#------------------------------------------------------------------------------ #$Date: 2023-11-10 04:00:10 +0200 (Fri, 10 Nov 2023) $ #$Revision: 287506 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247693.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_7247693 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.cc29gp6p _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 92.078(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.7836(11) _cell_length_b 8.0383(8) _cell_length_c 16.8670(12) _cell_measurement_reflns_used 2947 _cell_measurement_temperature 300.8 _cell_measurement_theta_max 25.02 _cell_measurement_theta_min 2.76 _cell_volume 2003.1(3) _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 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 300.8 _diffrn_measured_fraction_theta_full 0.549 _diffrn_measured_fraction_theta_max 0.506 _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 0.0445 _diffrn_reflns_av_unetI/netI 0.0483 _diffrn_reflns_Laue_measured_fraction_full 0.549 _diffrn_reflns_Laue_measured_fraction_max 0.506 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 10642 _diffrn_reflns_point_group_measured_fraction_full 0.549 _diffrn_reflns_point_group_measured_fraction_max 0.506 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.361 _diffrn_reflns_theta_min 2.417 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.197 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6758 _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 2.020 _exptl_crystal_description block _exptl_crystal_F_000 1224 _refine_diff_density_max 0.156 _refine_diff_density_min -0.192 _refine_diff_density_rms 0.043 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 391 _refine_ls_number_reflns 2068 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0445 _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^)+(0.0689P)^2^+0.6636P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1081 _refine_ls_wR_factor_ref 0.1236 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1435 _reflns_number_total 2068 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3cp04526a2.cif _cod_data_source_block 2tnp_p04 _cod_database_code 7247693 _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 ; ; _shelx_res_file ; TITL 2tnp_p04_a.res in P2(1)/c 2tnp_p04.res created by SHELXL-2018/3 at 20:29:32 on 08-Jul-2020 REM Old TITL 2TNP_P04 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.222, Rweak 0.007, Alpha 0.116, Orientation as input REM Formula found by SHELXT: C31 N2 O9 CELL 0.71073 14.7836 8.0383 16.867 90 92.078 90 ZERR 4 0.0011 0.0008 0.0012 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 36 12 60 72 L.S. 10 PLAN 20 TEMP 27.65 CONF BOND $H list 4 fmap 2 53 MORE -1 ACTA OMIT 1 2 7 OMIT 7 1 1 OMIT -2 2 7 OMIT 0 1 8 OMIT -5 3 1 OMIT 0 2 7 OMIT -1 1 8 REM REM REM WGHT 0.068900 0.663600 FVAR 0.61385 O001 4 0.683301 0.596142 0.650583 11.00000 0.05683 0.02940 = 0.04557 0.01224 0.00712 -0.01154 O002 4 0.522590 0.496367 0.812250 11.00000 0.04211 0.05041 = 0.03412 -0.00983 0.00362 0.01935 O003 4 0.661654 0.420901 0.833844 11.00000 0.03391 0.05557 = 0.03291 -0.00996 -0.00895 0.00056 O004 4 0.831787 0.598648 0.354377 11.00000 0.06331 0.03517 = 0.05359 -0.00999 0.01319 0.01574 N005 3 0.760699 0.936939 0.464518 11.00000 0.02800 0.02587 = 0.02121 -0.00008 0.00406 0.00038 O006 4 0.925340 0.107820 0.510464 11.00000 0.04639 0.07221 = 0.04185 0.03397 0.00202 -0.00682 O007 4 0.563317 0.127336 0.480874 11.00000 0.04983 0.05679 = 0.03774 -0.02572 0.00102 0.00471 N008 3 0.727157 0.941570 0.536435 11.00000 0.02656 0.02704 = 0.02230 -0.00078 0.00016 0.00038 O009 4 0.836483 0.410033 0.158108 11.00000 0.03360 0.08210 = 0.03616 0.02206 -0.00980 -0.00511 O00A 4 1.033175 0.285454 0.494593 11.00000 0.03728 0.07848 = 0.03948 0.01270 -0.01295 -0.01317 O00B 4 0.980320 0.459024 0.176101 11.00000 0.03284 0.07544 = 0.03602 0.01244 0.00421 -0.01608 O00C 4 1.122228 0.296919 0.340589 11.00000 0.02196 0.09384 = 0.05652 0.00952 0.00057 0.00704 O00D 4 0.456912 0.307827 0.498885 11.00000 0.03586 0.08125 = 0.03438 -0.01123 -0.00850 0.01423 N00E 3 0.639667 0.203205 0.625226 11.00000 0.02710 0.02446 = 0.02647 -0.00519 0.00468 0.00570 N00F 3 0.843702 0.208056 0.375138 11.00000 0.03018 0.02259 = 0.02763 0.00482 -0.00230 -0.00173 N00G 3 0.814726 0.742774 0.367335 11.00000 0.03524 0.02982 = 0.03014 0.00033 0.00390 0.00295 O00H 4 0.690848 0.418603 0.483852 11.00000 0.05388 0.03645 = 0.06555 -0.00474 -0.00199 -0.01772 N00I 3 0.687080 0.742749 0.634676 11.00000 0.03351 0.03309 = 0.02787 0.00236 0.00509 -0.00333 O00J 4 0.442924 0.596151 0.655757 11.00000 0.08672 0.04784 = 0.05530 -0.01068 -0.01527 0.03900 N00K 3 0.659925 0.251643 0.698896 11.00000 0.02858 0.03131 = 0.02075 -0.00065 0.00263 0.00462 O00L 4 0.828998 0.434389 0.527003 11.00000 0.06723 0.03571 = 0.06904 -0.00041 -0.02002 0.01924 N00M 3 0.907740 0.406198 0.196489 11.00000 0.02944 0.03557 = 0.02443 0.00448 -0.00103 -0.00133 N00N 3 0.831126 0.261265 0.300720 11.00000 0.02435 0.02696 = 0.02346 -0.00159 -0.00110 -0.00168 N00O 3 1.061129 0.399137 0.333381 11.00000 0.02456 0.05948 = 0.02503 0.00931 0.00310 -0.01097 N00P 3 0.438938 0.446062 0.657110 11.00000 0.03696 0.05253 = 0.01959 -0.00212 -0.00189 0.01495 N00Q 3 0.591644 0.425857 0.794021 11.00000 0.02747 0.02524 = 0.02465 0.00075 0.00165 0.00260 O00R 4 0.826429 0.859276 0.322620 11.00000 0.09085 0.04088 = 0.04060 0.00565 0.03362 0.00303 N00S 3 0.964683 0.211043 0.473043 11.00000 0.02721 0.04802 = 0.02775 0.01224 0.00192 0.00117 O00T 4 1.070639 0.546364 0.326251 11.00000 0.06991 0.06016 = 0.06129 0.02641 -0.02309 -0.03948 O00U 4 0.665012 0.855763 0.677177 11.00000 0.09746 0.04571 = 0.04191 -0.00108 0.03396 0.00830 N00V 3 0.757977 0.495792 0.504303 11.00000 0.04214 0.03056 = 0.02425 0.00232 0.00375 0.00138 O00W 4 0.371500 0.360694 0.656044 11.00000 0.02482 0.11025 = 0.05212 0.00435 0.00010 -0.00530 N00X 3 0.524558 0.229227 0.519651 11.00000 0.02998 0.04072 = 0.02767 -0.00582 -0.00220 -0.00462 C00Y 1 0.560074 0.263594 0.598586 11.00000 0.02490 0.02338 = 0.02453 -0.00201 -0.00176 -0.00222 C00Z 1 0.753051 0.675356 0.501902 11.00000 0.02107 0.01567 = 0.02561 0.00243 -0.00028 0.00168 C010 1 0.590403 0.344904 0.718389 11.00000 0.02419 0.01993 = 0.01987 0.00034 0.00284 -0.00313 C011 1 0.777812 0.780712 0.442126 11.00000 0.02017 0.02642 = 0.02148 -0.00192 0.00033 0.00262 C012 1 0.927680 0.251276 0.394586 11.00000 0.02467 0.01863 = 0.02377 0.00248 0.00037 0.00241 C013 1 0.905437 0.336921 0.273958 11.00000 0.02424 0.02451 = 0.01837 0.00149 0.00457 0.00236 C014 1 0.524779 0.357201 0.657499 11.00000 0.01718 0.02760 = 0.02699 -0.00164 0.00192 -0.00051 C015 1 0.970177 0.332366 0.334078 11.00000 0.01590 0.03802 = 0.02470 0.00265 0.00476 0.00173 C016 1 0.721578 0.785684 0.558974 11.00000 0.02014 0.02343 = 0.02397 0.00244 -0.00024 -0.00109 H00E 2 0.674691 0.131242 0.598393 11.00000 0.02171 H00N 2 0.773058 0.262908 0.272186 11.00000 0.07430 H005 2 0.779282 1.031498 0.431650 11.00000 0.08653 HKLF 4 REM 2tnp_p04_a.res in P2(1)/c REM wR2 = 0.123606, GooF = S = 1.05117, Restrained GooF = 1.05117 for all data REM R1 = 0.044476 for 1435 Fo > 4sig(Fo) and 0.076727 for all 2068 data REM 391 parameters refined using 0 restraints END WGHT 0.0690 0.6637 REM Highest difference peak 0.156, deepest hole -0.192, 1-sigma level 0.043 Q1 1 0.9454 0.2423 0.4205 11.00000 0.05 0.16 Q2 1 0.5580 0.3780 0.6915 11.00000 0.05 0.16 Q3 1 0.6298 0.3210 0.7014 11.00000 0.05 0.16 Q4 1 0.5728 0.1954 0.6194 11.00000 0.05 0.15 Q5 1 0.6099 0.2660 0.7161 11.00000 0.05 0.15 Q6 1 0.6599 0.9581 0.5587 11.00000 0.05 0.15 Q7 1 1.0107 0.6029 0.3608 11.00000 0.05 0.14 Q8 1 0.7966 0.2422 0.2799 11.00000 0.05 0.14 Q9 1 0.7635 0.1143 0.3143 11.00000 0.05 0.14 Q10 1 0.9573 0.2949 0.2870 11.00000 0.05 0.14 Q11 1 0.2784 0.3335 0.6548 11.00000 0.05 0.14 Q12 1 0.8898 0.2805 0.2844 11.00000 0.05 0.14 Q13 1 0.7550 0.4315 0.1763 11.00000 0.05 0.14 Q14 1 0.9165 0.3779 0.3084 11.00000 0.05 0.14 Q15 1 1.1375 0.6706 0.3380 11.00000 0.05 0.14 Q16 1 0.9348 0.5283 0.1577 11.00000 0.05 0.14 Q17 1 0.6583 0.1651 0.6119 11.00000 0.05 0.14 Q18 1 0.5876 0.8199 0.6975 11.00000 0.05 0.14 Q19 1 0.9381 0.3388 0.3024 11.00000 0.05 0.14 Q20 1 0.6769 0.3766 0.5607 11.00000 0.05 0.13 ; _shelx_res_checksum 45066 _shelx_hkl_file ; -2 0 0 338.77 15.10 2 0 0 329.27 15.00 3 0 0 154.08 7.40 -3 0 0 152.78 7.40 -4 0 0 39.50 3.20 4 0 0 37.70 2.90 4 0 0 42.40 3.10 -4 0 0 37.70 2.90 5 0 0 109.29 6.40 -5 0 0 109.29 6.30 -5 0 0 112.69 6.10 5 0 0 112.09 6.30 -1 -1 0 179.28 8.60 -1 -1 0 181.58 8.20 -1 -1 0 179.68 8.70 -1 -1 0 178.78 8.30 1 1 0 177.48 8.20 1 1 0 178.28 8.20 1 1 0 176.78 8.70 1 1 0 179.28 8.60 -2 -1 0 0.50 0.70 -2 -1 0 0.70 0.70 -2 -1 0 1.80 0.80 -2 -1 0 1.30 0.70 -2 -1 0 1.10 1.40 -2 -1 0 2.00 0.90 -2 -1 0 1.40 1.00 2 1 0 0.80 0.60 2 1 0 1.80 0.70 2 1 0 1.80 0.70 2 1 0 2.40 0.70 2 1 0 2.00 1.00 2 1 0 1.20 1.20 2 1 0 1.50 0.90 -4 -1 0 75.49 4.50 -4 -1 0 77.99 6.10 -4 -1 0 73.99 5.70 -4 -1 0 75.69 4.50 -4 -1 0 78.69 4.50 4 1 0 72.39 5.30 4 1 0 79.39 4.60 4 1 0 70.09 4.70 4 1 0 69.29 5.90 4 1 0 79.69 4.70 -5 -1 0 84.49 6.80 -5 -1 0 83.59 5.20 -5 -1 0 86.59 5.20 -5 -1 0 85.39 5.30 -5 -1 0 82.39 7.80 5 1 0 89.99 5.20 5 1 0 84.99 7.30 5 1 0 80.59 5.30 5 1 0 84.69 5.40 5 1 0 84.89 7.30 -6 -1 0 1.50 2.20 -6 -1 0 3.60 3.60 -6 -1 0 1.60 2.00 -6 -1 0 4.70 3.90 6 1 0 1.00 2.20 6 1 0 1.70 2.00 6 1 0 -1.40 2.90 6 1 0 0.00 3.50 6 1 0 0.30 1.80 -7 -1 0 534.85 24.20 -7 -1 0 558.34 24.40 7 1 0 455.25 24.20 7 1 0 545.75 24.60 7 1 0 484.05 24.20 -8 -1 0 12.70 3.40 -8 -1 0 21.80 4.20 -8 -1 0 10.10 5.70 -8 -1 0 12.60 3.60 8 1 0 18.40 3.50 8 1 0 16.50 3.60 8 1 0 16.60 4.10 8 1 0 24.80 6.00 8 1 0 21.30 3.80 -9 -1 0 15.50 4.30 -9 -1 0 17.00 6.70 -9 -1 0 23.50 4.40 -9 -1 0 21.30 4.70 9 1 0 19.30 4.50 9 1 0 20.40 4.50 9 1 0 32.30 7.20 9 1 0 17.60 4.50 9 1 0 19.30 4.30 -10 -1 0 138.09 10.00 -10 -1 0 110.19 11.90 10 1 0 117.09 9.60 10 1 0 158.98 13.40 -11 -1 0 450.95 23.10 -2 -2 0 15.40 1.80 -2 -2 0 19.90 2.10 -2 -2 0 20.20 2.70 -2 -2 0 18.80 2.80 2 2 0 20.60 1.80 2 2 0 20.50 2.00 2 2 0 16.80 2.50 2 2 0 21.10 2.10 2 2 0 18.20 2.60 -3 -2 0 14.00 2.10 -3 -2 0 16.40 2.40 -3 -2 0 12.80 2.10 -3 -2 0 15.20 2.70 -3 -2 0 13.40 2.80 -3 -2 0 17.40 2.20 3 2 0 12.50 1.90 3 2 0 11.50 1.90 3 2 0 10.80 2.90 3 2 0 12.40 2.50 3 2 0 11.00 1.90 3 2 0 7.30 2.30 3 2 0 12.00 3.60 3 2 0 12.10 2.00 -4 -2 0 558.34 27.70 -4 -2 0 558.44 25.40 -4 -2 0 564.24 25.70 -4 -2 0 562.64 26.70 4 2 0 561.04 25.50 4 2 0 576.24 27.00 4 2 0 588.54 25.60 4 2 0 540.05 26.20 4 2 0 545.75 25.60 4 2 0 529.55 26.40 -5 -2 0 28.00 3.10 -5 -2 0 28.70 5.60 -5 -2 0 37.50 4.90 -5 -2 0 33.70 5.00 -5 -2 0 32.40 3.50 -5 -2 0 34.70 3.20 5 2 0 28.30 3.20 5 2 0 29.30 3.20 5 2 0 30.40 3.10 5 2 0 25.50 3.20 5 2 0 36.30 3.40 5 2 0 41.30 3.40 5 2 0 34.80 5.90 5 2 0 41.20 4.50 5 2 0 40.70 4.40 5 2 0 33.10 5.10 -6 -2 0 927.41 43.40 -6 -2 0 1045.50 45.40 -6 -2 0 852.21 43.60 -6 -2 0 972.00 44.50 -6 -2 0 1041.50 45.90 -6 -2 0 876.61 43.00 6 2 0 989.90 44.00 6 2 0 988.00 43.10 6 2 0 902.91 43.20 6 2 0 820.22 44.00 6 2 0 958.90 43.30 6 2 0 935.11 43.00 6 2 0 1001.00 43.40 6 2 0 977.10 44.30 6 2 0 990.70 45.40 -7 -2 0 18.70 3.70 -7 -2 0 29.00 7.90 -7 -2 0 24.40 5.70 -7 -2 0 20.10 3.80 7 2 0 29.10 4.10 7 2 0 13.70 4.80 7 2 0 23.70 5.00 7 2 0 18.60 6.00 7 2 0 14.30 4.00 7 2 0 24.70 4.20 7 2 0 20.30 3.40 7 2 0 25.30 4.10 -8 -2 0 23.30 4.50 -8 -2 0 28.70 6.30 8 2 0 22.70 5.30 8 2 0 21.00 4.50 8 2 0 31.60 4.80 8 2 0 29.80 7.60 8 2 0 28.10 6.80 8 2 0 20.90 4.60 -9 -2 0 4.00 6.20 -9 -2 0 1.30 4.40 9 2 0 7.00 4.70 9 2 0 6.70 4.60 9 2 0 2.80 4.20 9 2 0 5.30 3.80 9 2 0 10.60 4.70 9 2 0 3.70 5.30 -10 -2 0 112.79 9.10 -10 -2 0 100.69 11.00 10 2 0 111.29 9.20 10 2 0 105.69 10.30 10 2 0 105.69 8.80 10 2 0 111.49 9.20 -11 -2 0 5.60 5.90 -11 -2 0 17.60 8.30 11 2 0 13.80 5.80 11 2 0 6.40 5.70 11 2 0 8.70 5.90 11 2 0 8.20 6.60 -12 -2 0 362.36 20.40 -12 -2 0 374.36 24.40 12 2 0 335.67 20.40 12 2 0 339.27 20.40 12 2 0 364.56 22.70 12 2 0 327.67 19.60 -13 -2 0 76.89 11.90 -13 -2 0 85.39 9.30 13 2 0 69.59 10.20 13 2 0 73.79 8.90 13 2 0 68.19 9.40 13 2 0 77.19 9.40 -3 -3 0 475.85 24.00 -3 -3 0 488.25 23.90 -3 -3 0 534.75 25.70 -3 -3 0 523.25 25.30 3 3 0 501.05 27.40 3 3 0 542.25 24.20 3 3 0 539.65 23.70 3 3 0 526.75 24.00 -4 -3 0 13.00 3.40 -4 -3 0 7.60 2.60 -4 -3 0 8.80 2.70 -4 -3 0 3.90 2.70 -4 -3 0 7.90 4.30 -4 -3 0 4.50 3.90 4 3 0 6.50 3.80 4 3 0 7.20 2.40 4 3 0 6.90 2.80 4 3 0 5.90 2.80 4 3 0 4.60 4.60 4 3 0 10.30 5.70 4 3 0 8.70 2.30 4 3 0 4.50 3.60 -5 -3 0 305.97 15.90 -5 -3 0 325.77 15.60 5 3 0 319.47 15.70 5 3 0 290.77 15.40 -6 -3 0 98.59 7.30 -6 -3 0 114.79 8.20 -6 -3 0 104.79 9.70 6 3 0 114.19 10.10 6 3 0 109.29 8.20 6 3 0 103.99 7.40 6 3 0 116.09 9.50 6 3 0 104.69 7.50 6 3 0 107.99 9.30 6 3 0 108.29 7.90 6 3 0 106.19 10.10 -7 -3 0 6.70 4.20 -7 -3 0 2.60 3.60 -7 -3 0 1.90 5.30 -7 -3 0 5.60 3.60 -7 -3 0 3.00 6.00 7 3 0 -2.70 3.20 7 3 0 6.40 3.90 7 3 0 6.40 3.60 7 3 0 -1.30 3.60 7 3 0 -0.90 4.50 7 3 0 0.30 6.00 7 3 0 -1.40 3.60 7 3 0 -2.80 4.30 -8 -3 0 2.50 4.30 -8 -3 0 7.10 4.30 -8 -3 0 5.50 4.10 8 3 0 -1.60 4.00 8 3 0 4.00 3.90 8 3 0 5.70 4.40 8 3 0 4.00 4.30 8 3 0 5.70 5.00 8 3 0 7.20 6.80 8 3 0 -3.50 4.00 8 3 0 2.60 5.10 -9 -3 0 692.13 32.80 -9 -3 0 709.73 38.10 -9 -3 0 677.13 32.90 -9 -3 0 686.13 32.70 9 3 0 675.83 34.60 9 3 0 718.73 33.20 9 3 0 721.53 33.20 9 3 0 642.24 33.20 9 3 0 727.33 37.50 9 3 0 674.83 34.20 -10 -3 0 235.68 14.30 -10 -3 0 230.28 24.00 -10 -3 0 213.18 13.80 10 3 0 217.28 14.20 10 3 0 218.28 16.40 10 3 0 208.88 17.30 10 3 0 223.48 14.30 10 3 0 215.68 15.70 -11 -3 0 275.87 22.10 -11 -3 0 259.37 26.00 11 3 0 315.07 19.10 11 3 0 295.47 23.60 11 3 0 307.57 19.40 11 3 0 284.17 20.10 -12 -3 0 3.40 6.30 -12 -3 0 14.50 6.20 -12 -3 0 -3.80 10.40 12 3 0 1.20 6.60 12 3 0 -9.10 7.30 12 3 0 3.40 7.60 12 3 0 6.00 6.90 12 3 0 -0.30 7.10 -13 -3 0 96.79 10.20 -13 -3 0 41.20 12.40 -13 -3 0 88.59 9.00 13 3 0 59.99 9.10 13 3 0 68.99 9.20 13 3 0 56.49 9.70 13 3 0 72.29 10.30 13 3 0 62.69 9.80 -14 -3 0 0.50 7.10 -14 -3 0 -4.00 7.60 -14 -3 0 -3.90 11.30 14 3 0 -2.10 7.80 14 3 0 -2.50 7.70 14 3 0 -8.20 7.20 14 3 0 -5.50 7.80 14 3 0 0.70 8.40 -15 -3 0 2.90 7.80 -15 -3 0 13.10 8.10 15 3 0 5.50 8.50 15 3 0 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-8.80 4.30 3 0 15 6.90 4.70 -4 0 -15 3.40 8.10 -4 0 -15 -4.70 6.70 -4 0 -15 -3.00 7.90 4 0 15 -1.10 4.70 -4 0 -15 -2.40 5.20 4 0 15 -13.10 17.30 4 0 15 3.30 4.80 4 0 15 -3.40 10.60 5 0 15 -0.40 4.90 -5 0 -15 -4.80 7.40 -5 0 -15 -7.00 5.50 5 0 15 -2.50 5.40 5 0 15 -3.80 4.80 -5 0 -15 -9.80 7.40 5 0 15 -20.50 13.90 -5 0 -15 2.00 5.30 -6 0 -15 0.30 5.50 -6 0 -15 -1.60 6.80 -6 0 -15 10.30 7.20 6 0 15 1.20 6.00 -7 0 -15 7.60 6.80 8 0 15 9.30 7.90 9 0 15 5.70 7.40 9 0 15 -5.10 7.10 10 0 15 -4.30 7.90 10 0 15 -5.60 7.30 11 0 15 -0.70 8.20 11 0 15 -7.20 8.30 12 0 15 3.50 9.00 12 0 15 -14.20 8.70 0 -1 15 4.90 3.30 0 -1 15 3.30 13.10 0 1 -15 -6.30 3.40 1 -1 15 14.10 12.90 1 -1 15 1.90 3.40 1 -1 15 1.60 3.30 -1 1 -15 -1.70 7.90 -1 1 -15 1.20 3.60 2 -1 15 862.01 39.30 2 -1 15 856.81 39.20 2 -1 15 817.02 47.20 2 -1 15 868.71 39.10 -2 1 -15 888.41 39.50 -2 1 -15 869.91 43.30 -2 1 -15 843.92 39.10 3 -1 15 1.20 4.20 3 -1 15 2.10 3.70 3 -1 15 6.00 17.50 3 -1 15 -7.80 10.60 -3 1 -15 -9.00 6.90 -3 1 -15 4.00 7.90 -3 1 -15 7.00 8.90 -3 1 -15 5.90 4.00 4 -1 15 320.37 17.30 4 -1 15 332.77 17.80 4 -1 15 355.16 28.30 -4 1 -15 333.87 22.60 -4 1 -15 346.17 24.00 5 -1 15 24.80 4.90 5 -1 15 28.30 5.70 -5 1 -15 26.10 8.90 -6 -1 -15 123.29 10.70 6 -1 15 134.59 9.90 6 -1 15 124.19 9.30 -6 1 -15 121.99 12.10 6 1 15 134.49 10.20 -6 1 -15 130.89 12.30 7 -1 15 -0.60 5.20 -7 -1 -15 9.20 6.40 7 -1 15 -3.60 6.10 -7 -1 -15 3.30 7.10 7 1 15 4.70 6.30 7 1 15 8.00 6.80 -8 -1 -15 203.38 14.90 8 -1 15 176.58 18.30 8 -1 15 221.38 15.00 8 1 15 190.78 14.20 9 -1 15 30.20 9.20 -9 -1 -15 23.30 7.80 9 1 15 19.10 8.40 10 -1 15 4.40 7.70 10 -1 15 -5.70 7.20 10 1 15 1.80 8.50 10 1 15 1.40 8.10 11 -1 15 6.90 8.00 11 1 15 9.40 9.00 11 1 15 4.00 8.80 12 -1 15 30.50 9.20 12 1 15 22.20 9.70 12 1 15 10.60 10.50 -2 -2 15 -18.50 13.50 2 2 -15 -6.30 8.40 -1 -2 15 336.67 28.90 1 2 -15 291.77 22.30 0 -2 15 13.10 44.40 0 2 -15 15.20 10.80 0 2 -15 9.90 11.90 1 -2 15 5.10 12.70 1 -2 15 17.00 19.60 -1 2 -15 -6.10 7.90 -1 2 -15 6.40 9.60 2 -2 15 153.48 26.10 -2 2 -15 113.69 22.10 3 -2 15 2.10 16.90 -3 2 -15 6.20 9.20 -4 2 -15 30.20 9.90 -5 2 -15 746.63 39.40 -5 2 -15 759.42 39.70 -5 2 -15 712.53 43.00 -6 2 -15 38.50 11.80 -6 2 -15 36.50 9.20 -6 2 -15 46.00 9.70 8 -2 15 7.20 6.10 -9 -2 -15 -7.20 8.40 9 -2 15 -5.70 6.20 -9 -2 -15 -4.40 7.50 9 2 15 5.50 8.30 9 2 15 -9.40 7.10 -10 -2 -15 9.10 8.50 10 -2 15 9.00 7.00 10 2 15 14.60 8.80 -11 -2 -15 4.40 8.60 11 2 15 7.60 10.40 -5 -3 15 4.90 17.60 5 3 -15 7.20 11.00 -4 -3 15 12.20 17.30 4 3 -15 2.50 10.40 -3 -3 15 151.48 28.80 -3 -3 15 99.59 20.00 3 3 -15 72.89 15.30 3 3 -15 81.49 13.30 -2 -3 15 470.35 40.10 -2 -3 15 385.96 35.00 2 3 -15 405.66 28.00 2 3 -15 406.86 29.60 -1 -3 15 39.30 15.50 -1 -3 15 4.90 21.60 1 3 -15 15.50 9.80 1 3 -15 21.20 12.00 0 -3 15 8.90 21.60 0 3 -15 29.30 12.30 1 -3 15 37.40 22.00 -1 3 -15 22.20 11.50 -2 3 -15 94.79 15.60 -3 3 -15 15.20 11.50 -4 3 -15 -16.50 9.90 -5 3 -15 55.89 11.60 -7 -4 15 290.17 29.90 -7 -4 15 312.57 37.60 7 4 -15 264.57 22.90 7 4 -15 295.57 26.60 -6 -4 15 -22.80 25.90 -6 -4 15 10.40 18.30 6 4 -15 -7.00 10.40 6 4 -15 10.30 13.20 -5 -4 15 11.90 21.50 -5 -4 15 30.20 16.00 5 4 -15 4.90 10.70 5 4 -15 30.60 13.90 -4 -4 15 4.00 21.10 -4 -4 15 5.80 16.20 4 4 -15 -6.70 10.40 4 4 -15 3.90 12.60 -3 -4 15 24.40 21.80 3 4 -15 -1.30 12.20 -2 -4 15 5.60 19.90 2 4 -15 -0.80 11.80 -1 -4 15 -21.00 20.00 1 4 -15 -10.60 10.90 0 4 -15 -2.80 11.30 -1 4 -15 42.50 13.20 -2 4 -15 33.80 12.70 3 -4 15 136.39 22.00 -3 4 -15 150.88 17.20 4 -4 15 -13.80 15.00 -4 4 -15 -3.00 10.70 5 -4 15 14.60 16.60 6 -4 15 7.00 14.80 -7 -5 15 -10.30 21.90 7 5 -15 -1.20 14.20 -6 -5 15 196.38 30.10 6 5 -15 189.08 22.40 -5 -5 15 0.40 24.10 5 5 -15 0.60 13.40 -4 -5 15 40.20 28.80 4 5 -15 18.20 15.90 3 5 -15 -6.00 12.70 2 5 -15 63.59 15.50 1 5 -15 -6.70 12.80 0 -5 15 3.80 19.40 0 5 -15 25.10 14.30 1 -5 15 102.59 23.70 -1 5 -15 41.00 14.10 2 -5 15 114.89 22.50 -2 5 -15 126.49 17.40 3 -5 15 14.40 16.80 4 -5 15 40.90 18.10 5 -5 15 -21.70 14.80 4 6 -15 3.80 14.50 3 6 -15 28.20 16.20 -2 -6 15 -1.30 20.20 2 6 -15 10.90 14.70 -1 -6 15 6.30 20.90 1 6 -15 1.10 13.80 0 6 -15 2.50 13.40 1 -6 15 -10.10 19.50 -1 6 -15 13.90 14.20 2 -6 15 36.10 20.90 4 0 16 531.75 43.10 -4 0 -16 482.55 23.70 -4 0 -16 473.95 23.00 -4 0 -16 455.75 26.10 4 0 16 409.76 22.90 4 0 16 423.26 23.00 -4 0 -16 494.75 28.40 4 0 16 427.16 23.20 -4 0 -16 497.85 28.10 5 0 16 0.50 5.70 5 0 16 -16.10 14.90 5 0 16 8.30 5.40 -5 0 -16 7.40 8.30 5 0 16 9.40 5.30 -5 0 -16 12.80 5.60 -5 0 -16 11.70 6.40 -5 0 -16 11.10 8.40 -6 0 -16 61.39 7.50 6 0 16 74.19 8.40 7 0 16 150.58 11.40 -7 0 -16 142.29 11.20 8 0 16 154.38 12.20 9 0 16 30.80 8.40 10 0 16 4.40 8.40 10 0 16 5.80 8.00 11 0 16 15.90 8.90 11 0 16 1.90 9.00 1 -1 16 164.98 9.40 1 -1 16 148.19 19.50 1 -1 16 164.38 9.80 1 -1 16 160.68 9.60 -1 1 -16 157.08 9.50 -1 1 -16 129.79 13.90 2 -1 16 2.60 4.10 2 -1 16 5.50 3.80 -2 1 -16 1.90 3.80 -2 1 -16 -14.10 14.60 3 -1 16 43.60 12.60 3 -1 16 46.10 20.50 3 -1 16 29.00 5.20 3 -1 16 24.50 4.70 -3 1 -16 33.50 10.50 -3 1 -16 27.60 5.20 -3 1 -16 29.60 8.60 4 -1 16 130.69 9.80 4 -1 16 104.59 20.40 4 -1 16 150.98 10.40 -4 1 -16 115.59 13.50 -4 1 -16 145.29 15.00 5 -1 16 101.59 8.00 5 -1 16 110.29 8.50 -5 1 -16 119.79 13.10 -5 1 -16 97.49 12.10 6 -1 16 4.30 5.90 6 -1 16 12.20 5.40 -7 -1 -16 -12.80 7.10 7 -1 16 10.30 6.40 -7 -1 -16 3.80 6.80 7 1 16 1.70 6.20 7 1 16 3.20 7.00 -8 -1 -16 9.60 7.50 8 -1 16 10.60 7.10 8 1 16 5.00 7.70 9 -1 16 10.20 7.60 -9 -1 -16 3.60 7.60 9 -1 16 8.70 7.00 9 1 16 8.90 8.00 10 -1 16 16.80 8.30 10 1 16 25.20 9.30 11 -1 16 130.79 12.40 11 1 16 135.69 13.40 -2 -2 16 309.17 27.70 2 2 -16 282.77 21.40 -1 -2 16 30.40 16.40 1 2 -16 57.99 12.00 0 -2 16 124.79 19.40 0 -2 16 209.98 30.70 0 2 -16 136.49 16.70 0 2 -16 140.39 14.60 1 -2 16 26.20 14.20 1 -2 16 23.10 21.90 -1 2 -16 5.50 10.60 -1 2 -16 -1.40 8.50 2 -2 16 544.85 46.70 -2 2 -16 519.75 33.10 3 -2 16 48.40 19.30 -3 2 -16 48.00 11.90 -5 2 -16 173.78 16.40 -6 2 -16 93.29 12.30 -6 2 -16 73.09 11.60 -4 -3 16 19.90 18.10 4 3 -16 10.10 11.50 -3 -3 16 7.30 16.10 -3 -3 16 2.30 25.80 3 3 -16 21.70 11.30 3 3 -16 0.00 12.30 -2 -3 16 16.10 15.90 -2 -3 16 0.90 24.30 2 3 -16 2.00 12.20 2 3 -16 20.70 10.40 -1 -3 16 247.48 24.40 -1 -3 16 260.77 32.30 1 3 -16 267.67 19.90 1 3 -16 245.28 22.20 0 -3 16 -18.50 21.80 0 3 -16 -2.00 11.80 1 -3 16 9.00 21.10 -1 3 -16 9.60 11.30 -2 3 -16 24.00 11.50 -3 3 -16 4.80 11.60 -4 3 -16 92.49 14.30 -5 3 -16 559.64 33.50 -6 -4 16 104.89 21.90 -6 -4 16 73.49 27.80 6 4 -16 90.59 14.80 6 4 -16 82.49 17.30 -5 -4 16 13.30 24.80 -5 -4 16 -0.90 15.90 5 4 -16 -10.10 11.20 5 4 -16 3.10 15.00 -4 -4 16 28.10 18.00 -4 -4 16 32.70 24.00 4 4 -16 -1.20 11.40 4 4 -16 2.30 13.80 -3 -4 16 26.80 24.20 3 4 -16 7.30 13.10 -2 -4 16 38.90 23.70 2 4 -16 57.09 15.10 -1 -4 16 17.90 22.20 1 4 -16 35.20 13.80 0 4 -16 471.55 33.20 -1 4 -16 21.70 13.70 -2 4 -16 210.28 21.50 -3 4 -16 14.40 13.40 -4 4 -16 15.60 11.90 -5 -5 16 28.00 27.40 5 5 -16 25.90 15.60 -4 -5 16 -18.80 23.70 4 5 -16 -5.90 14.30 3 5 -16 12.60 14.10 2 5 -16 18.50 16.70 1 5 -16 -0.10 14.60 0 5 -16 14.60 14.10 -1 5 -16 146.49 19.30 2 -5 16 9.20 19.00 -2 5 -16 16.10 13.60 3 -5 16 58.59 20.50 -3 5 -16 91.09 15.40 4 -5 16 -3.70 17.10 5 -5 16 139.09 21.90 2 6 -16 97.69 22.20 1 6 -16 44.50 16.40 0 -6 16 59.39 23.30 0 6 -16 46.40 16.00 1 -6 16 0.70 22.10 -1 6 -16 18.40 14.80 2 -6 16 -16.40 17.60 -6 0 -17 12.00 6.30 7 0 17 -10.00 7.90 8 0 17 0.10 7.40 9 0 17 2.70 8.20 10 0 17 15.10 8.90 2 -1 17 20.80 14.20 2 -1 17 -7.20 26.20 -2 1 -17 13.10 10.80 -2 1 -17 18.90 9.20 3 -1 17 -7.60 12.00 3 -1 17 -27.40 19.90 -3 1 -17 7.30 8.40 -3 1 -17 2.50 9.40 4 -1 17 63.29 19.70 -4 1 -17 48.30 11.30 -5 1 -17 5.70 10.50 -5 1 -17 11.60 9.40 10 1 17 1.60 8.70 -1 -2 17 202.18 23.80 1 2 -17 212.28 18.50 0 -2 17 26.00 26.60 0 -2 17 10.00 15.20 0 2 -17 9.50 10.20 0 2 -17 16.30 12.40 1 -2 17 26.30 14.00 1 -2 17 25.60 22.60 -1 2 -17 28.00 11.90 -1 2 -17 36.90 10.20 2 -2 17 -3.40 21.10 -2 2 -17 8.90 11.20 3 -2 17 91.29 22.50 -3 2 -17 92.79 15.70 -4 2 -17 4.50 10.80 -5 2 -17 125.49 16.60 -3 -3 17 59.19 29.10 -3 -3 17 -2.90 17.10 3 3 -17 14.40 13.70 3 3 -17 20.20 12.00 -2 -3 17 117.49 20.90 -2 -3 17 128.89 29.30 2 3 -17 112.49 14.60 2 3 -17 92.19 17.00 -1 -3 17 52.99 18.20 -1 -3 17 46.10 25.20 1 3 -17 46.40 14.40 1 3 -17 62.39 13.00 0 -3 17 15.40 23.70 0 3 -17 -5.50 12.50 1 -3 17 -9.50 20.90 -1 3 -17 2.40 12.10 -2 3 -17 371.46 29.40 -3 3 -17 -6.10 12.10 -4 3 -17 124.19 16.30 -5 3 -17 16.60 11.50 -5 -4 17 3.30 17.60 -5 -4 17 -9.10 23.50 5 4 -17 12.90 14.20 5 4 -17 -5.20 11.40 -4 -4 17 3.80 24.50 4 4 -17 18.50 14.80 -3 -4 17 49.50 42.30 3 4 -17 24.30 25.30 -2 -4 17 16.10 24.00 2 4 -17 11.80 13.80 -1 -4 17 30.20 24.80 1 4 -17 68.89 15.70 0 4 -17 6.80 13.40 -1 4 -17 9.70 14.30 -2 4 -17 12.20 15.40 -3 4 -17 134.99 18.60 -4 4 -17 89.59 15.60 4 5 -17 34.40 19.90 3 5 -17 -2.50 14.60 2 5 -17 14.50 14.70 1 5 -17 6.70 14.10 0 5 -17 15.20 14.40 -2 5 -17 109.39 19.90 -3 5 -17 7.40 12.70 0 -2 18 27.70 27.20 0 -2 18 23.60 16.80 0 2 -18 18.70 11.00 0 2 -18 17.40 13.30 1 -2 18 13.10 15.30 1 -2 18 19.20 25.10 -1 2 -18 -1.90 12.10 -1 2 -18 -3.40 10.30 2 -2 18 42.70 24.40 -2 2 -18 19.50 12.70 3 -2 18 30.00 21.00 -3 2 -18 73.39 14.00 -4 2 -18 211.98 19.10 -5 2 -18 30.40 13.30 -2 -3 18 30.30 26.50 -2 -3 18 5.50 16.50 2 3 -18 -4.20 13.20 2 3 -18 -8.00 10.30 -1 -3 18 95.89 29.50 1 3 -18 109.19 17.40 0 -3 18 -8.80 24.50 0 3 -18 2.90 13.50 1 -3 18 44.10 24.00 -1 3 -18 18.40 13.60 -2 3 -18 12.10 12.40 -3 3 -18 245.38 21.60 -4 3 -18 18.40 12.40 -5 3 -18 10.60 11.40 -4 -4 18 14.80 27.10 4 4 -18 7.00 14.70 -3 -4 18 3.60 24.90 3 4 -18 10.60 15.30 -2 -4 18 12.10 27.70 2 4 -18 28.60 14.90 -1 -4 18 9.80 24.10 1 4 -18 37.20 16.50 0 4 -18 38.70 16.00 -1 4 -18 40.90 15.50 -3 4 -18 0.80 13.70 -4 4 -18 6.40 13.00 1 5 -18 10.90 15.70 0 5 -18 26.90 16.70 -1 5 -18 19.40 15.70 -2 5 -18 6.20 14.50 2 -2 19 -19.30 21.80 -2 2 -19 20.50 12.70 -3 2 -19 5.30 11.90 0 -3 19 178.88 31.30 0 3 -19 152.98 19.80 1 -3 19 19.40 23.30 -1 3 -19 2.40 13.30 -2 3 -19 46.50 15.20 -3 3 -19 -13.60 12.80 -4 3 -19 180.28 19.60 -2 -4 19 -0.80 28.70 2 4 -19 10.80 15.30 -1 -4 19 37.90 23.90 1 4 -19 25.80 15.90 0 4 -19 7.90 15.10 -1 4 -19 106.69 18.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 55392 _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 0.68330(17) 0.5961(4) 0.65058(16) 0.0438(8) Uani 1 1 d . . . . . O002 O 0.52259(16) 0.4964(4) 0.81225(14) 0.0422(8) Uani 1 1 d . . . . . O003 O 0.66165(15) 0.4209(3) 0.83384(14) 0.0410(8) Uani 1 1 d . . . . . O004 O 0.83179(18) 0.5986(4) 0.35438(17) 0.0504(9) Uani 1 1 d . . . . . N005 N 0.7607(2) 0.9369(5) 0.4645(2) 0.0249(8) Uani 1 1 d . . . . . O006 O 0.92534(18) 0.1078(5) 0.51046(17) 0.0535(9) Uani 1 1 d . . . . . O007 O 0.56332(18) 0.1273(4) 0.48087(16) 0.0481(9) Uani 1 1 d . . . . . N008 N 0.72716(18) 0.9416(4) 0.53643(19) 0.0253(8) Uani 1 1 d . . . . . O009 O 0.83648(15) 0.4100(4) 0.15811(14) 0.0509(9) Uani 1 1 d . . . . . O00A O 1.03317(16) 0.2855(4) 0.49459(14) 0.0521(9) Uani 1 1 d . . . . . O00B O 0.98032(16) 0.4590(4) 0.17610(15) 0.0480(9) Uani 1 1 d . . . . . O00C O 1.12223(16) 0.2969(4) 0.34059(16) 0.0575(10) Uani 1 1 d . . . . . O00D O 0.45691(16) 0.3078(4) 0.49889(14) 0.0507(9) Uani 1 1 d . . . . . N00E N 0.6397(2) 0.2032(5) 0.62523(18) 0.0259(8) Uani 1 1 d . . . . . N00F N 0.84370(17) 0.2081(4) 0.37514(16) 0.0269(8) Uani 1 1 d . . . . . N00G N 0.8147(2) 0.7428(5) 0.3673(2) 0.0317(9) Uani 1 1 d . . . . . O00H O 0.69085(17) 0.4186(4) 0.48385(17) 0.0521(9) Uani 1 1 d . . . . . N00I N 0.6871(2) 0.7427(5) 0.6347(2) 0.0314(9) Uani 1 1 d . . . . . O00J O 0.4429(2) 0.5962(5) 0.65576(18) 0.0637(11) Uani 1 1 d . . . . . N00K N 0.65993(18) 0.2516(4) 0.69890(16) 0.0268(8) Uani 1 1 d . . . . . O00L O 0.82900(18) 0.4344(4) 0.52700(17) 0.0579(9) Uani 1 1 d . . . . . N00M N 0.90774(18) 0.4062(4) 0.19649(16) 0.0299(8) Uani 1 1 d . . . . . N00N N 0.83113(18) 0.2613(4) 0.30072(16) 0.0250(8) Uani 1 1 d . . . . . N00O N 1.0611(2) 0.3991(5) 0.33338(18) 0.0363(10) Uani 1 1 d . . . . . N00P N 0.4389(2) 0.4461(5) 0.65711(18) 0.0364(10) Uani 1 1 d . . . . . N00Q N 0.59164(17) 0.4259(4) 0.79402(16) 0.0258(8) Uani 1 1 d . . . . . O00R O 0.8264(2) 0.8593(4) 0.32262(17) 0.0567(9) Uani 1 1 d . . . . . N00S N 0.9647(2) 0.2110(5) 0.47304(18) 0.0343(9) Uani 1 1 d . . . . . O00T O 1.0706(2) 0.5464(5) 0.32625(18) 0.0644(13) Uani 1 1 d . . . . . O00U O 0.6650(2) 0.8558(5) 0.67718(18) 0.0609(10) Uani 1 1 d . . . . . N00V N 0.75798(18) 0.4958(5) 0.50430(15) 0.0323(9) Uani 1 1 d . . . . . O00W O 0.37150(17) 0.3607(4) 0.65604(17) 0.0624(10) Uani 1 1 d . . . . . N00X N 0.5246(2) 0.2292(5) 0.51965(18) 0.0329(9) Uani 1 1 d . . . . . C00Y C 0.5601(2) 0.2636(5) 0.5986(2) 0.0243(9) Uani 1 1 d . . . . . C00Z C 0.7531(2) 0.6754(5) 0.5019(2) 0.0208(9) Uani 1 1 d . . . . . C010 C 0.59040(19) 0.3449(5) 0.71839(19) 0.0213(9) Uani 1 1 d . . . . . C011 C 0.7778(2) 0.7807(5) 0.4421(2) 0.0227(10) Uani 1 1 d . . . . . C012 C 0.9277(2) 0.2513(4) 0.39459(19) 0.0224(9) Uani 1 1 d . . . . . C013 C 0.9054(2) 0.3369(5) 0.27396(18) 0.0223(9) Uani 1 1 d . . . . . C014 C 0.5248(2) 0.3572(5) 0.65750(19) 0.0239(9) Uani 1 1 d . . . . . C015 C 0.9702(2) 0.3324(5) 0.33408(19) 0.0261(9) Uani 1 1 d . . . . . C016 C 0.7216(2) 0.7857(5) 0.5590(2) 0.0225(9) Uani 1 1 d . . . . . H00E H 0.675(2) 0.131(5) 0.598(2) 0.022(9) Uiso 1 1 d . . . . . H00N H 0.773(3) 0.263(5) 0.272(2) 0.074(13) Uiso 1 1 d . . . . . H005 H 0.779(3) 1.031(7) 0.432(3) 0.087(17) 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 0.057(2) 0.029(3) 0.046(2) 0.0122(15) 0.0071(15) -0.0115(13) O002 0.0421(18) 0.050(3) 0.0341(17) -0.0098(13) 0.0036(14) 0.0194(13) O003 0.0339(16) 0.056(3) 0.0329(16) -0.0100(13) -0.0090(13) 0.0006(11) O004 0.063(2) 0.035(3) 0.054(2) -0.0100(17) 0.0132(16) 0.0157(14) N005 0.0280(19) 0.026(3) 0.021(2) -0.0001(17) 0.0041(16) 0.0004(12) O006 0.046(2) 0.072(3) 0.0419(19) 0.0340(17) 0.0020(16) -0.0068(14) O007 0.050(2) 0.057(3) 0.0377(19) -0.0257(16) 0.0010(16) 0.0047(13) N008 0.0266(19) 0.027(3) 0.022(2) -0.0008(16) 0.0002(16) 0.0004(11) O009 0.0336(17) 0.082(3) 0.0362(18) 0.0221(15) -0.0098(14) -0.0051(12) O00A 0.0373(18) 0.078(3) 0.0395(19) 0.0127(15) -0.0130(15) -0.0132(13) O00B 0.0328(18) 0.075(3) 0.0360(18) 0.0124(15) 0.0042(14) -0.0161(13) O00C 0.0220(18) 0.094(4) 0.057(2) 0.0095(17) 0.0006(15) 0.0070(13) O00D 0.0359(17) 0.081(3) 0.0344(18) -0.0112(15) -0.0085(14) 0.0142(13) N00E 0.027(2) 0.024(3) 0.026(2) -0.0052(14) 0.0047(16) 0.0057(12) N00F 0.0302(19) 0.023(3) 0.0276(19) 0.0048(14) -0.0023(15) -0.0017(11) N00G 0.035(2) 0.030(4) 0.030(2) 0.0003(19) 0.0039(18) 0.0029(14) O00H 0.054(2) 0.036(3) 0.066(2) -0.0047(15) -0.0020(16) -0.0177(13) N00I 0.034(2) 0.033(4) 0.028(2) 0.002(2) 0.0051(18) -0.0033(14) O00J 0.087(3) 0.048(3) 0.055(2) -0.011(2) -0.015(2) 0.0390(18) N00K 0.0286(19) 0.031(3) 0.0208(19) -0.0007(14) 0.0026(15) 0.0046(12) O00L 0.067(2) 0.036(3) 0.069(2) -0.0004(16) -0.0200(18) 0.0192(14) N00M 0.029(2) 0.036(3) 0.0244(19) 0.0045(14) -0.0010(16) -0.0013(12) N00N 0.0243(18) 0.027(3) 0.0235(19) -0.0016(14) -0.0011(15) -0.0017(11) N00O 0.025(2) 0.059(4) 0.025(2) 0.0093(18) 0.0031(16) -0.0110(16) N00P 0.037(2) 0.053(4) 0.020(2) -0.0021(18) -0.0019(17) 0.0150(17) N00Q 0.0275(19) 0.025(3) 0.0246(19) 0.0007(14) 0.0017(15) 0.0026(12) O00R 0.091(3) 0.041(3) 0.041(2) 0.0056(16) 0.0336(18) 0.0030(16) N00S 0.027(2) 0.048(3) 0.028(2) 0.0122(17) 0.0019(16) 0.0012(14) O00T 0.070(2) 0.060(4) 0.061(2) 0.026(2) -0.0231(18) -0.0395(19) O00U 0.097(3) 0.046(3) 0.042(2) -0.0011(17) 0.0340(19) 0.0083(17) N00V 0.042(2) 0.031(3) 0.024(2) 0.0023(16) 0.0037(17) 0.0014(14) O00W 0.0248(19) 0.110(4) 0.052(2) 0.0043(18) 0.0001(15) -0.0053(15) N00X 0.030(2) 0.041(3) 0.028(2) -0.0058(16) -0.0022(17) -0.0046(13) C00Y 0.025(2) 0.023(4) 0.025(2) -0.0020(17) -0.0018(19) -0.0022(13) C00Z 0.021(2) 0.016(4) 0.026(2) 0.002(2) 0.000(2) 0.0017(12) C010 0.024(2) 0.020(3) 0.020(2) 0.0003(16) 0.0028(17) -0.0031(13) C011 0.020(2) 0.026(4) 0.021(2) -0.0019(19) 0.0003(19) 0.0026(14) C012 0.025(2) 0.019(3) 0.024(2) 0.0025(17) 0.0004(18) 0.0024(13) C013 0.024(2) 0.025(3) 0.018(2) 0.0015(17) 0.0046(17) 0.0024(13) C014 0.017(2) 0.028(3) 0.027(2) -0.0016(18) 0.0019(18) -0.0005(13) C015 0.016(2) 0.038(4) 0.025(2) 0.0027(18) 0.0048(18) 0.0017(13) C016 0.020(2) 0.023(4) 0.024(2) 0.0024(19) -0.0002(19) -0.0011(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N008 N005 C011 111.4(3) . . ? N008 N005 H005 128(4) . . ? C011 N005 H005 120(4) . . ? C016 N008 N005 105.5(3) . . ? N00K N00E C00Y 112.0(3) . . ? N00K N00E H00E 122.7(18) . . ? C00Y N00E H00E 125.1(18) . . ? C012 N00F N00N 104.3(3) . . ? O004 N00G O00R 126.2(4) . . ? O004 N00G C011 117.0(4) . . ? O00R N00G C011 116.8(4) . . ? O001 N00I C016 116.9(4) . . ? O00U N00I O001 125.8(4) . . ? O00U N00I C016 117.3(5) . . ? C010 N00K N00E 104.4(2) . . ? O009 N00M C013 116.7(3) . . ? O00B N00M O009 126.7(3) . . ? O00B N00M C013 116.6(2) . . ? N00F N00N C013 111.9(3) . . ? N00F N00N H00N 124(2) . . ? C013 N00N H00N 123(2) . . ? O00C N00O C015 115.6(4) . . ? O00T N00O O00C 125.7(4) . . ? O00T N00O C015 118.6(3) . . ? O00J N00P O00W 127.4(4) . . ? O00J N00P C014 116.5(3) . . ? O00W N00P C014 116.1(4) . . ? O002 N00Q C010 116.9(2) . . ? O003 N00Q O002 125.6(3) . . ? O003 N00Q C010 117.5(3) . . ? O006 N00S O00A 126.4(3) . . ? O006 N00S C012 117.3(3) . . ? O00A N00S C012 116.4(3) . . ? O00H N00V C00Z 117.6(3) . . ? O00L N00V O00H 125.1(4) . . ? O00L N00V C00Z 117.3(3) . . ? O007 N00X O00D 126.5(3) . . ? O007 N00X C00Y 117.9(3) . . ? O00D N00X C00Y 115.6(3) . . ? N00E C00Y N00X 121.9(3) . . ? N00E C00Y C014 108.1(3) . . ? C014 C00Y N00X 130.0(3) . . ? C011 C00Z N00V 128.3(4) . . ? C011 C00Z C016 102.6(4) . . ? C016 C00Z N00V 129.1(4) . . ? N00K C010 N00Q 119.6(2) . . ? N00K C010 C014 112.6(3) . . ? C014 C010 N00Q 127.7(3) . . ? N005 C011 N00G 122.2(4) . . ? N005 C011 C00Z 108.2(4) . . ? C00Z C011 N00G 129.6(4) . . ? N00F C012 N00S 119.3(3) . . ? N00F C012 C015 112.9(3) . . ? C015 C012 N00S 127.8(3) . . ? N00N C013 N00M 122.1(3) . . ? N00N C013 C015 107.2(3) . . ? C015 C013 N00M 130.7(3) . . ? C00Y C014 N00P 128.6(3) . . ? C00Y C014 C010 102.9(3) . . ? C010 C014 N00P 128.5(3) . . ? C012 C015 N00O 128.9(3) . . ? C013 C015 N00O 127.5(3) . . ? C013 C015 C012 103.6(3) . . ? N008 C016 N00I 121.0(4) . . ? N008 C016 C00Z 112.3(4) . . ? C00Z C016 N00I 126.7(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 N00I 1.210(4) . ? O002 N00Q 1.217(3) . ? O003 N00Q 1.214(3) . ? O004 N00G 1.207(4) . ? N005 N008 1.328(5) . ? N005 C011 1.338(5) . ? N005 H005 0.99(5) . ? O006 N00S 1.205(4) . ? O007 N00X 1.206(4) . ? N008 C016 1.313(5) . ? O009 N00M 1.217(3) . ? O00A N00S 1.220(3) . ? O00B N00M 1.215(4) . ? O00C N00O 1.224(4) . ? O00D N00X 1.223(4) . ? N00E N00K 1.326(4) . ? N00E C00Y 1.336(4) . ? N00E H00E 0.91(3) . ? N00F N00N 1.333(4) . ? N00F C012 1.319(4) . ? N00G O00R 1.219(5) . ? N00G C011 1.426(5) . ? O00H N00V 1.210(4) . ? N00I O00U 1.209(5) . ? N00I C016 1.434(5) . ? O00J N00P 1.208(4) . ? N00K C010 1.323(4) . ? O00L N00V 1.210(3) . ? N00M C013 1.422(4) . ? N00N C013 1.348(4) . ? N00N H00N 0.97(4) . ? N00O O00T 1.198(4) . ? N00O C015 1.448(4) . ? N00P O00W 1.210(4) . ? N00P C014 1.456(4) . ? N00Q C010 1.432(4) . ? N00S C012 1.450(4) . ? N00V C00Z 1.446(5) . ? N00X C00Y 1.440(4) . ? C00Y C014 1.365(5) . ? C00Z C011 1.376(6) . ? C00Z C016 1.401(5) . ? C010 C014 1.391(4) . ? C012 C015 1.381(5) . ? C013 C015 1.369(4) . ? 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 N00I C016 N008 179.3(3) . . . . ? O001 N00I C016 C00Z -1.3(4) . . . . ? O002 N00Q C010 N00K -172.9(4) . . . . ? O002 N00Q C010 C014 10.6(6) . . . . ? O003 N00Q C010 N00K 8.3(5) . . . . ? O003 N00Q C010 C014 -168.2(4) . . . . ? O004 N00G C011 N005 176.5(3) . . . . ? O004 N00G C011 C00Z -4.2(5) . . . . ? N005 N008 C016 N00I -179.6(3) . . . . ? N005 N008 C016 C00Z 0.9(3) . . . . ? O006 N00S C012 N00F 16.6(6) . . . . ? O006 N00S C012 C015 -163.2(5) . . . . ? O007 N00X C00Y N00E 8.9(7) . . . . ? O007 N00X C00Y C014 -171.9(5) . . . . ? N008 N005 C011 N00G -179.6(3) . . . . ? N008 N005 C011 C00Z 0.9(3) . . . . ? O009 N00M C013 N00N 7.6(5) . . . . ? O009 N00M C013 C015 -171.5(4) . . . . ? O00A N00S C012 N00F -163.5(4) . . . . ? O00A N00S C012 C015 16.6(6) . . . . ? O00B N00M C013 N00N -174.0(4) . . . . ? O00B N00M C013 C015 6.9(6) . . . . ? O00C N00O C015 C012 63.9(5) . . . . ? O00C N00O C015 C013 -116.7(4) . . . . ? O00D N00X C00Y N00E -171.3(4) . . . . ? O00D N00X C00Y C014 8.0(7) . . . . ? N00E N00K C010 N00Q -176.9(3) . . . . ? N00E N00K C010 C014 0.1(5) . . . . ? N00E C00Y C014 N00P -179.0(4) . . . . ? N00E C00Y C014 C010 0.2(5) . . . . ? N00F N00N C013 N00M -179.0(3) . . . . ? N00F N00N C013 C015 0.2(4) . . . . ? N00F C012 C015 N00O 179.4(4) . . . . ? N00F C012 C015 C013 0.0(5) . . . . ? O00H N00V C00Z C011 -94.6(4) . . . . ? O00H N00V C00Z C016 84.9(4) . . . . ? O00J N00P C014 C00Y -109.9(5) . . . . ? O00J N00P C014 C010 71.1(5) . . . . ? N00K N00E C00Y N00X 179.2(4) . . . . ? N00K N00E C00Y C014 -0.2(5) . . . . ? N00K C010 C014 N00P 179.0(4) . . . . ? N00K C010 C014 C00Y -0.2(5) . . . . ? O00L N00V C00Z C011 85.7(4) . . . . ? O00L N00V C00Z C016 -94.8(4) . . . . ? N00M C013 C015 N00O -0.4(7) . . . . ? N00M C013 C015 C012 179.1(4) . . . . ? N00N N00F C012 N00S -179.7(3) . . . . ? N00N N00F C012 C015 0.2(4) . . . . ? N00N C013 C015 N00O -179.6(4) . . . . ? N00N C013 C015 C012 -0.1(4) . . . . ? N00Q C010 C014 N00P -4.3(7) . . . . ? N00Q C010 C014 C00Y 176.5(4) . . . . ? O00R N00G C011 N005 -3.2(4) . . . . ? O00R N00G C011 C00Z 176.1(3) . . . . ? N00S C012 C015 N00O -0.7(7) . . . . ? N00S C012 C015 C013 179.8(4) . . . . ? O00T N00O C015 C012 -115.8(5) . . . . ? O00T N00O C015 C013 63.5(5) . . . . ? O00U N00I C016 N008 -1.3(4) . . . . ? O00U N00I C016 C00Z 178.2(3) . . . . ? N00V C00Z C011 N005 179.3(3) . . . . ? N00V C00Z C011 N00G -0.1(5) . . . . ? N00V C00Z C016 N008 -179.9(3) . . . . ? N00V C00Z C016 N00I 0.6(5) . . . . ? O00W N00P C014 C00Y 68.2(6) . . . . ? O00W N00P C014 C010 -110.8(4) . . . . ? N00X C00Y C014 N00P 1.7(8) . . . . ? N00X C00Y C014 C010 -179.1(4) . . . . ? C00Y N00E N00K C010 0.1(5) . . . . ? C011 N005 N008 C016 -1.1(3) . . . . ? C011 C00Z C016 N008 -0.4(3) . . . . ? C011 C00Z C016 N00I -179.9(3) . . . . ? C012 N00F N00N C013 -0.2(4) . . . . ? C016 C00Z C011 N005 -0.3(3) . . . . ? C016 C00Z C011 N00G -179.7(3) . . . . ?