#------------------------------------------------------------------------------ #$Date: 2025-07-29 05:11:57 +0100 (Tue, 29 Jul 2025) $ #$Revision: 301393 $ #$URL: svn://www.crystallography.net/cod/cif/3/00/05/3000590.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_3000590 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 _audit_creation_date 2025-06-02 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _cell_angle_alpha 90 _cell_angle_beta 101.633(15) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.7562(16) _cell_length_b 6.8045(10) _cell_length_c 12.4297(19) _cell_measurement_reflns_used 1370 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.78850802421852 _cell_measurement_theta_min 3.747674960567056 _cell_volume 725.4(2) _computing_cell_refinement 'dials.two_theta_refine (Waterman et al., 2016)' _computing_data_collection ; ZOO (Hirata et al., 2019) BSS (Ueno et al., 2005) SHIKA (Barty et al., 2014) KUMA (Hirata et al., 2016) ; _computing_data_reduction 'dials.scale (Beilsten-Edmands et al., 2020)' _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 (Sheldrick, 2015)' _diffrn_ambient_temperature 100.15 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'EIGER2 16M XE' _diffrn_measurement_method 'Multiple small-wedge' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.700 _diffrn_reflns_av_R_equivalents 0.1363 _diffrn_reflns_av_unetI/netI 0.1008 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 11763 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 24.835 _diffrn_reflns_theta_max 27.815 _diffrn_reflns_theta_min 2.575 _exptl_absorpt_coefficient_mu 0.121 _exptl_crystal_colour 'clear yellowish yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.540 _exptl_crystal_description block _exptl_crystal_F_000 352 _refine_diff_density_max 0.402 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.088 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 141 _refine_ls_number_reflns 1788 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.958 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0700 _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^)+(0.1083P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1805 _refine_ls_wR_factor_ref 0.1898 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1056 _reflns_number_total 1788 _reflns_threshold_expression 'I > 2\s(I)' _journal_article_reference uoaf059 _cod_data_source_file SWSX-poly1.cif _cod_data_source_block poly-1-SWSX _cod_depositor_comments ;The structure was re-refined with the inclusion of unit cell parameter ESDs. Releasing structure 3000590 into public domain as published material. ; _cod_original_cell_volume 725.4 _cod_database_code 3000590 _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 ItoMie in P21/n #14 poly-1-swsx.res created by SHELXL-2018/3 at 13:12:24 on 02-Jun-2025 REM Best SHELXD solution FINAL CC 90.11 REM Fragments: 12 CELL 0.7 8.7562 6.8045 12.4297 90 101.633 90 ZERR 2 0.0016 0.001 0.0019 0 0.015 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O DISP C 0.003 0.0016 11.1819 DISP H 0 0 0.6234 DISP O 0.0105 0.0059 31.3712 UNIT 32 32 16 L.S. 4 0 0 PLAN 5 TEMP -173 CONF MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.108300 FVAR 1.10382 O14 3 0.311316 0.599083 0.170285 11.00000 0.05885 0.04937 = 0.04243 0.00040 0.01111 -0.00025 O13 3 0.556659 0.488448 0.207400 11.00000 0.06692 0.04162 = 0.04148 0.00045 0.00756 0.00592 O16 3 0.176078 0.631420 -0.093423 11.00000 0.05191 0.06685 = 0.06027 0.01599 0.00920 0.00329 O17 3 0.236355 0.338579 -0.015069 11.00000 0.05184 0.04345 = 0.05917 -0.00502 0.00766 -0.00502 C7 1 0.438066 0.572978 0.019966 11.00000 0.05148 0.03409 = 0.04013 0.00051 0.00738 0.00002 C9 1 0.444646 0.540918 0.143293 11.00000 0.05461 0.03643 = 0.04188 -0.00086 0.00694 -0.00353 C2 1 0.424886 0.895799 -0.091172 11.00000 0.05579 0.03984 = 0.03970 -0.00092 0.00550 0.00013 C10 1 0.268009 0.522990 -0.039431 11.00000 0.04915 0.04860 = 0.03974 -0.00203 0.00984 -0.00030 C3 1 0.456199 1.094544 -0.099123 11.00000 0.05867 0.03726 = 0.04036 0.00380 0.00661 0.00159 C1 1 0.469053 0.796569 0.008568 11.00000 0.05171 0.03453 = 0.04160 0.00104 0.00839 0.00032 C18 1 0.087541 0.260725 -0.070178 11.00000 0.05206 0.06962 = 0.05597 -0.01378 0.00815 -0.01273 C15 1 0.312603 0.605227 0.287491 11.00000 0.06512 0.05333 = 0.04681 -0.00061 0.01591 0.00109 H3 2 0.417447 1.161818 -0.170596 11.00000 0.03683 H2 2 0.369318 0.824223 -0.154535 11.00000 0.04486 H15A 2 0.396401 0.686165 0.322570 11.00000 0.05088 H15B 2 0.202680 0.650156 0.289930 11.00000 0.05952 H18A 2 0.003346 0.290201 -0.043530 11.00000 0.06925 H15C 2 0.326957 0.463475 0.317090 11.00000 0.05618 H18B 2 0.109757 0.115937 -0.059360 11.00000 0.07731 H18C 2 0.062219 0.333896 -0.141365 11.00000 0.09068 HKLF 4 REM ItoMie in P21/n #14 REM wR2 = 0.1898, GooF = S = 0.958, Restrained GooF = 0.958 for all data REM R1 = 0.0700 for 1056 Fo > 4sig(Fo) and 0.0938 for all 1788 data REM 141 parameters refined using 0 restraints END WGHT 0.1083 0.0000 REM Highest difference peak 0.402, deepest hole -0.309, 1-sigma level 0.088 Q1 1 0.3481 0.5466 -0.0055 11.00000 0.05 0.40 Q2 1 0.4505 0.4540 0.1887 11.00000 0.05 0.36 Q3 1 0.3913 0.6290 0.1673 11.00000 0.05 0.27 Q4 1 0.2968 0.7660 -0.1034 11.00000 0.05 0.26 Q5 1 0.2148 0.0001 -0.0769 11.00000 0.05 0.26 ; _shelx_res_checksum 58400 _shelx_hkl_file ; -11 0 1 30.03 15.93 -11 0 1 8.51 82.73 -11 0 1 75.54 54.25 -11 0 1 88.50 9.40 11 0 -1 203.09 449.29 11 0 -1 15.85 74.06 -11 0 2 -1.77 8.00 11 0 -2 -13.14 122.38 -11 0 3 1.14 30.06 11 0 -3 10.82 169.78 -11 0 4 15.79 131.10 11 0 -4 5.83 283.69 -11 0 5 0.05 4.07 11 0 -6 11.44 105.92 11 0 -7 5.60 42.21 11 0 -7 8.45 8.70 11 0 -8 -8.93 181.88 -11 1 1 0.91 10.13 -11 1 1 5.90 65.60 -11 1 1 5.13 43.15 -11 1 1 -1.82 24.21 -11 1 1 1.03 8.11 11 -1 -1 6.01 221.63 11 -1 -1 -5.97 87.49 11 1 -1 -6.63 67.01 -11 -1 1 2.06 13.37 -11 -1 1 10.16 83.25 -11 -1 1 17.67 48.93 -11 -1 1 3.08 6.83 -11 1 2 -0.00 42.57 -11 1 2 1.90 96.50 -11 1 2 3.19 32.02 -11 1 2 -0.81 30.92 11 -1 -2 -2.36 131.78 11 1 -2 22.95 113.67 -11 -1 2 2.20 5.54 -11 1 3 13.48 144.75 11 -1 -3 -41.10 216.55 11 1 -3 3.67 153.45 -11 -1 3 -1.34 6.47 11 1 -4 -26.60 238.49 -11 -1 4 0.03 17.54 -11 -1 5 1.65 4.26 -11 -1 5 6.90 86.96 11 -1 -6 -0.18 9.41 11 1 -6 0.70 31.49 11 -1 -7 10.20 5.56 11 1 -7 4.55 31.10 11 1 -7 1.95 9.24 11 -1 -8 -38.53 199.60 11 1 -8 0.29 5.71 11 1 -8 -6.13 193.20 -11 -1 8 -0.38 5.04 -11 2 1 3.07 5.42 -11 2 1 2.80 37.14 -11 2 1 3.71 27.74 -11 2 1 3.95 12.98 -11 2 1 1.06 19.59 11 -2 -1 45.75 207.88 11 -2 -1 15.06 129.30 11 2 -1 1.17 70.76 -11 -2 1 2.30 8.29 -11 -2 1 3.10 65.59 -11 -2 1 6.83 35.89 -11 -2 1 5.18 12.45 -11 2 2 6.21 28.24 -11 2 2 14.12 86.64 -11 2 2 4.10 18.06 -11 2 2 -2.44 128.26 11 -2 -2 -27.75 168.40 11 2 -2 18.86 119.22 -11 -2 2 0.44 42.83 -11 -2 2 19.20 98.31 -11 -2 2 7.21 10.45 11 -2 -3 24.35 246.27 11 2 -3 7.16 161.98 -11 -2 3 6.25 32.30 -11 -2 3 4.07 5.53 -11 2 4 3.82 31.46 11 2 -4 1.96 267.47 -11 -2 4 0.70 5.06 -11 -2 4 1.46 5.32 11 -2 -5 1.08 8.81 -11 -2 5 0.83 3.13 -11 -2 5 3.60 7.26 11 -2 -6 2.70 5.11 11 2 -6 -0.21 38.31 11 2 -6 -19.91 210.19 -11 -2 6 -0.22 21.36 11 2 -7 -4.61 26.59 -11 -2 7 0.02 101.21 -11 3 3 -1.92 44.24 -11 3 3 -10.43 112.65 11 -3 -3 1.81 10.12 11 3 -3 -11.61 199.65 -11 -3 3 2.77 5.48 -11 -3 3 8.60 12.21 11 -3 -4 3.92 6.97 -11 -3 4 3.10 4.36 -11 -3 4 8.07 11.02 -10 0 1 1.84 32.89 -10 0 1 -17.57 73.42 10 0 -1 -2.07 52.35 -10 0 2 -0.00 29.98 10 0 -2 1.07 78.45 -10 0 3 -23.91 125.28 10 0 -3 -28.65 117.08 10 0 -4 -31.54 192.47 -10 0 5 -0.24 4.77 10 0 -5 0.48 22.29 10 0 -5 4.02 25.51 10 0 -5 6.09 61.11 10 0 -6 8.26 21.21 10 0 -6 6.21 248.62 10 0 -7 -0.62 8.28 10 0 -7 0.25 8.14 10 0 -7 8.44 116.84 -10 0 8 5.35 6.10 10 0 -8 2.08 3.47 10 0 -8 2.27 4.52 10 0 -8 -0.58 51.53 -10 0 9 0.26 6.51 10 0 -9 0.05 1.92 10 0 -9 -0.06 2.73 10 0 -9 1.22 23.27 10 0 -9 -0.17 1.69 -10 0 10 16.81 17.65 -10 0 10 19.09 12.09 10 0 -10 17.46 2.64 10 0 -10 17.73 1.55 -10 0 11 -1.99 29.27 10 -1 -1 4.15 57.07 -10 -1 1 -3.92 32.59 -10 -1 1 0.34 74.62 -10 -1 1 -0.27 5.79 10 -1 -2 12.76 95.97 -10 -1 2 8.77 6.88 10 -1 -3 3.89 147.74 -10 -1 3 7.82 18.32 10 -1 -4 -25.45 265.29 -10 -1 4 5.42 23.61 -10 -1 4 0.53 100.60 -10 1 5 4.23 5.02 10 -1 -5 0.81 24.01 10 1 -5 0.77 30.40 10 1 -5 0.00 89.44 -10 -1 5 6.67 4.86 10 -1 -6 -1.44 32.92 10 -1 -6 3.05 9.43 10 1 -6 2.96 13.73 -10 1 7 -0.22 5.04 10 -1 -7 3.69 15.51 10 -1 -7 0.61 5.00 10 -1 -7 -2.99 125.40 10 1 -7 1.20 5.41 10 1 -7 3.86 7.81 -10 1 8 10.78 5.78 10 -1 -8 6.46 7.25 10 -1 -8 9.87 3.62 10 -1 -8 11.16 54.49 10 1 -8 5.92 2.56 10 1 -8 8.07 6.26 10 1 -8 8.67 65.91 -10 -1 8 14.25 6.25 -10 1 9 2.23 7.21 10 -1 -9 0.92 3.16 10 -1 -9 1.42 2.29 10 -1 -9 2.47 21.89 10 -1 -9 1.27 1.39 10 1 -9 1.42 1.42 10 1 -9 2.26 3.58 10 1 -9 1.46 26.36 10 1 -9 1.50 1.47 -10 -1 9 1.79 6.47 -10 1 10 4.77 11.84 10 -1 -10 2.85 1.29 10 -1 -10 3.07 0.68 10 1 -10 2.66 1.05 10 1 -10 2.78 2.33 10 1 -10 3.23 22.79 10 1 -10 3.14 0.67 -10 -1 10 3.49 19.96 -10 -1 10 5.09 11.61 10 1 -11 13.24 1.76 -10 -1 11 13.37 31.30 -10 2 1 16.13 18.33 -10 2 1 -3.56 84.79 -10 2 1 24.73 56.54 -10 2 1 14.67 15.84 -10 2 1 38.27 122.03 10 -2 -1 11.37 230.84 10 -2 -1 3.96 76.62 10 2 -1 8.46 56.17 -10 -2 1 9.21 26.97 -10 -2 1 21.52 68.53 -10 -2 1 64.80 16.21 -10 2 2 5.17 21.95 10 -2 -2 -27.06 119.33 10 2 -2 -8.43 79.11 -10 -2 2 0.04 6.37 -10 2 3 -0.61 28.80 10 -2 -3 -27.82 188.19 10 2 -3 11.61 114.92 -10 -2 3 2.00 5.75 10 2 -4 -14.18 202.54 -10 -2 4 5.27 6.46 -10 -2 4 5.81 8.02 -10 2 5 10.16 2.46 10 -2 -5 20.09 9.96 10 -2 -5 -4.44 47.07 10 2 -5 15.26 34.79 10 2 -5 -1.93 163.40 -10 -2 5 25.30 29.53 10 -2 -6 5.68 5.20 10 2 -6 -4.73 40.78 10 2 -6 19.19 63.54 -10 -2 6 6.61 113.76 -10 2 7 27.71 6.90 10 -2 -7 26.22 37.81 10 -2 -7 26.56 4.49 10 -2 -7 33.01 152.81 10 2 -7 17.37 4.92 10 2 -7 15.43 151.50 -10 2 8 32.63 7.20 10 -2 -8 34.71 18.45 10 -2 -8 32.88 3.95 10 -2 -8 19.66 74.63 10 -2 -8 18.41 6.77 10 2 -8 25.50 3.17 10 2 -8 30.46 9.45 10 2 -8 19.36 93.94 -10 -2 8 31.72 7.09 10 -2 -9 0.20 1.30 10 -2 -9 1.36 22.63 10 -2 -9 0.15 0.92 10 2 -9 0.21 1.13 10 2 -9 -0.49 4.08 10 2 -9 -5.56 43.88 10 2 -9 0.08 0.90 -10 -2 9 -2.66 30.79 -10 -2 9 0.05 6.89 10 2 -10 13.65 1.55 10 2 -10 10.93 2.83 10 2 -10 12.73 1.17 -10 -2 10 9.36 51.57 -10 -2 10 14.67 14.28 -10 3 1 7.08 6.65 -10 3 1 10.07 36.06 -10 3 1 10.41 30.14 -10 3 1 6.77 9.91 -10 3 1 -27.60 450.86 10 -3 -1 12.60 204.81 10 -3 -1 -10.34 125.09 10 3 -1 -10.37 71.65 10 3 -1 2.65 57.53 -10 -3 1 3.63 14.60 -10 -3 1 0.08 98.33 -10 -3 1 14.53 50.26 -10 3 2 4.44 30.43 -10 3 2 1.79 79.51 -10 3 2 3.76 12.02 10 -3 -2 -12.13 180.96 10 3 -2 2.71 99.71 -10 3 3 3.63 15.65 10 -3 -3 1.43 8.67 10 3 -3 11.03 142.26 -10 -3 3 4.60 7.10 -10 -3 3 15.70 14.76 -10 3 4 11.63 21.99 10 -3 -4 10.41 7.28 10 3 -4 -23.48 248.79 -10 -3 4 9.81 5.17 -10 -3 4 21.06 6.93 -10 3 5 -0.15 29.60 10 -3 -5 -0.01 4.34 10 3 -5 2.02 35.17 10 3 -5 15.05 188.64 -10 -3 5 0.07 2.64 -10 -3 5 0.22 5.39 -10 3 6 -3.24 28.07 10 -3 -6 6.68 3.13 10 -3 -6 6.49 51.11 10 -3 -6 0.00 112.95 10 3 -6 2.82 13.44 -10 -3 6 3.52 6.53 10 -3 -7 9.79 2.50 10 3 -7 7.86 4.43 10 3 -7 5.73 116.26 10 3 -7 24.29 63.09 10 3 -7 -1.53 201.03 -10 -3 7 6.82 16.69 10 -3 -8 -0.05 1.19 10 -3 -8 0.07 1.78 10 3 -8 -0.08 1.78 10 3 -8 5.24 145.47 -10 -3 8 2.84 73.86 10 -3 -9 12.94 43.85 10 3 -9 13.10 1.61 10 3 -9 18.62 5.24 10 3 -9 16.62 1.47 -10 -3 9 18.93 20.05 -10 4 1 1.95 2.62 -10 4 1 0.75 8.67 -10 4 1 2.79 11.67 -10 4 1 7.05 100.13 -10 4 1 4.08 19.99 10 -4 -1 0.42 9.02 10 -4 -1 37.93 128.41 10 -4 -1 4.57 188.89 10 4 -1 -13.93 186.44 10 4 -1 -5.60 81.13 -10 -4 1 1.52 4.00 -10 -4 1 1.60 30.28 -10 -4 1 3.47 18.52 -10 -4 1 7.26 39.69 -10 -4 1 -21.58 122.63 -10 4 2 5.92 8.67 -10 4 2 3.21 56.09 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-4 11.38 16.27 -9 1 -4 7.90 18.14 -9 -1 -5 9.34 2.28 -9 -1 -5 5.73 12.76 -9 -1 -5 -0.00 77.43 -9 1 -5 6.79 13.18 -9 1 -5 9.39 68.14 -9 -1 -6 38.12 4.73 -9 -1 -6 4.82 136.50 -9 1 -6 33.28 13.17 -9 1 -6 -6.84 136.48 -9 -1 -7 0.55 6.67 -9 -1 -7 -4.83 232.60 -9 1 -7 -1.82 25.02 9 2 0 13.20 23.24 9 2 0 21.83 78.82 -9 -2 0 15.39 13.88 -9 -2 0 21.84 63.05 -9 -2 0 33.59 40.50 -9 -2 0 47.19 17.39 -9 2 0 23.48 8.92 -9 2 0 14.57 34.72 -9 2 0 29.15 30.71 -9 2 0 27.32 13.89 -9 2 0 29.67 72.07 9 -2 0 17.12 158.24 9 -2 0 29.35 74.57 -9 -2 -1 5.29 3.31 -9 -2 -1 3.02 9.93 -9 -2 -1 7.81 11.01 -9 -2 -1 -7.90 96.60 -9 2 -1 8.46 3.27 -9 2 -1 2.25 1.07 -9 2 -1 5.17 7.46 -9 2 -1 6.53 10.64 -9 2 -1 3.86 9.55 -9 2 -1 8.39 11.76 -9 -2 -2 9.88 3.49 -9 -2 -2 5.95 54.51 -9 2 -2 10.54 1.90 -9 2 -2 10.17 3.21 -9 2 -2 1.61 81.97 -9 2 -2 7.47 12.38 -9 2 -2 13.47 6.82 -9 -2 -3 2.99 25.43 -9 -2 -3 3.74 22.94 -9 -2 -3 -0.03 21.79 -9 -2 -4 0.03 12.14 -9 -2 -4 -0.66 26.30 -9 2 -4 -0.16 3.37 -9 2 -4 -2.25 15.88 -9 2 -4 1.68 16.70 -9 -2 -5 5.90 1.29 -9 -2 -5 3.05 8.75 -9 -2 -5 5.12 60.88 -9 2 -5 4.47 7.37 -9 2 -5 4.43 34.21 -9 2 -5 2.51 30.27 -9 -2 -6 19.46 2.21 -9 -2 -6 12.03 19.26 -9 -2 -6 3.45 117.33 -9 2 -6 9.38 14.52 -9 -2 -7 1.95 1.96 -9 -2 -7 13.49 165.42 -9 2 -7 6.37 32.49 -9 2 -7 -22.33 189.75 9 3 0 16.58 109.07 9 3 0 -5.58 81.64 -9 -3 0 3.41 5.37 -9 -3 0 1.11 182.19 -9 3 0 6.06 4.18 -9 3 0 6.25 13.25 -9 3 0 4.21 16.91 -9 3 0 6.44 11.08 -9 3 0 6.95 131.00 9 -3 0 2.94 120.93 9 -3 0 7.69 56.04 -9 -3 -1 14.10 2.84 -9 -3 -1 9.24 5.55 -9 -3 -1 19.08 7.68 -9 -3 -1 6.23 98.95 -9 3 -1 11.69 4.53 -9 3 -1 16.53 7.16 -9 3 -1 -15.96 128.50 -9 3 -1 6.95 23.56 9 -3 1 12.54 14.35 9 -3 1 0.98 78.02 -9 -3 -2 8.62 37.13 -9 3 -2 6.21 1.60 -9 3 -2 3.09 56.63 -9 3 -2 0.36 19.76 -9 -3 -3 4.73 12.89 -9 3 -3 5.69 2.23 -9 3 -3 2.27 32.49 -9 3 -3 13.13 6.80 -9 -3 -4 2.29 16.72 -9 -3 -4 4.30 21.83 -9 3 -4 2.80 3.32 -9 3 -4 1.39 15.40 -9 3 -4 18.07 17.11 -9 -3 -5 1.66 8.32 -9 -3 -5 1.50 37.14 -9 3 -5 1.50 7.20 -9 -3 -6 4.08 17.09 -9 -3 -6 8.76 76.88 -9 3 -6 5.20 14.57 9 4 0 -6.35 68.28 -9 -4 0 3.97 2.66 -9 -4 0 4.63 9.23 -9 -4 0 6.40 9.13 -9 -4 0 16.75 116.26 -9 4 0 8.88 21.97 9 -4 0 4.17 45.97 9 -4 0 68.88 105.39 -9 -4 -1 10.51 2.76 -9 -4 -1 20.95 47.73 -9 4 -1 11.85 1.49 -9 4 -1 8.38 105.76 -9 4 -1 10.72 37.43 9 -4 1 41.70 62.77 -9 -4 -2 23.21 15.44 -9 4 -2 21.11 2.18 -9 4 -2 27.79 51.24 -9 4 -2 27.08 8.45 9 -4 2 30.30 79.97 -9 4 -3 4.64 1.80 -9 4 -3 -0.20 18.88 -9 4 -3 7.17 6.23 -9 -4 -4 2.68 24.02 -9 -4 -4 10.85 23.53 -9 4 -4 3.01 13.81 -9 4 -4 7.81 12.97 9 5 0 4.02 54.12 -9 -5 0 1.89 2.43 -9 -5 0 2.85 11.56 -9 5 0 -6.76 151.85 9 -5 0 1.68 5.51 9 -5 0 1.16 14.84 9 -5 0 103.55 171.41 9 5 1 11.26 75.12 -9 5 -1 17.44 65.74 -9 5 -1 20.29 46.33 9 -5 1 8.22 9.86 9 -5 1 131.68 148.23 9 5 2 17.03 87.14 -9 5 -2 2.37 25.27 9 -5 2 24.34 84.33 10 0 0 -4.39 56.30 -10 0 0 3.53 37.57 -10 0 0 14.38 22.45 -10 0 0 37.41 6.78 -10 0 -1 0.13 2.51 -10 0 -1 -0.03 7.35 -10 0 -1 0.94 9.49 -10 0 -1 -1.18 8.66 -10 0 -2 49.56 5.18 -10 0 -2 45.66 87.55 -10 0 -2 126.04 21.48 -10 0 -3 1.75 40.98 -10 0 -3 -0.00 8.54 -10 0 -4 18.25 1.93 -10 0 -4 10.73 15.68 -10 0 -4 15.44 13.74 -10 0 -5 0.05 1.15 -10 0 -5 0.18 18.09 -10 0 -5 -2.50 19.23 10 1 0 -10.47 84.84 -10 -1 0 0.39 6.79 -10 -1 0 -2.69 41.67 -10 1 0 0.06 5.75 -10 1 0 3.46 27.28 -10 1 0 2.14 24.85 -10 1 0 -0.06 7.58 10 -1 0 18.19 130.40 -10 -1 -1 32.79 3.88 -10 -1 -1 36.81 9.25 -10 -1 -1 15.21 133.68 -10 -1 -1 51.79 17.42 -10 1 -1 36.29 4.14 -10 1 -1 28.20 7.27 -10 1 -1 33.42 9.70 -10 1 -1 21.12 138.20 -10 1 -1 24.41 14.19 -10 1 -1 44.14 7.57 -10 -1 -2 8.68 2.64 -10 -1 -2 2.67 21.78 -10 1 -2 7.47 2.38 -10 1 -2 29.37 86.82 -10 1 -2 8.10 9.39 -10 1 -2 14.08 9.64 -10 -1 -3 26.32 35.38 -10 1 -3 19.85 2.07 -10 1 -3 19.66 43.93 -10 1 -3 17.55 13.41 -10 1 -3 22.99 15.39 -10 -1 -4 4.32 13.32 -10 1 -4 6.20 1.39 -10 1 -4 3.49 16.08 -10 1 -4 1.97 20.20 -10 -1 -5 14.27 17.19 -10 -1 -5 17.49 19.98 -10 1 -5 13.90 2.24 -10 1 -5 20.04 18.09 10 2 0 16.63 86.88 -10 -2 0 13.82 5.47 -10 -2 0 6.64 28.81 -10 -2 0 19.50 19.80 -10 2 0 17.19 4.52 -10 2 0 12.88 15.75 -10 2 0 17.28 17.01 -10 2 0 17.67 11.97 -10 2 0 19.35 17.68 10 -2 0 7.14 95.85 10 -2 0 6.32 63.55 -10 2 -1 0.14 2.00 -10 2 -1 -0.70 4.08 -10 2 -1 -0.90 7.69 -10 2 -1 -10.25 149.53 -10 2 -1 0.85 9.32 -10 2 -1 0.57 6.43 -10 -2 -2 -0.00 50.07 -10 -2 -2 2.87 23.59 -10 2 -2 -9.74 76.37 -10 2 -2 -0.21 14.53 -10 2 -2 -0.84 6.21 -10 -2 -3 -1.61 20.41 -10 -2 -3 -0.04 18.08 -10 2 -3 0.21 1.01 -10 2 -3 13.04 40.20 -10 2 -3 1.55 21.48 -10 2 -3 0.77 13.87 -10 -2 -4 -1.32 11.11 -10 -2 -4 -1.66 9.82 -10 2 -4 0.16 1.26 -10 2 -4 0.85 15.24 10 3 0 0.92 78.64 -10 -3 0 9.97 3.21 -10 -3 0 9.10 12.03 -10 -3 0 8.26 10.77 -10 -3 0 0.65 124.76 -10 3 0 10.81 2.88 -10 3 0 9.46 7.00 -10 3 0 6.61 9.73 -10 3 0 5.64 130.91 -10 3 0 11.86 12.83 -10 3 0 15.10 39.96 10 -3 0 11.27 43.22 10 -3 0 -13.11 73.59 10 3 1 -9.15 100.05 -10 -3 -1 -3.25 87.42 -10 3 -1 0.35 2.50 -10 3 -1 2.59 12.98 -10 3 -1 -1.43 153.01 -10 3 -1 2.58 18.43 -10 3 -1 0.79 8.13 -10 -3 -2 3.67 37.31 -10 3 -2 3.36 0.89 -10 3 -2 -10.92 66.88 -10 3 -2 5.84 6.07 -10 -3 -3 0.62 27.97 -10 3 -3 2.99 1.05 -10 3 -3 2.09 28.44 -10 3 -3 7.80 8.97 10 4 0 -4.16 58.09 -10 -4 0 2.51 1.69 -10 -4 0 1.49 3.83 -10 -4 0 4.70 5.43 -10 -4 0 9.49 135.43 -10 4 0 3.98 1.51 -10 4 0 2.03 2.87 -10 4 0 3.78 6.32 -10 4 0 -11.16 194.98 -10 4 0 -10.06 19.67 -10 4 0 -0.32 69.58 10 -4 0 4.74 15.56 10 -4 0 -0.00 123.46 10 4 1 12.87 89.38 -10 -4 -1 -3.46 48.52 -10 4 -1 9.51 102.87 -10 4 -1 -0.16 10.31 11 0 0 -5.79 75.32 -11 0 0 0.07 2.91 -11 0 0 0.44 13.19 -11 0 0 -0.25 13.94 -11 0 0 14.84 113.04 -11 0 0 -2.49 27.82 -11 0 0 0.92 6.16 11 0 1 0.01 106.89 -11 0 -1 3.84 1.61 -11 0 -1 3.58 3.41 -11 0 -1 6.17 6.22 -11 0 -1 30.09 176.35 -11 0 -1 5.02 16.67 -11 0 -1 5.51 14.18 -11 0 -2 18.02 76.01 -11 0 -2 -0.89 10.01 11 1 0 -12.02 77.65 -11 -1 0 2.03 2.85 -11 -1 0 1.14 13.13 -11 -1 0 0.83 12.42 -11 -1 0 -9.89 116.74 -11 -1 0 8.09 16.17 -11 1 0 1.97 2.66 -11 1 0 1.86 10.63 -11 1 0 2.39 11.63 -11 1 0 -4.05 118.79 -11 1 0 1.80 15.05 -11 1 0 2.65 5.68 11 -1 0 0.08 67.91 11 1 1 -0.00 101.58 -11 -1 -1 0.02 1.37 -11 -1 -1 -0.06 2.97 -11 -1 -1 0.06 5.31 -11 -1 -1 16.21 159.05 -11 1 -1 0.04 1.23 -11 1 -1 -0.01 2.90 -11 1 -1 -0.60 4.85 -11 1 -1 27.33 178.33 -11 1 -1 0.07 9.94 11 -1 1 0.00 101.81 11 2 0 -7.26 70.14 -11 -2 0 -0.10 8.52 -11 -2 0 0.81 8.75 -11 -2 0 -13.56 163.98 -11 2 0 -0.35 6.20 -11 2 0 11.90 168.95 -11 2 0 0.01 9.08 11 -2 0 3.82 73.69 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 1237 _olex2_submission_special_instructions 'No special instructions were received' 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 O14 O 0.3113(2) 0.5991(3) 0.17029(14) 0.0501(5) Uani 1 1 d . . . . . O13 O 0.5567(2) 0.4884(2) 0.20740(14) 0.0505(5) Uani 1 1 d . . . . . O16 O 0.1761(2) 0.6314(3) -0.09342(17) 0.0600(6) Uani 1 1 d . . . . . O17 O 0.2364(2) 0.3386(3) -0.01507(16) 0.0520(5) Uani 1 1 d . . . . . C7 C 0.4381(3) 0.5730(3) 0.01997(19) 0.0422(5) Uani 1 1 d . . . . . C9 C 0.4446(3) 0.5409(3) 0.14329(19) 0.0447(6) Uani 1 1 d . . . . . C2 C 0.4249(3) 0.8958(4) -0.09117(19) 0.0457(6) Uani 1 1 d . . . . . C10 C 0.2680(3) 0.5230(4) -0.03943(19) 0.0457(6) Uani 1 1 d . . . . . C3 C 0.4562(3) 1.0945(4) -0.09912(19) 0.0459(6) Uani 1 1 d . . . . . C1 C 0.4691(3) 0.7966(3) 0.00857(18) 0.0428(5) Uani 1 1 d . . . . . C18 C 0.0875(4) 0.2607(5) -0.0702(3) 0.0596(7) Uani 1 1 d . . . . . C15 C 0.3126(4) 0.6052(5) 0.2875(2) 0.0544(7) Uani 1 1 d . . . . . H3 H 0.417(3) 1.162(4) -0.171(2) 0.037(6) Uiso 1 1 d . . . . . H2 H 0.369(3) 0.824(4) -0.155(2) 0.045(7) Uiso 1 1 d . . . . . H15A H 0.396(4) 0.686(4) 0.323(2) 0.051(8) Uiso 1 1 d . . . . . H15B H 0.203(4) 0.650(5) 0.290(3) 0.060(9) Uiso 1 1 d . . . . . H18A H 0.003(4) 0.290(5) -0.044(3) 0.069(10) Uiso 1 1 d . . . . . H15C H 0.327(4) 0.463(5) 0.317(2) 0.056(8) Uiso 1 1 d . . . . . H18B H 0.110(4) 0.116(6) -0.059(3) 0.077(11) Uiso 1 1 d . . . . . H18C H 0.062(5) 0.334(6) -0.141(4) 0.091(13) 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 O14 0.0589(12) 0.0494(10) 0.0424(9) 0.0004(7) 0.0111(8) -0.0003(8) O13 0.0669(12) 0.0416(9) 0.0415(9) 0.0005(7) 0.0076(8) 0.0059(8) O16 0.0519(12) 0.0668(13) 0.0603(12) 0.0160(9) 0.0092(9) 0.0033(9) O17 0.0518(11) 0.0434(10) 0.0592(11) -0.0050(8) 0.0077(9) -0.0050(7) C7 0.0515(14) 0.0341(11) 0.0401(11) 0.0005(8) 0.0074(10) 0.0000(9) C9 0.0546(15) 0.0364(11) 0.0419(12) -0.0009(9) 0.0069(10) -0.0035(10) C2 0.0558(14) 0.0398(12) 0.0397(11) -0.0009(9) 0.0055(10) 0.0001(10) C10 0.0492(14) 0.0486(13) 0.0397(11) -0.0020(9) 0.0098(10) -0.0003(10) C3 0.0587(16) 0.0373(11) 0.0404(11) 0.0038(8) 0.0066(11) 0.0016(10) C1 0.0517(14) 0.0345(11) 0.0416(11) 0.0010(8) 0.0084(10) 0.0003(9) C18 0.0521(16) 0.0696(19) 0.0560(15) -0.0138(14) 0.0082(13) -0.0127(14) C15 0.0651(19) 0.0533(16) 0.0468(14) -0.0006(11) 0.0159(13) 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 0.0030 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 0.0105 0.0059 '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 C9 O14 C15 115.4(2) . . C10 O17 C18 116.5(2) . . C9 C7 C7 109.0(2) . 3_665 C9 C7 C10 106.3(2) . . C9 C7 C1 104.90(18) . . C10 C7 C7 110.8(2) . 3_665 C1 C7 C7 115.6(2) . 3_665 C1 C7 C10 109.70(19) . . O14 C9 C7 110.4(2) . . O13 C9 O14 124.4(2) . . O13 C9 C7 124.9(2) . . C3 C2 C1 120.8(2) . . C3 C2 H2 120.4(16) . . C1 C2 H2 118.8(16) . . O16 C10 O17 124.2(3) . . O16 C10 C7 127.0(2) . . O17 C10 C7 108.7(2) . . C2 C3 C1 121.8(2) . 3_675 C2 C3 H3 118.3(14) . . C1 C3 H3 119.7(14) 3_675 . C2 C1 C7 122.1(2) . . C3 C1 C7 120.5(2) 3_675 . C3 C1 C2 117.4(2) 3_675 . O17 C18 H18A 118(2) . . O17 C18 H18B 99(2) . . O17 C18 H18C 105(2) . . H18A C18 H18B 109(3) . . H18A C18 H18C 99(3) . . H18B C18 H18C 127(3) . . O14 C15 H15A 109.0(18) . . O14 C15 H15B 102.8(18) . . O14 C15 H15C 107.8(17) . . H15A C15 H15B 117(3) . . H15A C15 H15C 111(3) . . H15B C15 H15C 109(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O14 C9 1.338(3) . O14 C15 1.455(3) . O13 C9 1.187(3) . O16 C10 1.194(3) . O17 C10 1.333(3) . O17 C18 1.445(3) . C7 C7 1.621(5) 3_665 C7 C9 1.538(3) . C7 C10 1.560(4) . C7 C1 1.557(3) . C2 C3 1.387(3) . C2 C1 1.396(3) . C2 H2 0.97(3) . C3 C1 1.395(3) 3_675 C3 H3 1.00(3) . C18 H18A 0.89(4) . C18 H18B 1.01(4) . C18 H18C 1.00(5) . C15 H15A 0.95(3) . C15 H15B 1.02(3) . C15 H15C 1.03(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 C7 C7 C9 O14 -157.1(2) 3_665 . . . C7 C7 C9 O13 29.1(4) 3_665 . . . C7 C7 C10 O16 -123.3(3) 3_665 . . . C7 C7 C10 O17 60.3(3) 3_665 . . . C7 C7 C1 C2 80.8(3) 3_665 . . . C7 C7 C1 C3 -98.8(3) 3_665 . . 3_675 C9 C7 C10 O16 118.4(3) . . . . C9 C7 C10 O17 -58.0(2) . . . . C9 C7 C1 C2 -159.2(2) . . . . C9 C7 C1 C3 21.2(3) . . . 3_675 C10 C7 C9 O14 -37.6(2) . . . . C10 C7 C9 O13 148.6(2) . . . . C10 C7 C1 C2 -45.3(3) . . . . C10 C7 C1 C3 135.0(2) . . . 3_675 C3 C2 C1 C7 -179.0(2) . . . . C3 C2 C1 C3 0.6(4) . . . 3_675 C1 C7 C9 O14 78.6(2) . . . . C1 C7 C9 O13 -95.2(3) . . . . C1 C7 C10 O16 5.5(3) . . . . C1 C7 C10 O17 -170.89(18) . . . . C1 C2 C3 C1 -0.7(4) . . . 3_675 C18 O17 C10 O16 8.4(4) . . . . C18 O17 C10 C7 -175.1(2) . . . . C15 O14 C9 O13 3.2(3) . . . . C15 O14 C9 C7 -170.6(2) . . . . loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code _cod_related_entry_description 1 XRDa 00331 DOI:10.51093/xrd-00331