#------------------------------------------------------------------------------ #$Date: 2025-07-29 05:08:36 +0100 (Tue, 29 Jul 2025) $ #$Revision: 301392 $ #$URL: svn://www.crystallography.net/cod/cif/3/00/05/3000589.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_3000589 loop_ _publ_author_name 'Sasaki, Toshiyuki' 'Nakane, Takanori' 'Takimoto, Kazuyoshi' 'Ichiyanagi, Kouhei' 'Mori, Yuki' 'Baba, Seiki' 'Sakai, Naoki' 'Kurisu, Genji' 'Miyata, Mikiji' 'Uno, Takahiro' 'Itoh, Takahito' _publ_section_title ; Application of multiple small-wedge synchrotron crystallography for post-reaction structural characterization of a stimuli-responsive small-molecule crystal ; _journal_name_full 'Bulletin of the Chemical Society of Japan' _journal_paper_doi 10.1093/bulcsj/uoaf059 _journal_volume 98 _journal_year 2025 _chemical_formula_moiety 'C16 H16 O8' _chemical_formula_sum 'C16 H16 O8' _chemical_formula_weight 336.29 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _audit_creation_date 2025-06-03 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _cell_angle_alpha 90 _cell_angle_beta 101.692(6) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.7157(5) _cell_length_b 6.7991(3) _cell_length_c 12.3904(7) _cell_measurement_reflns_used 2474 _cell_measurement_temperature 100 _cell_measurement_theta_max 70.6110 _cell_measurement_theta_min 5.1070 _cell_volume 719.01(7) _computing_cell_refinement 'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)' _computing_data_collection 'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)' _computing_data_reduction 'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.00 _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -100.00 -75.00 0.50 0.06 -- 0.00 0.00 120.00 50 2 \w -99.00 -74.00 0.50 0.06 -- 0.00 0.00 90.00 50 3 \w -100.00 -75.00 0.50 0.06 -- 0.00 0.00 -60.00 50 4 \w -100.00 -75.00 0.50 0.06 -- 0.00 0.00-120.00 50 5 \w -100.00 -75.00 0.50 0.06 -- 0.00 0.00-180.00 50 6 \w -37.00 16.00 0.50 0.22 -- 55.62 -19.00-150.00 106 7 \w 27.00 58.00 0.50 0.22 -- 111.23 -50.00-180.00 62 8 \w 49.00 78.00 0.50 0.22 -- 111.23 -63.00-180.00 58 9 \w 29.00 58.00 0.50 0.22 -- 111.23 -50.00 -90.00 58 10 \w 27.00 54.00 0.50 0.22 -- 111.23 -50.00 60.00 54 11 \w 27.00 54.00 0.50 0.22 -- 111.23 -50.00 -30.00 54 12 \w 29.00 57.00 0.50 0.22 -- 111.23 -50.00 -60.00 56 13 \w 33.00 58.00 0.50 0.22 -- 111.23 -50.00 90.00 50 14 \w 46.00 71.00 0.50 0.22 -- 111.23 -63.00 120.00 50 15 \w 30.00 57.00 0.50 0.22 -- 111.23 -50.00 150.00 54 16 \w 65.00 90.00 0.50 0.22 -- 111.23 -86.00 119.00 50 17 \w 29.00 106.00 0.50 0.22 -- 111.23-111.00 90.00 154 18 \w 40.00 85.00 0.50 0.22 -- 55.62-125.00 0.00 90 19 \w 83.00 151.00 0.50 0.22 -- 111.23-178.00 30.00 136 20 \w 69.00 108.00 0.50 0.22 -- 111.23-111.00 30.00 78 21 \w 32.00 90.00 0.50 0.22 -- 111.23-111.00 0.00 116 22 \w 64.00 107.00 0.50 0.22 -- 111.23-111.00-180.00 86 23 \w 28.00 53.00 0.50 0.22 -- 111.23-111.00-180.00 50 24 \w 6.00 105.00 0.50 0.22 -- 55.62 -99.00 0.00 198 25 \w 13.00 43.00 0.50 0.06 -- 0.00 -86.00 119.00 60 26 \w -17.00 59.00 0.50 0.22 -- 55.62 -86.00 119.00 152 27 \w 115.00 153.00 0.50 0.22 -- 111.23 0.00 30.00 76 28 \w 147.00 176.00 0.50 0.22 -- 111.23 0.00 60.00 58 29 \w 107.00 134.00 0.50 0.22 -- 55.62 0.00 -30.00 54 30 \w 111.00 136.00 0.50 0.22 -- 55.62 0.00 -60.00 50 31 \w 112.00 137.00 0.50 0.22 -- 55.62 0.00 -90.00 50 32 \w 108.00 133.00 0.50 0.22 -- 55.62 0.00-150.00 50 33 \w 112.00 174.00 0.50 0.22 -- 111.23 0.00 -30.00 124 34 \w 140.00 172.00 0.50 0.22 -- 111.23 86.00-122.00 64 35 \w 115.00 144.00 0.50 0.22 -- 111.23 178.00 0.00 58 36 \w 64.00 108.00 0.50 0.22 -- 111.23 178.00 0.00 88 37 \w 65.00 127.00 0.50 0.22 -- 111.23 178.00 120.00 124 38 \w 18.00 43.00 0.50 0.06 -- 0.00 86.00-122.00 50 39 \w -21.00 6.00 0.50 0.06 -- 0.00 86.00-122.00 54 40 \w -52.00 -25.00 0.50 0.22 -- -106.00 50.00-180.00 54 41 \w -51.00 -24.00 0.50 0.22 -- -106.00 50.00-150.00 54 42 \w -52.00 -23.00 0.50 0.22 -- -106.00 50.00-120.00 58 43 \w -11.00 23.00 0.50 0.22 -- -55.62 19.00-150.00 68 44 \w -17.00 8.00 0.50 0.22 -- -55.62 19.00 -30.00 50 45 \w -52.00 -27.00 0.50 0.22 -- -106.00 50.00 90.00 50 46 \w -15.00 16.00 0.50 0.22 -- -55.62 19.00 150.00 62 47 \w -35.00 25.00 0.50 0.22 -- -55.62 37.00 60.00 120 48 \w -11.00 16.00 0.50 0.22 -- -55.62 19.00 0.00 54 49 \w -131.00 -74.00 0.50 0.22 -- -106.00 0.00-180.00 114 50 \w -165.00-134.00 0.50 0.22 -- -106.00 0.00-180.00 62 51 \w -100.00 -61.00 0.50 0.22 -- -106.00 86.00-122.00 78 52 \w -69.00 -7.00 0.50 0.22 -- -55.62 86.00-122.00 124 53 \w -146.00-119.00 0.50 0.22 -- -106.00 86.00-122.00 54 54 \w -172.00 -83.00 0.50 0.22 -- -106.00-111.00 150.00 178 55 \w -92.00 -41.00 0.50 0.22 -- -106.00-178.00 -30.00 102 56 \w -126.00 -98.00 0.50 0.22 -- -106.00-178.00 -30.00 56 57 \w -117.00 -90.00 0.50 0.22 -- -106.00-111.00-180.00 54 58 \w -131.00-104.00 0.50 0.22 -- -55.62 -99.00 -90.00 54 59 \w -145.00 -88.00 0.50 0.22 -- -55.62 -99.00 30.00 114 60 \w -127.00 -97.00 0.50 0.22 -- -55.62 -86.00 119.00 60 61 \w -123.00 -80.00 0.50 0.22 -- -106.00 -86.00 119.00 86 62 \w -165.00-131.00 0.50 0.22 -- -106.00 -86.00 119.00 68 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_unetI/netI 0.0249 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4755 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.250 _diffrn_reflns_theta_min 5.702 _exptl_absorpt_coefficient_mu 1.080 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.72007 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.142a (Rigaku Oxford Diffraction, 2024) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.553 _exptl_crystal_description plate _exptl_crystal_F_000 352 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.296 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.069 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 141 _refine_ls_number_reflns 1307 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.077 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0477 _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^)+(0.0971P)^2^+0.1225P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1378 _refine_ls_wR_factor_ref 0.1472 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1157 _reflns_number_total 1307 _reflns_threshold_expression 'I > 2\s(I)' _journal_article_reference uoaf059 _cod_data_source_file Lab-Poly-1.cif _cod_data_source_block poly1 _cod_depositor_comments ;Re-refinement of the structure. Hydrogen atoms were located from difference Fourier maps and refined, replacing the previous riding model (AFIX) treatment. Releasing structure 3000589 into public domain as published material. ; _cod_database_code 3000589 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.900 _shelx_estimated_absorpt_t_min 0.724 _olex2_refinement_description ; ; _shelx_res_file ; TITL exp_54_auto_a.res in P2(1)/n poly1.res created by SHELXL-2018/3 at 18:45:11 on 03-Jun-2025 REM Old TITL exp_54_auto in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.140, Rweak 0.522, Alpha 0.016, Orientation as input REM Formula found by SHELXT: C6 O9 CELL 1.54184 8.7157 6.7991 12.3904 90 101.692 90 ZERR 2 0.0005 0.0003 0.0007 0 0.006 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O UNIT 32 32 16 L.S. 10 PLAN 5 SIZE 0.1 0.2 0.32 TEMP -173.15 CONF BOND $H MORE -1 fmap 2 acta SHEL 99 0.83 REM REM REM WGHT 0.097100 0.122500 FVAR 1.20919 O10 3 0.764292 0.337288 0.515034 11.00000 0.05647 0.04279 = 0.04643 0.00236 0.01507 0.00235 O11 3 0.443585 0.487018 0.291488 11.00000 0.06169 0.04277 = 0.03804 -0.00018 0.01432 -0.00195 O12 3 0.690877 0.599263 0.329873 11.00000 0.05840 0.04864 = 0.03828 0.00018 0.01926 -0.00213 O9 3 0.825179 0.629820 0.595099 11.00000 0.05625 0.05699 = 0.04761 -0.00846 0.01413 -0.00040 C7 1 0.556343 0.541705 0.356526 11.00000 0.05457 0.03652 = 0.03961 0.00060 0.01721 0.00209 C1 1 0.530764 0.795817 0.491872 11.00000 0.05448 0.04160 = 0.03962 0.00122 0.01832 -0.00096 C5 1 0.732463 0.521819 0.539736 11.00000 0.05706 0.04534 = 0.03598 0.00043 0.01930 -0.00127 C3 1 0.544439 1.094560 0.599164 11.00000 0.05743 0.04413 = 0.03732 -0.00304 0.01671 -0.00347 C4 1 0.563289 0.572826 0.480459 11.00000 0.05615 0.04173 = 0.03589 -0.00046 0.01607 -0.00101 C2 1 0.575011 0.896055 0.591668 11.00000 0.05565 0.04349 = 0.03791 0.00178 0.01613 -0.00139 C8 1 0.688845 0.606827 0.212182 11.00000 0.06645 0.05324 = 0.03882 0.00092 0.02213 -0.00095 C6 1 0.914034 0.258407 0.569813 11.00000 0.05802 0.05769 = 0.04719 0.00721 0.01662 0.00842 H2 2 0.624436 0.827864 0.655711 11.00000 0.04619 H3 2 0.577752 1.159416 0.671097 11.00000 0.05044 H8A 2 0.791574 0.655744 0.207329 11.00000 0.04313 H8B 2 0.669776 0.471917 0.181767 11.00000 0.05033 H6A 2 0.930261 0.297357 0.644999 11.00000 0.06865 H6B 2 0.903247 0.114313 0.564086 11.00000 0.05462 H8C 2 0.603664 0.699552 0.177652 11.00000 0.05329 H6C 2 1.000757 0.289566 0.533614 11.00000 0.05909 HKLF 4 REM exp_54_auto_a.res in P2(1)/n REM wR2 = 0.1472, GooF = S = 1.077, Restrained GooF = 1.077 for all data REM R1 = 0.0477 for 1157 Fo > 4sig(Fo) and 0.0541 for all 1307 data REM 141 parameters refined using 0 restraints END WGHT 0.0971 0.1225 REM Highest difference peak 0.296, deepest hole -0.202, 1-sigma level 0.069 Q1 1 0.5000 0.5000 0.5000 10.50000 0.05 0.30 Q2 1 0.6434 0.5652 0.4923 11.00000 0.05 0.26 Q3 1 0.4444 0.7909 0.4560 11.00000 0.05 0.24 Q4 1 0.3575 0.4701 0.2253 11.00000 0.05 0.23 Q5 1 0.5474 0.8908 0.4536 11.00000 0.05 0.22 ; _shelx_res_checksum 90718 _shelx_hkl_file ; 0 0 1 3.42 0.63 0 0 2 5695.62 91.92 0 0 3 1.86 1.28 0 0 -4 156.73 3.48 0 0 -5 3.09 0.77 0 0 -6 533.46 11.63 0 0 -7 -0.30 1.07 0 0 -7 0.57 1.09 0 0 -8 12.51 1.87 0 0 -8 15.08 2.14 0 0 -9 0.07 1.26 0 0 -10 543.78 14.95 0 0 -11 -0.15 1.29 0 0 -11 0.16 0.90 0 0 -12 37.56 3.53 0 0 -13 1.65 1.13 0 0 -14 11.17 1.82 0 1 0 1.75 0.86 0 -1 -1 5670.17 90.83 0 1 -1 5684.39 91.61 0 -1 2 409.65 10.16 0 1 2 431.57 10.42 0 -1 3 3.30 0.71 0 -1 -3 2.82 0.67 0 -1 -4 201.77 8.46 0 -1 -4 200.44 4.84 0 -1 -4 197.57 4.53 0 -1 4 209.66 5.18 0 -1 -4 198.88 4.96 0 -1 4 203.47 4.36 0 -1 -5 2003.44 33.63 0 -1 5 2062.19 33.42 0 -1 5 2137.60 34.83 0 -1 -5 2050.53 34.28 0 -1 -6 159.97 4.57 0 -1 -6 169.01 5.16 0 -1 -7 305.05 7.86 0 -1 -7 280.83 6.87 0 -1 7 300.39 6.78 0 -1 -8 1023.22 20.29 0 1 -9 38.71 4.12 0 1 -10 4.24 1.49 0 1 -10 3.88 1.57 0 -1 -10 3.15 1.17 0 1 -10 2.31 1.70 0 -1 -10 5.32 1.53 0 -1 -11 38.93 2.75 0 1 -11 36.33 3.37 0 -1 -11 42.39 3.48 0 -1 -12 9.70 1.56 0 -1 -12 11.67 2.01 0 1 -12 9.99 1.90 0 1 -13 1.32 1.24 0 -1 -13 1.95 0.95 0 -1 -13 0.95 1.23 0 -1 -14 20.23 2.26 0 1 -14 14.55 2.18 0 2 0 1874.91 35.13 0 2 0 1818.99 33.46 0 2 -1 1185.98 24.09 0 -2 -1 1304.62 25.33 0 2 -1 1229.10 25.65 0 -2 -1 1306.98 25.04 0 -2 1 1195.31 25.36 0 2 -1 1147.41 19.99 0 -2 -1 1254.05 20.56 0 2 -2 2037.19 33.47 0 -2 -2 2169.11 38.77 0 -2 -3 496.97 10.32 0 -2 -3 505.40 9.49 0 -2 -4 103.34 3.22 0 -2 -4 96.51 3.34 0 -2 -5 84.15 3.14 0 -2 5 84.46 3.65 0 -2 -5 85.04 3.20 0 -2 -5 79.67 3.04 0 -2 -5 82.31 3.34 0 -2 -6 8.54 1.37 0 -2 -6 10.73 1.47 0 -2 -6 7.80 1.47 0 -2 6 5.83 1.55 0 -2 -7 1050.01 19.36 0 -2 7 1001.64 21.20 0 -2 -7 1049.61 20.30 0 -2 -7 1041.89 19.90 0 -2 -8 44.50 3.32 0 -2 -8 43.99 2.92 0 -2 8 46.07 3.68 0 -2 -9 107.00 5.77 0 -2 -9 121.81 5.57 0 2 -9 118.79 8.70 0 2 -9 116.48 5.35 0 2 -10 -0.60 1.76 0 -2 10 1.46 2.14 0 -2 -10 1.52 1.25 0 2 -10 0.98 1.25 0 -2 -10 0.41 1.37 0 2 -10 1.94 1.43 0 2 -11 1.97 1.25 0 -2 -11 0.34 1.21 0 2 -11 -0.07 1.17 0 -2 11 -1.55 2.58 0 -2 -12 148.65 5.44 0 -2 -12 166.36 6.67 0 2 -13 3.25 1.17 0 -2 -13 4.53 1.15 0 -2 -14 9.60 1.20 0 2 -14 7.12 1.36 0 -3 0 1.89 0.69 0 3 1 44.11 2.21 0 -3 -1 49.02 2.55 0 3 1 45.23 1.78 0 -3 1 45.33 1.99 0 3 -2 0.85 0.80 0 -3 -2 0.68 0.81 0 -3 2 -0.21 1.16 0 -3 -2 1.96 1.25 0 -3 3 364.19 9.60 0 -3 -3 373.26 9.62 0 3 -3 382.95 8.35 0 -3 -4 566.35 11.28 0 -3 -4 537.16 12.48 0 3 -4 550.70 11.57 0 -3 -5 382.94 9.28 0 3 -5 389.38 9.24 0 -3 -5 379.53 8.75 0 -3 6 155.03 6.27 0 3 -6 170.66 5.93 0 -3 -6 168.52 5.99 0 3 -7 103.89 4.81 0 -3 -7 105.03 4.91 0 3 -8 602.01 14.82 0 -3 8 612.46 16.28 0 -3 -8 646.12 14.15 0 -3 -8 639.29 15.09 0 -3 -8 556.44 15.60 0 3 -8 595.69 20.23 0 -3 -9 7.13 1.47 0 -3 -9 8.89 1.91 0 -3 -9 8.09 1.97 0 -3 -9 7.53 1.87 0 3 -9 6.55 3.14 0 -3 9 12.24 3.38 0 3 -9 10.45 1.95 0 -3 -10 0.70 1.03 0 -3 10 -1.78 2.72 0 3 -10 2.66 2.36 0 -3 -10 0.17 1.15 0 -3 11 107.64 8.43 0 -3 -11 102.06 4.54 0 3 -11 93.47 8.27 0 3 -11 81.08 5.13 0 -3 12 7.80 2.73 0 -3 -12 11.42 1.60 0 3 -12 8.22 1.63 0 -3 -13 2.66 1.10 0 -4 0 510.85 10.34 0 -4 0 490.71 11.73 0 -4 -1 65.75 2.73 0 -4 -1 55.50 3.42 0 -4 1 57.78 3.95 0 -4 -1 54.79 3.90 0 -4 -2 33.99 3.23 0 -4 -2 36.41 2.05 0 -4 2 32.59 3.24 0 -4 3 0.87 1.01 0 -4 3 2.34 1.52 0 -4 -3 0.60 0.90 0 -4 -3 0.93 1.40 0 -4 -4 257.56 8.91 0 4 -4 263.93 7.59 0 4 -5 123.63 5.21 0 -4 -5 131.87 4.91 0 -4 -5 136.65 5.61 0 -4 -6 25.06 2.38 0 -4 -6 25.27 2.72 0 -4 6 22.80 2.93 0 4 -6 25.20 2.67 0 4 -7 12.58 2.22 0 -4 -7 13.46 1.98 0 -4 -7 14.66 2.33 0 -4 7 8.84 2.42 0 -4 -7 12.28 1.98 0 -4 -8 20.74 2.52 0 4 -8 21.70 4.23 0 -4 8 19.92 3.09 0 4 -8 21.66 2.81 0 -4 8 20.19 4.20 0 -4 -8 24.22 2.79 0 -4 -9 10.38 2.09 0 -4 -9 10.41 1.68 0 -4 9 12.06 3.53 0 4 -9 13.20 3.62 0 -4 -10 135.60 5.15 0 -4 10 125.26 9.78 0 -4 -10 144.31 6.03 0 4 -10 131.33 9.63 0 -4 -10 137.68 7.25 0 -4 -11 9.34 1.71 0 4 -11 9.91 3.08 0 -4 11 13.60 3.15 0 -4 -11 10.74 1.57 0 -4 12 95.75 6.47 0 -4 -12 96.96 3.78 0 -5 0 -1.09 1.50 0 -5 -1 39.83 3.98 0 -5 1 33.51 3.32 0 -5 1 41.18 4.06 0 -5 -1 41.25 2.66 0 -5 2 214.65 6.95 0 -5 -2 227.87 6.48 0 -5 -2 219.36 9.21 0 -5 2 202.69 8.92 0 -5 -3 16.77 3.01 0 -5 3 17.60 2.94 0 -5 3 19.66 2.31 0 -5 4 24.32 2.70 0 -5 -4 18.18 2.35 0 -5 -4 20.97 3.12 0 -5 -5 27.59 2.59 0 -5 -5 23.55 2.51 0 -5 5 20.73 3.10 0 -5 -6 83.39 4.69 0 -5 -6 87.48 4.87 0 -5 -6 91.18 4.73 0 -5 6 73.70 5.32 0 5 -7 365.24 15.84 0 -5 -7 376.78 10.81 0 -5 -7 344.20 10.57 0 -5 -8 12.83 2.35 0 -5 8 17.33 3.78 0 5 -8 13.12 3.77 0 -5 9 58.53 6.45 0 -5 10 9.90 3.22 0 5 -10 11.21 3.19 0 -5 -10 14.26 2.04 0 -5 11 19.31 3.45 0 -5 -11 28.09 2.26 0 -6 0 14.31 2.12 0 -6 1 7.97 2.12 0 -6 -1 5.93 2.64 0 -6 1 7.06 2.69 0 -6 1 7.53 1.77 0 -6 1 12.08 2.47 0 -6 -1 12.41 2.49 0 -6 -2 0.68 1.91 0 -6 -2 -0.16 1.34 0 -6 -2 1.80 1.95 0 -6 2 3.18 1.90 0 -6 2 2.04 1.41 0 -6 -3 81.55 4.64 0 6 3 94.02 9.94 0 6 -4 87.94 9.79 0 -6 -4 148.63 6.17 0 -6 -5 41.72 3.41 0 -6 -5 40.53 3.17 0 6 -5 27.07 5.28 0 6 -5 37.90 5.67 0 -6 6 36.20 5.34 0 -6 -6 31.61 3.01 0 6 -6 22.87 4.83 0 6 -6 25.62 4.64 0 -6 -7 79.18 5.57 0 -6 -7 72.97 4.36 0 6 -7 57.31 5.80 0 6 -7 61.73 7.02 0 -6 -7 79.13 4.74 0 -6 -8 5.87 1.45 0 6 -8 5.18 2.55 0 -6 9 2.41 2.06 0 6 -9 1.02 1.89 0 -6 -9 0.61 1.17 0 -6 10 2.10 1.68 0 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-0.40 1.27 -7 -6 2 5.95 1.80 -7 -6 2 0.77 2.28 -7 6 2 5.56 1.56 -7 -6 1 23.06 2.91 -7 -6 1 10.13 3.58 -7 6 1 24.21 4.21 -7 -6 1 13.14 2.87 -7 -6 0 9.50 3.44 -7 6 0 26.93 2.77 -7 6 -1 0.91 0.72 -8 0 12 12.01 1.18 -8 0 11 -1.06 0.91 -8 0 10 130.19 5.45 -8 0 9 -0.75 1.36 -8 0 9 2.63 1.56 -8 0 8 2.08 1.77 -8 0 7 0.29 0.98 -8 0 7 1.23 1.55 -8 0 6 21.38 2.02 -8 0 6 28.81 2.73 -8 0 5 0.66 1.14 -8 0 5 -0.48 0.99 -8 0 4 54.32 3.06 -8 0 4 61.85 3.97 -8 0 3 -1.41 1.20 -8 0 2 60.92 3.30 -8 0 2 68.20 5.93 -8 0 2 76.26 6.37 -8 0 2 68.28 6.81 -8 0 1 0.98 1.96 -8 0 1 1.30 1.72 -8 0 1 1.46 1.81 -8 0 1 -0.90 2.10 -8 0 0 592.00 18.02 -8 0 0 519.79 17.88 -8 0 0 497.62 17.92 -8 0 0 578.97 19.86 -8 0 -1 1.58 2.00 -8 0 -1 -0.51 1.17 -8 0 -1 0.92 1.68 -8 0 -1 -1.18 1.93 -8 0 -1 -0.42 2.15 -8 0 -2 54.50 3.20 -8 0 -2 51.09 5.56 -8 0 -3 -0.24 1.19 -8 0 -3 -0.40 1.95 -8 0 -4 77.28 3.49 -8 0 -4 64.41 6.08 -8 0 -5 -0.59 1.31 -8 0 -5 0.74 1.35 -8 0 -6 1.66 1.46 -8 0 -7 0.79 1.03 -8 1 11 0.52 0.90 -8 1 11 -1.10 0.85 -8 -1 11 0.97 1.08 -8 1 10 6.74 1.46 -8 1 10 6.39 1.21 -8 -1 10 5.27 1.72 -8 1 9 1.73 1.22 -8 -1 9 0.36 1.38 -8 1 9 0.07 1.09 -8 -1 9 0.38 1.58 -8 -1 8 16.19 2.23 -8 1 8 8.51 1.54 -8 -1 7 7.33 1.96 -8 -1 7 13.18 2.12 -8 -1 7 7.15 2.21 -8 -1 6 74.05 3.53 -8 1 6 91.28 4.75 -8 -1 6 84.50 5.00 -8 -1 6 111.55 5.27 -8 -1 6 103.79 5.61 -8 -1 6 73.63 5.76 -8 -1 5 24.38 3.79 -8 1 5 29.69 2.31 -8 -1 5 23.87 2.09 -8 1 5 32.70 2.80 -8 -1 5 35.67 3.15 -8 -1 5 35.80 3.43 -8 1 4 70.60 3.51 -8 -1 4 72.50 4.54 -8 -1 4 80.21 4.84 -8 -1 4 70.75 5.67 -8 1 3 12.92 1.73 -8 -1 3 10.05 2.87 -8 -1 3 11.03 1.57 -8 1 3 14.42 3.66 -8 -1 2 13.42 2.95 -8 1 2 13.20 1.69 -8 -1 2 15.01 3.06 -8 -1 2 13.07 1.72 -8 -1 2 7.91 2.81 -8 -1 1 10.96 3.03 -8 -1 1 11.55 1.76 -8 1 1 11.58 3.40 -8 -1 1 10.94 2.89 -8 1 1 14.07 2.79 -8 1 1 10.14 2.96 -8 1 1 18.18 3.38 -8 -1 1 8.48 2.83 -8 -1 0 65.88 5.71 -8 -1 0 54.74 5.59 -8 1 0 49.91 5.39 -8 1 0 58.52 5.79 -8 1 0 52.83 6.14 -8 -1 0 54.59 5.41 -8 -1 -1 5.40 2.18 -8 -1 -1 1.42 2.10 -8 -1 -1 3.95 2.06 -8 1 -1 3.05 1.90 -8 1 -1 3.83 2.42 -8 -1 -2 8.00 2.61 -8 -1 -2 5.70 1.43 -8 1 -2 8.14 2.44 -8 1 -2 6.60 2.58 -8 -1 -3 115.91 4.74 -8 -1 -3 103.36 7.86 -8 1 -3 100.25 7.78 -8 -1 -4 2.04 1.19 -8 1 -4 2.92 1.14 -8 -1 -4 1.01 1.76 -8 1 -4 2.04 1.79 -8 1 -4 6.12 2.36 -8 -1 -5 4.13 2.27 -8 1 -5 7.84 2.22 -8 1 -5 9.86 2.68 -8 -1 -6 13.99 2.62 -8 1 -6 9.75 2.62 -8 1 -7 6.07 1.93 -8 -2 11 -0.38 0.99 -8 -2 11 1.60 1.05 -8 2 10 13.83 1.44 -8 2 10 12.66 1.73 -8 -2 10 10.24 2.02 -8 2 9 3.67 1.28 -8 -2 9 4.15 1.50 -8 2 9 2.35 1.11 -8 2 8 36.24 2.46 -8 2 8 35.09 2.92 -8 -2 8 33.84 3.14 -8 -2 8 31.20 3.43 -8 2 7 154.11 5.26 -8 -2 7 160.76 6.65 -8 -2 7 145.08 6.91 -8 2 6 66.02 3.48 -8 -2 6 72.81 4.38 -8 -2 6 66.61 4.52 -8 2 6 51.36 6.40 -8 2 6 54.58 5.90 -8 -2 6 43.97 4.94 -8 -2 5 10.81 2.92 -8 2 5 11.89 1.74 -8 -2 5 12.84 2.27 -8 2 5 16.20 3.66 -8 2 5 12.35 3.19 -8 -2 4 33.90 4.71 -8 -2 4 34.05 6.01 -8 -2 4 35.71 3.47 -8 2 4 35.33 3.28 -8 2 4 39.98 5.89 -8 2 4 43.66 5.00 -8 -2 4 36.22 4.64 -8 -2 3 6.85 2.36 -8 -2 3 3.03 2.67 -8 -2 3 3.45 2.09 -8 2 3 4.41 1.56 -8 -2 3 2.69 1.21 -8 2 3 3.07 2.45 -8 2 3 4.05 2.28 -8 -2 2 1.40 2.12 -8 2 2 3.22 1.50 -8 -2 2 2.61 1.30 -8 -2 2 0.79 1.85 -8 2 2 3.98 2.32 -8 -2 1 82.97 6.73 -8 -2 1 73.58 8.33 -8 2 1 78.32 5.03 -8 -2 1 76.36 3.78 -8 -2 1 72.31 6.74 -8 2 1 84.56 8.14 -8 2 1 80.68 7.05 -8 2 1 72.26 7.39 -8 -2 1 80.07 6.84 -8 -2 0 97.54 7.21 -8 -2 0 84.57 8.64 -8 -2 0 87.98 4.18 -8 2 0 78.02 8.48 -8 -2 0 92.22 7.32 -8 2 0 88.80 6.96 -8 2 0 96.46 8.37 -8 -2 0 96.54 7.11 -8 -2 -1 -0.26 2.06 -8 2 -1 2.07 1.44 -8 2 -1 2.09 2.01 -8 2 -1 4.12 1.87 -8 2 -1 -0.42 2.05 -8 -2 -2 29.48 2.58 -8 -2 -2 29.70 4.36 -8 -2 -2 31.77 4.50 -8 2 -2 38.09 4.54 -8 2 -2 27.06 5.10 -8 -2 -3 39.13 4.77 -8 -2 -3 35.90 4.52 -8 2 -3 30.35 4.58 -8 -2 -3 30.23 4.70 -8 -2 -4 8.86 2.52 -8 -2 -4 5.18 2.48 -8 2 -4 8.17 2.79 -8 -2 -5 29.26 3.56 -8 -2 -5 23.71 3.57 -8 2 -5 22.45 3.75 -8 2 -5 20.33 4.04 -8 -2 -6 4.15 1.56 -8 2 -6 2.83 1.57 -8 2 -6 1.22 1.54 -8 -3 10 21.09 2.63 -8 -3 9 109.39 5.59 -8 -3 9 114.20 5.68 -8 -3 8 259.87 8.75 -8 -3 8 240.33 8.63 -8 3 7 48.35 2.66 -8 -3 7 44.58 3.45 -8 -3 6 0.36 1.87 -8 3 6 1.27 1.17 -8 -3 6 2.27 1.43 -8 -3 6 3.59 1.89 -8 -3 6 1.66 1.42 -8 -3 6 3.23 2.58 -8 3 6 1.21 1.95 -8 -3 5 76.15 6.20 -8 3 5 96.28 4.12 -8 -3 5 76.81 6.72 -8 -3 5 68.26 8.05 -8 -3 5 92.53 8.43 -8 3 5 83.62 8.14 -8 3 5 73.20 6.78 -8 -3 4 10.73 2.80 -8 -3 4 3.49 3.19 -8 -3 4 5.48 2.68 -8 3 4 7.64 1.68 -8 -3 4 7.45 3.20 -8 3 4 5.38 3.28 -8 3 4 9.13 2.71 -8 -3 3 2.73 2.27 -8 -3 3 0.57 2.41 -8 -3 3 -0.63 1.83 -8 3 3 2.16 1.27 -8 -3 3 2.99 2.32 -8 3 3 0.45 2.03 -8 3 3 0.10 2.07 -8 -3 2 17.75 3.93 -8 3 2 25.05 3.06 -8 3 2 23.03 4.33 -8 -3 1 3.32 2.41 -8 -3 1 3.50 2.15 -8 -3 1 3.91 2.44 -8 3 1 4.67 1.62 -8 3 1 3.49 2.32 -8 3 1 7.02 2.45 -8 -3 0 31.47 4.50 -8 -3 0 28.56 5.07 -8 3 0 33.58 5.10 -8 3 0 25.81 4.84 -8 -3 -1 1.25 2.15 -8 -3 -1 3.35 2.08 -8 -3 -1 1.98 2.25 -8 3 -1 1.81 1.45 -8 3 -1 1.88 2.33 -8 3 -1 3.66 1.73 -8 3 -1 5.19 2.49 -8 -3 -2 1.37 1.99 -8 3 -2 2.74 1.30 -8 3 -2 2.80 1.90 -8 3 -2 2.46 1.73 -8 3 -2 0.63 2.01 -8 -3 -3 4.40 1.90 -8 -3 -3 4.18 2.31 -8 3 -3 4.43 2.18 -8 3 -3 5.26 2.38 -8 3 -4 2.43 1.41 -8 3 -4 -0.10 1.55 -8 3 -5 5.78 2.10 -8 3 -6 1.13 0.87 -8 -4 8 57.61 2.94 8 -4 -8 31.01 2.88 -8 -4 7 10.46 2.32 8 -4 -7 8.35 1.73 -8 -4 6 10.10 2.87 -8 -4 6 7.70 2.62 -8 4 6 11.48 3.17 -8 -4 5 -0.71 2.13 -8 -4 5 1.66 1.77 -8 -4 5 3.76 2.18 -8 4 5 1.86 1.86 -8 -4 4 4.41 2.92 -8 -4 4 5.01 2.42 -8 4 4 9.30 1.72 -8 -4 4 9.94 2.85 -8 4 4 5.48 2.89 -8 -4 3 2.43 1.74 -8 -4 3 3.66 2.05 -8 4 3 0.35 1.11 -8 -4 3 0.87 1.89 -8 4 3 -0.79 1.81 -8 4 2 9.49 2.05 -8 -4 1 2.33 1.93 -8 -4 1 3.02 2.25 -8 4 1 5.00 2.01 -8 -4 0 16.77 3.66 -8 -4 0 18.74 4.19 -8 4 0 24.28 2.89 -8 4 0 24.91 4.41 -8 4 0 25.78 4.40 -8 -4 -1 41.60 5.32 -8 -4 -1 44.38 5.85 -8 4 -1 63.98 4.48 -8 4 -1 54.32 6.22 -8 4 -1 63.10 6.82 -8 -4 -2 0.32 1.47 -8 4 -2 0.77 0.99 -8 4 -2 1.37 1.22 -8 4 -2 1.20 1.55 -8 4 -3 12.01 2.57 -8 4 -3 3.61 2.66 -8 4 -4 6.29 1.97 -8 -5 6 1.46 1.26 -8 -5 5 1.33 1.82 -8 -5 5 0.05 1.75 8 -5 -5 4.55 1.31 -8 -5 4 4.69 2.43 -8 5 4 11.52 1.60 -8 5 4 8.32 2.87 8 -5 -4 11.72 1.59 -8 -5 3 9.43 2.99 -8 -5 3 10.54 3.39 -8 5 3 21.09 2.43 -8 5 3 21.93 4.19 8 -5 -3 22.23 1.99 -8 -5 2 12.75 2.93 -8 5 2 23.12 2.54 -8 -5 1 2.96 1.70 -8 -5 1 1.72 1.85 -8 5 1 0.96 1.79 -8 -5 0 -0.25 1.29 -8 -5 0 1.12 1.43 -8 5 0 0.38 0.97 -8 5 0 -0.15 1.38 -8 5 -1 0.33 0.79 -9 0 9 0.22 1.07 -9 0 9 1.54 0.83 -9 0 8 0.86 1.07 -9 0 8 0.32 1.07 -9 0 8 -0.49 0.95 -9 0 7 11.75 1.52 -9 0 7 12.50 2.00 -9 0 6 3.12 1.61 -9 0 6 -0.14 1.15 -9 0 6 -0.10 0.97 -9 0 5 95.17 3.81 -9 0 5 80.35 6.80 -9 0 4 0.19 1.75 -9 0 4 -0.43 1.02 -9 0 3 19.55 1.80 -9 0 3 18.48 1.80 -9 0 3 20.22 3.53 -9 0 2 -0.78 1.09 -9 0 2 1.01 1.73 -9 0 1 8.17 2.82 -9 0 1 12.32 1.66 -9 0 1 10.89 2.74 -9 0 1 8.65 2.85 -9 0 0 -0.10 1.52 -9 0 -1 88.55 3.92 -9 0 -1 85.85 6.77 -9 0 -1 97.04 6.24 -9 0 -2 0.69 1.00 -9 0 -2 1.09 1.42 -9 0 -3 21.06 1.81 -9 0 -4 0.02 0.80 -9 0 -4 0.28 1.12 -9 0 -5 5.49 1.77 -9 1 10 1.36 0.77 -9 -1 10 2.16 0.72 -9 1 9 1.40 1.48 -9 1 9 -0.08 0.88 -9 -1 9 1.60 1.08 -9 -1 9 1.92 0.79 -9 -1 8 41.44 2.20 -9 1 8 29.73 4.22 -9 1 7 10.19 2.72 -9 -1 7 10.67 1.31 -9 1 7 10.03 1.81 -9 1 6 59.62 3.06 -9 -1 6 53.42 2.60 -9 1 6 67.06 3.73 -9 1 6 45.44 5.24 -9 -1 6 46.34 4.43 -9 -1 5 0.89 1.68 -9 1 5 1.12 1.03 -9 1 5 0.55 1.14 -9 1 5 -0.28 1.81 -9 -1 4 10.28 3.05 -9 -1 4 14.73 3.00 -9 1 4 17.25 1.83 -9 -1 3 4.31 2.37 -9 -1 3 7.44 1.35 -9 -1 3 3.85 2.30 -9 -1 2 46.60 4.97 -9 -1 2 48.30 2.82 -9 -1 2 40.85 4.77 -9 1 2 50.68 5.47 -9 -1 2 42.21 4.80 -9 -1 1 21.28 3.50 -9 -1 1 16.73 3.49 -9 -1 1 18.70 1.91 -9 -1 1 14.36 3.33 -9 1 1 19.56 3.69 -9 1 1 18.20 3.66 -9 -1 0 13.87 2.88 -9 -1 0 11.14 2.87 -9 -1 0 10.78 2.66 -9 1 0 11.08 2.67 -9 1 0 9.58 3.04 -9 -1 -1 2.63 2.05 -9 -1 -1 3.42 2.16 -9 1 -1 4.28 1.24 -9 -1 -1 5.23 2.08 -9 1 -1 3.30 1.88 -9 1 -1 0.68 1.97 -9 -1 -2 4.68 1.22 -9 1 -2 2.57 1.11 -9 1 -2 3.49 1.85 -9 1 -2 1.49 2.04 -9 1 -3 26.81 3.87 -9 -1 -3 19.83 3.97 -9 1 -4 31.76 1.76 -9 -1 -4 15.83 3.15 -9 -1 -5 5.77 1.68 -9 1 -5 3.82 1.63 -9 2 9 10.61 1.23 -9 2 9 6.13 1.47 -9 2 8 25.05 1.98 -9 -2 8 30.65 2.31 -9 2 8 23.81 3.10 -9 2 7 14.27 1.71 -9 2 7 15.43 2.06 -9 -2 7 18.99 1.96 -9 -2 6 72.85 5.54 -9 2 6 86.71 6.90 -9 -2 5 7.09 2.42 -9 2 5 9.03 1.63 -9 2 5 6.32 2.49 -9 -2 4 66.72 6.02 -9 -2 4 59.90 6.28 -9 -2 3 80.40 6.94 -9 2 3 102.79 7.71 -9 -2 3 93.94 7.01 -9 -2 2 15.56 3.30 -9 2 2 13.44 3.47 -9 -2 1 5.80 2.25 -9 -2 1 3.50 2.26 -9 2 1 0.75 2.10 -9 -2 0 50.80 4.78 -9 -2 0 32.25 4.75 -9 2 0 45.40 4.58 -9 2 0 37.52 5.11 -9 -2 -1 11.22 2.54 -9 -2 -1 7.20 2.65 -9 2 -1 10.44 2.41 -9 2 -1 7.26 2.78 -9 2 -2 15.20 1.56 -9 -2 -2 8.05 2.74 -9 2 -2 8.76 2.67 -9 2 -2 7.69 2.85 -9 2 -3 4.31 1.00 -9 2 -3 3.43 1.60 -9 2 -4 1.65 1.15 -9 3 7 3.73 1.23 -9 3 6 13.51 1.66 -9 -3 5 8.22 2.31 -9 3 5 13.20 1.66 -9 -3 5 10.29 2.28 -9 -3 4 16.44 3.83 -9 -3 4 28.45 4.01 -9 -3 3 9.03 3.22 -9 -3 3 10.86 3.19 -9 3 3 12.72 3.93 -9 -3 2 8.33 3.49 -9 -3 1 99.25 7.27 -9 -3 1 82.21 7.33 -9 -3 0 8.11 2.52 -9 3 0 7.38 2.72 -9 -3 -1 9.13 2.85 -9 3 -1 10.81 3.10 -9 3 -2 6.06 1.92 -9 3 -2 4.53 2.13 -9 -4 5 0.44 1.13 -9 -4 4 1.89 1.46 -9 -4 3 16.12 3.64 -9 4 3 27.22 5.17 -9 -4 2 5.99 2.21 -9 -4 0 3.67 1.62 -10 0 8 6.30 1.95 -10 0 7 0.50 0.68 -10 0 6 14.15 2.28 -10 0 6 8.30 2.69 -10 0 5 -1.44 1.47 -10 0 5 0.13 1.37 -10 0 4 0.12 1.61 -10 0 4 1.60 1.63 -10 0 3 -0.47 1.38 -10 0 3 0.11 0.78 -10 0 3 -0.07 1.39 -10 0 2 0.47 1.38 -10 0 2 0.22 0.83 -10 0 1 -0.82 1.53 -10 0 1 -0.12 0.84 -10 0 1 2.78 1.33 -10 0 0 40.25 3.82 -10 0 0 42.23 3.69 -10 0 -1 1.65 1.25 -10 0 -2 56.60 2.55 -10 0 -2 44.77 4.30 -10 1 7 2.63 1.58 -10 -1 7 0.84 1.39 -10 1 6 6.54 1.84 -10 -1 6 10.26 1.96 -10 1 6 4.56 2.37 -10 -1 6 6.74 2.11 -10 1 5 10.80 2.47 -10 -1 5 11.32 2.49 -10 1 5 11.19 2.89 -10 -1 5 12.96 2.49 -10 1 4 5.36 2.04 -10 -1 4 2.95 2.07 -10 -1 4 2.28 1.89 -10 1 3 18.85 1.46 -10 -1 3 13.14 2.47 -10 1 2 10.62 2.53 -10 -1 2 8.91 2.52 -10 1 2 13.84 1.39 -10 1 1 0.05 1.32 -10 -1 1 0.21 1.46 -10 1 1 0.75 0.82 -10 1 0 0.72 1.19 -10 -1 0 0.88 1.38 -10 1 -1 31.76 2.10 -10 1 -1 29.84 3.35 -10 2 6 3.63 2.03 -10 -2 5 18.42 3.08 -10 -2 4 2.39 1.81 -10 -2 3 0.79 1.37 -10 2 3 2.25 0.79 -10 -2 2 -1.13 1.45 -10 -2 2 -1.28 1.49 -10 2 2 -0.40 0.83 -10 -2 1 29.45 3.66 -10 2 1 43.97 2.27 -10 2 -1 0.12 0.59 0 0 0 0.00 0.00 TITL exp_54_auto in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 8.715683 6.799131 12.390389 90.0000 101.6920 90.0000 ZERR 2.00 0.000500 0.000341 0.000718 0.0000 0.0056 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H O UNIT 32.00 36.00 16.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 86028 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 O10 O 0.76429(17) 0.3373(2) 0.51503(12) 0.0479(4) Uani 1 1 d . . . . . O11 O 0.44359(17) 0.4870(2) 0.29149(10) 0.0469(4) Uani 1 1 d . . . . . O12 O 0.69088(18) 0.5993(2) 0.32987(11) 0.0471(4) Uani 1 1 d . . . . . O9 O 0.82518(18) 0.6298(2) 0.59510(12) 0.0531(5) Uani 1 1 d . . . . . C7 C 0.5563(2) 0.5417(3) 0.35653(16) 0.0425(5) Uani 1 1 d . . . . . C1 C 0.5308(2) 0.7958(3) 0.49187(16) 0.0440(5) Uani 1 1 d . . . . . C5 C 0.7325(2) 0.5218(3) 0.53974(15) 0.0447(5) Uani 1 1 d . . . . . C3 C 0.5444(2) 1.0946(3) 0.59916(16) 0.0453(5) Uani 1 1 d . . . . . C4 C 0.5633(2) 0.5728(3) 0.48046(15) 0.0436(5) Uani 1 1 d . . . . . C2 C 0.5750(3) 0.8961(3) 0.59167(17) 0.0447(5) Uani 1 1 d . . . . . C8 C 0.6888(3) 0.6068(4) 0.21218(17) 0.0512(6) Uani 1 1 d . . . . . C6 C 0.9140(3) 0.2584(4) 0.5698(2) 0.0535(6) Uani 1 1 d . . . . . H2 H 0.624(3) 0.828(3) 0.656(2) 0.046(6) Uiso 1 1 d . . . . . H3 H 0.578(3) 1.159(3) 0.671(2) 0.050(6) Uiso 1 1 d . . . . . H8A H 0.792(3) 0.656(3) 0.2073(18) 0.043(6) Uiso 1 1 d . . . . . H8B H 0.670(3) 0.472(4) 0.182(2) 0.050(6) Uiso 1 1 d . . . . . H6A H 0.930(3) 0.297(4) 0.645(3) 0.069(8) Uiso 1 1 d . . . . . H6B H 0.903(3) 0.114(4) 0.564(2) 0.055(7) Uiso 1 1 d . . . . . H8C H 0.604(3) 0.700(4) 0.178(2) 0.053(6) Uiso 1 1 d . . . . . H6C H 1.001(3) 0.290(4) 0.534(2) 0.059(7) 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 O10 0.0565(9) 0.0428(8) 0.0464(8) 0.0024(6) 0.0151(6) 0.0024(6) O11 0.0617(9) 0.0428(8) 0.0380(8) -0.0002(6) 0.0143(7) -0.0020(6) O12 0.0584(9) 0.0486(9) 0.0383(8) 0.0002(6) 0.0193(6) -0.0021(6) O9 0.0563(9) 0.0570(10) 0.0476(8) -0.0085(7) 0.0141(7) -0.0004(7) C7 0.0546(11) 0.0365(10) 0.0396(10) 0.0006(8) 0.0172(9) 0.0021(8) C1 0.0545(12) 0.0416(11) 0.0396(10) 0.0012(8) 0.0183(9) -0.0010(8) C5 0.0571(12) 0.0453(11) 0.0360(9) 0.0004(8) 0.0193(9) -0.0013(9) C3 0.0574(12) 0.0441(11) 0.0373(10) -0.0030(8) 0.0167(9) -0.0035(9) C4 0.0561(12) 0.0417(11) 0.0359(10) -0.0005(8) 0.0161(8) -0.0010(9) C2 0.0557(11) 0.0435(11) 0.0379(10) 0.0018(8) 0.0161(8) -0.0014(8) C8 0.0664(15) 0.0532(13) 0.0388(11) 0.0009(9) 0.0221(10) -0.0010(11) C6 0.0580(13) 0.0577(15) 0.0472(11) 0.0072(10) 0.0166(10) 0.0084(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 '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 C5 O10 C6 116.80(18) . . C7 O12 C8 115.07(17) . . O11 C7 O12 124.41(17) . . O11 C7 C4 125.13(17) . . O12 C7 C4 110.27(17) . . C3 C1 C4 120.70(18) 3_676 . C2 C1 C3 117.01(19) . 3_676 C2 C1 C4 122.28(18) . . O10 C5 C4 108.93(17) . . O9 C5 O10 124.0(2) . . O9 C5 C4 126.94(19) . . C1 C3 H3 119.7(14) 3_676 . C2 C3 C1 122.08(19) . 3_676 C2 C3 H3 118.2(14) . . C7 C4 C1 104.71(15) . . C7 C4 C5 106.48(15) . . C7 C4 C4 108.74(19) . 3_666 C1 C4 C4 114.80(19) . 3_666 C5 C4 C1 110.44(17) . . C5 C4 C4 111.1(2) . 3_666 C1 C2 H2 120.1(14) . . C3 C2 C1 120.9(2) . . C3 C2 H2 119.0(14) . . O12 C8 H8A 104.5(14) . . O12 C8 H8B 108.3(14) . . O12 C8 H8C 107.9(14) . . H8A C8 H8B 112.3(19) . . H8A C8 H8C 112(2) . . H8B C8 H8C 112(2) . . O10 C6 H6A 107.3(17) . . O10 C6 H6B 105.7(14) . . O10 C6 H6C 114.4(15) . . H6A C6 H6B 110(2) . . H6A C6 H6C 114(2) . . H6B C6 H6C 105(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O10 C5 1.334(3) . O10 C6 1.447(3) . O11 C7 1.197(2) . O12 C7 1.339(2) . O12 C8 1.456(2) . O9 C5 1.199(3) . C7 C4 1.539(3) . C1 C3 1.399(3) 3_676 C1 C4 1.554(3) . C1 C2 1.396(3) . C5 C4 1.548(3) . C3 C2 1.382(3) . C3 H3 0.98(3) . C4 C4 1.628(4) 3_666 C2 H2 0.94(2) . C8 H8A 0.97(2) . C8 H8B 0.99(3) . C8 H8C 1.00(3) . C6 H6A 0.95(3) . C6 H6B 0.99(3) . C6 H6C 0.98(3) . 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 O10 C5 C4 C7 -57.9(2) . . . . O10 C5 C4 C1 -171.01(14) . . . . O10 C5 C4 C4 60.4(2) . . . 3_666 O11 C7 C4 C1 -95.7(2) . . . . O11 C7 C4 C5 147.3(2) . . . . O11 C7 C4 C4 27.5(3) . . . 3_666 O12 C7 C4 C1 79.48(19) . . . . O12 C7 C4 C5 -37.5(2) . . . . O12 C7 C4 C4 -157.36(19) . . . 3_666 O9 C5 C4 C7 118.9(2) . . . . O9 C5 C4 C1 5.7(3) . . . . O9 C5 C4 C4 -122.9(2) . . . 3_666 C1 C3 C2 C1 -0.3(3) 3_676 . . . C3 C1 C4 C7 20.7(2) 3_676 . . . C3 C1 C4 C5 134.96(19) 3_676 . . . C3 C1 C4 C4 -98.5(2) 3_676 . . 3_666 C3 C1 C2 C3 0.3(3) 3_676 . . . C4 C1 C2 C3 179.98(18) . . . . C2 C1 C4 C7 -158.96(18) . . . . C2 C1 C4 C5 -44.7(2) . . . . C2 C1 C4 C4 81.9(3) . . . 3_666 C8 O12 C7 O11 4.8(3) . . . . C8 O12 C7 C4 -170.43(17) . . . . C6 O10 C5 O9 7.6(3) . . . . C6 O10 C5 C4 -175.53(16) . . . . loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code _cod_related_entry_description 1 XRDa 00330 DOI:10.51093/xrd-00330