#------------------------------------------------------------------------------ #$Date: 2019-05-18 08:14:21 +0300 (Sat, 18 May 2019) $ #$Revision: 215299 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/83/2108395.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2108395 loop_ _publ_author_name 'Tcho\'n, Daniel' 'Makal, Anna' _publ_section_title ; Structure and piezochromism of pyrene-1-carbaldehyde at high pressure ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first ; ; _journal_paper_doi 10.1107/S2052520619003354 _journal_volume 75 _journal_year 2019 _chemical_formula_moiety 'C17 H10 O' _chemical_formula_sum 'C17 H10 O' _chemical_formula_weight 230.25 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2018-06-25 _audit_creation_method ; Olex2 1.2 (compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 109.691(17) _cell_angle_beta 99.378(15) _cell_angle_gamma 100.628(12) _cell_formula_units_Z 2 _cell_length_a 6.7049(9) _cell_length_b 8.1989(12) _cell_length_c 10.329(2) _cell_measurement_reflns_used 850 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.2310 _cell_measurement_theta_min 1.8410 _cell_volume 509.66(16) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.689 _diffrn_measured_fraction_theta_max 0.477 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -150.00 -94.00 0.2000 0.1970 omega____ theta____ kappa____ phi______ frames - -20.0000 70.0000 -24.2319 280 #__ type_ start__ end____ width___ exp.time_ 2 omega -150.00 -94.00 0.2000 0.1970 omega____ theta____ kappa____ phi______ frames - -20.0000 70.0000 155.7681 280 #__ type_ start__ end____ width___ exp.time_ 3 omega -105.00 -77.20 0.2000 0.1970 omega____ theta____ kappa____ phi______ frames - 20.0000 70.0000 155.7700 139 #__ type_ start__ end____ width___ exp.time_ 4 omega -105.00 -74.80 0.2000 0.1970 omega____ theta____ kappa____ phi______ frames - 20.0000 70.0000 -24.2300 151 #__ type_ start__ end____ width___ exp.time_ 5 omega -96.00 -30.00 0.2000 0.1970 omega____ theta____ kappa____ phi______ frames - 20.0000 -70.0000 24.2300 330 #__ type_ start__ end____ width___ exp.time_ 6 omega -101.40 -66.00 0.2000 0.1970 omega____ theta____ kappa____ phi______ frames - -20.0000 -70.0000 -155.7700 177 #__ type_ start__ end____ width___ exp.time_ 7 omega -102.80 -66.00 0.2000 0.1970 omega____ theta____ kappa____ phi______ frames - -20.0000 -70.0000 24.2300 184 #__ type_ start__ end____ width___ exp.time_ 8 omega -96.00 -30.00 0.2000 0.1970 omega____ theta____ kappa____ phi______ frames - 20.0000 -70.0000 -155.7700 330 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'dectris-CrysAlisPro-abstract goniometer imported dectris images' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0161120000 _diffrn_orient_matrix_UB_12 -0.0283252000 _diffrn_orient_matrix_UB_13 -0.0513633000 _diffrn_orient_matrix_UB_21 0.0718074000 _diffrn_orient_matrix_UB_22 0.0254330000 _diffrn_orient_matrix_UB_23 0.0007208000 _diffrn_orient_matrix_UB_31 0.0190445000 _diffrn_orient_matrix_UB_32 -0.0528641000 _diffrn_orient_matrix_UB_33 0.0038434000 _diffrn_radiation_monochromator synchrotron _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.4859 _diffrn_reflns_av_R_equivalents 0.163 _diffrn_reflns_av_unetI/netI 0.0390 _diffrn_reflns_Laue_measured_fraction_full 0.689 _diffrn_reflns_Laue_measured_fraction_max 0.477 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 2730 _diffrn_reflns_point_group_measured_fraction_full 0.689 _diffrn_reflns_point_group_measured_fraction_max 0.477 _diffrn_reflns_theta_full 16.950 _diffrn_reflns_theta_max 22.683 _diffrn_reflns_theta_min 1.476 _diffrn_source synchrotron _exptl_absorpt_coefficient_mu 0.048 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.27480 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.500 _exptl_crystal_description ; ; _exptl_crystal_F_000 240 _refine_diff_density_max 0.918 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.219 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.579 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 165 _refine_ls_number_reflns 2730 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.579 _refine_ls_R_factor_all 0.2224 _refine_ls_R_factor_gt 0.1596 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.4088 _refine_ls_wR_factor_ref 0.4539 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1587 _reflns_number_total 2730 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file xk5054sup1.cif _cod_data_source_block 8kbar _cod_original_cell_volume 509.65(16) _cod_database_code 2108395 _shelx_shelxl_version_number 2016/6 _chemical_oxdiff_formula 'C17 H10 O1' _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. ; _diffrn_oxdiff_twin_integration_method simultaneous _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.690(6) 0.111(3) 0.199(5) 2. Fixed Uiso At 1.2 times of: All C(H) groups 3.a Aromatic/amide H refined with riding coordinates: C10(H10), C3(H3), C13(H13), C4(H4), C11(H11), C14(H14), C6(H6), C8(H8), C17(H17), C7(H7) ; _shelx_res_file ; TITL 3d_twin1_hklf4_a.res in P-1 3d_twin1_hklf4.res created by SHELXL-2016/6 at 18:46:45 on 25-Jun-2018 REM Old TITL 3d_twin1_hklf4 in P-1 REM SHELXT solution in P-1 REM R1 0.413, Rweak 0.015, Alpha 0.120, Orientation as input REM Formula found by SHELXT: C17 O CELL 0.4859 6.7049 8.1989 10.3289 109.691 99.378 100.628 ZERR 2 0.0009 0.0012 0.0023 0.017 0.015 0.012 LATT 1 SFAC C H O DISP C 0.001 0.001 6.068 DISP H -0 0 0.607 DISP O 0.004 0.003 13.336 UNIT 34 20 2 L.S. 10 PLAN 20 BOND $H list 4 fmap 2 acta OMIT 3 0 -7 OMIT 1 2 3 OMIT -4 -8 9 REM REM REM WGHT 0.200000 BASF 0.11145 0.19898 FVAR 9.17014 C15 1 0.242225 0.476157 0.456410 11.00000 0.02067 0.01673 = 0.01895 0.00665 0.01012 0.00695 C16 1 0.236906 0.435157 0.310128 11.00000 0.02003 0.01718 = 0.02302 0.00638 0.00798 0.00627 O1 3 0.406305 1.015184 0.805673 11.00000 0.07181 0.01976 = 0.02845 -0.00786 0.01747 -0.00003 C2 1 0.289288 0.656748 0.552200 11.00000 0.01922 0.01453 = 0.01943 0.00214 0.00501 0.00377 C12 1 0.200093 0.331301 0.504700 11.00000 0.02447 0.01970 = 0.01693 0.00857 0.00824 0.00860 C10 1 0.152298 0.113654 0.265721 11.00000 0.02828 0.01887 = 0.02694 0.00641 -0.00054 0.00591 AFIX 43 H10 2 0.122280 -0.004977 0.203340 11.00000 -1.20000 AFIX 0 C3 1 0.326393 0.796005 0.496366 11.00000 0.02196 0.01671 = 0.02882 0.00609 0.00156 0.00278 AFIX 43 H3 2 0.355438 0.915232 0.557311 11.00000 -1.20000 AFIX 0 C13 1 0.206749 0.370165 0.647557 11.00000 0.02869 0.02907 = 0.01698 0.01302 0.00416 0.00681 AFIX 43 H13 2 0.180832 0.277422 0.680176 11.00000 -1.20000 AFIX 0 C5 1 0.278490 0.577508 0.259934 11.00000 0.02647 0.01966 = 0.01946 0.00571 0.00668 0.00615 C4 1 0.319924 0.757326 0.358674 11.00000 0.03353 0.01785 = 0.02582 0.01122 0.00722 0.00749 AFIX 43 H4 2 0.343184 0.850676 0.326493 11.00000 -1.20000 AFIX 0 C11 1 0.154837 0.151327 0.403998 11.00000 0.02734 0.01624 = 0.02460 0.00869 0.00448 0.00693 AFIX 43 H11 2 0.126203 0.057093 0.434724 11.00000 -1.20000 AFIX 0 C14 1 0.251393 0.544752 0.740419 11.00000 0.03149 0.02798 = 0.00814 0.00310 0.00969 0.00844 AFIX 43 H14 2 0.253049 0.568083 0.835216 11.00000 -1.20000 AFIX 0 C9 1 0.195640 0.255654 0.214853 11.00000 0.02191 0.01964 = 0.02386 0.00310 0.00088 0.00528 C6 1 0.276882 0.535545 0.116760 11.00000 0.05092 0.03043 = 0.01737 0.01416 0.01138 0.01189 AFIX 43 H6 2 0.300993 0.627298 0.082925 11.00000 -1.20000 AFIX 0 C8 1 0.196700 0.219271 0.071799 11.00000 0.03877 0.02278 = 0.01850 -0.00078 0.00309 0.00915 AFIX 43 H8 2 0.168542 0.101425 0.008264 11.00000 -1.20000 AFIX 0 C1 1 0.294644 0.689194 0.696546 11.00000 0.02340 0.02211 = 0.01430 0.00099 0.00685 0.00686 C17 1 0.351572 0.868442 0.811410 11.00000 0.03789 0.02722 = 0.02103 -0.00132 0.00912 0.00610 AFIX 43 H17 2 0.344531 0.869089 0.900757 11.00000 -1.20000 AFIX 0 C7 1 0.240209 0.360773 0.025346 11.00000 0.05444 0.04036 = 0.01450 0.01130 0.01141 0.01254 AFIX 43 H7 2 0.244369 0.336192 -0.068749 11.00000 -1.20000 AFIX 0 HKLF 5 REM 3d_twin1_hklf4_a.res in P-1 REM R1 = 0.1596 for 1587 Fo > 4sig(Fo) and 0.2224 for all 2730 data REM 165 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.918, deepest hole -0.829, 1-sigma level 0.219 Q1 1 0.1302 0.2501 0.5416 11.00000 0.05 0.92 Q2 1 0.2219 0.6227 0.5979 11.00000 0.05 0.86 Q3 1 0.3588 0.7318 0.5189 11.00000 0.05 0.86 Q4 1 0.1958 0.4343 0.6473 11.00000 0.05 0.82 Q5 1 0.1781 0.6407 0.3721 11.00000 0.05 0.81 Q6 1 0.1996 0.5170 0.2970 11.00000 0.05 0.76 Q7 1 0.2075 0.6657 0.3497 11.00000 0.05 0.76 Q8 1 0.1843 0.3525 0.5644 11.00000 0.05 0.75 Q9 1 0.3502 0.7527 0.6805 11.00000 0.05 0.74 Q10 1 0.0333 0.0040 0.2980 11.00000 0.05 0.74 Q11 1 0.2103 0.3074 0.5620 11.00000 0.05 0.73 Q12 1 0.4146 0.9506 0.7465 11.00000 0.05 0.70 Q13 1 0.1432 0.3645 0.3353 11.00000 0.05 0.69 Q14 1 -0.0016 -0.0369 0.2815 11.00000 0.05 0.69 Q15 1 0.4441 0.7523 0.2410 11.00000 0.05 0.69 Q16 1 0.1751 0.4122 0.4941 11.00000 0.05 0.69 Q17 1 0.0415 0.1960 0.5367 11.00000 0.05 0.69 Q18 1 0.3739 0.5869 0.4284 11.00000 0.05 0.69 Q19 1 0.2996 0.8609 0.5772 11.00000 0.05 0.68 Q20 1 0.4509 0.8231 0.5254 11.00000 0.05 0.68 ; _shelx_res_checksum 80097 _shelx_hkl_file ; 0 -1 1 133181. 122.257 1 0 -1 0 68673.7 241.163 1 0 -2 2 26241.5 79.8659 1 0 2 -1 62800.2 78.5002 1 0 -2 0 647.783 21.6808 1 0 -3 3 3148.26 50.7233 1 0 -3 2 22825.8 68.3646 1 0 -3 1 1340.24 17.6290 1 0 -4 4 183.433 26.1627 1 0 -4 3 17744.0 64.2046 1 0 4 -2 3650.25 25.9620 1 0 4 -1 668.371 20.9573 1 0 4 0 17.0358 27.6179 1 0 -5 5 4215.18 65.1540 1 0 -5 4 1194.53 38.7594 1 0 5 -3 3097.06 31.2628 1 0 -5 2 8.11721 12.9880 1 0 -5 1-5.86377 21.9576 1 0 6 -6 1476.73 57.3105 1 0 6 -5 509.587 46.7343 1 0 -6 4 1385.69 45.9319 1 0 6 -3 12.5925 29.7666 1 0 -6 2 37209.1 170.262 1 0 -6 1 28956.9 173.577 1 0 -7 7 7516.56 137.602 1 0 -7 6 4580.43 84.8154 1 0 -7 5 1330.29 59.1211 1 0 -7 4 719.019 39.9495 1 0 7 -3 1744.13 49.6988 1 0 7 -2 62279.2 243.827 1 0 7 -1 504.798 66.9394 1 0 -8 7 5916.48 162.590 1 0 -8 5 489.805 79.2923 1 0 -8 4 1732.97 76.1351 1 0 8 -3 422.560 84.9027 1 0 -9 8 1160.11 97.4458 1 0 9 -7 322.785 78.3381 1 0 9 -6-12.9296 53.6803 1 0 9 -5 1022.27 59.3847 1 0 -9 4 327.430 51.7149 1 0 9 -3 486.522 55.0974 1 0 -9 2 21.6045 66.1834 1 0 -10 9 5345.50 212.447 1 0 -10 8-4.35646 94.1962 1 0 -10 7 214.597 72.5087 1 0 -10 6 18.2706 63.2288 1 0 10 -5 4717.68 89.9144 1 0 10 -4 4565.34 90.1945 1 0 10 -3-6.57393 62.8052 1 2 0 11-90.8123 323.999 -3 -8 5 4-90.8123 323.999 -2 0 -10 2-90.8123 323.999 1 0 -11 9 6126.17 172.706 1 0 -11 8 258.306 83.4856 1 0 -11 7 190.556 80.9766 1 0 -11 6 136.837 72.6307 1 0 -11 5 437.658 65.0375 1 0 -11 4 617.886 75.2174 1 0 -11 3 113.628 76.9637 1 0 12 -9 488.749 177.453 1 0 -12 8 244.282 95.9816 1 0 -12 7-34.8124 84.3860 1 0 12 -6 49.0623 79.0174 1 0 12 -5 322.655 82.0828 1 0 -12 4 606.813 90.8987 1 1 -12 3 554.712 122.481 1 1 -12 4 105.835 77.6425 1 1 -12 5 145.398 73.8657 1 -1 12 -6-29.3852 74.7325 1 1 -12 7 259.356 88.1284 1 -1 12 -8 28.7484 88.7540 1 -1 12 -9-37.1080 91.1307 1 -1 11 -3 176.186 72.6864 1 -1 11 -4 2.28526 64.7487 1 1 -11 5 983.421 70.1456 1 1 -11 6 456.657 71.4934 1 -1 11 -7 152.389 76.4461 1 1 -11 8 179.711 77.5271 1 1 -11 9 1510.87 217.946 1 -1 10 -2 159.850 88.0697 1 -1 10 -3 80.1762 58.1070 1 1 -10 4 143.861 51.2216 1 -1 10 -6 351.738 63.6273 1 1 -10 7 120.988 63.9507 1 1 -10 8 121.130 88.0867 1 -1 9 -2-37.8537 50.8786 1 -1 9 -3 220.631 47.3427 1 -1 9 -4 165.206 65.5246 1 1 -9 5 106.909 64.5943 1 1 -9 6 259.251 69.7726 1 -1 9 -7 53.7046 68.3440 1 1 -9 8 123.045 126.908 1 1 -8 1 459.589 121.852 1 -1 8 -2-5.39811 49.7518 1 -1 8 -3 35.2676 37.7271 1 1 -8 4 2438.19 55.0132 1 -1 8 -5 985.177 63.0464 1 -1 8 -6 1061.68 67.0963 1 -1 8 -7 1392.14 98.0001 1 -1 7 -1 8745.31 132.090 1 1 -7 2 27429.7 129.367 1 1 -7 3 425.845 37.0789 1 -1 7 -4 1629.15 43.9647 1 -1 7 -5 264.320 46.6023 1 1 -7 6 6299.96 144.512 1 1 -6 1 35791.0 136.019 1 1 -6 2 34.7462 17.3347 1 -1 6 -3 26.3910 18.3823 1 1 -6 4 2740.95 40.2020 1 1 -6 5 191.886 39.7839 1 1 -6 6 171.597 64.6144 1 1 -5 0 6694.61 145.309 1 1 -5 1 2455.53 46.8140 1 -1 5 -2 1378.20 58.4894 1 1 -5 3 1182.84 32.3419 1 -1 5 -4 15954.6 91.4745 1 1 -5 5 1620.79 71.0749 1 -1 4 0 15.5876 25.3305 1 1 -4 1 159.445 16.7259 1 -1 4 -2 2053.56 27.5230 1 1 -4 3 95283.9 247.015 1 1 -4 4 30092.6 204.067 1 1 -3 0 645.892 14.5714 1 -1 3 -1 12.3979 9.14117 1 -1 3 -2 378.012 13.8014 1 1 -3 3 80295.4 272.543 1 1 -2 0 2300.50 17.9726 1 1 -2 1 299.557 7.67788 1 -1 2 -2 11236.6 121.768 1 -1 1 0 314.316 8.64262 1 1 -1 1 53096.4 183.824 1 1 0 0 5008.09 33.1620 1 -1 -1 1 25081.0 59.2000 1 -1 -1 0 12205.5 65.1612 1 -1 -2 3 24938.7 96.8616 1 1 2 -2 1222.38 19.7279 1 -1 -2 1 7675.49 48.9044 1 1 2 0 4905.12 56.5092 1 1 3 -4 8644.00 71.5117 1 -1 -3 3 142171. 394.032 1 1 3 0 3943.25 64.2681 1 -1 -4 5 5468.42 70.9359 1 1 4 -4 36100.0 145.404 1 -1 -4 3 31175.9 119.906 1 1 4 -2 4730.69 46.4646 1 1 4 -1 707.264 31.7046 1 -1 -4 0 11923.9 192.669 1 -1 -5 6 114.375 41.9472 1 1 5 -5 56.4707 36.4162 1 -1 -5 4 184.310 47.7518 1 1 -1 -6 2612.65 248.077 -3 1 5 -4 2612.65 248.077 1 1 5 -3 9014.39 69.8586 1 -1 -5 2 2268.12 51.3885 1 -1 -5 1 4064.73 68.3206 1 -1 -6 6 266.921 48.9136 1 -1 -6 5 1655.59 56.9043 1 -1 -6 4 308.716 41.9333 1 -1 -6 3 2784.77 53.3189 1 -1 -6 2 16411.6 122.026 1 -1 -6 1 43029.3 213.896 1 -1 -7 7 336.736 56.6859 1 -1 -7 6 7049.47 106.979 1 -1 -7 5 3863.36 81.0820 1 1 7 -4 83.6906 39.1620 1 -1 -7 3 695.929 45.0177 1 1 7 -1 161.643 56.2525 1 1 8 -8 279.780 72.2402 1 1 8 -7 240.201 73.5402 1 1 -2 -9 77.6153 217.664 -3 5 -7 0 77.6153 217.664 -2 1 8 -6 77.6153 217.664 1 1 8 -5 17.7992 65.2838 1 1 8 -4 738.425 74.1055 1 -1 -8 3 882.141 69.2632 1 1 8 -2 59.1270 58.7231 1 -1 -9 8 17.1844 85.2771 1 1 9 -7 232.514 99.0756 1 1 9 -6 35.1553 59.9244 1 1 9 -5 4055.47 80.7405 1 1 9 -4 499.597 58.0308 1 1 9 -3 80.2843 57.4892 1 1 9 -2 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197.673 3 -2 -6 1 5351.91 98.3773 3 -2 -6 0 335.007 75.9626 3 2 6 1 102.570 79.7104 3 2 6 2 517.749 119.739 3 -2 -6 -4-88.7845 158.167 3 2 7 -8 150.277 184.288 3 2 7 -7 1743.68 205.296 3 -2 -7 6 742.364 214.699 3 -2 -7 5-153.576 126.856 3 2 7 -4 407.897 130.543 3 2 7 -3 453.299 211.343 3 -2 -7 1 150.332 155.778 3 -2 -7 0 408.173 96.5346 3 -2 -7 -1-31.3874 102.503 3 2 7 2-5.57112 109.568 3 2 7 3-33.4557 114.522 3 2 7 4 68.7871 122.399 3 2 8 -5 826.038 250.451 3 -2 -8 4 74.3886 149.831 3 -2 -8 3 961.848 151.234 3 -2 -8 2-272.633 178.080 3 2 8 -1 39.0959 164.135 3 -2 -8 0 311.582 118.785 3 -2 -8 -1 238.252 127.029 3 2 8 2-53.2006 129.280 3 2 8 3-10.5151 133.842 3 -2 -9 1 156.040 188.296 3 -2 -9 0 742.201 180.625 3 2 9 1 156.527 187.571 3 2 9 2 84.4425 210.430 3 2 9 3 560.807 219.553 3 3 -2 -13-1120.99 364.336 3 3 -2 -12-4764.30 811.258 3 -3 2 11 4503.95 328.263 3 -3 2 10-558.980 292.542 3 -3 2 9-256.453 279.912 3 -3 1 14 351.515 284.780 3 -3 1 13 170.313 284.994 3 -3 1 12 666.109 285.957 3 -3 1 11 1507.29 268.370 3 -3 1 10 276.978 237.168 3 -3 1 8 447.102 212.370 3 -3 1 7 3027.41 266.205 3 -3 0 14 767.713 235.869 3 -3 0 13 1034.82 232.455 3 -3 0 12 1224.09 223.997 3 -3 0 11 844.409 228.345 3 -3 0 9 710.651 183.149 3 -3 0 8 139.658 164.248 3 -3 0 7 72.6928 251.557 3 -3 -1 15 2274.80 231.690 3 3 1 -14 2379.36 213.899 3 -3 -1 13 613.222 179.323 3 -3 -1 12 596.022 162.846 3 -3 -1 11 569.197 164.781 3 -3 -1 10 2243.39 161.422 3 -3 -1 9 235.273 143.688 3 -3 -1 8 283.915 122.868 3 -3 -1 7 1403.74 117.236 3 -3 -1 6-25.9751 43.4125 3 -3 -1 5 240.476 124.615 3 3 1 5 320.026 206.922 3 3 1 6 9016.28 117.512 3 3 1 7 4398.60 330.798 3 3 1 9 3428.59 510.814 3 -3 -2 15 1311.18 201.847 3 -3 -2 14 352.784 175.333 3 -3 -2 13 245.583 145.679 3 3 2 -12 35.1229 134.580 3 -3 -2 10-74.6412 117.302 3 -3 -2 9 205.181 96.2927 3 -3 -2 8 139.917 89.7981 3 -3 -2 7 182.844 81.3288 3 -3 -2 6 431.045 80.1384 3 -3 -2 5 44.7467 41.1842 3 -3 -2 4 219.910 35.0850 3 3 2 -3 9111.66 64.8846 3 3 2 -2 1125.06 37.6147 3 -3 -2 1 106.634 32.8531 3 3 2 0 106.159 35.3532 3 3 2 1 11891.9 85.8154 3 3 2 2 8298.42 78.8791 3 -3 -2 -3-56.8207 68.3047 3 3 2 4-36.5741 49.6114 3 3 2 5 197.233 72.5196 3 3 2 6 5231.65 395.273 3 3 2 7 257.480 411.585 3 3 2 8-190.090 260.165 3 -3 -2 -9-87.2737 292.496 3 -3 -2 -10 436.322 366.202 3 -3 -3 14 236.800 155.639 3 -3 -3 13-0.14511 120.387 3 3 3 -12 748.793 114.425 3 3 3 -11 174.780 81.2259 3 -3 -3 10 112.361 68.9636 3 3 3 -9 147.198 62.0877 3 -3 -3 8 13711.1 121.024 3 3 3 -7 4928.01 55.8426 3 3 3 -6 25.1440 43.9947 3 -3 -3 5 155.288 28.6282 3 -3 -3 4 2052.28 47.5145 3 -3 -3 3 20755.6 101.013 3 -3 -3 2 110.491 39.7546 3 -3 -3 1 118.624 41.7831 3 -3 -3 0 248.457 44.0803 3 3 3 1 1465.06 57.1510 3 3 3 2 718.153 57.9019 3 3 3 3 16.4299 74.5905 3 3 3 4 324.780 59.0899 3 3 3 5 188.753 69.2269 3 -3 -4 7 283.164 43.6756 3 -3 -4 6 402.557 45.6200 3 3 4 -5 49.0597 47.5923 3 -3 -4 4 1847.86 56.9048 3 -3 -4 3 508.838 50.8470 3 -3 -4 2 255.021 64.9475 3 -3 -4 1 559.436 57.0517 3 -3 -4 0 338.973 56.8350 3 -3 -4 -1 246.322 61.9271 3 -3 -4 -2 181.718 69.1437 3 -3 -4 -3 249.199 70.1721 3 3 4 4 535.861 80.5589 3 3 4 5 233.231 96.3344 3 -3 -5 7 239.356 57.2411 3 -3 -5 6 177.467 56.2505 3 3 5 -5 311.345 56.6938 3 3 5 -4 304.494 58.1808 3 3 5 -3 69.3150 57.7700 3 -3 -5 2 91.3643 96.4544 3 -3 -5 1 11224.8 108.024 3 3 5 0 76.4001 67.0156 3 -3 -5 -1 241.937 73.4712 3 -3 -5 -2 417.529 81.6220 3 -3 -5 -4 368.766 121.670 3 3 6 -7 70.9912 77.3010 3 -3 -6 6 1464.51 74.8727 3 -3 -6 5 107.293 72.8472 3 -3 -6 4 603.136 73.8173 3 -3 -6 3 155.394 72.5891 3 -3 -6 2 3323.53 87.4317 3 3 6 1 200.418 84.5630 3 -3 -6 -2 226.638 90.4407 3 -3 -6 -3 232.663 104.145 3 -3 -6 -4 54.7397 105.840 3 -3 -7 8 10.0654 77.1843 3 3 7 -7 147.387 90.5831 3 -3 -7 4 579.720 169.483 3 3 7 -3 110.322 87.0217 3 3 7 -2-12.6864 90.8323 3 3 7 -1 203.522 95.2514 3 -3 -7 0 88.0892 150.151 3 -3 -7 -1 145.360 108.209 3 -3 -7 -2 285.555 113.906 3 -3 -7 -3 162.691 124.200 3 -3 -7 -4 397.702 178.422 3 -3 -8 8-3616.03 707.250 3 -3 -8 7-177.358 97.8948 3 -3 -8 6-15.5140 101.317 3 3 8 -5-22.3904 100.266 3 -3 -8 4 47.7358 107.246 3 -3 -8 3 55.2240 115.282 3 3 8 -1 79.8778 119.494 3 3 8 0 362.790 127.587 3 3 8 1-23.7787 137.336 3 3 8 2 111.634 142.516 3 -3 -8 -3 116.806 150.821 3 -3 -9 8 5.42170 118.716 3 -3 -9 7 13.5978 127.171 3 -3 -9 6-234.340 113.601 3 -3 -9 5 406.536 124.840 3 3 9 -4-85.7093 126.414 3 3 9 -3 2.41468 130.601 3 3 9 -2 143.086 147.026 3 3 9 -1 505.940 147.880 3 3 9 0 224.361 195.571 3 3 9 1 48.1221 160.750 3 3 9 2 223.122 168.618 3 -3 -9 -3-141.980 175.510 3 3 10 -4 146.139 179.268 3 3 10 -3-79.3422 154.552 3 3 10 -2-11.9403 164.912 3 -3 -10 1 160.537 172.158 3 -4 1 14 539.550 384.271 3 4 0 -14 705.211 291.623 3 -4 0 13 101.513 300.924 3 -4 0 12 371.395 263.978 3 -4 0 11-292.612 280.715 3 -4 0 9 4650.16 264.389 3 4 1 -14 8167.21 259.031 3 -4 -1 13 634.233 274.348 3 -4 -1 12 98.4139 224.901 3 -4 -1 11 135.857 203.590 3 -4 -1 10 711.907 175.205 3 -4 -1 9 437.496 169.838 3 -4 -1 8 85.8678 160.608 3 -4 -1 7 87.1949 177.417 3 -4 -2 14 1093.08 212.504 3 -4 -2 13 301.332 179.484 3 -4 -2 12 143.555 148.168 3 -4 -2 10-67.9365 128.104 3 -4 -2 9 693.810 123.253 3 -4 -2 8 90.3526 119.907 3 -4 -2 7 2.41822 114.214 3 -4 -2 6 156.981 55.0101 3 4 2 -5 22.9877 63.4709 3 4 2 -4 8.34906 66.7818 3 4 2 -2 2657.02 89.9781 3 -4 -2 1-38.2822 43.2036 3 4 3 -7 2001.20 84.9006 3 -4 -3 6 574.465 49.3932 3 -4 -3 5 165.758 48.5390 3 4 3 -4 120.151 56.3705 3 -4 -3 3 620.619 63.8834 3 -4 -3 2 168.841 59.2108 3 4 3 -1 126.756 52.1743 3 -4 -3 0 173.765 55.8079 3 4 3 1 118.511 60.0753 3 -4 -3 -2 22.4219 66.7326 3 -4 -3 -4-159.042 71.9790 3 -4 -4 7 278.065 53.4933 3 -4 -4 6-50.7019 55.9396 3 -4 -4 5 185.215 57.4770 3 -4 -4 4 357.141 60.9173 3 -4 -4 3-23.7936 59.4930 3 -4 -4 2 48.1864 61.5946 3 -4 -4 1 2.91490 66.4761 3 4 4 0 33.1942 68.6461 3 -4 -4 -2 716.089 110.207 3 4 4 4 510.384 93.8242 3 -4 -4 -5-123.304 95.9445 3 -4 -5 7 79.4533 63.6624 3 -4 -5 6 133.326 63.9203 3 -4 -5 5 40.5956 64.3832 3 -4 -5 4 372.788 69.5993 3 -4 -5 3 94.9309 69.1850 3 -4 -5 2 5999.75 100.138 3 4 5 0 44.7744 119.137 3 -4 -5 -1 290.654 90.3299 3 -4 -5 -2-6.70228 94.6912 3 4 5 3 1886.70 104.677 3 -4 -5 -4 465.926 106.608 3 -4 -6 7 689.494 75.5028 3 -4 -6 6 1827.94 99.8744 3 4 6 -4 225.198 138.362 3 -4 -6 3 224.906 79.0892 3 -4 -6 2 8566.32 118.303 3 -4 -6 1 251.698 88.2653 3 -4 -6 0 116.418 94.0610 3 -4 -6 -1 121.672 103.834 3 4 6 2 81.3722 107.094 3 4 6 3-131.964 111.531 3 -4 -6 -4 647.797 117.534 3 -4 -7 8-2.12430 194.329 3 -4 -7 7 803.088 94.2476 3 -4 -7 6 187.614 89.0506 3 4 7 -5 124.157 90.4972 3 4 7 -4 87.1314 91.6582 3 4 7 -3 442.340 97.8788 3 -4 -7 2 284.006 100.083 3 -4 -7 1 116.451 100.967 3 -4 -7 0 283.441 111.637 3 -4 -7 -1 433.229 121.801 3 -4 -7 -2 117.871 130.423 3 -4 -7 -3 453.147 150.576 3 -4 -7 -4-330.750 229.438 3 4 8 -8 44.7257 100.459 3 4 8 -7 94.0158 105.791 3 -4 -8 6 143.737 111.599 3 4 8 -5 254.475 118.026 3 4 8 -4 397.659 125.274 3 4 8 -3 85.7098 116.657 3 -4 -8 2 277.985 121.633 3 -4 -8 1-19.8041 142.035 3 4 8 0 1187.93 142.099 3 -4 -8 -1 414.413 150.215 3 -4 -8 -2 276.449 160.483 3 -4 -8 -3 28.6006 169.754 3 4 9 -8-98.7636 119.578 3 4 9 -7 114.732 123.193 3 4 9 -6-39.6663 128.648 3 4 9 -5 659.499 137.057 3 4 9 -4 715.783 143.076 3 4 9 -3 30.7747 145.848 3 4 9 -2 147.836 151.772 3 -4 -9 1 134.235 162.734 3 -4 -9 0 202.680 174.436 3 4 10 -8 379.713 156.559 3 -4 -10 7 131.053 146.026 3 4 10 -6 49.3312 152.975 3 4 10 -5 369.747 160.205 3 -5 -1 13-348.241 262.314 3 -5 -1 12 1147.64 250.539 3 -5 -1 11 228.179 249.704 3 5 3 -7 2152.20 115.466 3 5 3 -6 64.1094 95.6174 3 5 3 -5 292.655 100.539 3 5 3 -4 1836.39 105.569 3 -5 -3 3 1346.11 65.9255 3 -5 -3 2 219.253 59.9491 3 -5 -3 1 441.860 69.7505 3 -5 -4 7 228.200 66.7700 3 -5 -4 6 20.8971 68.2140 3 -5 -4 5 213.612 77.6923 3 -5 -4 4 248.497 68.8282 3 -5 -4 3 371.799 71.4313 3 5 4 -1 1245.83 124.468 3 -5 -4 0 148.304 81.2461 3 -5 -4 -1 523.969 89.5116 3 -5 -4 -2-110.121 90.4371 3 -5 -4 -3 256.716 101.565 3 5 4 4 647.771 149.201 3 5 4 5 781.584 159.372 3 -5 -5 7 279.468 74.0872 3 -5 -5 6 997.507 94.9003 3 5 5 -4 441.651 139.175 3 5 5 -3 563.209 84.4297 3 5 5 -2 2524.50 97.5262 3 5 5 -1 7254.22 122.673 3 -5 -5 0 442.787 96.5514 3 -5 -5 -1 559.740 104.652 3 -5 -5 -2 223.522 111.457 3 -5 -5 -3 256.265 117.760 3 -5 -5 -4-178.799 124.193 3 -5 -6 7-219.248 86.9596 3 -5 -6 6 625.189 93.5332 3 -5 -6 5 179.341 90.3208 3 -5 -6 4-59.6514 92.6530 3 -5 -6 3 20.2321 99.4280 3 -5 -6 2 112.130 100.949 3 -5 -6 1 273.901 107.606 3 -5 -6 0 339.322 116.599 3 5 6 1 664.848 119.341 3 -5 -6 -2 703.979 129.621 3 -5 -6 -3 353.637 139.873 3 -5 -6 -4 179.806 139.048 3 5 7 -8 154.176 204.396 3 -5 -7 7 34.1095 99.1369 3 -5 -7 6 173.433 103.770 3 -5 -7 5-41.7919 106.925 3 -5 -7 4-221.033 121.796 3 -5 -7 3 4.33214 110.768 3 -5 -7 2 122.359 117.280 3 -5 -7 1-142.630 126.705 3 -5 -7 0-202.012 127.429 3 5 7 1 162.108 145.562 3 -5 -7 -2 690.791 144.363 3 -5 -7 -3 732.870 149.651 3 -5 -7 -4 1866.47 302.047 3 -5 -8 8 86.9358 115.222 3 -5 -8 7 213.944 116.629 3 -5 -8 6 281.700 120.755 3 -5 -8 5 477.362 124.535 3 -5 -8 4 172.849 127.868 3 -5 -8 3 184.684 134.383 3 -5 -8 2 122.392 145.110 3 -5 -8 1 120.736 150.218 3 5 8 0 339.721 162.074 3 -5 -8 -1-311.560 232.897 3 -5 -9 8 57.9133 134.247 3 -5 -9 7-39.1804 137.655 3 -5 -9 6 179.842 145.826 3 -5 -9 5 544.633 151.700 3 -5 -9 4 341.805 162.308 3 -5 -9 3 7.91688 148.415 3 6 4 -6 4.30011 130.234 3 6 4 -5 13.1412 126.160 3 6 4 -4 22.5804 129.675 3 6 4 -3 55.9003 131.532 3 -6 -5 7-109.924 85.4724 3 -6 -5 6 718.211 95.8055 3 -6 -5 5 293.029 95.4498 3 -6 -5 4 162.495 96.1034 3 -6 -5 3 165.652 98.6717 3 6 5 -2 7635.30 139.446 3 -6 -5 1 2238.39 119.276 3 -6 -5 0 191.476 113.046 3 -6 -5 -1-475.792 154.160 3 6 5 2 1360.07 192.337 3 -6 -6 7 1059.09 102.557 3 -6 -6 6 1262.13 110.382 3 -6 -6 5 588.465 109.517 3 -6 -6 4 677.801 113.402 3 -6 -6 3 394.685 116.644 3 -6 -6 2 902.119 124.457 3 -6 -6 1 433.624 131.451 3 -6 -6 0 173.158 136.106 3 -6 -6 -1 202.859 145.824 3 -6 -6 -2-176.476 152.650 3 -6 -6 -3-615.417 163.841 3 -6 -7 7 743.203 112.457 3 -6 -7 6 762.306 118.846 3 6 7 -5 876.102 121.384 3 -6 -7 4 796.407 126.643 3 -6 -7 3 1042.44 135.776 3 -6 -7 2 728.523 144.117 3 -6 -7 1 688.574 150.022 3 -6 -7 0 789.405 160.487 3 6 8 -8 183.861 252.129 3 -6 -8 7-157.152 135.152 3 -6 -8 6-33.8998 133.559 3 -6 -8 5 162.317 141.541 3 -6 -8 4 710.586 155.504 3 -6 -8 3 1141.29 198.836 3 -6 -9 8-202.336 176.938 3 7 6 -7-37.9603 207.774 3 -7 -6 6-287.689 137.617 3 -7 -6 5-196.254 128.867 3 -7 -6 4-302.990 131.085 3 -7 -6 3-492.224 133.888 3 7 6 -2 35.4743 219.918 3 -7 -7 7-85.9134 130.450 3 -7 -7 6 201.418 139.496 3 -7 -7 5 131.513 145.047 3 -7 -7 4 228.476 190.511 3 ; _shelx_hkl_checksum 2959 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 C15 C 0.2422(7) 0.4762(6) 0.4564(7) 0.0178(13) Uani 1 1 d . C16 C 0.2369(7) 0.4352(6) 0.3101(7) 0.0199(13) Uani 1 1 d . O1 O 0.4063(7) 1.0152(5) 0.8057(5) 0.0456(14) Uani 1 1 d . C2 C 0.2893(7) 0.6567(6) 0.5522(7) 0.0189(12) Uani 1 1 d . C12 C 0.2001(7) 0.3313(6) 0.5047(7) 0.0191(12) Uani 1 1 d . C10 C 0.1523(8) 0.1137(7) 0.2657(8) 0.0262(15) Uani 1 1 d . H10 H 0.122280 -0.004977 0.203340 0.031 Uiso 1 1 calc R C3 C 0.3264(8) 0.7960(7) 0.4964(8) 0.0241(14) Uani 1 1 d . H3 H 0.355438 0.915232 0.557311 0.029 Uiso 1 1 calc R C13 C 0.2067(8) 0.3702(7) 0.6476(7) 0.0240(13) Uani 1 1 d . H13 H 0.180832 0.277422 0.680176 0.029 Uiso 1 1 calc R C5 C 0.2785(8) 0.5775(7) 0.2599(7) 0.0222(13) Uani 1 1 d . C4 C 0.3199(8) 0.7573(7) 0.3587(8) 0.0248(15) Uani 1 1 d . H4 H 0.343184 0.850676 0.326493 0.030 Uiso 1 1 calc R C11 C 0.1548(8) 0.1513(6) 0.4040(7) 0.0225(14) Uani 1 1 d . H11 H 0.126203 0.057093 0.434724 0.027 Uiso 1 1 calc R C14 C 0.2514(8) 0.5448(6) 0.7404(7) 0.0228(12) Uani 1 1 d . H14 H 0.253049 0.568083 0.835216 0.027 Uiso 1 1 calc R C9 C 0.1956(8) 0.2557(7) 0.2149(7) 0.0238(14) Uani 1 1 d . C6 C 0.2769(9) 0.5355(7) 0.1168(7) 0.0309(15) Uani 1 1 d . H6 H 0.300993 0.627298 0.082925 0.037 Uiso 1 1 calc R C8 C 0.1967(9) 0.2193(7) 0.0718(8) 0.0293(15) Uani 1 1 d . H8 H 0.168542 0.101425 0.008264 0.035 Uiso 1 1 calc R C1 C 0.2946(8) 0.6892(7) 0.6965(7) 0.0211(13) Uani 1 1 d . C17 C 0.3516(9) 0.8684(7) 0.8114(8) 0.0316(15) Uani 1 1 d . H17 H 0.344531 0.869089 0.900757 0.038 Uiso 1 1 calc R C7 C 0.2402(9) 0.3608(7) 0.0253(7) 0.0358(15) Uani 1 1 d . H7 H 0.244369 0.336192 -0.068749 0.043 Uiso 1 1 calc R 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 C15 0.021(3) 0.017(3) 0.019(3) 0.007(3) 0.010(3) 0.0069(19) C16 0.020(3) 0.017(3) 0.023(4) 0.006(3) 0.008(3) 0.006(2) O1 0.072(3) 0.020(2) 0.028(3) -0.008(2) 0.017(3) 0.0000(19) C2 0.019(3) 0.015(3) 0.019(3) 0.002(3) 0.005(3) 0.0038(18) C12 0.024(3) 0.020(3) 0.017(3) 0.009(3) 0.008(3) 0.009(2) C10 0.028(3) 0.019(3) 0.027(4) 0.006(3) -0.001(4) 0.006(2) C3 0.022(3) 0.017(3) 0.029(4) 0.006(3) 0.002(3) 0.0028(19) C13 0.029(3) 0.029(3) 0.017(3) 0.013(3) 0.004(3) 0.007(2) C5 0.026(3) 0.020(3) 0.019(3) 0.006(3) 0.007(3) 0.006(2) C4 0.034(3) 0.018(3) 0.026(4) 0.011(3) 0.007(4) 0.007(2) C11 0.027(3) 0.016(3) 0.025(4) 0.009(3) 0.004(3) 0.007(2) C14 0.031(3) 0.028(3) 0.008(3) 0.003(3) 0.010(3) 0.008(2) C9 0.022(3) 0.020(3) 0.024(4) 0.003(3) 0.001(3) 0.005(2) C6 0.051(4) 0.030(3) 0.017(3) 0.014(3) 0.011(4) 0.012(3) C8 0.039(3) 0.023(3) 0.019(3) -0.001(3) 0.003(4) 0.009(2) C1 0.023(3) 0.022(3) 0.014(3) 0.001(3) 0.007(3) 0.007(2) C17 0.038(3) 0.027(3) 0.021(4) -0.001(3) 0.009(4) 0.006(2) C7 0.054(4) 0.040(4) 0.014(3) 0.011(3) 0.011(4) 0.013(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0010 0.0010 '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 0.0040 0.0030 '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 C16 C15 C12 118.8(5) C2 C15 C16 120.5(4) C2 C15 C12 120.8(6) C15 C16 C5 119.6(5) C9 C16 C15 120.8(4) C9 C16 C5 119.6(6) C15 C2 C3 118.0(6) C1 C2 C15 117.9(4) C1 C2 C3 124.1(5) C13 C12 C15 119.1(5) C13 C12 C11 122.2(4) C11 C12 C15 118.6(6) C11 C10 H10 119.8 C11 C10 C9 120.3(6) C9 C10 H10 119.8 C2 C3 H3 119.3 C4 C3 C2 121.5(6) C4 C3 H3 119.3 C12 C13 H13 119.9 C14 C13 C12 120.2(5) C14 C13 H13 119.9 C4 C5 C16 118.3(6) C6 C5 C16 119.0(5) C6 C5 C4 122.7(5) C3 C4 C5 122.1(5) C3 C4 H4 119.0 C5 C4 H4 119.0 C12 C11 H11 118.9 C10 C11 C12 122.2(5) C10 C11 H11 118.9 C13 C14 H14 119.0 C13 C14 C1 121.9(6) C1 C14 H14 119.0 C16 C9 C10 119.3(6) C8 C9 C16 119.6(5) C8 C9 C10 121.2(6) C5 C6 H6 119.5 C7 C6 C5 121.0(5) C7 C6 H6 119.5 C9 C8 H8 120.1 C7 C8 C9 119.8(6) C7 C8 H8 120.1 C2 C1 C17 125.0(5) C14 C1 C2 120.0(5) C14 C1 C17 114.9(6) O1 C17 C1 129.2(6) O1 C17 H17 115.4 C1 C17 H17 115.4 C6 C7 C8 120.9(6) C6 C7 H7 119.5 C8 C7 H7 119.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C15 C16 1.426(9) C15 C2 1.418(8) C15 C12 1.435(6) C16 C5 1.430(6) C16 C9 1.413(8) O1 C17 1.216(6) C2 C3 1.444(7) C2 C1 1.417(9) C12 C13 1.392(9) C12 C11 1.431(8) C10 H10 0.9300 C10 C11 1.352(9) C10 C9 1.433(7) C3 H3 0.9300 C3 C4 1.340(9) C13 H13 0.9300 C13 C14 1.372(8) C5 C4 1.426(8) C5 C6 1.399(9) C4 H4 0.9300 C11 H11 0.9300 C14 H14 0.9300 C14 C1 1.403(7) C9 C8 1.407(9) C6 H6 0.9300 C6 C7 1.374(8) C8 H8 0.9300 C8 C7 1.399(7) C1 C17 1.478(8) C17 H17 0.9300 C7 H7 0.9300 loop_ _diffrn_oxdiff_twin_id _diffrn_oxdiff_twin_ratio _diffrn_oxdiff_twin_reflns_isolated _diffrn_oxdiff_twin_reflns_overlapped 1 0.3333 2982 42 2 0.3333 2982 41 3 0.3333 2772 48 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.690(6) 2 0.111(3) 3 0.199(5) _cod_database_fobs_code 2108395