#------------------------------------------------------------------------------ #$Date: 2024-04-19 06:02:53 +0300 (Fri, 19 Apr 2024) $ #$Revision: 291285 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/99/7159908.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_7159908 loop_ _publ_author_name 'Neto, Brenno A. D.' 'Beck, Pedro' 'Leit\~ao, Arthur' 'Santana, Yasmin' 'Correa, Jose R.' 'Rodrigues, Carime Vit\'oria da Silva' 'Machado, Daniel' 'Matos, Guilherme' 'Machado Ramos, Luciana' 'Gatto, Claudia Cristina' 'Z. Andrade, Carlos Kleber' 'Caldas, Sarah' _publ_section_title ; Revisiting Biginelli-like Reactions: Solvent Effects, Mechanisms, Biological Applications and Correction of Several Literature Reports ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D4OB00272E _journal_year 2024 _chemical_formula_sum 'C25 H16 O6' _chemical_formula_weight 412.38 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-01-02 deposited with the CCDC. 2024-04-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.965(3) _cell_length_b 12.839(4) _cell_length_c 18.595(6) _cell_measurement_reflns_used 2646 _cell_measurement_temperature 273.(2) _cell_measurement_theta_max 19.2426 _cell_measurement_theta_min 2.1905 _cell_volume 1901.6(11) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_collection 'Bruker Instrument Service v2018.1.0.3' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.1935 _diffrn_reflns_av_unetI/netI 0.0939 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 30028 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 24.990 _diffrn_reflns_theta_max 24.990 _diffrn_reflns_theta_min 1.928 _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.440 _exptl_crystal_description prism _exptl_crystal_F_000 856 _exptl_crystal_size_max 0.468 _exptl_crystal_size_mid 0.390 _exptl_crystal_size_min 0.125 _refine_diff_density_max 0.180 _refine_diff_density_min -0.191 _refine_diff_density_rms 0.054 _refine_ls_abs_structure_details ; Refined as a perfect inversion twin. ; _refine_ls_abs_structure_Flack 0.5 _refine_ls_extinction_coef 0.0136(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 283 _refine_ls_number_reflns 3349 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.884 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0441 _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^)+(0.0315P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0894 _refine_ls_wR_factor_ref 0.1036 _reflns_Friedel_coverage 0.733 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 2018 _reflns_number_total 3349 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ob00272e2.cif _cod_data_source_block shelx _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_original_cell_volume 1901.6(10) _cod_database_code 7159908 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.953 _shelx_estimated_absorpt_t_max 0.987 _shelx_res_file ; TITL P212121_a.res in P2(1)2(1)2(1) shelx.res created by SHELXL-2018/3 at 17:03:18 on 02-Aug-2022 CELL 0.71073 7.9654 12.8387 18.5948 90 90 90 ZERR 4 0.0025 0.004 0.0059 0 0 0 LATT -1 SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5-X,-Y,0.5+Z SFAC C H O UNIT 100 64 24 L.S. 15 PLAN 5 SIZE 0.125 0.39 0.468 TEMP 0 HTAB O5 O4 HTAB O2 O6 CONF BOND $H HTAB fmap 2 acta MORE -1 TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT -4 50 WGHT 0.031500 EXTI 0.013615 FVAR 0.45876 O1 3 0.162745 0.562585 0.680557 11.00000 0.05375 0.05236 = 0.03540 -0.00302 0.00718 -0.00452 O2 3 0.244136 0.357589 0.482035 11.00000 0.06098 0.03656 = 0.04768 0.00487 -0.00465 -0.00308 AFIX 147 H2 2 0.272462 0.383345 0.520521 11.00000 -1.50000 AFIX 0 O3 3 0.091097 0.579263 0.337514 11.00000 0.06462 0.05158 = 0.03906 0.00380 -0.01504 0.00114 O4 3 0.211626 0.704368 0.399261 11.00000 0.07919 0.03910 = 0.04628 0.00729 -0.01437 0.00302 O5 3 0.269777 0.787765 0.531472 11.00000 0.10301 0.03702 = 0.04565 0.00647 0.00043 0.01341 AFIX 147 H5 2 0.265460 0.764422 0.490466 11.00000 -1.50000 AFIX 0 O6 3 0.259100 0.438973 0.611341 11.00000 0.06333 0.03504 = 0.04373 0.00631 0.00545 0.00147 C1 1 0.011713 0.790848 0.774327 11.00000 0.06335 0.09467 = 0.06376 -0.03406 0.00640 0.00567 AFIX 43 H1 2 -0.043427 0.807510 0.816884 11.00000 -1.20000 AFIX 0 C2 1 0.050248 0.687858 0.759329 11.00000 0.05593 0.07504 = 0.04369 -0.01359 0.00282 -0.00198 AFIX 43 H2A 2 0.024081 0.635013 0.791648 11.00000 -1.20000 AFIX 0 C3 1 0.129426 0.666090 0.694286 11.00000 0.04044 0.05021 = 0.04181 -0.01103 -0.00031 0.00282 C4 1 0.239620 0.532364 0.617955 11.00000 0.03814 0.04177 = 0.03294 -0.00031 0.00030 0.00058 C5 1 0.285701 0.609890 0.566585 11.00000 0.03921 0.03296 = 0.02977 0.00016 -0.00340 0.00647 C6 1 0.376833 0.575481 0.498747 11.00000 0.04559 0.02991 = 0.03183 0.00243 -0.00058 0.00291 AFIX 13 H6 2 0.420144 0.640244 0.477915 11.00000 -1.20000 AFIX 0 C7 1 0.257407 0.533127 0.442025 11.00000 0.03910 0.03259 = 0.03162 -0.00054 0.00244 0.00194 C8 1 0.206391 0.433274 0.435574 11.00000 0.04075 0.03972 = 0.03640 0.00057 0.00578 0.00571 C9 1 0.108107 0.400497 0.374616 11.00000 0.03768 0.04659 = 0.03521 -0.00403 0.00433 -0.00154 C10 1 0.054025 0.475740 0.327403 11.00000 0.04723 0.04930 = 0.03758 -0.00364 0.00036 -0.00439 C11 1 -0.042785 0.451637 0.267589 11.00000 0.06393 0.06903 = 0.04049 -0.00264 -0.01073 -0.01017 AFIX 43 H11 2 -0.078314 0.503279 0.235991 11.00000 -1.20000 AFIX 0 C12 1 -0.084321 0.349199 0.256615 11.00000 0.06377 0.08934 = 0.04127 -0.01436 -0.00843 -0.01888 AFIX 43 H12 2 -0.149142 0.331439 0.216865 11.00000 -1.20000 AFIX 0 C13 1 0.054138 0.868446 0.726990 11.00000 0.08347 0.06486 = 0.06910 -0.02793 -0.01411 0.02501 AFIX 43 H13 2 0.029922 0.937396 0.738280 11.00000 -1.20000 AFIX 0 C14 1 0.132349 0.845174 0.662827 11.00000 0.08322 0.05263 = 0.05353 -0.01195 -0.01027 0.02244 AFIX 43 H14 2 0.160018 0.898241 0.630914 11.00000 -1.20000 AFIX 0 C15 1 0.169739 0.742495 0.645914 11.00000 0.04800 0.04708 = 0.03824 -0.00501 -0.00983 0.01048 C16 1 0.534396 0.509867 0.513779 11.00000 0.03916 0.03345 = 0.03551 0.00609 0.00122 0.00086 C17 1 0.594889 0.436697 0.465873 11.00000 0.04472 0.04863 = 0.04724 0.00408 0.00385 0.00178 AFIX 43 H17 2 0.533638 0.421814 0.424553 11.00000 -1.20000 AFIX 0 C18 1 0.744197 0.385255 0.478032 11.00000 0.05432 0.05262 = 0.07005 0.00852 0.01956 0.00931 AFIX 43 H18 2 0.783108 0.336305 0.445149 11.00000 -1.20000 AFIX 0 C19 1 0.834607 0.406676 0.538717 11.00000 0.04200 0.07712 = 0.07554 0.02002 0.00711 0.01044 AFIX 43 H19 2 0.933404 0.370454 0.547929 11.00000 -1.20000 AFIX 0 C20 1 0.780780 0.480796 0.585780 11.00000 0.04014 0.09650 = 0.05578 0.01690 -0.00782 -0.00230 AFIX 43 H20 2 0.844993 0.496947 0.626034 11.00000 -1.20000 AFIX 0 C21 1 0.630356 0.532157 0.573705 11.00000 0.04569 0.05604 = 0.04089 0.00677 0.00243 -0.00013 AFIX 43 H21 2 0.593640 0.582158 0.606296 11.00000 -1.20000 AFIX 0 C22 1 0.062584 0.296045 0.362033 11.00000 0.04937 0.05117 = 0.04865 -0.00352 0.00350 -0.00579 AFIX 43 H22 2 0.096758 0.243935 0.393538 11.00000 -1.20000 AFIX 0 C23 1 -0.032487 0.271978 0.302955 11.00000 0.06257 0.06136 = 0.05157 -0.01228 0.00403 -0.01842 AFIX 43 H23 2 -0.062192 0.203111 0.294090 11.00000 -1.20000 AFIX 0 C24 1 0.189799 0.609644 0.393951 11.00000 0.05147 0.04039 = 0.03178 0.00219 -0.00324 0.00414 C25 1 0.245237 0.710758 0.578589 11.00000 0.05321 0.03751 = 0.03711 0.00262 -0.00477 0.01038 HKLF 4 REM P212121_a.res in P2(1)2(1)2(1) REM wR2 = 0.1036, GooF = S = 0.884, Restrained GooF = 0.884 for all data REM R1 = 0.0441 for 2018 Fo > 4sig(Fo) and 0.0865 for all 3349 data REM 283 parameters refined using 0 restraints END WGHT 0.0317 0.0000 REM Instructions for potential hydrogen bonds HTAB O2 O6 HTAB O5 O4 REM Highest difference peak 0.180, deepest hole -0.191, 1-sigma level 0.054 Q1 1 0.7800 0.2730 0.5203 11.00000 0.05 0.18 Q2 1 0.2245 0.4448 0.5600 11.00000 0.05 0.18 Q3 1 0.2388 0.5561 0.5788 11.00000 0.05 0.18 Q4 1 0.0536 0.4308 0.3617 11.00000 0.05 0.17 Q5 1 -0.0023 0.4474 0.3017 11.00000 0.05 0.17 ; _shelx_res_checksum 14580 _shelx_hkl_file ; 0 0 -1 0.83 0.64 0 0 -1 -0.08 0.39 0 0 -1 0.31 0.45 0 0 -1 0.81 0.50 0 0 -1 0.05 0.33 0 0 1 -0.16 0.37 0 0 1 1.29 0.75 0 0 1 0.48 0.55 0 0 1 0.37 0.30 0 0 1 0.81 0.56 0 0 -2 705.04 15.13 0 0 -2 804.50 16.24 0 0 -2 659.98 9.85 0 0 -2 579.66 13.49 0 0 -2 548.97 10.86 0 0 -2 915.71 17.39 0 0 2 702.13 15.18 0 0 2 794.71 16.05 0 0 2 634.09 9.61 0 0 2 549.47 13.07 0 0 2 552.22 10.91 0 0 2 862.10 16.78 0 0 -3 -0.09 1.65 0 0 -3 -0.37 1.00 0 0 -3 -0.14 0.69 0 0 -3 1.32 1.60 0 0 -3 -0.12 1.12 0 0 -3 -0.34 0.76 0 0 3 -0.45 0.97 0 0 3 0.14 1.75 0 0 3 -0.02 0.44 0 0 3 -0.56 0.97 0 0 3 -0.56 0.86 0 0 -4 81.94 7.73 0 0 -4 73.40 4.83 0 0 -4 60.45 6.53 0 0 -4 61.84 5.38 0 0 -4 108.94 9.07 0 0 4 85.70 7.82 0 0 4 62.84 4.47 0 0 4 65.57 5.70 0 0 -5 0.84 1.95 0 0 -5 -0.11 0.75 0 0 -5 -1.23 1.28 0 0 -5 -0.79 1.68 0 0 5 -2.21 1.26 0 0 5 -0.16 1.18 0 0 5 1.25 1.89 0 0 -6 20.54 3.88 0 0 -6 6.75 4.36 0 0 6 18.63 5.76 0 0 6 22.20 3.86 0 0 6 18.46 4.52 0 0 -7 0.47 2.63 0 0 -7 -1.26 1.37 0 0 -7 -0.69 2.12 0 0 -7 -0.45 2.24 0 0 7 1.04 2.68 0 0 7 1.29 1.85 0 0 -8 113.43 16.17 0 0 -8 103.35 8.20 0 0 -8 87.00 13.73 0 0 -8 136.38 15.22 0 0 8 108.57 15.24 0 0 8 77.73 8.71 0 0 -9 5.87 4.66 0 0 -9 3.55 2.46 0 0 -9 0.12 2.80 0 0 -9 -1.37 3.02 0 0 9 2.54 3.21 0 0 -10 -2.17 5.03 0 0 -10 5.38 3.16 0 0 -10 4.04 4.00 0 0 -10 5.41 5.31 0 0 10 0.79 4.27 0 0 10 0.90 3.49 0 0 10 2.51 4.43 0 0 -11 -0.90 2.21 0 0 -11 -0.97 3.91 0 0 -11 0.83 5.05 0 0 11 2.59 4.13 0 0 11 -0.45 3.57 0 0 11 0.65 5.48 0 0 -12 95.70 9.74 0 0 -12 69.38 14.88 0 0 -12 128.26 20.38 0 0 12 99.02 17.98 0 0 12 91.94 13.60 0 0 12 121.13 19.71 0 0 -13 -1.46 3.10 0 0 -13 -7.10 5.59 0 0 -13 -7.06 5.50 0 0 13 -5.47 5.87 0 0 13 0.76 4.69 0 0 13 -2.09 5.98 0 0 -14 81.27 9.94 0 0 -14 68.12 16.24 0 0 -14 89.08 18.81 0 0 14 97.30 19.66 0 0 14 54.58 11.86 0 0 14 86.09 17.96 0 0 -15 -2.23 3.82 0 0 -15 1.31 8.34 0 0 15 -2.01 7.53 0 0 15 0.45 3.24 0 0 15 -5.95 7.71 0 0 -16 -0.70 8.94 0 0 -16 21.83 10.91 0 0 16 15.22 10.00 0 0 16 17.15 7.46 0 0 16 24.82 12.18 0 0 -17 8.66 7.81 0 0 -17 -10.56 7.21 0 0 17 -1.15 8.63 0 0 17 -0.53 4.16 0 0 17 9.22 11.50 0 0 -18 0.75 9.18 0 0 -18 14.66 12.95 0 0 18 2.45 7.65 0 0 18 8.06 11.45 0 0 -19 1.40 7.42 0 0 -19 -1.00 7.06 0 0 19 -4.19 6.36 0 0 19 7.35 9.72 0 0 -20 12.45 11.17 0 0 -20 30.96 18.00 0 0 20 34.59 18.65 0 0 20 10.31 14.18 0 0 -21 1.12 12.39 0 0 -21 4.77 9.69 0 0 21 2.06 9.24 0 0 21 1.18 6.64 0 0 -22 14.57 13.31 0 0 -22 28.53 18.85 0 0 22 12.61 17.05 0 0 22 21.86 17.36 0 0 -23 -2.18 8.54 0 0 -23 2.82 16.48 0 0 23 -1.00 10.14 0 0 23 -3.63 13.62 0 -1 0 0.76 0.62 0 -1 0 0.58 0.56 0 -1 0 0.69 0.56 0 -1 0 1.00 0.69 0 -1 0 1.14 0.90 0 1 0 0.06 0.44 0 1 0 1.11 0.79 0 1 0 0.53 0.51 0 1 0 0.30 0.44 0 1 0 0.26 0.62 0 1 0 0.93 0.72 0 -1 -1 386.61 9.05 0 -1 -1 334.85 9.82 0 -1 -1 278.09 8.69 0 -1 -1 214.02 4.44 0 -1 -1 435.23 11.09 0 -1 1 373.90 9.63 0 -1 1 339.12 7.25 0 -1 1 323.45 7.96 0 -1 1 284.85 9.13 0 -1 1 429.35 10.97 0 1 -1 380.57 9.72 0 1 -1 343.38 7.28 0 1 -1 288.83 7.56 0 1 -1 278.04 8.99 0 1 -1 442.92 11.19 0 1 1 373.28 8.91 0 1 1 349.28 9.97 0 1 1 267.98 8.51 0 1 1 281.83 5.08 0 1 1 436.91 11.16 0 -1 -2 43.30 4.13 0 -1 -2 40.28 4.05 0 -1 -2 35.00 4.04 0 -1 -2 47.55 4.74 0 -1 2 39.68 4.30 0 -1 2 35.34 1.96 0 -1 2 27.66 3.23 0 -1 2 29.04 4.10 0 -1 2 52.01 4.83 0 1 -2 46.54 4.38 0 1 -2 32.08 1.89 0 1 -2 25.35 2.93 0 1 -2 33.47 4.49 0 1 -2 47.34 4.50 0 1 2 43.86 4.10 0 1 2 34.18 3.74 0 1 2 30.79 4.33 0 1 2 55.28 4.83 0 1 2 50.62 4.81 0 -1 -3 229.15 10.02 0 -1 -3 190.14 10.52 0 -1 -3 178.00 5.38 0 -1 -3 291.63 12.87 0 -1 3 216.34 4.49 0 -1 3 296.66 5.17 0 -1 3 197.55 9.60 0 -1 3 180.60 9.68 0 1 -3 289.48 12.67 0 1 -3 194.45 9.46 0 1 -3 329.23 13.65 0 1 3 257.84 11.51 0 1 3 218.09 9.71 0 1 3 189.51 5.55 0 1 3 179.51 5.39 0 1 3 312.40 13.35 0 -1 -4 167.68 9.44 0 -1 -4 154.61 10.72 0 -1 -4 144.16 6.28 0 -1 -4 222.98 12.75 0 -1 4 194.87 11.95 0 -1 4 194.09 5.00 0 -1 4 186.40 4.83 0 -1 4 160.03 10.14 0 1 -4 216.45 12.59 0 1 -4 228.76 5.34 0 1 -4 162.49 10.30 0 1 -4 256.48 13.63 0 1 4 205.17 11.83 0 1 4 146.01 6.33 0 1 4 145.89 6.28 0 1 4 235.79 13.12 0 -1 -5 332.33 14.07 0 -1 -5 279.42 15.94 0 -1 -5 305.54 10.67 0 -1 -5 416.61 19.24 0 -1 5 377.51 18.53 0 -1 5 334.59 7.73 0 -1 5 263.57 13.99 0 1 -5 417.40 19.43 0 1 -5 451.96 9.01 0 1 -5 281.16 15.00 0 1 -5 466.70 20.43 0 1 5 362.09 17.40 0 1 5 278.46 10.24 0 1 5 257.17 9.80 0 1 5 448.45 19.96 0 -1 -6 216.62 12.04 0 -1 -6 174.24 13.73 0 -1 -6 177.27 9.32 0 -1 -6 263.02 16.81 0 -1 6 233.31 15.95 0 -1 6 217.67 7.26 0 -1 6 161.82 12.25 0 1 -6 275.32 17.23 0 1 -6 289.50 8.37 0 1 -6 183.69 13.62 0 1 -6 316.84 18.37 0 1 6 224.29 15.55 0 1 6 177.08 9.36 0 1 6 172.70 9.22 0 1 6 293.13 17.86 0 -1 -7 0.33 2.42 0 -1 -7 -0.22 1.89 0 -1 -7 1.51 2.98 0 -1 7 2.90 3.27 0 -1 7 -0.45 0.79 0 -1 7 -0.09 1.62 0 1 -7 0.56 2.77 0 1 -7 0.55 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2 5.34 9.47 9 -3 -2 15.77 15.44 9 -3 2 3.77 10.02 9 3 -2 -3.29 7.71 9 3 -2 -1.60 7.82 9 3 2 -0.39 8.65 9 3 2 0.83 11.22 -9 -3 -3 -1.22 9.29 -9 -3 3 5.62 11.05 -9 3 -3 -1.60 13.68 -9 3 -3 -3.69 9.27 -9 3 3 1.87 15.39 -9 3 3 6.98 13.06 9 -3 -3 3.04 13.06 9 -3 3 -0.93 11.89 9 3 -3 8.94 14.62 9 3 -3 0.00 8.90 9 3 3 -5.13 11.64 9 3 3 2.27 12.50 -9 -3 -4 11.31 12.95 -9 -3 4 9.41 16.02 -9 3 -4 0.95 15.57 -9 3 -4 24.01 16.70 -9 3 4 16.42 13.42 -9 3 4 7.29 14.96 9 -3 -4 11.72 16.34 9 -3 4 13.62 15.24 9 3 -4 13.56 14.88 9 3 -4 19.59 16.41 9 3 4 0.75 9.50 9 3 4 26.77 13.48 -9 -3 -5 39.25 20.21 -9 -3 5 13.01 12.31 -9 3 -5 16.28 17.01 -9 3 -5 2.91 14.05 -9 3 5 22.22 14.80 -9 3 5 14.72 11.56 9 -3 -5 -4.77 13.38 9 -3 5 7.46 10.60 9 3 -5 13.31 12.45 9 3 -5 15.27 15.35 9 3 5 19.06 16.59 9 3 5 9.26 12.36 -9 -3 -6 17.59 17.14 -9 -3 6 1.28 9.50 -9 3 -6 6.64 14.99 -9 3 -6 24.21 14.72 -9 3 6 12.42 17.12 9 -3 -6 10.00 15.44 9 -3 6 3.24 11.59 9 3 -6 -0.19 14.23 9 3 -6 7.37 10.70 9 3 6 8.37 16.22 9 3 6 2.62 8.85 -9 -3 -7 6.75 16.25 -9 -3 7 26.15 18.28 -9 3 -7 -2.32 9.43 -9 3 -7 6.51 10.84 -9 3 7 0.25 10.81 9 -3 -7 12.65 15.30 9 -3 7 0.12 7.71 9 3 -7 0.00 13.38 9 3 -7 4.64 11.28 9 3 7 0.02 10.08 9 3 7 -3.46 11.39 -9 -3 -8 5.47 14.99 -9 -3 8 -6.73 12.73 -9 -3 8 -8.91 7.95 -9 3 -8 -7.17 8.71 -9 3 -8 -6.62 12.04 -9 3 8 -2.49 8.37 9 -3 -8 -0.98 9.93 9 -3 8 -5.56 11.28 9 3 -8 5.41 11.27 9 3 -8 -3.57 7.17 9 3 8 -4.07 10.98 9 3 8 -0.33 11.79 -9 -3 -9 -2.37 9.18 -9 -3 9 9.57 12.09 -9 3 9 9.38 12.65 -9 -4 0 3.91 14.43 -9 4 0 7.03 11.95 -9 4 0 -1.34 11.78 9 -4 0 -1.39 11.78 9 4 0 7.57 10.44 9 4 0 4.95 12.59 -9 -4 -1 5.86 11.45 -9 -4 1 13.82 13.13 -9 4 -1 -9.41 14.09 -9 4 -1 3.69 13.54 -9 4 1 1.40 10.94 -9 4 1 2.68 10.02 9 -4 -1 0.70 12.89 9 -4 1 7.87 13.03 9 4 -1 4.41 13.70 9 4 -1 3.94 8.04 9 4 1 7.82 15.21 9 4 1 7.59 9.24 -9 -4 -2 -1.67 9.63 -9 -4 2 -0.05 12.95 -9 4 -2 -1.17 14.16 -9 4 -2 2.94 12.53 -9 4 2 17.78 16.84 -9 4 2 6.51 10.31 9 -4 -2 0.55 13.35 9 -4 2 5.50 9.80 9 4 -2 -2.31 8.35 9 4 -2 2.65 8.87 9 4 2 3.90 10.74 9 4 2 6.22 12.65 -9 -4 -3 18.95 17.70 -9 -4 3 15.29 13.98 -9 4 -3 -1.76 10.67 -9 4 -3 3.58 10.39 -9 4 3 12.14 15.66 -9 4 3 4.99 12.87 9 -4 -3 16.53 14.97 9 -4 3 7.42 11.14 9 4 -3 3.63 14.05 9 4 -3 1.92 12.82 9 4 3 0.22 12.95 9 4 3 0.09 7.43 -9 -4 -4 1.84 14.65 -9 -4 4 4.63 14.38 -9 4 -4 -2.17 10.50 -9 4 -4 -5.67 11.58 -9 4 4 -0.12 13.35 -9 4 4 15.69 16.06 9 -4 -4 1.75 13.13 9 -4 4 -10.91 10.35 9 4 -4 5.76 11.28 9 4 -4 -2.74 11.22 9 4 4 3.80 14.83 9 4 4 0.70 11.19 -9 -4 -5 2.98 16.47 -9 -4 5 6.90 11.55 -9 4 -5 4.38 11.72 -9 4 -5 7.40 14.23 -9 4 5 0.86 14.71 -9 4 5 5.56 15.78 9 -4 -5 5.84 14.52 9 -4 5 1.42 9.89 9 4 -5 -11.56 12.67 9 4 -5 5.53 11.19 9 4 5 0.19 9.88 9 4 5 12.51 11.22 -9 -4 -6 2.99 16.91 -9 -4 6 1.46 10.30 -9 -4 6 3.26 11.28 -9 4 -6 1.29 15.88 -9 4 -6 -16.59 11.30 -9 4 6 11.59 12.46 -9 4 6 -2.38 9.58 9 -4 -6 7.35 14.49 9 -4 6 3.07 9.40 9 4 -6 -0.78 14.51 9 4 -6 0.56 9.04 9 4 6 -7.18 8.71 9 4 6 -4.43 10.78 -9 -4 -7 2.09 11.14 -9 -4 7 -4.69 13.13 -9 -4 7 1.17 13.49 -9 4 -7 -8.16 13.88 -9 4 -7 7.63 11.95 -9 4 7 8.83 11.59 -9 4 7 -2.27 9.18 9 -4 -7 -1.54 10.27 9 -4 -7 -8.85 14.16 9 -4 7 5.67 14.65 9 4 -7 -1.67 10.38 9 4 -7 -9.44 11.67 9 4 7 0.09 8.96 -9 -4 -8 -2.18 9.08 -9 -4 8 6.39 14.32 -9 -4 8 -2.17 13.62 -9 4 -8 0.42 10.63 -9 4 8 6.23 16.30 -9 4 8 8.04 15.38 9 -4 -8 5.05 15.74 9 -4 -8 -2.29 15.21 9 -4 8 7.12 10.77 9 4 -8 5.30 16.94 9 4 -8 -2.46 14.71 -9 -5 0 -0.83 12.01 -9 5 0 17.29 18.03 -9 5 0 -1.22 14.32 9 -5 0 0.95 11.70 9 5 0 3.09 10.95 9 5 0 5.48 13.74 -9 -5 -1 15.49 14.46 -9 -5 1 6.37 11.94 -9 5 -1 13.54 13.13 -9 5 -1 14.54 15.50 -9 5 1 9.44 13.03 -9 5 1 10.47 12.26 9 -5 -1 1.36 13.76 9 -5 1 26.77 17.50 9 5 -1 -6.03 14.04 9 5 -1 0.81 8.60 9 5 1 23.17 17.51 9 5 1 2.37 9.30 -9 -5 -2 8.62 12.65 -9 -5 2 2.62 14.68 -9 5 -2 8.44 11.86 -9 5 -2 3.43 9.96 -9 5 2 -3.26 14.49 -9 5 2 6.53 11.41 9 -5 -2 -0.55 13.35 9 -5 2 7.60 10.66 9 5 -2 8.43 12.37 9 5 -2 0.75 8.34 9 5 2 -2.26 12.62 9 5 2 0.02 12.61 -9 -5 -3 11.55 16.56 -9 -5 3 2.74 11.45 -9 -5 3 3.41 16.03 -9 5 -3 4.27 10.72 -9 5 -3 10.58 12.43 -9 5 3 3.49 12.40 -9 5 3 -1.34 10.35 9 -5 -3 15.35 12.70 9 -5 -3 -1.04 8.97 9 -5 3 1.11 8.57 9 5 -3 7.29 15.78 9 5 -3 -6.00 12.57 9 5 3 5.34 11.62 9 5 3 4.47 8.90 -9 -5 -4 2.23 12.22 -9 -5 4 5.24 15.47 -9 -5 4 22.67 16.55 -9 5 -4 11.48 16.72 -9 5 -4 30.07 20.29 -9 5 4 11.19 15.21 9 -5 -4 8.37 14.04 9 -5 -4 18.85 13.79 9 -5 4 12.04 14.15 9 5 -4 6.96 11.86 9 5 -4 11.72 13.57 9 5 4 11.56 16.47 9 5 4 10.25 13.57 -9 -5 -5 4.27 12.57 -9 -5 5 11.23 13.59 -9 -5 5 -0.98 9.96 -9 5 -5 6.25 16.16 -9 5 -5 2.66 15.24 -9 5 5 -4.69 9.82 9 -5 -5 -3.74 7.96 9 -5 -5 -0.81 14.15 9 -5 5 -0.95 8.52 9 5 -5 -3.19 15.39 9 5 -5 -1.03 9.60 9 5 5 7.14 14.72 9 5 5 5.27 8.97 -9 -5 -6 -5.41 8.12 -9 -5 6 5.48 10.81 -9 -5 6 9.43 15.44 -9 5 -6 2.96 10.60 -9 5 -6 -4.46 12.85 -9 5 6 5.67 17.73 -9 5 6 0.31 15.57 9 -5 -6 21.47 16.70 9 -5 -6 5.36 15.88 9 -5 6 -2.54 8.93 9 5 -6 11.62 13.91 9 5 -6 -4.33 12.04 9 5 6 7.00 17.06 9 5 6 5.10 13.84 9 -5 -7 -8.77 12.90 -9 -6 0 -7.87 12.68 -9 -6 0 11.61 16.80 -9 6 0 3.82 11.67 -9 6 0 -4.67 15.64 9 -6 0 10.11 15.04 9 6 0 3.60 15.81 9 6 0 -7.42 9.46 -9 -6 -1 12.23 13.95 -9 -6 1 15.80 13.51 -9 -6 1 18.17 13.80 -9 6 -1 18.17 15.44 -9 6 -1 14.46 12.75 -9 6 1 5.44 17.00 -9 6 1 32.77 20.43 9 -6 -1 13.01 16.86 9 -6 -1 -2.93 12.62 9 -6 1 12.04 15.30 9 6 -1 24.28 19.46 9 6 -1 6.06 10.17 9 6 1 18.39 15.05 9 6 1 14.96 12.32 -9 -6 -2 22.58 17.84 -9 -6 2 -5.41 11.42 -9 -6 2 3.18 11.25 -9 6 -2 1.32 15.67 -9 6 -2 3.65 11.44 -9 6 2 3.10 10.53 -9 6 2 -2.60 14.35 9 -6 -2 -6.76 8.73 9 -6 -2 -1.50 12.09 9 -6 2 -1.37 8.15 9 6 -2 6.33 12.46 9 6 -2 0.26 9.61 9 6 2 -1.75 16.52 9 6 2 8.23 13.03 -9 -6 -3 21.38 15.22 -9 -6 3 -0.26 10.00 -9 -6 3 3.07 15.64 -9 6 -3 1.68 15.57 -9 6 -3 18.40 17.70 -9 6 3 13.31 16.98 -9 6 3 8.41 15.91 9 -6 -3 -5.19 12.25 9 -6 -3 7.45 15.60 9 -6 3 -0.48 8.21 9 6 -3 9.78 17.01 9 6 -3 3.82 14.05 9 6 3 -10.89 14.79 9 6 3 7.57 12.40 -9 -6 -4 5.44 10.14 -9 -6 4 0.20 15.47 -9 -6 4 -6.56 10.08 -9 6 -4 4.00 15.81 -9 6 -4 0.17 14.93 -9 6 4 11.19 12.82 -9 6 4 3.26 10.66 9 -6 -4 -1.22 8.85 9 -6 -4 -2.73 15.57 9 -6 4 8.29 15.13 9 6 -4 3.94 12.04 9 6 -4 3.94 11.33 9 6 4 -10.02 14.58 9 6 4 1.62 9.01 9 -6 -5 -6.95 8.51 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 13389 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, 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 O1 O 0.1627(4) 0.5626(2) 0.68056(14) 0.0472(8) Uani 1 1 d . . . . . O2 O 0.2441(4) 0.35759(19) 0.48203(15) 0.0484(8) Uani 1 1 d . . . . . H2 H 0.272462 0.383345 0.520521 0.073 Uiso 1 1 calc R U . . . O3 O 0.0911(4) 0.5793(2) 0.33751(15) 0.0518(9) Uani 1 1 d . . . . . O4 O 0.2116(4) 0.7044(2) 0.39926(15) 0.0549(9) Uani 1 1 d . . . . . O5 O 0.2698(5) 0.7878(2) 0.53147(15) 0.0619(10) Uani 1 1 d . . . . . H5 H 0.265460 0.764422 0.490466 0.093 Uiso 1 1 calc R U . . . O6 O 0.2591(4) 0.4390(2) 0.61134(14) 0.0474(8) Uani 1 1 d . . . . . C1 C 0.0117(7) 0.7908(5) 0.7743(3) 0.0739(17) Uani 1 1 d . . . . . H1 H -0.043427 0.807510 0.816884 0.089 Uiso 1 1 calc R U . . . C2 C 0.0502(6) 0.6879(4) 0.7593(2) 0.0582(14) Uani 1 1 d . . . . . H2A H 0.024081 0.635013 0.791648 0.070 Uiso 1 1 calc R U . . . C3 C 0.1294(6) 0.6661(4) 0.6943(2) 0.0442(11) Uani 1 1 d . . . . . C4 C 0.2396(5) 0.5324(3) 0.6180(2) 0.0376(10) Uani 1 1 d . . . . . C5 C 0.2857(5) 0.6099(3) 0.56659(19) 0.0340(10) Uani 1 1 d . . . . . C6 C 0.3768(5) 0.5755(3) 0.49875(19) 0.0358(10) Uani 1 1 d . . . . . H6 H 0.420144 0.640244 0.477915 0.043 Uiso 1 1 calc R U . . . C7 C 0.2574(5) 0.5331(3) 0.4420(2) 0.0344(10) Uani 1 1 d . . . . . C8 C 0.2064(5) 0.4333(3) 0.4356(2) 0.0390(11) Uani 1 1 d . . . . . C9 C 0.1081(5) 0.4005(3) 0.3746(2) 0.0398(11) Uani 1 1 d . . . . . C10 C 0.0540(6) 0.4757(4) 0.3274(2) 0.0447(12) Uani 1 1 d . . . . . C11 C -0.0428(6) 0.4516(4) 0.2676(2) 0.0578(14) Uani 1 1 d . . . . . H11 H -0.078314 0.503279 0.235991 0.069 Uiso 1 1 calc R U . . . C12 C -0.0843(7) 0.3492(4) 0.2566(3) 0.0648(15) Uani 1 1 d . . . . . H12 H -0.149142 0.331439 0.216865 0.078 Uiso 1 1 calc R U . . . C13 C 0.0541(7) 0.8684(4) 0.7270(3) 0.0725(17) Uani 1 1 d . . . . . H13 H 0.029922 0.937396 0.738280 0.087 Uiso 1 1 calc R U . . . C14 C 0.1323(7) 0.8452(4) 0.6628(3) 0.0631(15) Uani 1 1 d . . . . . H14 H 0.160018 0.898241 0.630914 0.076 Uiso 1 1 calc R U . . . C15 C 0.1697(6) 0.7425(4) 0.6459(2) 0.0444(12) Uani 1 1 d . . . . . C16 C 0.5344(5) 0.5099(3) 0.5138(2) 0.0360(10) Uani 1 1 d . . . . . C17 C 0.5949(6) 0.4367(3) 0.4659(2) 0.0469(12) Uani 1 1 d . . . . . H17 H 0.533638 0.421814 0.424553 0.056 Uiso 1 1 calc R U . . . C18 C 0.7442(7) 0.3853(4) 0.4780(3) 0.0590(13) Uani 1 1 d . . . . . H18 H 0.783108 0.336305 0.445149 0.071 Uiso 1 1 calc R U . . . C19 C 0.8346(7) 0.4067(4) 0.5387(3) 0.0649(15) Uani 1 1 d . . . . . H19 H 0.933404 0.370454 0.547929 0.078 Uiso 1 1 calc R U . . . C20 C 0.7808(6) 0.4808(4) 0.5858(3) 0.0641(15) Uani 1 1 d . . . . . H20 H 0.844993 0.496947 0.626034 0.077 Uiso 1 1 calc R U . . . C21 C 0.6304(6) 0.5322(3) 0.5737(2) 0.0475(12) Uani 1 1 d . . . . . H21 H 0.593640 0.582158 0.606296 0.057 Uiso 1 1 calc R U . . . C22 C 0.0626(5) 0.2960(4) 0.3620(2) 0.0497(12) Uani 1 1 d . . . . . H22 H 0.096758 0.243935 0.393538 0.060 Uiso 1 1 calc R U . . . C23 C -0.0325(6) 0.2720(4) 0.3030(3) 0.0585(14) Uani 1 1 d . . . . . H23 H -0.062192 0.203111 0.294090 0.070 Uiso 1 1 calc R U . . . C24 C 0.1898(6) 0.6096(4) 0.3940(2) 0.0412(11) Uani 1 1 d . . . . . C25 C 0.2452(6) 0.7108(3) 0.5786(2) 0.0426(11) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.054(2) 0.0524(19) 0.0354(17) -0.0030(15) 0.0072(15) -0.0045(17) O2 0.061(2) 0.0366(16) 0.0477(18) 0.0049(14) -0.0047(18) -0.0031(17) O3 0.065(2) 0.052(2) 0.0391(18) 0.0038(15) -0.0150(16) 0.0011(18) O4 0.079(3) 0.0391(19) 0.0463(18) 0.0073(15) -0.0144(17) 0.0030(18) O5 0.103(3) 0.0370(17) 0.0457(18) 0.0065(15) 0.000(2) 0.013(2) O6 0.063(2) 0.0350(18) 0.0437(17) 0.0063(14) 0.0054(16) 0.0015(17) C1 0.063(4) 0.095(5) 0.064(4) -0.034(4) 0.006(3) 0.006(4) C2 0.056(4) 0.075(4) 0.044(3) -0.014(3) 0.003(3) -0.002(3) C3 0.040(3) 0.050(3) 0.042(3) -0.011(2) 0.000(2) 0.003(2) C4 0.038(3) 0.042(3) 0.033(2) 0.000(2) 0.000(2) 0.001(2) C5 0.039(3) 0.033(2) 0.030(2) 0.0002(19) -0.0034(19) 0.006(2) C6 0.046(3) 0.030(2) 0.032(2) 0.0024(18) -0.001(2) 0.003(2) C7 0.039(2) 0.033(3) 0.032(2) -0.0005(18) 0.002(2) 0.002(2) C8 0.041(3) 0.040(3) 0.036(2) 0.001(2) 0.006(2) 0.006(2) C9 0.038(3) 0.047(3) 0.035(2) -0.004(2) 0.004(2) -0.002(2) C10 0.047(3) 0.049(3) 0.038(3) -0.004(2) 0.000(2) -0.004(2) C11 0.064(3) 0.069(4) 0.040(3) -0.003(3) -0.011(3) -0.010(3) C12 0.064(4) 0.089(4) 0.041(3) -0.014(3) -0.008(3) -0.019(3) C13 0.083(4) 0.065(4) 0.069(4) -0.028(3) -0.014(3) 0.025(3) C14 0.083(4) 0.053(3) 0.054(3) -0.012(3) -0.010(3) 0.022(3) C15 0.048(3) 0.047(3) 0.038(3) -0.005(2) -0.010(2) 0.010(2) C16 0.039(3) 0.033(2) 0.036(2) 0.006(2) 0.001(2) 0.001(2) C17 0.045(3) 0.049(3) 0.047(3) 0.004(2) 0.004(2) 0.002(3) C18 0.054(3) 0.053(3) 0.070(3) 0.009(3) 0.020(3) 0.009(3) C19 0.042(3) 0.077(4) 0.076(4) 0.020(3) 0.007(3) 0.010(3) C20 0.040(3) 0.097(4) 0.056(3) 0.017(3) -0.008(3) -0.002(3) C21 0.046(3) 0.056(3) 0.041(3) 0.007(2) 0.002(2) 0.000(3) C22 0.049(3) 0.051(3) 0.049(3) -0.004(2) 0.004(3) -0.006(2) C23 0.063(4) 0.061(3) 0.052(3) -0.012(3) 0.004(3) -0.018(3) C24 0.051(3) 0.040(3) 0.032(2) 0.002(2) -0.003(2) 0.004(2) C25 0.053(3) 0.038(3) 0.037(2) 0.003(2) -0.005(2) 0.010(2) 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' 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 C4 O1 C3 121.0(3) . . ? C8 O2 H2 109.5 . . ? C24 O3 C10 120.3(3) . . ? C25 O5 H5 109.5 . . ? C13 C1 C2 120.6(5) . . ? C13 C1 H1 119.7 . . ? C2 C1 H1 119.7 . . ? C1 C2 C3 117.8(5) . . ? C1 C2 H2A 121.1 . . ? C3 C2 H2A 121.1 . . ? C15 C3 O1 121.6(4) . . ? C15 C3 C2 122.2(4) . . ? O1 C3 C2 116.2(4) . . ? O6 C4 O1 115.0(4) . . ? O6 C4 C5 126.0(4) . . ? O1 C4 C5 119.0(4) . . ? C25 C5 C4 119.7(4) . . ? C25 C5 C6 121.9(4) . . ? C4 C5 C6 118.4(3) . . ? C7 C6 C5 112.4(3) . . ? C7 C6 C16 116.2(3) . . ? C5 C6 C16 113.5(3) . . ? C7 C6 H6 104.4 . . ? C5 C6 H6 104.4 . . ? C16 C6 H6 104.4 . . ? C8 C7 C24 118.8(4) . . ? C8 C7 C6 126.1(4) . . ? C24 C7 C6 115.0(3) . . ? O2 C8 C7 124.5(4) . . ? O2 C8 C9 114.8(4) . . ? C7 C8 C9 120.7(4) . . ? C10 C9 C22 118.8(4) . . ? C10 C9 C8 117.9(4) . . ? C22 C9 C8 123.3(4) . . ? O3 C10 C9 121.7(4) . . ? O3 C10 C11 116.4(4) . . ? C9 C10 C11 121.9(4) . . ? C12 C11 C10 117.8(5) . . ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C11 C12 C23 121.7(5) . . ? C11 C12 H12 119.2 . . ? C23 C12 H12 119.2 . . ? C1 C13 C14 120.6(5) . . ? C1 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C15 119.9(5) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C3 C15 C14 118.8(4) . . ? C3 C15 C25 117.6(4) . . ? C14 C15 C25 123.6(4) . . ? C21 C16 C17 117.9(4) . . ? C21 C16 C6 119.0(4) . . ? C17 C16 C6 122.7(4) . . ? C18 C17 C16 121.4(4) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C19 C18 C17 119.6(5) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C20 C19 C18 120.3(5) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 120.0(5) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C16 C21 C20 120.7(5) . . ? C16 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C23 C22 C9 119.4(5) . . ? C23 C22 H22 120.3 . . ? C9 C22 H22 120.3 . . ? C22 C23 C12 120.4(5) . . ? C22 C23 H23 119.8 . . ? C12 C23 H23 119.8 . . ? O4 C24 O3 115.1(4) . . ? O4 C24 C7 125.0(4) . . ? O3 C24 C7 119.9(4) . . ? O5 C25 C5 124.4(4) . . ? O5 C25 C15 114.8(4) . . ? C5 C25 C15 120.7(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 O1 C4 1.371(5) . ? O1 C3 1.379(5) . ? O2 C8 1.335(5) . ? O2 H2 0.8200 . ? O3 C24 1.368(5) . ? O3 C10 1.374(5) . ? O4 C24 1.232(5) . ? O5 C25 1.335(5) . ? O5 H5 0.8200 . ? O6 C4 1.215(4) . ? C1 C13 1.372(7) . ? C1 C2 1.386(7) . ? C1 H1 0.9300 . ? C2 C3 1.392(6) . ? C2 H2A 0.9300 . ? C3 C15 1.369(6) . ? C4 C5 1.428(5) . ? C5 C25 1.353(5) . ? C5 C6 1.521(5) . ? C6 C7 1.521(5) . ? C6 C16 1.537(5) . ? C6 H6 0.9800 . ? C7 C8 1.350(5) . ? C7 C24 1.433(5) . ? C8 C9 1.440(5) . ? C9 C10 1.375(6) . ? C9 C22 1.409(6) . ? C10 C11 1.388(6) . ? C11 C12 1.371(6) . ? C11 H11 0.9300 . ? C12 C23 1.377(6) . ? C12 H12 0.9300 . ? C13 C14 1.379(7) . ? C13 H13 0.9300 . ? C14 C15 1.388(6) . ? C14 H14 0.9300 . ? C15 C25 1.447(6) . ? C16 C21 1.381(6) . ? C16 C17 1.381(5) . ? C17 C18 1.379(6) . ? C17 H17 0.9300 . ? C18 C19 1.367(7) . ? C18 H18 0.9300 . ? C19 C20 1.362(7) . ? C19 H19 0.9300 . ? C20 C21 1.386(6) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.370(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O5 H5 O4 0.82 1.91 2.721(4) 169.0 . yes O2 H2 O6 0.82 1.84 2.624(4) 160.6 . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 C1 C2 C3 -1.4(8) . . . . ? C4 O1 C3 C15 0.7(6) . . . . ? C4 O1 C3 C2 179.7(4) . . . . ? C1 C2 C3 C15 0.2(7) . . . . ? C1 C2 C3 O1 -178.7(4) . . . . ? C3 O1 C4 O6 -178.5(4) . . . . ? C3 O1 C4 C5 0.1(5) . . . . ? O6 C4 C5 C25 175.0(4) . . . . ? O1 C4 C5 C25 -3.4(6) . . . . ? O6 C4 C5 C6 -3.8(6) . . . . ? O1 C4 C5 C6 177.7(3) . . . . ? C25 C5 C6 C7 -97.8(5) . . . . ? C4 C5 C6 C7 81.0(4) . . . . ? C25 C5 C6 C16 127.9(4) . . . . ? C4 C5 C6 C16 -53.2(5) . . . . ? C5 C6 C7 C8 -88.6(5) . . . . ? C16 C6 C7 C8 44.4(5) . . . . ? C5 C6 C7 C24 88.5(4) . . . . ? C16 C6 C7 C24 -138.5(4) . . . . ? C24 C7 C8 O2 -171.6(4) . . . . ? C6 C7 C8 O2 5.3(7) . . . . ? C24 C7 C8 C9 10.2(6) . . . . ? C6 C7 C8 C9 -172.8(4) . . . . ? O2 C8 C9 C10 175.2(3) . . . . ? C7 C8 C9 C10 -6.4(6) . . . . ? O2 C8 C9 C22 -3.5(6) . . . . ? C7 C8 C9 C22 174.8(4) . . . . ? C24 O3 C10 C9 2.7(6) . . . . ? C24 O3 C10 C11 -178.1(4) . . . . ? C22 C9 C10 O3 178.6(4) . . . . ? C8 C9 C10 O3 -0.2(6) . . . . ? C22 C9 C10 C11 -0.5(6) . . . . ? C8 C9 C10 C11 -179.3(4) . . . . ? O3 C10 C11 C12 -178.9(4) . . . . ? C9 C10 C11 C12 0.2(7) . . . . ? C10 C11 C12 C23 0.0(8) . . . . ? C2 C1 C13 C14 1.5(9) . . . . ? C1 C13 C14 C15 -0.4(8) . . . . ? O1 C3 C15 C14 179.8(4) . . . . ? C2 C3 C15 C14 0.9(7) . . . . ? O1 C3 C15 C25 1.5(6) . . . . ? C2 C3 C15 C25 -177.4(4) . . . . ? C13 C14 C15 C3 -0.8(7) . . . . ? C13 C14 C15 C25 177.4(4) . . . . ? C7 C6 C16 C21 -167.3(4) . . . . ? C5 C6 C16 C21 -34.9(5) . . . . ? C7 C6 C16 C17 19.9(5) . . . . ? C5 C6 C16 C17 152.3(4) . . . . ? C21 C16 C17 C18 1.6(6) . . . . ? C6 C16 C17 C18 174.5(4) . . . . ? C16 C17 C18 C19 0.1(7) . . . . ? C17 C18 C19 C20 -2.2(7) . . . . ? C18 C19 C20 C21 2.5(7) . . . . ? C17 C16 C21 C20 -1.3(6) . . . . ? C6 C16 C21 C20 -174.4(4) . . . . ? C19 C20 C21 C16 -0.7(7) . . . . ? C10 C9 C22 C23 0.7(6) . . . . ? C8 C9 C22 C23 179.4(4) . . . . ? C9 C22 C23 C12 -0.5(7) . . . . ? C11 C12 C23 C22 0.2(8) . . . . ? C10 O3 C24 O4 -178.1(4) . . . . ? C10 O3 C24 C7 1.1(6) . . . . ? C8 C7 C24 O4 171.6(4) . . . . ? C6 C7 C24 O4 -5.8(6) . . . . ? C8 C7 C24 O3 -7.6(6) . . . . ? C6 C7 C24 O3 175.1(3) . . . . ? C4 C5 C25 O5 -174.1(4) . . . . ? C6 C5 C25 O5 4.7(7) . . . . ? C4 C5 C25 C15 5.8(6) . . . . ? C6 C5 C25 C15 -175.4(4) . . . . ? C3 C15 C25 O5 175.1(4) . . . . ? C14 C15 C25 O5 -3.1(7) . . . . ? C3 C15 C25 C5 -4.9(6) . . . . ? C14 C15 C25 C5 177.0(5) . . . . ?