . . . ? N00L N00N C012 C014 0.9(5) . . . . ? O00M N00O C013 C010 70.7(6) . . . . ? O00M N00O C013 C011 -109.9(5) . . . . ? N00N N00L C015 N00X -179.3(4) . . . . ? N00N N00L C015 C014 0.1(5) . . . . ? N00N C012 C014 N00T 179.8(4) . . . . ? N00N C012 C014 C015 -0.8(5) . . . . ? N00P N00E C011 N00V -179.7(4) . . . . ? N00P N00E C011 C013 -0.2(6) . . . . ? N00P C010 C013 N00O 178.7(4) . . . . ? N00P C010 C013 C011 -0.8(5) . . . . ? N00Q C010 C013 N00O -5.3(8) . . . . ? N00Q C010 C013 C011 175.2(4) . . . . ? O00R N00B C00Y N00A -1.4(5) . . . . ? O00R N00B C00Y C016 178.2(4) . . . . ? O00S N00O C013 C010 -109.1(5) . . . . ? O00S N00O C013 C011 70.3(6) . . . . ? N00T C014 C015 N00L 179.8(4) . . . . ? N00T C014 C015 N00X -0.9(8) . . . . ? N00U C012 C014 N00T -0.3(8) . . . . ? N00U C012 C014 C015 179.1(4) . . . . ? N00V C011 C013 N00O 0.4(8) . . . . ? N00V C011 C013 C010 179.9(4) . . . . ? C00Z N007 N00A C00Y -1.2(4) . . . . ? C011 N00E N00P C010 -0.2(5) . . . . ? C012 C014 C015 N00L 0.4(5) . . . . ? C012 C014 C015 N00X 179.7(4) . . . . ? C015 N00L N00N C012 -0.6(5) . . . . ?