#------------------------------------------------------------------------------ #$Date: 2024-01-06 11:53:54 +0200 (Sat, 06 Jan 2024) $ #$Revision: 288906 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247696.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_7247696 loop_ _publ_author_name 'Atceken, Nurunnisa' 'Hemingway, Jack' 'Bull, Craig L.' 'Liu, Xiaojiao' 'Michalchuk, Adam A. L.' 'Konar, Sumit' 'Morrison, Carole A.' 'Pulham, Colin R.' _publ_section_title ; High-pressure structural studies and pressure-induced sensitisation of 3,4,5-trinitro-1H-pyrazole. ; _journal_issue 46 _journal_name_full 'Physical chemistry chemical physics : PCCP' _journal_page_first 31646 _journal_page_last 31654 _journal_paper_doi 10.1039/d3cp04526a _journal_volume 25 _journal_year 2023 _chemical_formula_moiety '3(C6 H2 N10 O12)' _chemical_formula_sum 'C18 H6 N30 O36' _chemical_formula_weight 1218.53 _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.cc29gp5n _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 92.170(7) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 14.9370(17) _cell_length_b 8.1341(11) _cell_length_c 16.9890(17) _cell_measurement_reflns_used 2256 _cell_measurement_temperature 298.0 _cell_measurement_theta_max 24.74 _cell_measurement_theta_min 2.73 _cell_volume 2062.7(4) _computing_cell_refinement 'SAINT V8.40A (?, 2016)' _computing_data_reduction 'SAINT V8.40A (?, 2016)' _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 298.0 _diffrn_measured_fraction_theta_full 0.553 _diffrn_measured_fraction_theta_max 0.507 _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 0.0563 _diffrn_reflns_av_unetI/netI 0.0651 _diffrn_reflns_Laue_measured_fraction_full 0.553 _diffrn_reflns_Laue_measured_fraction_max 0.507 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 11940 _diffrn_reflns_point_group_measured_fraction_full 0.553 _diffrn_reflns_point_group_measured_fraction_max 0.507 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.380 _diffrn_reflns_theta_min 2.399 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.191 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0839 before and 0.0558 after correction. The Ratio of minimum to maximum transmission is 0.8771. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.962 _exptl_crystal_description block _exptl_crystal_F_000 1224 _refine_diff_density_max 0.181 _refine_diff_density_min -0.192 _refine_diff_density_rms 0.046 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 391 _refine_ls_number_reflns 2144 _refine_ls_number_restraints 306 _refine_ls_restrained_S_all 0.981 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0512 _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^)+(0.0568P)^2^+2.7225P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1246 _refine_ls_wR_factor_ref 0.1499 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1313 _reflns_number_total 2144 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3cp04526a2.cif _cod_data_source_block 2tnp_p02 _cod_depositor_comments 'Adding full bibliography for 7247689--7247697.cif.' _cod_database_code 7247696 _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_p02_a.res in P2(1)/c 2tnp_p02.res created by SHELXL-2018/3 at 21:28:01 on 31-Mar-2020 REM Old TITL 2TNP_P02 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.236, Rweak 0.006, Alpha 0.090 REM 0.513 for 98 systematic absences, Orientation as input REM Formula found by SHELXT: C32 N O9 CELL 0.71073 14.937 8.1341 16.989 90 92.17 90 ZERR 2 0.0017 0.0011 0.0017 0 0.007 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 20 TEMP 24.85 CONF BOND list 4 fmap 2 53 MORE -1 ACTA BOND $H OMIT 1 2 7 OMIT 1 6 11 OMIT 2 4 16 OMIT 5 3 0 OMIT -1 1 8 OMIT -4 3 3 OMIT 5 0 6 OMIT -2 2 7 OMIT 7 1 1 OMIT 6 1 4 OMIT -5 3 1 OMIT -4 2 6 OMIT 7 0 2 OMIT 1 1 8 OMIT 2 3 5 OMIT 0 1 8 OMIT -2 1 8 REM REM REM WGHT 0.056800 2.722500 FVAR 0.63187 O001 4 0.827368 0.597235 0.354493 11.00000 0.06291 0.04171 = 0.05468 -0.01183 0.01747 0.01506 O002 4 0.682079 0.599474 0.649316 11.00000 0.06019 0.03956 = 0.05062 0.01520 0.00788 -0.01241 O003 4 0.525245 0.492530 0.812488 11.00000 0.04589 0.05685 = 0.03520 -0.00883 0.00537 0.01885 O004 4 0.663060 0.419615 0.833665 11.00000 0.03745 0.06287 = 0.03606 -0.01408 -0.01048 0.00272 O005 4 0.925990 0.111789 0.510945 11.00000 0.04198 0.08107 = 0.04559 0.03777 0.00284 -0.00551 O006 4 0.565483 0.125129 0.483902 11.00000 0.05761 0.05906 = 0.04367 -0.02776 0.00180 0.00514 O007 4 0.978258 0.463371 0.178583 11.00000 0.04271 0.06630 = 0.04351 0.01803 -0.00316 -0.01583 N008 3 0.762489 0.933226 0.465087 11.00000 0.02643 0.03169 = 0.02237 0.00124 0.00398 -0.00172 O009 4 1.120924 0.304066 0.340298 11.00000 0.02412 0.10343 = 0.06042 0.00881 0.00167 0.00724 N00A 3 0.833825 0.259035 0.300984 11.00000 0.02634 0.03251 = 0.02315 -0.00264 -0.00034 -0.00223 O00B 4 1.033201 0.285347 0.493406 11.00000 0.03848 0.08261 = 0.04568 0.01881 -0.01516 -0.01575 O00C 4 0.836712 0.409121 0.159933 11.00000 0.04028 0.08555 = 0.03673 0.02007 -0.01332 -0.00594 O00D 4 0.458631 0.300718 0.501389 11.00000 0.04056 0.09194 = 0.03458 -0.00954 -0.00861 0.01678 N00E 3 0.729114 0.940657 0.536271 11.00000 0.03170 0.02767 = 0.02366 0.00050 -0.00213 -0.00025 O00F 4 0.446112 0.590148 0.656548 11.00000 0.08291 0.05724 = 0.06280 -0.01198 -0.01380 0.03956 N00G 3 0.687440 0.744832 0.633161 11.00000 0.02930 0.03869 = 0.03100 0.00266 0.00710 -0.00472 O00H 4 0.825556 0.434666 0.524502 11.00000 0.06868 0.04489 = 0.07313 -0.00183 -0.01674 0.02225 N00I 3 0.846040 0.205769 0.374965 11.00000 0.03054 0.02882 = 0.02542 0.00313 -0.00061 -0.00204 O00J 4 0.687588 0.425185 0.485325 11.00000 0.06466 0.03865 = 0.07553 -0.00149 -0.00715 -0.02031 N00K 3 0.641042 0.202266 0.626960 11.00000 0.02800 0.03431 = 0.02868 -0.00439 0.00644 0.00860 N00L 3 0.814005 0.741697 0.368091 11.00000 0.03481 0.04045 = 0.02932 -0.00339 0.00875 0.00358 N00M 3 0.661819 0.252527 0.699711 11.00000 0.02979 0.03019 = 0.02466 -0.00239 -0.00022 0.00596 N00N 3 0.442489 0.441573 0.657681 11.00000 0.03419 0.06312 = 0.02234 -0.00414 0.00009 0.01900 N00O 3 0.593962 0.423584 0.794333 11.00000 0.02940 0.02853 = 0.03582 -0.00506 -0.00062 0.00006 N00P 3 0.907098 0.408856 0.198693 11.00000 0.03778 0.03754 = 0.02489 0.00431 -0.00032 -0.00148 O00Q 4 0.665314 0.856548 0.675588 11.00000 0.11497 0.04446 = 0.04446 -0.00049 0.04027 0.00591 O00R 4 0.828725 0.855972 0.324614 11.00000 0.10881 0.04561 = 0.03938 0.00398 0.03575 -0.00090 N00S 3 0.755372 0.498092 0.503341 11.00000 0.04743 0.02592 = 0.03231 -0.00150 0.00223 -0.00147 N00T 3 0.965722 0.212522 0.472494 11.00000 0.02953 0.05087 = 0.02657 0.01135 0.00378 -0.00008 O00U 4 0.375038 0.358106 0.657300 11.00000 0.01799 0.12494 = 0.05540 0.00216 0.00559 -0.00316 C00V 1 0.721820 0.784985 0.558408 11.00000 0.02175 0.02079 = 0.02932 0.00112 -0.00070 -0.00536 C00W 1 0.777883 0.778329 0.442686 11.00000 0.02421 0.03011 = 0.02395 -0.00384 0.00257 -0.00126 N00X 3 0.526302 0.225146 0.522232 11.00000 0.03193 0.04439 = 0.02890 -0.00612 -0.00295 -0.00260 C00Y 1 0.591938 0.343804 0.718662 11.00000 0.02389 0.02031 = 0.02648 -0.00137 0.00451 -0.00570 N00Z 3 1.059277 0.402821 0.334483 11.00000 0.03209 0.06040 = 0.02578 0.01056 0.00100 -0.01304 C010 1 0.562045 0.260541 0.599659 11.00000 0.03004 0.02564 = 0.02516 0.00214 -0.00027 -0.00240 C011 1 0.929047 0.251770 0.394315 11.00000 0.02664 0.02305 = 0.02875 0.00567 -0.00095 0.00293 O012 4 1.067053 0.549183 0.329081 11.00000 0.07955 0.06373 = 0.06867 0.02898 -0.02552 -0.04115 C013 1 0.751851 0.675740 0.502053 11.00000 0.02286 0.02621 = 0.02763 0.00167 0.00116 0.00269 C014 1 0.969873 0.334882 0.335060 11.00000 0.02046 0.03136 = 0.02402 0.00247 0.00264 -0.00028 C015 1 0.905572 0.337850 0.275298 11.00000 0.02860 0.03064 = 0.02353 0.00175 0.00078 0.00173 C016 1 0.527137 0.353088 0.658558 11.00000 0.01838 0.02852 = 0.03026 0.00174 0.00107 0.00129 H008 2 0.783417 1.028202 0.432161 11.00000 0.09394 H00K 2 0.672547 0.137648 0.601081 11.00000 0.00387 H00A 2 0.779894 0.254087 0.274200 11.00000 0.07042 HKLF 4 REM 2tnp_p02_a.res in P2(1)/c REM wR2 = 0.1499, GooF = S = 1.045, Restrained GooF = 0.981 for all data REM R1 = 0.0512 for 1313 Fo > 4sig(Fo) and 0.0998 for all 2144 data REM 391 parameters refined using 306 restraints END WGHT 0.0571 2.7125 REM Highest difference peak 0.181, deepest hole -0.192, 1-sigma level 0.046 Q1 1 0.9651 0.2758 0.2830 11.00000 0.05 0.18 Q2 1 0.7510 1.1327 0.5211 11.00000 0.05 0.18 Q3 1 1.1101 0.1604 0.2444 11.00000 0.05 0.16 Q4 1 0.3925 0.1832 0.7453 11.00000 0.05 0.16 Q5 1 0.3359 0.3671 0.6015 11.00000 0.05 0.16 Q6 1 0.9684 0.2753 0.3639 11.00000 0.05 0.16 Q7 1 0.6778 0.5181 0.5617 11.00000 0.05 0.16 Q8 1 0.5411 0.3461 0.6806 11.00000 0.05 0.16 Q9 1 0.6034 0.2549 0.7178 11.00000 0.05 0.15 Q10 1 0.8339 0.1010 0.4040 11.00000 0.05 0.15 Q11 1 0.8478 0.1259 0.5163 11.00000 0.05 0.15 Q12 1 0.8771 0.8646 0.3765 11.00000 0.05 0.15 Q13 1 0.7559 0.4508 0.1848 11.00000 0.05 0.15 Q14 1 0.7999 1.2059 0.4967 11.00000 0.05 0.15 Q15 1 0.6252 -0.0039 0.5569 11.00000 0.05 0.14 Q16 1 0.7633 0.5828 0.6059 11.00000 0.05 0.14 Q17 1 0.4735 0.5219 0.5970 11.00000 0.05 0.14 Q18 1 0.5246 0.2636 0.6434 11.00000 0.05 0.14 Q19 1 0.8354 0.4734 0.3814 11.00000 0.05 0.14 Q20 1 0.6860 1.1170 0.4691 11.00000 0.05 0.14 ; _shelx_res_checksum 30217 _shelx_hkl_file ; 2 0 0 388.66 30.80 -2 0 0 404.06 30.80 2 0 0 400.56 30.80 -3 0 0 93.59 8.20 -3 0 0 95.69 8.10 3 0 0 96.89 8.10 3 0 0 93.59 8.00 4 0 0 19.10 2.90 -4 0 0 23.30 3.40 -4 0 0 21.10 3.20 4 0 0 22.50 3.00 -1 -1 0 203.48 16.20 -1 -1 0 206.78 16.10 -1 -1 0 204.48 16.20 -1 -1 0 200.68 16.20 1 1 0 201.48 16.20 1 1 0 202.58 16.10 1 1 0 211.98 16.20 1 1 0 204.68 16.10 -2 -1 0 0.30 1.60 -2 -1 0 1.50 1.40 -2 -1 0 -0.30 1.30 -2 -1 0 0.70 1.40 -2 -1 0 -0.30 1.30 -2 -1 0 1.10 1.10 -2 -1 0 1.10 1.10 -2 -1 0 -0.30 1.50 2 1 0 0.50 1.00 2 1 0 0.00 1.30 2 1 0 0.40 0.90 2 1 0 0.50 1.20 2 1 0 -0.50 1.30 2 1 0 0.60 0.90 2 1 0 1.80 1.20 2 1 0 0.30 1.30 -4 -1 0 35.50 4.80 -4 -1 0 37.60 4.70 -4 -1 0 32.70 4.70 -4 -1 0 33.40 4.50 -4 -1 0 30.90 4.50 -4 -1 0 43.00 5.00 4 1 0 43.40 5.40 4 1 0 38.10 4.20 4 1 0 44.60 4.60 4 1 0 42.60 4.10 4 1 0 27.30 3.90 4 1 0 38.30 4.60 -5 -1 0 36.10 5.60 -5 -1 0 45.40 5.50 -5 -1 0 45.10 5.80 -5 -1 0 45.20 5.80 -5 -1 0 42.70 9.00 5 1 0 39.40 5.10 5 1 0 50.59 5.50 5 1 0 41.40 5.80 5 1 0 42.20 5.70 -6 -1 0 6.10 3.90 -6 -1 0 4.50 4.20 -6 -1 0 0.50 3.90 -6 -1 0 2.20 4.30 -6 -1 0 3.20 4.70 6 1 0 1.40 3.30 6 1 0 2.00 2.90 6 1 0 -6.70 3.50 6 1 0 -1.10 3.60 6 1 0 -3.10 3.10 -7 -1 0 756.72 60.19 -7 -1 0 912.31 60.09 -7 -1 0 828.52 60.39 -7 -1 0 768.22 60.39 7 1 0 688.33 59.59 7 1 0 668.03 59.59 7 1 0 745.83 60.19 7 1 0 717.63 60.29 -8 -1 0 14.10 6.50 -8 -1 0 15.30 6.00 -8 -1 0 10.30 6.20 -8 -1 0 15.40 7.80 -8 -1 0 3.80 5.80 8 1 0 11.80 6.70 8 1 0 21.50 5.10 8 1 0 19.40 5.90 8 1 0 6.40 5.00 8 1 0 15.50 6.50 -9 -1 0 17.80 8.50 -9 -1 0 12.70 8.40 -9 -1 0 18.90 7.90 9 1 0 4.50 5.20 9 1 0 21.30 9.40 9 1 0 6.60 7.70 9 1 0 8.10 5.80 -10 -1 0 101.79 14.40 -10 -1 0 99.09 15.10 -10 -1 0 104.29 15.30 10 1 0 93.19 15.30 10 1 0 98.69 13.10 10 1 0 93.39 14.80 10 1 0 86.79 11.40 -2 -2 0 22.00 3.80 -2 -2 0 13.30 3.40 -2 -2 0 19.50 3.50 -2 -2 0 22.60 3.40 2 2 0 17.00 3.90 2 2 0 19.20 3.00 2 2 0 15.60 3.10 2 2 0 19.80 3.40 2 2 0 20.90 3.10 2 2 0 24.30 3.20 -3 -2 0 15.00 3.30 -3 -2 0 14.90 3.30 -3 -2 0 11.20 3.00 -3 -2 0 19.80 3.80 3 2 0 18.10 3.00 3 2 0 8.60 2.90 3 2 0 6.90 3.30 3 2 0 10.20 3.50 -4 -2 0 727.73 54.29 -4 -2 0 687.43 54.39 -4 -2 0 716.93 54.59 -4 -2 0 705.83 54.09 -4 -2 0 657.43 54.69 4 2 0 715.93 54.39 4 2 0 678.13 54.69 4 2 0 676.83 54.49 4 2 0 723.03 54.19 4 2 0 709.23 54.39 4 2 0 658.23 54.49 4 2 0 672.73 54.59 4 2 0 665.53 54.39 4 2 0 701.33 53.99 -5 -2 0 8.90 3.40 -5 -2 0 8.30 5.10 -5 -2 0 11.10 4.90 -5 -2 0 18.70 5.10 -5 -2 0 17.10 4.90 -5 -2 0 12.50 5.20 -5 -2 0 12.60 4.00 -5 -2 0 16.10 5.10 5 2 0 6.50 4.20 5 2 0 11.90 5.10 5 2 0 16.30 3.80 5 2 0 9.00 4.00 5 2 0 13.90 3.80 5 2 0 12.40 4.40 5 2 0 14.30 4.30 5 2 0 10.50 4.00 5 2 0 16.20 5.60 5 2 0 18.40 4.50 5 2 0 13.30 3.70 -6 -2 0 842.72 72.29 -6 -2 0 953.00 71.79 -6 -2 0 827.52 71.89 6 2 0 961.20 71.29 6 2 0 949.90 70.89 6 2 0 958.20 71.19 6 2 0 943.21 70.99 6 2 0 897.31 71.69 6 2 0 830.52 71.39 6 2 0 992.10 71.59 6 2 0 821.22 71.79 -7 -2 0 5.60 6.50 -7 -2 0 -3.10 6.50 -7 -2 0 9.40 6.50 7 2 0 13.50 4.80 7 2 0 4.60 4.90 7 2 0 2.50 5.20 7 2 0 -1.40 6.10 7 2 0 1.70 4.80 7 2 0 2.50 5.10 7 2 0 -2.80 5.60 7 2 0 8.50 4.50 -8 -2 0 7.70 7.40 -8 -2 0 3.20 7.00 8 2 0 9.90 6.40 8 2 0 2.00 6.80 8 2 0 4.50 5.70 8 2 0 3.40 4.80 8 2 0 10.50 5.20 -9 -2 0 -0.20 8.00 -9 -2 0 5.40 8.10 9 2 0 7.20 6.10 9 2 0 2.60 5.30 9 2 0 9.60 7.80 9 2 0 1.20 6.20 -10 -2 0 39.70 11.00 -10 -2 0 44.20 11.90 10 2 0 56.59 8.80 10 2 0 50.69 9.00 -11 -2 0 -10.40 10.20 -11 -2 0 -1.00 9.90 11 2 0 6.10 7.00 11 2 0 8.40 7.90 -12 -2 0 234.98 26.20 -12 -2 0 222.68 24.70 12 2 0 244.18 23.90 12 2 0 252.27 23.00 -13 -2 0 48.20 13.70 -13 -2 0 45.40 15.30 13 2 0 60.89 10.70 -3 -3 0 585.34 46.40 -3 -3 0 601.34 46.90 -3 -3 0 580.14 46.70 -3 -3 0 572.64 47.00 3 3 0 617.74 46.70 3 3 0 564.94 46.20 3 3 0 558.24 46.30 3 3 0 591.34 46.30 3 3 0 639.44 47.10 3 3 0 542.15 47.70 -4 -3 0 5.80 4.90 -4 -3 0 2.00 5.40 -4 -3 0 -2.40 5.40 -4 -3 0 1.50 4.40 4 3 0 5.80 3.70 4 3 0 5.90 4.50 4 3 0 7.80 5.10 4 3 0 0.50 5.40 4 3 0 8.30 4.70 4 3 0 1.70 4.10 -5 -3 0 614.64 54.79 -5 -3 0 653.23 54.29 5 3 0 550.54 54.19 5 3 0 717.03 54.39 5 3 0 696.63 54.09 5 3 0 842.32 55.89 5 3 0 767.42 55.09 -6 -3 0 91.49 11.30 -6 -3 0 77.89 9.60 -6 -3 0 82.79 10.40 -6 -3 0 72.79 9.90 6 3 0 91.99 11.20 6 3 0 93.39 10.90 6 3 0 94.69 11.20 6 3 0 71.79 9.50 6 3 0 109.69 11.50 6 3 0 87.79 9.80 6 3 0 68.69 10.70 6 3 0 64.09 10.50 6 3 0 97.89 10.90 -7 -3 0 -1.20 7.50 -7 -3 0 -0.60 7.10 -7 -3 0 5.00 6.40 -7 -3 0 7.00 7.90 -7 -3 0 7.70 7.30 -7 -3 0 3.40 5.90 7 3 0 5.20 6.20 7 3 0 -3.70 6.50 7 3 0 3.00 6.00 7 3 0 10.50 7.60 7 3 0 -2.10 6.20 7 3 0 5.90 5.20 7 3 0 12.80 5.30 7 3 0 -0.50 6.00 7 3 0 -8.10 5.70 7 3 0 3.70 6.50 -8 -3 0 -9.20 8.50 -8 -3 0 -3.00 7.80 -8 -3 0 8.80 8.80 -8 -3 0 8.00 8.40 8 3 0 1.20 6.40 8 3 0 1.70 7.50 8 3 0 2.40 7.80 8 3 0 1.60 8.80 8 3 0 7.50 6.60 8 3 0 -4.00 5.40 8 3 0 -7.20 5.10 8 3 0 1.90 6.70 8 3 0 9.40 8.00 -9 -3 0 698.73 57.49 -9 -3 0 656.23 56.49 -9 -3 0 607.94 56.69 -9 -3 0 627.84 55.99 9 3 0 661.83 56.59 9 3 0 708.33 56.69 9 3 0 669.83 55.89 9 3 0 679.23 55.09 9 3 0 700.63 57.59 9 3 0 687.63 55.59 9 3 0 707.73 55.19 9 3 0 748.23 56.49 9 3 0 717.83 54.89 -10 -3 0 132.69 18.10 -10 -3 0 124.29 17.60 -10 -3 0 121.29 16.90 10 3 0 143.39 17.50 10 3 0 122.89 14.40 10 3 0 153.38 16.50 10 3 0 150.48 15.20 10 3 0 107.69 17.50 -11 -3 0 352.36 32.10 -11 -3 0 320.07 31.70 -11 -3 0 331.87 33.20 -11 -3 0 261.67 31.50 11 3 0 348.57 30.20 11 3 0 305.67 31.70 11 3 0 316.97 30.70 11 3 0 372.76 34.90 11 3 0 338.57 29.80 11 3 0 373.66 30.10 -12 -3 0 -15.00 11.80 -12 -3 0 -3.40 11.90 -12 -3 0 -27.00 11.70 -12 -3 0 -3.20 14.30 12 3 0 -14.90 12.00 12 3 0 -7.20 7.90 12 3 0 6.10 9.30 12 3 0 -9.70 8.40 12 3 0 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143.99 16.60 9 3 -4 165.58 18.00 9 3 -4 144.39 16.30 9 3 -4 151.98 16.70 9 3 -4 155.08 15.30 9 3 -4 131.69 16.40 -8 -3 4 12.30 8.80 -8 -3 4 20.10 12.90 8 3 -4 -3.90 7.20 8 3 -4 6.20 6.20 8 3 -4 16.00 10.00 8 3 -4 0.50 5.70 8 3 -4 10.30 7.80 8 3 -4 4.80 7.30 8 3 -4 2.30 7.80 8 3 -4 7.20 7.40 -7 -3 4 233.08 21.60 -7 -3 4 226.08 23.60 7 3 -4 215.98 21.90 7 3 -4 219.38 20.90 7 3 -4 217.88 21.40 7 3 -4 216.68 19.70 7 3 -4 218.28 21.30 7 3 -4 233.18 20.00 7 3 -4 199.58 22.00 7 3 -4 196.48 20.60 -6 -3 4 9.50 6.00 -6 -3 4 3.20 9.80 -6 -3 4 15.20 7.70 -6 -3 4 15.30 6.30 6 3 -4 13.30 6.80 6 3 -4 4.70 5.80 6 3 -4 12.60 7.30 6 3 -4 18.20 5.20 6 3 -4 7.80 6.00 6 3 -4 21.90 5.10 6 3 -4 9.40 7.00 6 3 -4 15.10 7.70 6 3 -4 13.70 6.90 -5 -3 4 16.70 5.80 -5 -3 4 24.00 5.40 -5 -3 4 15.50 10.00 -5 -3 4 21.30 7.80 -5 -3 4 19.70 9.80 5 3 -4 18.70 4.80 5 3 -4 14.70 6.30 5 3 -4 7.00 6.80 5 3 -4 12.70 7.90 5 3 -4 19.10 4.70 5 3 -4 16.50 6.50 5 3 -4 22.50 5.90 5 3 -4 24.50 6.10 5 3 -4 20.30 5.80 5 3 -4 10.50 7.40 -4 -3 4 16.80 4.40 -4 -3 4 12.60 7.80 -4 -3 4 7.90 6.40 4 3 -4 -28.30 6.10 4 3 -4 -10.90 3.70 4 3 -4 15.50 6.00 -3 -3 4 8357.76 635.74 3 3 -4 8562.64 635.24 3 3 -4 8171.58 632.74 3 3 -4 8301.87 632.74 3 3 -4 8013.20 634.24 -2 -3 4 90.99 8.80 -2 -3 4 89.99 13.30 -2 -3 4 109.79 11.10 -2 -3 4 105.29 9.00 2 3 -4 84.59 11.90 2 3 -4 91.79 9.00 2 3 -4 77.29 9.90 2 3 -4 86.89 10.70 -1 -3 4 -1.40 4.80 -1 -3 4 2.00 5.30 -1 -3 4 -0.20 2.90 -1 -3 4 0.90 3.10 1 3 -4 -0.20 4.30 1 3 -4 -1.50 5.90 1 3 -4 1.00 4.30 1 3 -4 1.60 2.30 0 -3 4 120.49 11.50 0 -3 4 77.49 9.90 0 -3 4 87.19 10.10 0 3 -4 88.19 12.10 0 3 -4 72.19 11.00 0 3 -4 112.59 10.50 0 3 -4 89.29 9.90 1 -3 4 2059.39 158.08 1 -3 4 2015.10 157.88 -1 3 -4 2097.99 157.88 -1 3 -4 1949.51 158.98 -1 3 -4 2090.59 157.68 -4 -3 -4 4.30 6.90 -4 -3 -4 17.90 7.50 4 3 4 18.50 5.70 4 3 4 6.20 6.70 4 3 4 -1.60 5.60 -5 -3 -4 142.99 12.90 -5 -3 -4 126.29 15.40 -5 -3 -4 117.59 15.00 -5 -3 -4 135.09 15.10 5 3 4 122.79 14.40 5 3 4 162.88 14.90 5 3 4 128.09 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24.20 -6 -4 15 -24.00 23.50 6 4 -15 25.40 17.00 6 4 -15 -5.20 16.90 6 4 -15 9.30 15.80 -5 -4 15 47.40 25.80 -5 -4 15 51.49 24.70 5 4 -15 69.39 18.80 5 4 -15 48.40 18.00 5 4 -15 58.49 19.10 -4 -4 15 -12.90 20.40 -4 -4 15 -0.90 23.10 4 4 -15 6.50 16.90 4 4 -15 -5.30 14.40 4 4 -15 1.10 16.00 -3 -4 15 -31.60 20.30 -3 -4 15 9.50 23.10 3 4 -15 -7.70 13.20 3 4 -15 4.90 16.80 3 4 -15 4.60 14.70 -2 -4 15 11.10 22.30 2 4 -15 -5.90 13.80 2 4 -15 -26.60 15.80 -1 -4 15 4.30 20.70 1 4 -15 -2.20 13.80 1 4 -15 4.60 17.40 0 -4 15 10.90 19.70 0 4 -15 -0.70 12.50 0 4 -15 -20.30 11.70 -1 4 -15 60.79 15.60 -1 4 -15 41.10 14.90 -2 4 -15 6.00 15.70 -2 4 -15 21.70 13.20 -3 4 -15 138.59 21.00 -3 4 -15 96.09 17.90 -4 4 -15 -0.80 13.10 -4 4 -15 8.10 12.30 -5 4 -15 26.80 13.40 -6 4 -15 1.90 12.50 -7 4 -15 49.10 14.80 -7 -5 15 -29.60 24.70 -7 -5 15 3.10 27.00 7 5 -15 3.10 18.90 7 5 -15 -3.40 17.50 7 5 -15 -6.40 17.50 -6 -5 15 195.98 37.60 6 5 -15 230.88 29.80 6 5 -15 254.07 32.80 -5 -5 15 13.20 25.20 5 5 -15 -2.30 16.60 5 5 -15 16.40 23.30 4 5 -15 42.90 38.20 -3 -5 15 17.60 23.10 3 5 -15 22.30 16.00 3 5 -15 1.20 15.50 -2 -5 15 56.89 24.00 2 5 -15 42.70 16.90 2 5 -15 46.50 17.00 1 5 -15 7.40 14.90 1 5 -15 13.80 15.00 0 5 -15 23.30 15.00 0 5 -15 22.50 15.40 -1 5 -15 36.40 17.50 -1 5 -15 29.00 16.20 2 -5 15 149.79 23.60 -2 5 -15 141.39 23.40 -2 5 -15 208.38 25.50 3 -5 15 10.50 15.70 -3 5 -15 -8.80 15.20 -3 5 -15 1.60 15.60 4 -5 15 34.40 16.60 -4 5 -15 48.00 17.10 5 -5 15 -12.60 14.20 -5 5 -15 13.80 15.40 5 6 -15 -5.90 17.40 5 6 -15 -44.20 27.90 4 6 -15 22.40 16.10 4 6 -15 12.20 17.20 3 6 -15 44.60 17.70 3 6 -15 59.09 19.00 2 6 -15 20.80 18.10 2 6 -15 29.20 18.30 1 6 -15 40.30 17.50 0 -6 15 9.90 17.30 0 6 -15 -6.30 17.20 0 6 -15 1.70 17.60 1 -6 15 40.00 21.00 -2 6 -15 -19.80 17.90 -2 6 -15 -5.60 14.30 3 -6 15 36.70 19.60 -3 6 -15 19.30 17.60 4 0 16 402.66 33.40 4 0 16 254.17 26.70 4 0 16 261.97 28.30 5 0 16 -10.60 12.70 -5 0 -16 11.30 10.80 -5 0 -16 5.90 9.30 5 0 16 22.50 10.40 -5 0 -16 8.80 10.90 -5 0 -16 3.70 8.70 5 0 16 -8.10 9.70 5 0 16 0.60 12.10 -5 0 -16 18.40 8.70 6 0 16 86.39 16.00 -7 0 -16 53.39 13.80 7 0 16 64.09 13.00 8 0 16 162.68 19.90 9 0 16 8.70 11.40 10 0 16 6.30 11.60 10 0 16 19.90 11.40 11 0 16 15.20 12.80 11 0 16 24.50 16.70 2 -1 16 -2.10 7.30 2 -1 16 -3.70 7.20 2 -1 16 -14.60 14.20 2 -1 16 18.20 7.50 -2 1 -16 3.80 8.10 -2 1 -16 -4.20 10.60 -2 1 -16 -4.90 7.40 3 -1 16 44.40 9.40 3 -1 16 47.50 16.50 3 -1 16 40.90 9.40 3 -1 16 42.30 17.80 -3 1 -16 27.60 12.20 -3 1 -16 60.09 13.10 -3 1 -16 52.89 10.30 4 -1 16 92.99 12.00 4 -1 16 85.09 18.60 4 -1 16 98.79 12.10 -4 1 -16 85.29 12.80 -4 1 -16 52.79 13.80 -4 1 -16 77.19 13.40 5 -1 16 84.89 12.60 5 -1 16 65.59 11.60 -5 1 -16 91.49 12.80 -5 1 -16 71.39 13.20 6 -1 16 8.40 8.70 6 -1 16 4.20 8.60 7 -1 16 6.90 9.00 -7 -1 -16 -20.70 11.80 -7 -1 -16 5.90 12.90 7 1 16 -4.90 11.50 7 1 16 -10.30 11.20 -8 -1 -16 1.50 13.70 8 -1 16 -2.60 9.40 8 1 16 -0.30 12.30 9 -1 16 14.10 10.70 9 -1 16 1.20 9.50 -9 -1 -16 -4.60 14.10 9 1 16 3.20 12.30 10 -1 16 2.00 15.10 10 -1 16 -3.70 14.00 10 1 16 -5.30 12.60 11 -1 16 200.78 26.00 11 1 16 161.78 22.90 -1 -2 16 2.80 17.40 1 2 -16 9.30 12.50 0 -2 16 83.99 21.90 0 2 -16 142.19 18.90 1 -2 16 27.90 20.70 1 -2 16 29.60 19.30 2 -2 16 572.24 54.09 2 -2 16 500.85 51.99 -2 2 -16 557.04 48.50 -2 2 -16 521.15 47.50 3 -2 16 34.90 18.10 -3 2 -16 3.30 11.50 -4 2 -16 91.49 15.20 -5 2 -16 94.99 17.60 -6 2 -16 133.29 15.30 -6 2 -16 115.39 17.10 -11 -2 -16 23.90 18.00 11 2 16 33.70 15.60 -3 -3 16 -22.00 19.70 3 3 -16 -22.60 13.20 -2 -3 16 20.40 20.70 -2 -3 16 6.40 21.10 2 3 -16 23.00 14.40 2 3 -16 -5.90 14.10 -1 -3 16 313.07 39.70 -1 -3 16 313.77 41.20 1 3 -16 370.46 36.00 1 3 -16 426.66 37.70 1 3 -16 359.66 36.90 0 -3 16 -10.40 18.40 0 -3 16 -6.60 20.40 0 3 -16 -14.30 14.30 0 3 -16 -0.30 13.10 0 3 -16 -15.90 12.60 1 -3 16 -14.30 17.90 -1 3 -16 4.10 14.30 -1 3 -16 -25.20 11.90 2 -3 16 -5.10 17.30 -2 3 -16 9.40 12.10 -2 3 -16 8.80 14.00 -3 3 -16 0.50 11.60 -3 3 -16 -17.40 13.50 -4 3 -16 42.80 30.00 -4 3 -16 26.50 27.30 -5 3 -16 565.54 50.19 -5 3 -16 566.34 51.49 -6 3 -16 -18.90 11.60 -4 -4 16 45.70 25.40 -4 -4 16 45.60 24.20 4 4 -16 20.10 17.70 4 4 -16 -15.50 15.60 4 4 -16 19.20 18.60 -3 -4 16 -25.50 20.80 -3 -4 16 -13.30 22.20 3 4 -16 16.50 15.40 3 4 -16 -18.10 17.20 3 4 -16 15.10 16.00 -2 -4 16 68.79 24.60 2 4 -16 13.90 15.30 2 4 -16 18.50 18.30 -1 -4 16 0.00 21.60 1 4 -16 -2.80 14.50 1 4 -16 0.30 17.20 0 -4 16 534.15 53.39 0 4 -16 562.24 52.59 0 4 -16 490.95 48.90 -1 4 -16 8.00 17.50 -1 4 -16 -4.10 13.00 -2 4 -16 1655.03 132.89 -3 4 -16 9.50 17.70 -3 4 -16 -11.90 11.70 -4 4 -16 36.60 15.80 -4 4 -16 13.50 13.60 -5 4 -16 23.60 13.40 -6 4 -16 53.59 14.90 -6 -5 16 -22.80 27.30 6 5 -16 -3.80 17.40 6 5 -16 2.60 22.30 -5 -5 16 4.60 27.00 5 5 -16 9.90 17.20 5 5 -16 18.10 21.10 -4 -5 16 36.90 26.00 4 5 -16 -30.90 20.70 4 5 -16 -12.50 15.90 -3 -5 16 -14.40 23.30 3 5 -16 49.00 18.10 3 5 -16 52.69 25.90 1 5 -16 -21.10 13.60 1 5 -16 -5.80 14.20 0 5 -16 26.60 15.70 0 5 -16 4.80 15.30 -1 5 -16 136.29 21.70 -1 5 -16 139.49 23.70 -2 5 -16 -7.60 14.20 -2 5 -16 -3.30 16.30 -3 5 -16 26.70 15.40 -3 5 -16 44.30 17.60 -4 5 -16 9.90 14.60 5 -5 16 147.69 21.70 -5 5 -16 107.49 20.90 3 6 -16 -2.80 27.50 3 6 -16 26.30 28.00 2 6 -16 134.09 23.20 2 6 -16 95.59 23.10 1 6 -16 41.80 17.70 1 6 -16 3.60 17.80 0 6 -16 69.89 19.20 0 6 -16 40.60 18.80 -1 6 -16 27.30 17.90 -1 6 -16 7.10 16.30 2 -6 16 16.30 19.50 -2 6 -16 0.50 15.50 -3 6 -16 -30.90 25.00 -6 0 -17 11.70 12.10 6 0 17 0.10 10.40 -7 0 -17 7.60 11.90 8 0 17 2.50 10.30 9 0 17 5.70 11.40 10 0 17 -15.40 11.00 3 -1 17 -0.20 17.70 4 -1 17 51.49 17.00 -4 1 -17 60.99 13.60 -5 1 -17 -9.80 9.80 -5 1 -17 -0.10 8.90 -9 -1 -17 -8.60 14.10 9 1 17 7.00 12.50 10 1 17 13.30 13.50 0 -2 17 -1.30 17.00 0 2 -17 1.10 13.30 1 -2 17 52.19 20.50 1 -2 17 66.89 19.70 -1 2 -17 57.19 15.40 -1 2 -17 44.70 14.80 2 -2 17 -7.90 17.60 2 -2 17 0.80 16.10 -2 2 -17 18.20 12.70 -2 2 -17 -23.70 10.90 -3 2 -17 143.49 20.90 -4 2 -17 -12.40 10.70 -5 2 -17 116.69 21.50 -2 -3 17 88.79 26.00 -2 -3 17 136.09 26.00 2 3 -17 107.89 20.10 2 3 -17 86.59 19.80 -1 -3 17 4.90 20.50 -1 -3 17 23.90 22.60 1 3 -17 33.30 15.30 1 3 -17 -3.60 15.30 0 -3 17 -15.80 18.30 0 -3 17 -34.90 20.20 0 3 -17 -17.50 13.50 0 3 -17 14.20 13.60 1 -3 17 2.50 19.90 -1 3 -17 0.20 13.70 -1 3 -17 -7.80 14.50 2 -3 17 377.06 40.20 -2 3 -17 387.96 36.70 -2 3 -17 324.77 35.50 -3 3 -17 7.60 14.80 -3 3 -17 5.90 12.90 -4 3 -17 177.28 22.20 -4 3 -17 125.69 23.00 -5 3 -17 14.20 13.80 -5 3 -17 -10.00 13.90 -6 3 -17 47.10 26.20 -4 -4 17 21.20 24.00 -4 -4 17 -11.50 25.00 4 4 -17 -8.00 16.60 4 4 -17 -22.20 16.50 3 4 -17 -4.20 30.40 3 4 -17 37.60 19.40 3 4 -17 4.90 26.70 -2 -4 17 -23.00 22.70 2 4 -17 9.60 18.50 2 4 -17 -19.70 15.20 -1 -4 17 69.69 26.20 1 4 -17 87.39 19.20 1 4 -17 90.29 21.60 0 -4 17 -12.60 20.00 0 4 -17 26.20 18.60 0 4 -17 7.50 13.90 -1 4 -17 -2.20 17.70 -1 4 -17 25.00 15.50 -2 4 -17 45.40 17.40 -2 4 -17 -3.00 17.30 -3 4 -17 95.79 21.20 -3 4 -17 99.09 22.80 -4 4 -17 60.09 17.50 -4 4 -17 34.80 18.00 -5 4 -17 139.29 22.90 -6 4 -17 13.90 16.20 -4 -5 17 15.70 25.50 4 5 -17 37.80 17.90 4 5 -17 32.80 22.90 -3 -5 17 -4.70 24.00 3 5 -17 9.90 16.70 3 5 -17 25.00 21.10 2 5 -17 25.00 16.70 2 5 -17 8.70 20.80 1 5 -17 11.00 15.40 1 5 -17 2.00 32.70 0 5 -17 4.50 20.00 0 5 -17 9.00 21.80 -1 5 -17 5.60 19.70 -1 5 -17 -7.80 22.20 -2 5 -17 128.99 23.20 -2 5 -17 93.19 19.80 -3 5 -17 -10.00 16.10 -3 5 -17 -6.30 14.20 -4 5 -17 211.88 27.00 -5 5 -17 26.90 15.10 0 6 -17 0.10 19.50 0 6 -17 -2.00 17.30 -1 6 -17 111.49 22.80 -1 6 -17 99.39 21.30 2 -2 18 -8.30 17.00 2 -2 18 48.10 20.70 -2 2 -18 26.00 13.40 -2 2 -18 -5.50 12.70 3 -2 18 44.90 20.10 -3 2 -18 35.30 14.00 -4 2 -18 208.88 26.30 -1 -3 18 142.19 26.80 -1 -3 18 108.99 27.60 1 3 -18 115.19 20.80 1 3 -18 121.69 21.60 0 -3 18 15.20 20.60 0 -3 18 -27.50 21.20 0 3 -18 -13.70 14.20 0 3 -18 14.40 15.20 1 -3 18 36.70 22.20 -1 3 -18 20.10 15.20 2 -3 18 22.20 19.70 -2 3 -18 14.60 13.60 -3 3 -18 207.48 25.80 -4 3 -18 10.60 16.60 -5 3 -18 -35.00 13.00 -3 -4 18 25.50 26.60 -3 -4 18 42.80 25.20 3 4 -18 -0.50 17.00 3 4 -18 33.20 17.70 -2 -4 18 26.70 25.00 2 4 -18 76.69 25.90 2 4 -18 15.00 17.40 0 -4 18 83.69 25.30 0 4 -18 104.69 18.90 0 4 -18 42.90 20.70 -1 4 -18 34.40 18.70 -1 4 -18 17.10 15.70 -2 4 -18 -9.60 17.20 -2 4 -18 -4.50 18.90 -3 4 -18 -13.50 16.30 -3 4 -18 6.20 17.50 -4 4 -18 18.60 16.50 -4 4 -18 40.60 17.50 -5 4 -18 11.60 16.40 2 5 -18 -23.90 14.40 2 5 -18 29.40 24.20 1 5 -18 22.80 17.20 1 5 -18 12.00 20.50 0 5 -18 15.60 20.20 0 5 -18 22.50 16.40 -1 5 -18 0.20 20.80 -1 5 -18 -12.60 18.10 -2 5 -18 -11.30 17.90 -2 5 -18 8.30 30.90 -3 5 -18 6.20 22.00 -3 5 -18 24.70 21.50 1 -3 19 -6.40 20.00 -1 3 -19 -8.40 14.10 2 -3 19 57.69 22.10 -2 3 -19 63.39 16.50 -3 3 -19 -14.90 13.00 -4 3 -19 259.67 31.40 -2 -4 19 14.60 24.30 2 4 -19 22.30 17.20 -1 -4 19 52.29 24.90 1 4 -19 11.60 16.40 0 -4 19 14.80 22.80 0 4 -19 15.90 15.70 -1 4 -19 114.19 25.40 -2 4 -19 2.20 19.70 -2 4 -19 -13.20 21.20 -3 4 -19 35.90 19.10 -3 4 -19 32.10 18.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 43562 _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 0.8274(3) 0.5972(5) 0.3545(2) 0.0527(12) Uani 1 1 d . . . . . O002 O 0.6821(2) 0.5995(5) 0.6493(2) 0.0500(11) Uani 1 1 d . . . . . O003 O 0.5252(2) 0.4925(5) 0.8125(2) 0.0459(11) Uani 1 1 d . . . . . O004 O 0.6631(2) 0.4196(5) 0.83367(19) 0.0458(10) Uani 1 1 d . . . . . O005 O 0.9260(3) 0.1118(6) 0.5109(2) 0.0562(13) Uani 1 1 d . . . . . O006 O 0.5655(3) 0.1251(6) 0.4839(2) 0.0534(12) Uani 1 1 d . . . . . O007 O 0.9783(2) 0.4634(5) 0.1786(2) 0.0510(12) Uani 1 1 d . . . . . N008 N 0.7625(3) 0.9332(6) 0.4651(3) 0.0268(10) Uani 1 1 d . . . . . O009 O 1.1209(2) 0.3041(6) 0.3403(2) 0.0627(13) Uani 1 1 d . . . . . N00A N 0.8338(3) 0.2590(5) 0.3010(2) 0.0274(10) Uani 1 1 d . . . . . O00B O 1.0332(2) 0.2853(5) 0.4934(2) 0.0560(12) Uani 1 1 d . . . . . O00C O 0.8367(2) 0.4091(5) 0.1599(2) 0.0546(12) Uani 1 1 d . . . . . O00D O 0.4586(2) 0.3007(5) 0.5014(2) 0.0559(12) Uani 1 1 d . . . . . N00E N 0.7291(3) 0.9407(5) 0.5363(2) 0.0278(10) Uani 1 1 d . . . . . O00F O 0.4461(3) 0.5901(6) 0.6565(2) 0.0681(15) Uani 1 1 d . . . . . N00G N 0.6874(3) 0.7448(7) 0.6332(3) 0.0328(11) Uani 1 1 d . . . . . O00H O 0.8256(3) 0.4347(5) 0.5245(2) 0.0627(13) Uani 1 1 d . . . . . N00I N 0.8460(2) 0.2058(5) 0.3750(2) 0.0283(10) Uani 1 1 d . . . . . O00J O 0.6876(3) 0.4252(5) 0.4853(2) 0.0599(12) Uani 1 1 d . . . . . N00K N 0.6410(3) 0.2023(6) 0.6270(3) 0.0302(11) Uani 1 1 d . . . . . N00L N 0.8140(3) 0.7417(6) 0.3681(3) 0.0347(11) Uani 1 1 d . . . . . N00M N 0.6618(2) 0.2525(5) 0.6997(2) 0.0282(10) Uani 1 1 d . . . . . N00N N 0.4425(3) 0.4416(7) 0.6577(2) 0.0399(12) Uani 1 1 d . . . . . N00O N 0.5940(3) 0.4236(5) 0.7943(2) 0.0313(11) Uani 1 1 d . . . . . N00P N 0.9071(3) 0.4089(5) 0.1987(2) 0.0334(11) Uani 1 1 d . . . . . O00Q O 0.6653(3) 0.8565(6) 0.6756(2) 0.0670(14) Uani 1 1 d . . . . . O00R O 0.8287(3) 0.8560(6) 0.3246(2) 0.0638(13) Uani 1 1 d . . . . . N00S N 0.7554(3) 0.4981(6) 0.5033(2) 0.0352(10) Uani 1 1 d . . . . . N00T N 0.9657(3) 0.2125(6) 0.4725(2) 0.0356(11) Uani 1 1 d . . . . . O00U O 0.3750(3) 0.3581(6) 0.6573(2) 0.0660(13) Uani 1 1 d . . . . . C00V C 0.7218(3) 0.7850(6) 0.5584(3) 0.0240(11) Uani 1 1 d . . . . . C00W C 0.7779(3) 0.7783(7) 0.4427(3) 0.0260(12) Uani 1 1 d . . . . . N00X N 0.5263(3) 0.2251(6) 0.5222(2) 0.0352(11) Uani 1 1 d . . . . . C00Y C 0.5919(3) 0.3438(6) 0.7187(3) 0.0235(11) Uani 1 1 d . . . . . N00Z N 1.0593(3) 0.4028(7) 0.3345(2) 0.0394(12) Uani 1 1 d . . . . . C010 C 0.5620(3) 0.2605(6) 0.5997(3) 0.0270(12) Uani 1 1 d . . . . . C011 C 0.9290(3) 0.2518(6) 0.3943(3) 0.0262(12) Uani 1 1 d . . . . . O012 O 1.0671(3) 0.5492(6) 0.3291(2) 0.0714(16) Uani 1 1 d . . . . . C013 C 0.7519(3) 0.6757(6) 0.5021(3) 0.0256(10) Uani 1 1 d . . . . . C014 C 0.9699(3) 0.3349(6) 0.3351(3) 0.0252(12) Uani 1 1 d . . . . . C015 C 0.9056(3) 0.3378(6) 0.2753(3) 0.0276(12) Uani 1 1 d . . . . . C016 C 0.5271(3) 0.3531(6) 0.6586(3) 0.0257(12) Uani 1 1 d . . . . . H008 H 0.783(4) 1.028(9) 0.432(4) 0.09(2) Uiso 1 1 d . . . . . H00K H 0.673(3) 0.138(6) 0.601(2) 0.004(11) Uiso 1 1 d . . . . . H00A H 0.780(4) 0.254(7) 0.274(3) 0.070(18) 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 0.063(3) 0.042(3) 0.055(3) -0.012(2) 0.017(2) 0.0151(19) O002 0.060(3) 0.040(3) 0.051(3) 0.015(2) 0.008(2) -0.0124(18) O003 0.046(3) 0.057(4) 0.035(2) -0.0088(18) 0.005(2) 0.0188(19) O004 0.037(2) 0.063(4) 0.036(2) -0.0141(17) -0.010(2) 0.0027(16) O005 0.042(3) 0.081(4) 0.046(3) 0.038(2) 0.003(2) -0.0055(19) O006 0.058(3) 0.059(4) 0.044(3) -0.028(2) 0.002(2) 0.0051(19) O007 0.043(3) 0.066(4) 0.044(3) 0.0180(19) -0.003(2) -0.0158(19) N008 0.026(3) 0.032(3) 0.022(2) 0.001(2) 0.004(2) -0.0017(17) O009 0.024(3) 0.103(4) 0.060(3) 0.009(2) 0.002(2) 0.0072(19) N00A 0.026(3) 0.033(4) 0.023(2) -0.0026(18) 0.000(2) -0.0022(17) O00B 0.038(3) 0.083(4) 0.046(3) 0.019(2) -0.015(2) -0.0158(19) O00C 0.040(3) 0.086(4) 0.037(2) 0.0201(19) -0.013(2) -0.0059(18) O00D 0.041(3) 0.092(4) 0.035(3) -0.010(2) -0.009(2) 0.0168(19) N00E 0.032(3) 0.028(3) 0.024(2) 0.0005(19) -0.002(2) -0.0003(16) O00F 0.083(3) 0.057(4) 0.063(3) -0.012(3) -0.014(3) 0.040(2) N00G 0.029(3) 0.039(4) 0.031(3) 0.003(2) 0.007(2) -0.0047(19) O00H 0.069(3) 0.045(4) 0.073(3) -0.002(2) -0.017(3) 0.022(2) N00I 0.031(3) 0.029(4) 0.025(2) 0.0031(17) -0.001(2) -0.0020(16) O00J 0.065(3) 0.039(4) 0.076(3) -0.001(2) -0.007(2) -0.0203(19) N00K 0.028(3) 0.034(4) 0.029(3) -0.0044(19) 0.006(2) 0.0086(18) N00L 0.035(3) 0.040(4) 0.029(3) -0.003(2) 0.009(2) 0.004(2) N00M 0.030(3) 0.030(4) 0.025(2) -0.0024(18) 0.000(2) 0.0060(17) N00N 0.034(3) 0.063(4) 0.022(3) -0.004(2) 0.000(2) 0.019(2) N00O 0.029(3) 0.029(4) 0.036(3) -0.0051(19) -0.001(2) 0.0001(16) N00P 0.038(3) 0.038(4) 0.025(3) 0.0043(19) 0.000(2) -0.0015(18) O00Q 0.115(4) 0.044(4) 0.044(3) 0.000(2) 0.040(3) 0.006(2) O00R 0.109(4) 0.046(4) 0.039(3) 0.004(2) 0.036(3) -0.001(2) N00S 0.047(3) 0.026(3) 0.032(3) -0.001(2) 0.002(2) -0.0015(19) N00T 0.030(3) 0.051(4) 0.027(3) 0.011(2) 0.004(2) -0.0001(19) O00U 0.018(3) 0.125(5) 0.055(3) 0.002(2) 0.006(2) -0.003(2) C00V 0.022(3) 0.021(4) 0.029(3) 0.001(2) -0.001(2) -0.0054(17) C00W 0.024(3) 0.030(4) 0.024(3) -0.004(2) 0.003(2) -0.0013(19) N00X 0.032(3) 0.044(4) 0.029(3) -0.006(2) -0.003(2) -0.0026(19) C00Y 0.024(3) 0.020(4) 0.026(3) -0.001(2) 0.005(2) -0.0057(18) N00Z 0.032(3) 0.060(4) 0.026(3) 0.011(2) 0.001(2) -0.013(2) C010 0.030(3) 0.026(4) 0.025(3) 0.002(2) 0.000(2) -0.0024(19) C011 0.027(3) 0.023(4) 0.029(3) 0.006(2) -0.001(2) 0.0029(18) O012 0.080(3) 0.064(4) 0.069(3) 0.029(3) -0.026(3) -0.041(2) C013 0.023(3) 0.026(3) 0.028(3) 0.002(2) 0.001(2) 0.0027(19) C014 0.020(3) 0.031(4) 0.024(3) 0.002(2) 0.003(2) -0.0003(18) C015 0.029(3) 0.031(4) 0.024(3) 0.002(2) 0.001(2) 0.0017(19) C016 0.018(3) 0.029(4) 0.030(3) 0.002(2) 0.001(2) 0.0013(18) 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 N00E N008 C00W 112.1(4) . . ? N00E N008 H008 127(5) . . ? C00W N008 H008 120(5) . . ? N00I N00A C015 112.4(4) . . ? N00I N00A H00A 123(3) . . ? C015 N00A H00A 124(3) . . ? C00V N00E N008 104.6(4) . . ? O002 N00G C00V 116.9(4) . . ? O00Q N00G O002 124.9(6) . . ? O00Q N00G C00V 118.2(6) . . ? C011 N00I N00A 103.6(4) . . ? N00M N00K C010 112.7(4) . . ? N00M N00K H00K 124(2) . . ? C010 N00K H00K 123(2) . . ? O001 N00L C00W 116.2(4) . . ? O00R N00L O001 126.2(6) . . ? O00R N00L C00W 117.7(5) . . ? N00K N00M C00Y 103.8(3) . . ? O00F N00N O00U 126.6(5) . . ? O00F N00N C016 117.1(5) . . ? O00U N00N C016 116.4(5) . . ? O003 N00O C00Y 116.3(3) . . ? O004 N00O O003 125.6(4) . . ? O004 N00O C00Y 118.1(4) . . ? O007 N00P O00C 126.5(4) . . ? O007 N00P C015 116.7(4) . . ? O00C N00P C015 116.8(4) . . ? O00H N00S C013 117.4(4) . . ? O00J N00S O00H 125.2(5) . . ? O00J N00S C013 117.3(4) . . ? O005 N00T C011 117.7(4) . . ? O00B N00T O005 126.1(4) . . ? O00B N00T C011 116.2(4) . . ? N00E C00V N00G 120.5(5) . . ? N00E C00V C013 112.5(5) . . ? C013 C00V N00G 127.0(5) . . ? N008 C00W N00L 121.6(5) . . ? N008 C00W C013 107.8(5) . . ? C013 C00W N00L 130.6(5) . . ? O006 N00X O00D 126.5(4) . . ? O006 N00X C010 117.4(4) . . ? O00D N00X C010 116.1(4) . . ? N00M C00Y N00O 118.5(4) . . ? N00M C00Y C016 112.7(4) . . ? C016 C00Y N00O 128.7(4) . . ? O009 N00Z C014 116.2(5) . . ? O012 N00Z O009 125.7(5) . . ? O012 N00Z C014 118.2(5) . . ? N00K C010 N00X 122.8(4) . . ? N00K C010 C016 107.2(4) . . ? C016 C010 N00X 130.0(4) . . ? N00I C011 N00T 118.8(4) . . ? N00I C011 C014 113.2(4) . . ? C014 C011 N00T 128.0(4) . . ? C00V C013 N00S 129.8(5) . . ? C00W C013 N00S 127.3(5) . . ? C00W C013 C00V 103.0(5) . . ? C011 C014 N00Z 128.9(4) . . ? C015 C014 N00Z 127.6(4) . . ? C015 C014 C011 103.5(4) . . ? N00A C015 N00P 122.2(4) . . ? N00A C015 C014 107.3(4) . . ? C014 C015 N00P 130.4(4) . . ? C00Y C016 N00N 128.2(4) . . ? C010 C016 N00N 128.2(4) . . ? C010 C016 C00Y 103.5(4) . . ? 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 N00L 1.216(6) . ? O002 N00G 1.217(6) . ? O003 N00O 1.220(5) . ? O004 N00O 1.209(4) . ? O005 N00T 1.216(5) . ? O006 N00X 1.207(5) . ? O007 N00P 1.213(5) . ? N008 N00E 1.327(6) . ? N008 C00W 1.339(7) . ? N008 H008 1.01(7) . ? O009 N00Z 1.223(6) . ? N00A N00I 1.335(5) . ? N00A C015 1.336(6) . ? N00A H00A 0.91(5) . ? O00B N00T 1.211(5) . ? O00C N00P 1.219(4) . ? O00D N00X 1.224(5) . ? N00E C00V 1.327(6) . ? O00F N00N 1.210(6) . ? N00G O00Q 1.213(6) . ? N00G C00V 1.426(7) . ? O00H N00S 1.211(5) . ? N00I C011 1.325(5) . ? O00J N00S 1.203(5) . ? N00K N00M 1.327(5) . ? N00K C010 1.338(5) . ? N00K H00K 0.84(4) . ? N00L O00R 1.213(6) . ? N00L C00W 1.427(7) . ? N00M C00Y 1.330(6) . ? N00N O00U 1.215(6) . ? N00N C016 1.454(6) . ? N00O C00Y 1.439(6) . ? N00P C015 1.425(6) . ? N00S C013 1.446(7) . ? N00T C011 1.453(5) . ? C00V C013 1.393(7) . ? C00W C013 1.376(7) . ? N00X C010 1.430(5) . ? C00Y C016 1.382(5) . ? N00Z O012 1.200(6) . ? N00Z C014 1.446(6) . ? C010 C016 1.371(7) . ? C011 C014 1.374(6) . ? C014 C015 1.371(6) . ? 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 N00L C00W N008 178.3(4) . . . . ? O001 N00L C00W C013 -2.8(7) . . . . ? O002 N00G C00V N00E 179.5(4) . . . . ? O002 N00G C00V C013 -1.4(6) . . . . ? O003 N00O C00Y N00M -173.0(5) . . . . ? O003 N00O C00Y C016 10.0(9) . . . . ? O004 N00O C00Y N00M 8.3(8) . . . . ? O004 N00O C00Y C016 -168.7(5) . . . . ? O005 N00T C011 N00I 14.4(9) . . . . ? O005 N00T C011 C014 -166.2(6) . . . . ? O006 N00X C010 N00K 7.7(10) . . . . ? O006 N00X C010 C016 -172.1(7) . . . . ? O007 N00P C015 N00A -173.0(5) . . . . ? O007 N00P C015 C014 7.7(9) . . . . ? N008 N00E C00V N00G -179.8(4) . . . . ? N008 N00E C00V C013 1.0(5) . . . . ? N008 C00W C013 N00S 179.4(4) . . . . ? N008 C00W C013 C00V -0.4(5) . . . . ? O009 N00Z C014 C011 64.0(8) . . . . ? O009 N00Z C014 C015 -115.5(6) . . . . ? N00A N00I C011 N00T -179.7(5) . . . . ? N00A N00I C011 C014 0.8(6) . . . . ? O00B N00T C011 N00I -165.0(5) . . . . ? O00B N00T C011 C014 14.4(9) . . . . ? O00C N00P C015 N00A 7.1(8) . . . . ? O00C N00P C015 C014 -172.2(5) . . . . ? O00D N00X C010 N00K -172.0(5) . . . . ? O00D N00X C010 C016 8.2(10) . . . . ? N00E N008 C00W N00L -179.9(4) . . . . ? N00E N008 C00W C013 1.0(5) . . . . ? N00E C00V C013 N00S 179.9(4) . . . . ? N00E C00V C013 C00W -0.4(5) . . . . ? O00F N00N C016 C00Y 69.4(7) . . . . ? O00F N00N C016 C010 -109.8(7) . . . . ? N00G C00V C013 N00S 0.8(8) . . . . ? N00G C00V C013 C00W -179.5(4) . . . . ? O00H N00S C013 C00V -96.0(6) . . . . ? O00H N00S C013 C00W 84.4(6) . . . . ? N00I N00A C015 N00P -178.5(4) . . . . ? N00I N00A C015 C014 1.0(6) . . . . ? N00I C011 C014 N00Z -179.8(5) . . . . ? N00I C011 C014 C015 -0.2(6) . . . . ? O00J N00S C013 C00V 82.1(6) . . . . ? O00J N00S C013 C00W -97.5(6) . . . . ? N00K N00M C00Y N00O -177.9(5) . . . . ? N00K N00M C00Y C016 -0.4(7) . . . . ? N00K C010 C016 N00N -179.8(5) . . . . ? N00K C010 C016 C00Y 0.9(7) . . . . ? N00L C00W C013 N00S 0.3(8) . . . . ? N00L C00W C013 C00V -179.4(4) . . . . ? N00M N00K C010 N00X 179.0(5) . . . . ? N00M N00K C010 C016 -1.2(7) . . . . ? N00M C00Y C016 N00N -179.7(5) . . . . ? N00M C00Y C016 C010 -0.3(7) . . . . ? N00O C00Y C016 N00N -2.5(10) . . . . ? N00O C00Y C016 C010 176.9(5) . . . . ? O00Q N00G C00V N00E -0.1(6) . . . . ? O00Q N00G C00V C013 179.0(5) . . . . ? O00R N00L C00W N008 -1.5(6) . . . . ? O00R N00L C00W C013 177.4(5) . . . . ? N00T C011 C014 N00Z 0.7(10) . . . . ? N00T C011 C014 C015 -179.6(5) . . . . ? O00U N00N C016 C00Y -111.3(6) . . . . ? O00U N00N C016 C010 69.4(8) . . . . ? C00W N008 N00E C00V -1.2(4) . . . . ? N00X C010 C016 N00N 0.0(11) . . . . ? N00X C010 C016 C00Y -179.3(5) . . . . ? N00Z C014 C015 N00A 179.2(5) . . . . ? N00Z C014 C015 N00P -1.4(10) . . . . ? C010 N00K N00M C00Y 1.0(7) . . . . ? C011 C014 C015 N00A -0.4(6) . . . . ? C011 C014 C015 N00P 178.9(5) . . . . ? O012 N00Z C014 C011 -115.4(6) . . . . ? O012 N00Z C014 C015 65.1(7) . . . . ? C015 N00A N00I C011 -1.1(6) . . . . ?