#------------------------------------------------------------------------------ #$Date: 2020-04-28 02:29:12 +0300 (Tue, 28 Apr 2020) $ #$Revision: 251203 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/04/7240412.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_7240412 loop_ _publ_author_name 'Charpe, Vaibhav Pramod' 'Sagadevan, Arunachalam' 'Hwang, Kuo Chu' _publ_section_title ; Visible Light-Induced Aerobic Oxidation of Diarylalkynes to -Diketones Catalyzed by Copper-superoxo at Room Temperature ; _journal_name_full 'Green Chemistry' _journal_paper_doi 10.1039/D0GC00975J _journal_year 2020 _chemical_absolute_configuration rm _chemical_formula_sum 'C14 H10 O2' _chemical_formula_weight 210.22 _space_group_crystal_system trigonal _space_group_IT_number 154 _space_group_name_Hall 'P 32 2"' _space_group_name_H-M_alt 'P 32 2 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/6 _audit_update_record ; 2018-07-30 deposited with the CCDC. 2020-04-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 8.3601(7) _cell_length_b 8.3601(7) _cell_length_c 13.3968(12) _cell_measurement_reflns_used 7075 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.2697 _cell_measurement_theta_min 2.8134 _cell_volume 810.88(12) _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.3333 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.996 _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 0.0333 _diffrn_reflns_av_unetI/netI 0.0261 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 10682 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.509 _diffrn_reflns_theta_min 2.813 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_T_max 0.9485 _exptl_absorpt_correction_T_min 0.7698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/4 (Bruker AXS Inc.)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description lump _exptl_crystal_F_000 330 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.144 _refine_diff_density_min -0.131 _refine_diff_density_rms 0.026 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 74 _refine_ls_number_reflns 1127 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.105 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0295 _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^)+(0.0281P)^2^+0.0979P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.0695 _reflns_Friedel_coverage 0.665 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 1070 _reflns_number_total 1127 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0gc00975j2.cif _cod_data_source_block 180116LT_0m_a _cod_depositor_comments ; The following automatic conversions were performed: data item '_chemical_absolute_configuration' value 'RM' was changed to 'rm' 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. data item '_exptl_crystal_density_meas' value 'not measured' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_cell_volume 810.88(15) _cod_database_code 7240412 _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. ; _shelxl_version_number 2014/6 _shelx_res_file ; TITL 180116LT_0m_a.res in P3(2)21 CELL 0.71073 8.3601 8.3601 13.3968 90.000 90.000 120.000 ZERR 3.000 0.0007 0.0007 0.0012 0.000 0.000 0.000 LATT -1 SYMM -Y, X-Y, 2/3+Z SYMM -X+Y, -X, 1/3+Z SYMM Y, X, -Z SYMM X-Y, -Y, 1/3-Z SYMM -X, -X+Y, 2/3-Z SFAC C H O UNIT 42 30 6 L.S. 4 ACTA BOND $H TWIN FMAP 2 PLAN 5 TEMP -173.000 WGHT 0.028100 0.097900 BASF -0.27250 FVAR 1.04093 C1 1 0.234571 0.208482 0.245038 11.00000 0.02517 0.02585 = 0.04116 0.00667 0.00655 0.00959 C2 1 0.182640 0.296374 0.174870 11.00000 0.03076 0.03563 = 0.04460 0.01014 0.00849 0.01594 AFIX 43 H2 2 0.147229 0.246317 0.109642 11.00000 -1.20000 AFIX 0 C3 1 0.182532 0.457050 0.200089 11.00000 0.04785 0.04079 = 0.05977 0.01833 0.01610 0.02809 AFIX 43 H3 2 0.145815 0.516669 0.152476 11.00000 -1.20000 AFIX 0 C4 1 0.236076 0.530293 0.294832 11.00000 0.05640 0.03456 = 0.06906 0.00894 0.02422 0.02580 AFIX 43 H4 2 0.236685 0.640882 0.311922 11.00000 -1.20000 AFIX 0 C5 1 0.288776 0.444061 0.364982 11.00000 0.05060 0.03437 = 0.05188 -0.00047 0.01075 0.01630 AFIX 43 H5 2 0.325491 0.495542 0.429848 11.00000 -1.20000 AFIX 0 C6 1 0.287983 0.283115 0.340667 11.00000 0.03695 0.03132 = 0.04298 0.00477 0.00428 0.01255 AFIX 43 H6 2 0.323626 0.223398 0.388794 11.00000 -1.20000 AFIX 0 C7 1 0.230519 0.034438 0.221006 11.00000 0.03049 0.02599 = 0.04289 0.00514 0.00136 0.01072 O1 3 0.262260 -0.055263 0.281114 11.00000 0.06288 0.03552 = 0.05146 0.00342 -0.00983 0.02737 HKLF 4 REM 180116LT_0m_a.res in P3(2)21 REM R1 = 0.0295 for 1070 Fo > 4sig(Fo) and 0.0313 for all 1127 data REM 74 parameters refined using 0 restraints END WGHT 0.0281 0.0979 REM Highest difference peak 0.144, deepest hole -0.131, 1-sigma level 0.026 Q1 1 0.1774 0.0000 0.1667 10.50000 0.05 0.14 Q2 1 0.2683 0.1438 0.2290 11.00000 0.05 0.13 Q3 1 0.3127 0.2685 0.2833 11.00000 0.05 0.10 Q4 1 0.3521 0.3918 0.3470 11.00000 0.05 0.09 Q5 1 0.2540 0.5292 0.2382 11.00000 0.05 0.09 ; _shelx_res_checksum 60533 _shelx_hkl_file ; 1 0 0 551.53 19.58 1 0 0 535.79 18.79 1 0 0 545.88 18.46 0 -1 0 571.18 18.66 0 -1 0 509.33 18.79 0 -1 0 519.65 19.47 0 -1 0 518.24 18.43 -1 1 0 525.95 18.42 -1 1 0 516.42 18.66 1 0 0 620.39 20.69 -1 1 0 519.69 18.50 -1 1 0 520.37 18.87 -1 1 0 553.18 19.88 0 1 0 521.93 18.67 0 1 0 548.95 18.97 0 1 0 510.78 19.06 1 -1 0 542.52 18.75 0 1 0 559.26 18.76 1 -1 0 530.70 19.26 1 -1 0 535.92 18.62 -1 0 0 564.00 20.01 -1 0 0 533.56 19.13 -1 0 0 524.44 18.83 -1 0 0 531.57 18.50 1 -1 0 497.27 18.51 0 1 0 510.20 18.44 1 -1 0 542.57 19.36 1 -2 0 1204.95 43.68 1 -2 0 1265.35 42.97 1 -2 0 1264.80 42.89 1 1 0 1160.14 43.51 1 1 0 1275.25 44.37 1 1 0 1284.00 43.02 1 1 0 1250.02 42.38 -2 1 0 1195.35 43.36 -2 1 0 1262.97 43.20 1 1 0 1212.63 43.30 -2 1 0 1283.64 44.94 2 -1 0 1301.67 42.88 -1 2 0 1332.92 45.72 2 -1 0 1276.85 43.25 -1 -1 0 1263.88 44.39 -1 -1 0 1278.17 44.35 -1 -1 0 1200.24 42.61 -1 2 0 1277.24 43.30 -1 2 0 1157.72 43.33 0 -2 0 4615.27 153.17 -2 2 0 4510.06 155.59 2 0 0 5086.11 157.87 2 0 0 4645.85 154.15 2 0 0 4481.00 151.52 -2 2 0 4395.40 151.46 -2 2 0 4478.82 153.48 0 2 0 4376.46 153.11 -2 0 0 4567.36 151.60 0 2 0 4368.60 153.94 0 2 0 4514.67 153.54 -2 0 0 4479.86 154.80 -2 0 0 4512.15 154.27 2 -2 0 4438.59 151.09 2 -2 0 4573.01 154.13 2 -2 0 4380.85 151.47 2 -3 0 111.15 4.48 2 -3 0 107.88 4.08 1 2 0 104.28 4.50 -3 1 0 104.07 4.73 -3 1 0 102.83 4.70 -3 1 0 107.28 4.22 2 -3 0 109.68 4.05 1 2 0 109.47 4.67 1 2 0 106.56 4.11 -2 3 0 106.98 4.10 -2 3 0 105.12 4.75 -2 3 0 105.07 4.16 -1 -2 0 107.95 4.43 3 -1 0 102.81 4.22 -1 -2 0 108.39 4.46 -1 -2 0 104.24 4.33 2 1 0 105.95 4.61 -3 2 0 99.99 4.22 -3 2 0 103.43 4.79 -3 2 0 103.15 4.59 1 -3 0 105.43 4.42 1 -3 0 105.26 4.56 1 -3 0 108.36 4.07 2 1 0 116.55 4.92 2 1 0 110.49 4.21 -1 3 0 107.18 4.47 3 -2 0 107.65 4.16 3 -2 0 108.75 4.57 3 -2 0 108.79 4.30 -2 -1 0 112.04 4.17 -1 3 0 106.08 4.72 -1 3 0 107.66 4.11 -2 -1 0 110.16 4.70 -2 -1 0 108.53 4.59 0 -3 0 31.98 1.93 0 -3 0 30.04 1.45 -3 3 0 31.16 2.18 3 0 0 28.85 1.66 -3 3 0 29.42 1.61 -3 3 0 29.33 1.68 0 -3 0 32.15 1.89 3 0 0 25.39 2.34 -3 3 0 30.95 1.79 0 3 0 29.32 1.42 0 3 0 31.88 2.08 0 3 0 30.37 1.59 3 -3 0 29.82 1.60 -3 0 0 30.77 1.66 -3 0 0 32.23 2.21 0 3 0 30.14 1.89 -3 0 0 29.81 2.03 3 -3 0 28.90 1.91 1 3 0 145.96 5.56 3 -4 0 147.48 6.09 1 3 0 145.83 6.30 -4 1 0 147.04 6.44 3 -4 0 144.92 5.53 -4 1 0 144.40 5.69 -4 1 0 146.51 6.47 -1 -3 0 142.14 5.70 4 -1 0 137.08 5.72 -3 4 0 145.89 5.58 -1 -3 0 138.49 5.95 4 -1 0 140.88 7.31 -3 4 0 143.84 6.49 -3 4 0 136.16 5.61 -1 -3 0 144.52 5.99 -4 2 0 413.64 16.17 -4 2 0 438.50 16.07 2 2 0 436.02 16.16 2 -4 0 437.37 15.71 -4 2 0 468.01 15.47 2 2 0 454.73 15.33 2 -4 0 441.04 15.16 -2 4 0 427.09 15.19 -2 4 0 452.69 16.23 4 -2 0 438.34 15.45 -2 -2 0 445.19 15.79 -2 -2 0 423.59 15.74 1 -4 0 129.63 5.31 3 1 0 144.91 6.58 1 -4 0 141.57 5.84 1 -4 0 143.96 6.07 3 1 0 149.23 5.63 -4 3 0 138.87 6.38 -4 3 0 141.93 5.64 -4 3 0 142.44 6.03 4 -3 0 136.75 5.45 -1 4 0 137.94 5.39 4 -3 0 142.18 6.04 -3 -1 0 142.62 6.09 -3 -1 0 138.30 6.19 -3 -1 0 141.05 5.48 -1 4 0 137.79 6.25 -4 4 0 2076.80 71.02 0 -4 0 2040.20 71.17 -4 4 0 2159.19 73.45 4 0 0 2106.78 69.88 0 -4 0 2083.01 75.51 -4 4 0 2021.52 69.66 4 0 0 2308.91 72.09 -4 0 0 2112.33 70.66 -4 0 0 2103.98 78.14 -4 0 0 2017.28 70.71 0 4 0 2077.52 71.15 4 -4 0 2178.92 70.74 0 4 0 2039.84 70.40 4 -4 0 2114.44 73.81 0 4 0 2043.44 72.12 -5 1 0 103.06 5.36 1 4 0 103.64 4.42 4 -5 0 101.59 4.99 -5 1 0 98.02 4.51 -5 1 0 99.87 5.34 1 4 0 104.25 5.27 4 -5 0 104.45 4.39 -4 5 0 95.41 4.46 -4 5 0 97.40 5.41 -1 -4 0 102.74 4.87 -1 -4 0 99.37 4.40 -1 -4 0 108.76 4.98 5 -1 0 120.24 6.87 -4 5 0 97.68 4.39 -5 2 0 5.33 1.30 -5 2 0 3.75 1.07 -5 2 0 4.71 0.86 3 -5 0 5.21 0.59 3 -5 0 3.97 0.96 2 3 0 4.46 0.81 2 3 0 5.69 1.36 3 -5 0 5.16 0.81 -3 5 0 5.00 1.21 -2 -3 0 5.56 1.09 -3 5 0 4.72 0.85 5 -2 0 5.40 1.92 -2 -3 0 4.37 0.98 -5 3 0 3.45 1.12 2 -5 0 4.52 1.05 2 -5 0 5.30 1.06 2 -5 0 4.94 0.78 3 2 0 5.88 1.37 -5 3 0 5.37 0.99 3 2 0 5.88 0.96 -5 3 0 3.99 1.07 5 -3 0 4.15 0.76 5 -3 0 4.01 0.99 -3 -2 0 5.39 1.23 -2 5 0 5.01 1.22 -3 -2 0 4.78 1.06 5 -3 0 4.83 1.74 -3 -2 0 5.89 0.87 -2 5 0 5.88 0.87 -5 4 0 97.99 4.82 1 -5 0 100.83 4.98 -5 4 0 95.88 5.39 1 -5 0 100.58 4.80 4 1 0 103.02 5.83 4 1 0 101.88 4.53 -5 4 0 100.94 4.54 5 -4 0 103.81 5.06 5 -4 0 101.33 4.39 -4 -1 0 99.54 5.23 -4 -1 0 104.98 5.14 -4 -1 0 98.88 4.36 -1 5 0 97.69 5.21 -1 5 0 103.34 4.33 5 0 0 20.19 3.31 0 -5 0 24.56 2.11 5 0 0 23.45 1.88 -5 5 0 24.98 1.89 0 -5 0 26.01 2.07 -5 5 0 27.58 2.65 0 -5 0 27.22 1.69 0 5 0 27.80 2.46 5 -5 0 23.60 1.72 -5 0 0 29.25 2.63 -5 0 0 26.19 2.41 -5 0 0 24.91 1.02 0 5 0 25.71 1.75 -5 0 0 25.84 1.84 5 -5 0 26.66 2.27 0 5 0 24.62 1.41 -6 1 0 30.82 2.13 -6 1 0 25.14 2.60 1 5 0 27.38 1.97 5 -6 0 27.51 1.95 1 5 0 28.01 2.66 5 -6 0 26.46 2.41 -6 1 0 27.70 2.81 -1 -5 0 24.55 1.76 -5 6 0 29.43 2.91 -1 -5 0 29.47 2.35 -5 6 0 26.50 2.06 -1 -5 0 28.64 2.38 6 -1 0 28.57 4.47 -6 2 0 18.78 2.32 2 4 0 21.71 2.35 -6 2 0 22.47 2.39 -6 2 0 20.56 1.77 2 4 0 21.13 1.66 4 -6 0 20.57 2.04 4 -6 0 20.86 1.60 -2 -4 0 20.53 1.92 6 -2 0 19.63 3.78 -4 6 0 22.10 2.43 -4 6 0 22.26 1.86 -2 -4 0 20.21 1.53 -2 -4 0 20.64 1.85 3 -6 0 95.33 5.24 3 -6 0 93.83 4.20 3 -6 0 99.76 4.90 3 3 0 94.17 5.44 3 3 0 94.15 4.38 -6 3 0 96.84 5.49 -6 3 0 99.02 5.30 -6 3 0 93.36 4.49 -3 6 0 88.65 4.23 -3 -3 0 94.65 4.91 6 -3 0 93.87 4.38 -3 -3 0 94.92 4.91 -3 6 0 91.59 5.33 2 -6 0 19.90 2.12 4 2 0 21.94 2.59 -6 4 0 20.72 2.11 4 2 0 21.41 1.76 -6 4 0 19.42 2.76 2 -6 0 18.74 1.85 -6 4 0 20.48 1.76 -4 -2 0 20.81 1.60 -2 6 0 19.08 1.55 -4 -2 0 19.95 2.16 -4 -2 0 17.87 1.93 -2 6 0 19.85 2.26 6 -4 0 19.74 1.62 6 -4 0 21.33 2.09 -6 5 0 28.89 2.16 5 1 0 26.44 2.09 1 -6 0 26.76 2.42 1 -6 0 26.60 2.26 -6 5 0 29.64 2.95 5 1 0 27.51 3.35 1 -6 0 25.50 1.78 -5 -1 0 27.19 1.96 -1 6 0 25.68 2.60 -5 -1 0 27.53 2.55 6 -5 0 30.91 2.61 -1 6 0 26.57 1.91 6 -5 0 30.32 2.07 -5 -1 0 27.83 2.73 -6 6 0 3.02 1.27 -6 6 0 2.16 0.79 6 0 0 3.60 1.77 0 -6 0 1.45 0.71 0 -6 0 2.47 0.92 -6 0 0 2.11 1.05 -6 0 0 2.83 1.36 6 -6 0 2.90 1.05 -6 0 0 2.29 0.75 0 6 0 2.78 1.14 6 -6 0 3.06 0.80 -7 1 0 20.21 3.14 6 -7 0 21.68 2.39 6 -7 0 19.91 2.27 1 6 0 16.21 2.58 -7 1 0 18.87 2.94 7 -1 0 12.28 3.25 -6 7 0 18.54 2.95 -1 -6 0 18.95 2.15 5 -7 0 8.93 1.35 5 -7 0 8.36 1.71 2 5 0 8.81 2.00 -7 2 0 7.51 1.31 -7 2 0 5.78 1.77 -7 2 0 10.42 2.22 7 -2 0 10.38 3.21 -5 7 0 7.64 1.94 4 -7 0 22.89 2.27 4 -7 0 22.52 1.79 4 -7 0 23.42 2.61 3 4 0 23.80 2.73 -7 3 0 20.84 2.45 -7 3 0 23.95 2.73 -7 3 0 22.57 2.01 -3 -4 0 23.52 2.22 -3 -4 0 22.64 2.22 -4 7 0 22.66 2.70 3 -7 0 24.61 2.30 -7 4 0 24.35 2.08 3 -7 0 29.79 2.65 4 3 0 24.16 3.54 -7 4 0 17.80 2.28 -7 4 0 22.98 2.75 -3 7 0 26.18 2.83 -4 -3 0 24.53 2.50 7 -4 0 14.05 3.72 7 -4 0 21.32 2.34 7 -4 0 26.58 2.02 -4 -3 0 23.47 2.32 -7 5 0 7.81 1.94 2 -7 0 8.02 1.65 -7 5 0 8.40 1.46 5 2 0 10.11 2.49 2 -7 0 7.91 1.60 7 -5 0 7.72 1.33 -5 -2 0 8.21 1.85 -5 -2 0 7.61 1.73 -2 7 0 6.91 1.74 7 -5 0 9.47 1.94 -7 6 0 17.76 2.94 6 1 0 16.15 3.34 -7 6 0 20.05 2.32 1 -7 0 22.28 2.35 -6 -1 0 21.78 3.19 7 -6 0 21.90 2.28 -6 -1 0 19.14 2.75 -1 7 0 20.84 2.55 7 -6 0 18.60 2.29 -7 7 0 57.23 3.57 7 0 0 45.24 5.46 -7 7 0 58.49 4.80 0 -7 0 58.29 3.95 -7 0 0 56.50 4.47 -7 0 0 50.21 4.13 0 7 0 56.95 4.45 7 -7 0 54.82 4.10 -8 1 0 59.78 4.77 1 7 0 51.55 4.42 7 -8 0 56.68 4.27 -1 -7 0 52.81 4.05 -7 8 0 56.40 4.92 6 -8 0 78.67 5.08 -8 2 0 78.36 5.49 2 6 0 70.74 5.32 -8 2 0 83.35 5.56 -6 8 0 76.18 5.64 -8 3 0 11.52 2.42 3 5 0 12.43 2.61 5 -8 0 16.51 2.87 -8 3 0 10.55 2.29 -5 8 0 11.89 2.47 8 -3 0 3.06 2.54 4 4 0 22.16 3.50 4 -8 0 33.92 3.00 -8 4 0 26.96 2.36 -8 4 0 29.14 3.29 8 -4 0 28.58 3.02 -4 8 0 24.84 3.06 8 -4 0 27.15 2.31 5 3 0 13.47 2.95 -8 5 0 13.22 1.91 -8 5 0 10.69 2.38 -3 8 0 11.72 2.43 -5 -3 0 13.17 2.33 8 -5 0 12.17 1.79 8 -5 0 12.05 2.31 -8 6 0 82.21 5.91 -8 6 0 76.85 4.54 2 -8 0 81.79 5.27 8 -6 0 83.21 4.43 8 -6 0 77.58 5.23 -2 8 0 80.98 5.56 -6 -2 0 81.62 5.37 1 -8 0 56.98 4.27 -8 7 0 51.67 4.73 -8 7 0 55.36 3.66 7 1 0 35.24 5.54 8 -7 0 58.14 4.34 -7 -1 0 54.46 4.49 -1 8 0 54.56 4.56 8 0 0 21.05 4.85 -8 8 0 34.06 4.02 0 -8 0 45.16 3.63 8 -8 0 30.51 3.59 0 8 0 36.63 3.79 1 8 0 36.18 3.88 9 -1 0 15.08 4.96 -8 9 0 32.88 4.84 2 7 0 0.37 1.06 -7 9 0 2.98 1.71 9 -2 0 0.90 2.31 -9 3 0 29.78 3.55 3 6 0 26.59 3.90 -6 9 0 33.96 3.88 -9 4 0 2.45 1.59 4 5 0 2.38 1.62 -5 9 0 3.13 1.56 9 -4 0 0.37 2.00 9 -4 0 3.44 1.56 9 -4 0 1.71 1.00 4 -9 0 1.78 1.34 -9 5 0 1.49 1.31 5 4 0 5.02 2.05 9 -5 0 2.22 1.23 9 -5 0 3.81 1.19 -4 9 0 2.35 1.60 6 3 0 28.01 4.72 3 -9 0 41.14 3.93 -9 6 0 32.35 3.91 9 -6 0 34.01 3.53 -3 9 0 34.36 3.85 7 2 0 3.00 2.11 -9 7 0 1.58 0.95 -9 7 0 1.71 1.38 -2 9 0 1.56 1.35 9 -7 0 2.20 1.23 8 1 0 21.60 5.27 1 -9 0 35.36 3.55 -9 8 0 31.55 2.94 -9 8 0 31.02 4.80 -1 9 0 36.43 4.06 -9 9 0 -0.31 1.39 9 0 0 1.66 2.31 0 9 0 0.38 1.29 3 7 0 31.38 4.58 7 -10 0 50.01 4.62 10 -3 0 13.04 4.95 -7 10 0 33.24 4.92 4 6 0 6.91 2.49 10 -4 0 8.91 2.57 10 -4 0 10.88 2.36 -6 10 0 10.58 2.92 10 -4 0 2.19 2.75 5 -10 0 10.47 3.01 5 5 0 14.06 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7 2 -1 14.23 3.73 -9 7 -1 19.74 2.59 9 -7 1 17.67 2.94 -2 9 1 18.48 3.27 8 1 -1 3.19 2.62 -9 8 -1 3.18 1.91 -9 8 -1 3.21 1.24 -1 9 1 2.86 1.62 9 0 -1 1.89 2.31 -9 9 -1 0.26 1.26 0 9 1 0.44 1.31 7 -10 -1 46.59 4.65 3 7 -1 31.76 3.95 -7 10 1 29.44 4.72 4 6 -1 33.99 4.35 6 -10 -1 68.03 6.11 -10 4 -1 49.92 5.05 10 -4 1 51.68 4.84 -6 10 1 50.30 5.17 5 5 -1 18.29 3.78 5 -10 -1 25.96 4.15 -10 5 -1 23.24 3.93 10 -5 1 24.61 3.85 -5 10 1 21.63 4.03 -10 6 -1 23.02 3.94 6 4 -1 16.03 3.67 -4 10 1 24.84 4.03 10 -6 1 24.73 3.77 -10 7 -1 20.61 3.87 7 3 -1 16.03 4.29 -3 10 1 19.87 3.56 0 0 -2 0.22 0.08 0 0 -2 -0.04 0.11 0 0 -2 0.47 0.18 0 0 -2 0.67 0.15 0 0 2 0.00 0.04 0 0 2 0.12 0.13 0 0 2 0.08 0.06 0 0 2 0.09 0.08 -1 0 -2 2028.29 69.83 1 -1 -2 1996.88 69.04 -1 0 -2 2009.46 70.12 -1 0 -2 1968.99 70.44 1 -1 -2 1977.21 67.57 0 1 -2 1975.53 70.63 -1 0 -2 2009.86 68.28 1 -1 -2 2066.46 70.19 -1 1 2 1968.83 67.43 1 0 2 2018.94 67.77 1 0 2 1956.49 69.00 -1 1 2 2031.65 69.50 -1 1 2 1975.53 67.64 -1 1 2 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-15 1.83 0.99 -1 2 -15 1.48 0.85 -1 2 -15 5.44 2.07 2 -1 -15 2.05 0.81 -1 2 -15 4.34 0.91 2 -1 -15 0.93 0.84 -1 -1 -15 0.67 1.18 -1 2 -15 1.46 0.94 1 -2 15 0.60 1.10 -1 3 -15 10.14 1.64 3 -2 -15 8.94 1.95 -2 -1 -15 7.45 2.03 -1 3 -15 12.43 2.92 -2 -1 -15 8.77 1.49 -1 3 -15 9.13 1.59 -2 -1 -15 7.13 2.34 -1 3 -15 8.90 1.17 3 -2 -15 8.27 1.43 -2 -1 -15 7.57 1.64 1 -3 15 9.13 2.39 2 -2 -15 4.36 1.92 -2 0 -15 3.96 1.09 0 2 -15 3.77 1.89 -2 0 -15 6.85 1.86 2 -2 -15 2.50 1.32 2 -2 -15 4.87 1.18 2 -2 -15 5.86 1.35 0 2 -15 4.80 1.22 -2 0 -15 2.49 1.56 0 2 -15 3.56 1.08 -2 0 -15 4.93 1.25 1 -2 -15 1.58 0.84 1 1 -15 1.21 0.80 -2 1 -15 0.27 1.08 -2 1 -15 -0.59 0.76 1 1 -15 2.51 0.69 1 -2 -15 1.40 1.06 -2 1 -15 1.11 0.80 1 -2 -15 2.34 1.54 1 1 -15 1.30 0.77 1 -2 -15 1.42 0.81 -2 1 -15 1.78 1.09 2 -1 15 1.00 0.91 0 -2 -15 1.12 0.80 2 0 -15 0.55 0.75 2 0 -15 0.77 1.13 0 -2 -15 1.35 1.04 0 -2 -15 1.99 0.98 -2 2 -15 2.03 0.95 -2 2 -15 0.33 0.87 2 0 -15 0.09 0.67 -2 2 -15 1.83 1.76 2 0 -15 -0.08 0.54 0 -2 -15 0.70 1.26 -2 2 -15 1.21 0.73 2 -2 15 1.16 1.10 3 -1 -15 1.03 0.73 -1 -2 -15 -0.35 0.68 -1 -2 -15 0.11 1.02 -2 3 -15 0.93 0.87 3 -1 -15 0.17 0.76 -1 -2 -15 1.66 1.21 -1 -2 -15 -0.09 0.69 -2 3 -15 2.40 0.77 -2 3 -15 -0.36 1.24 -2 3 -15 0.70 0.80 3 -1 -15 0.84 0.77 2 -3 15 -0.20 0.88 -2 -2 -15 6.79 1.34 -2 4 -15 12.03 1.91 4 -2 -15 8.03 2.05 -2 -2 -15 8.25 2.28 4 -2 -15 8.71 1.49 -2 -2 -15 8.10 1.85 -2 -2 -15 9.49 2.82 -2 4 -15 2.35 2.08 -2 4 -15 8.47 1.24 2 -4 15 9.10 2.47 -3 -1 -15 2.91 1.21 -1 4 -15 4.96 1.37 -3 -1 -15 2.56 1.52 -3 -1 -15 3.03 1.82 -1 4 -15 4.59 0.74 4 -3 -15 4.21 1.25 -3 -1 -15 4.34 1.10 -1 4 -15 3.65 1.86 -1 4 -15 4.14 1.00 4 -3 -15 3.95 1.48 1 -4 15 2.97 1.81 -3 0 -15 19.91 2.24 0 3 -15 19.19 2.25 3 -3 -15 20.64 3.10 3 -3 -15 22.04 2.44 -3 0 -15 20.19 3.27 0 3 -15 19.88 3.72 0 3 -15 18.60 1.37 0 3 -15 18.69 1.74 -3 0 -15 20.68 3.65 -3 0 -15 17.74 2.41 3 -3 -15 20.17 3.90 0 -3 15 21.13 3.66 1 2 -15 7.58 1.31 2 -3 -15 7.99 1.58 -3 1 -15 10.93 2.66 1 2 -15 8.26 1.52 -3 1 -15 6.21 1.35 2 -3 -15 8.89 2.72 -3 1 -15 9.31 2.19 -3 1 -15 7.81 1.56 2 -3 -15 7.62 1.99 1 2 -15 12.48 2.99 1 -3 -15 0.86 0.78 2 1 -15 0.49 0.70 1 -3 -15 1.46 1.45 -3 2 -15 -0.82 1.12 2 1 -15 1.36 0.79 -3 2 -15 0.50 0.58 -3 2 -15 0.00 0.71 1 -3 -15 0.48 1.10 -3 2 -15 2.58 1.24 2 1 -15 0.35 0.54 3 -2 15 0.01 0.87 3 0 -15 6.04 1.42 0 -3 -15 6.63 2.11 3 0 -15 3.92 1.16 0 -3 -15 4.00 1.35 3 0 -15 5.18 0.97 0 -3 -15 5.50 2.25 -3 3 -15 6.22 1.45 -3 3 -15 6.92 2.35 -3 3 -15 5.00 1.14 -3 3 -15 8.23 1.84 3 -3 15 5.58 1.86 -1 -3 -15 0.50 0.83 -3 4 -15 -0.26 0.36 -3 4 -15 -0.32 0.79 -1 -3 -15 0.32 1.08 4 -1 -15 -0.01 0.87 -1 -3 -15 1.46 1.46 4 -1 -15 -0.33 0.61 3 -4 15 0.88 1.30 4 -4 -15 -0.08 0.85 4 -4 -15 -0.40 0.65 -4 0 -15 0.70 1.25 -4 0 -15 0.31 1.46 -4 0 -15 0.11 0.87 0 4 -15 2.17 1.27 -4 1 -15 5.44 1.25 -4 1 -15 2.77 1.18 -4 1 -15 4.13 2.19 -4 1 -15 2.43 1.56 1 3 -15 3.35 0.82 3 -4 -15 2.73 1.18 3 -4 -15 3.69 1.90 1 3 -15 6.64 2.25 1 3 -15 4.78 1.21 3 -4 -15 2.96 1.41 2 2 -15 7.49 0.93 -4 2 -15 7.62 2.45 2 2 -15 11.93 1.77 -4 2 -15 9.98 1.68 2 2 -15 12.60 1.33 2 -4 -15 8.82 2.64 2 -4 -15 9.66 1.82 2 -4 -15 7.63 2.14 -4 2 -15 6.43 2.03 -4 2 -15 10.04 1.82 1 -4 -15 -0.12 0.84 3 1 -15 1.63 0.89 1 -4 -15 1.59 1.29 3 1 -15 -0.07 0.68 1 -4 -15 0.33 1.34 -4 3 -15 0.68 1.14 -4 3 -15 -1.63 1.23 -4 3 -15 -0.56 0.52 3 1 -15 0.42 0.54 4 -3 15 1.28 1.21 -4 4 -15 3.22 1.68 0 -4 -15 0.38 1.16 0 -4 -15 0.71 0.93 4 0 -15 0.60 0.69 -4 4 -15 0.19 1.01 -4 4 -15 1.87 0.78 4 0 -15 1.66 0.91 0 -4 -15 -0.53 0.94 0 0 -16 -0.21 0.65 0 0 -16 1.54 1.01 -1 0 -16 1.69 0.87 0 1 -16 -0.69 0.61 1 -1 -16 -0.85 0.82 1 -1 -16 -0.99 0.56 0 1 -16 3.42 1.95 1 -1 -16 1.25 1.32 0 1 -16 2.03 1.00 1 -1 -16 0.78 0.87 0 1 -16 -1.14 0.72 -1 0 -16 -1.14 0.85 -1 0 -16 4.56 1.83 -1 0 -16 0.73 0.82 -1 1 -16 -0.31 0.95 1 0 -16 1.15 0.88 0 -1 -16 2.25 1.18 -1 1 -16 -1.47 1.23 1 0 -16 0.31 0.88 0 -1 -16 -0.64 0.60 -1 1 -16 2.43 1.02 1 0 -16 3.51 1.99 0 -1 -16 0.85 0.76 0 -1 -16 0.22 1.34 -1 -1 -16 5.60 1.28 -1 2 -16 1.42 0.85 -1 -1 -16 4.18 2.06 -1 2 -16 5.39 1.39 -1 2 -16 5.97 1.51 -1 -1 -16 3.15 1.17 2 -1 -16 4.36 1.37 -1 2 -16 3.87 2.57 -1 -1 -16 3.87 1.61 2 -1 -16 4.07 0.98 2 -1 -16 9.14 2.19 2 -1 -16 3.40 1.19 1 -2 16 2.31 1.55 -2 -1 -16 6.41 2.04 -1 3 -16 10.68 2.84 3 -2 -16 4.86 1.18 -1 3 -16 6.76 1.43 3 -2 -16 5.31 2.25 3 -2 -16 3.85 1.49 -1 3 -16 6.64 1.09 2 -2 -16 14.07 2.02 0 2 -16 6.25 2.75 -2 0 -16 11.61 2.62 -2 0 -16 12.20 1.81 0 2 -16 17.98 2.24 0 2 -16 10.17 1.37 0 2 -16 12.90 1.97 -2 0 -16 13.01 2.03 2 -2 -16 12.83 2.44 2 -2 -16 9.85 2.77 -2 0 -16 13.30 3.11 1 -2 -16 2.62 1.43 1 1 -16 7.16 1.51 1 1 -16 3.03 0.85 1 -2 -16 4.08 1.17 1 -2 -16 5.03 2.24 1 1 -16 3.71 1.22 -2 1 -16 5.65 1.34 -2 1 -16 2.21 1.70 1 -2 -16 3.30 1.17 -2 1 -16 5.97 1.71 2 0 -16 1.82 1.02 2 0 -16 2.15 0.96 0 -2 -16 1.26 1.37 -2 2 -16 1.12 1.13 -2 2 -16 1.76 0.99 -2 2 -16 0.82 0.79 0 -2 -16 -1.55 0.82 0 -2 -16 0.63 0.86 2 0 -16 2.94 0.77 0 -2 -16 1.41 0.93 2 0 -16 0.30 1.29 2 -2 16 1.43 1.24 -2 3 -16 7.92 1.36 3 -1 -16 6.31 1.26 -2 3 -16 8.21 1.86 -1 -2 -16 8.08 2.41 2 -3 -16 5.04 2.21 2 -3 -16 5.65 1.81 2 -3 -16 7.16 1.54 -3 1 -16 3.45 1.70 -3 1 -16 4.17 1.33 1 2 -16 5.72 1.35 1 2 -16 9.94 2.94 2 1 -16 8.74 1.23 2 1 -16 13.22 3.16 1 -3 -16 5.23 2.32 2 1 -16 8.26 1.52 -3 2 -16 7.92 2.08 -3 2 -16 8.85 1.61 1 -3 -16 6.69 2.05 _exptl_absorpt_process_details 'SADABS 2014/4' _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_max 0.9485 _exptl_absorpt_correction_T_min 0.7698 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71073 8.366 8.371 13.381 90.010 90.035 119.887 ) _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 28505 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' 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 C1 C 0.2346(2) 0.2085(2) 0.24504(11) 0.0321(3) Uani 1 1 d . . . . . C2 C 0.1826(2) 0.2964(2) 0.17487(12) 0.0373(4) Uani 1 1 d . . . . . H2 H 0.1472 0.2463 0.1096 0.045 Uiso 1 1 calc R U . . . C3 C 0.1825(3) 0.4570(2) 0.20009(14) 0.0468(5) Uani 1 1 d . . . . . H3 H 0.1458 0.5167 0.1525 0.056 Uiso 1 1 calc R U . . . C4 C 0.2361(3) 0.5303(3) 0.29483(14) 0.0520(5) Uani 1 1 d . . . . . H4 H 0.2367 0.6409 0.3119 0.062 Uiso 1 1 calc R U . . . C5 C 0.2888(3) 0.4441(3) 0.36498(14) 0.0478(5) Uani 1 1 d . . . . . H5 H 0.3255 0.4955 0.4298 0.057 Uiso 1 1 calc R U . . . C6 C 0.2880(2) 0.2831(2) 0.34067(12) 0.0391(4) Uani 1 1 d . . . . . H6 H 0.3236 0.2234 0.3888 0.047 Uiso 1 1 calc R U . . . C7 C 0.2305(2) 0.0344(2) 0.22101(11) 0.0346(4) Uani 1 1 d . . . . . O1 O 0.26226(18) -0.05526(16) 0.28111(8) 0.0487(4) 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 C1 0.0252(8) 0.0259(8) 0.0412(7) 0.0067(6) 0.0066(6) 0.0096(6) C2 0.0308(8) 0.0356(9) 0.0446(8) 0.0101(7) 0.0085(7) 0.0159(7) C3 0.0478(11) 0.0408(10) 0.0598(10) 0.0183(8) 0.0161(8) 0.0281(9) C4 0.0564(12) 0.0346(10) 0.0691(11) 0.0089(9) 0.0242(10) 0.0258(9) C5 0.0506(11) 0.0344(10) 0.0519(9) -0.0005(8) 0.0107(8) 0.0163(9) C6 0.0370(9) 0.0313(9) 0.0430(8) 0.0048(7) 0.0043(7) 0.0125(7) C7 0.0305(8) 0.0260(8) 0.0429(8) 0.0051(7) 0.0014(6) 0.0107(7) O1 0.0629(9) 0.0355(7) 0.0515(7) 0.0034(5) -0.0098(6) 0.0274(7) 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 C2 C1 C6 119.92(16) . . ? C2 C1 C7 121.01(15) . . ? C6 C1 C7 119.06(14) . . ? C3 C2 C1 119.97(17) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 119.74(17) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 120.64(17) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 119.98(17) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 119.75(16) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? O1 C7 C1 124.02(14) . . ? O1 C7 C7 116.95(15) . 5 ? C1 C7 C7 118.92(14) . 5 ? 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 C1 C2 1.390(2) . ? C1 C6 1.397(2) . ? C1 C7 1.474(2) . ? C2 C3 1.386(2) . ? C2 H2 0.9500 . ? C3 C4 1.383(3) . ? C3 H3 0.9500 . ? C4 C5 1.384(3) . ? C4 H4 0.9500 . ? C5 C6 1.381(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O1 1.2166(19) . ? C7 C7 1.539(3) 5 ?