#------------------------------------------------------------------------------ #$Date: 2020-01-31 02:29:41 +0200 (Fri, 31 Jan 2020) $ #$Revision: 247396 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/71/1557196.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_1557196 loop_ _publ_author_name 'Shibuya, Yusuke' 'Aonuma, Kazuhiro' 'Kimura, Tomohiro' 'Kaneko, Takuro' 'Fujiwara, Wataru' 'Yamaguchi, Yuji' 'Kumaki, Daisuke' 'Tokito, Shizuo' 'Katagiri, Hiroshi' _publ_section_title ; Linear Biazulene Isomers: Effects of Molecular and Packing Structure on Optoelectronic and Charge-Transport Properties ; _journal_name_full 'The Journal of Physical Chemistry C' _journal_paper_doi 10.1021/acs.jpcc.9b11214 _journal_year 2020 _chemical_formula_moiety 'C20 H14' _chemical_formula_sum 'C20 H14' _chemical_formula_weight 254.31 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 97.942(2) _cell_angle_beta 95.597(2) _cell_angle_gamma 90.921(3) _cell_formula_units_Z 2 _cell_length_a 6.0870(2) _cell_length_b 7.5639(3) _cell_length_c 14.4293(5) _cell_measurement_reflns_used 6858 _cell_measurement_temperature 296 _cell_measurement_theta_max 68.23 _cell_measurement_theta_min 3.11 _cell_volume 654.54(4) _computing_cell_refinement 'PROCESS-AUTO (Rigaku, 1998)' _computing_data_collection 'PROCESS-AUTO (Rigaku, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2003)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'Yadokari-XG 2009 (Wakita, 2001, Kabuto et al., 2009)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 296 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54187 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_unetI/netI 0.0268 _diffrn_reflns_Laue_measured_fraction_full 0.983 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 11019 _diffrn_reflns_point_group_measured_fraction_full 0.983 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_theta_full 67.497 _diffrn_reflns_theta_max 67.497 _diffrn_reflns_theta_min 6.282 _diffrn_source 'rotating anode' _exptl_absorpt_coefficient_mu 0.552 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8872 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_crystal_colour Blue _exptl_crystal_density_diffrn 1.290 _exptl_crystal_description Platelet _exptl_crystal_F_000 268 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.030 _refine_diff_density_max 0.220 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.101 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 2321 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.157 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0492 _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^)+(0.0622P)^2^+0.1253P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1129 _refine_ls_wR_factor_ref 0.1286 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1910 _reflns_number_total 2321 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jp9b11214_si_004.cif _cod_data_source_block BiAz3_rt_20180918 _cod_database_code 1557196 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.922 _shelx_estimated_absorpt_t_max 0.984 _exptl_absorpt_special_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _shelx_res_file ; BiAz3_rt.res created by SHELXL-2014/7 TITL BiAz3_rt_a.res in P-1 REM Yadorkari-X generated CELL 1.54187 6.0870 7.5639 14.4293 97.9420 95.5970 90.9210 ZERR 2.0 0.0002 0.0003 0.0005 0.0020 0.0020 0.0030 LATT 1 REM SPGR P-1 triclinic SFAC C H UNIT 40 28 SIZE 0.15 0.09 0.03 TEMP 23.0 L.S. 50 FMAP 2 PLAN -20 ACTA CONF LIST 4 BOND $H OMIT -10.000000 135.000000 OMIT 0 0 1 OMIT 0 0 2 OMIT 0 1 0 WGHT 0.062200 0.125300 FVAR 7.95188 C1 1 0.861982 0.663977 0.372443 11.00000 0.03668 0.04230 = 0.04632 0.00815 0.00728 0.00727 AFIX 43 H1 2 0.989825 0.622284 0.401795 11.00000 -1.20000 AFIX 0 C2 1 0.849079 0.642906 0.275123 11.00000 0.04104 0.04111 = 0.04797 0.00489 0.01478 0.00678 AFIX 43 H2 2 0.968918 0.588345 0.248994 11.00000 -1.20000 AFIX 0 C3 1 0.684345 0.690963 0.210909 11.00000 0.04469 0.04064 = 0.04211 0.00487 0.00965 0.00227 C4 1 0.682415 0.665833 0.113102 11.00000 0.06008 0.06019 = 0.04380 0.00342 0.01322 0.00802 AFIX 43 H4 2 0.791617 0.611306 0.079398 11.00000 -1.20000 AFIX 0 C5 1 0.490260 0.735798 0.074432 11.00000 0.07035 0.07425 = 0.04053 0.00633 0.00281 0.00633 AFIX 43 H5 2 0.451261 0.735772 0.010488 11.00000 -1.20000 AFIX 0 C6 1 0.364866 0.805979 0.145901 11.00000 0.05402 0.06159 = 0.04783 0.00653 -0.00189 0.00931 AFIX 43 H6 2 0.229577 0.860030 0.137552 11.00000 -1.20000 AFIX 0 C7 1 0.476566 0.781434 0.232006 11.00000 0.04113 0.04075 = 0.04388 0.00518 0.00279 0.00093 C8 1 0.405285 0.830464 0.319672 11.00000 0.03450 0.04031 = 0.04874 0.00378 0.00392 0.00401 AFIX 43 H8 2 0.269334 0.884841 0.319634 11.00000 -1.20000 AFIX 0 C9 1 0.506842 0.810417 0.407627 11.00000 0.03473 0.04123 = 0.04245 0.00249 0.00936 0.00258 AFIX 43 H9 2 0.426593 0.851001 0.457588 11.00000 -1.20000 AFIX 0 C10 1 0.711498 0.738668 0.433501 11.00000 0.03580 0.03373 = 0.04170 0.00629 0.00793 0.00013 C11 1 0.774172 0.744255 0.536915 11.00000 0.03501 0.03397 = 0.04156 0.00560 0.00602 0.00246 C12 1 0.985088 0.817024 0.572092 11.00000 0.03422 0.04347 = 0.04564 0.01207 0.00794 0.00189 AFIX 43 H12 2 1.070764 0.849190 0.526787 11.00000 -1.20000 AFIX 0 C13 1 1.085158 0.848289 0.663375 11.00000 0.03325 0.04120 = 0.05400 0.01080 0.00197 0.00138 AFIX 43 H13 2 1.224838 0.903035 0.670414 11.00000 -1.20000 AFIX 0 C14 1 1.008121 0.810140 0.745711 11.00000 0.03944 0.03875 = 0.04595 0.00749 0.00017 0.00437 C15 1 1.118612 0.843826 0.836184 11.00000 0.05228 0.05723 = 0.05297 0.00820 -0.00583 0.00066 AFIX 43 H15 2 1.257564 0.898730 0.852043 11.00000 -1.20000 AFIX 0 C16 1 0.985508 0.781300 0.898545 11.00000 0.06578 0.07029 = 0.04368 0.01002 0.00018 0.00753 AFIX 43 H16 2 1.022207 0.788439 0.963073 11.00000 -1.20000 AFIX 0 C17 1 0.790361 0.706875 0.850443 11.00000 0.05633 0.06080 = 0.04530 0.01165 0.01080 0.00480 AFIX 43 H17 2 0.676577 0.655394 0.877164 11.00000 -1.20000 AFIX 0 C18 1 0.792842 0.721960 0.755280 11.00000 0.04391 0.04072 = 0.04106 0.00841 0.00838 0.00629 C19 1 0.625803 0.668622 0.684818 11.00000 0.03965 0.04187 = 0.04653 0.00836 0.01246 0.00036 AFIX 43 H19 2 0.501533 0.616730 0.704062 11.00000 -1.20000 AFIX 0 C20 1 0.615791 0.680977 0.589315 11.00000 0.03596 0.04101 = 0.04348 0.00464 0.00581 -0.00201 AFIX 43 H20 2 0.483002 0.640905 0.554821 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM BiAz3_rt_a.res in P-1 REM R1 = 0.0492 for 1910 Fo > 4sig(Fo) and 0.0602 for all 2321 data REM 181 parameters refined using 0 restraints END WGHT 0.0622 0.1253 REM Highest difference peak 0.220, deepest hole -0.344, 1-sigma level 0.101 Q1 1 0.5591 1.0342 0.3454 11.00000 0.05 0.22 Q2 1 0.5119 1.0783 0.2653 11.00000 0.05 0.20 Q3 1 0.4139 1.0563 0.1871 11.00000 0.05 0.20 Q4 1 1.2038 0.5345 0.2594 11.00000 0.05 0.19 Q5 1 0.0000 0.5000 0.5000 10.50000 0.05 0.19 Q6 1 0.5328 0.4566 0.6954 11.00000 0.05 0.19 Q7 1 0.7198 0.4533 0.2964 11.00000 0.05 0.19 Q8 1 0.0534 0.9504 0.3108 11.00000 0.05 0.19 Q9 1 1.1231 0.5753 0.1880 11.00000 0.05 0.19 Q10 1 1.2072 0.5812 0.2755 11.00000 0.05 0.19 Q11 1 0.7866 0.4887 0.7974 11.00000 0.05 0.19 Q12 1 0.6867 0.4801 0.6674 11.00000 0.05 0.18 Q13 1 0.4991 0.9805 0.1676 11.00000 0.05 0.18 Q14 1 0.6584 0.4951 0.8546 11.00000 0.05 0.18 Q15 1 0.5912 0.5494 0.8140 11.00000 0.05 0.18 Q16 1 1.1848 0.5813 0.3224 11.00000 0.05 0.18 Q17 1 0.5519 0.9880 0.2360 11.00000 0.05 0.18 Q18 1 0.4235 1.0319 0.1026 11.00000 0.05 0.18 Q19 1 0.3231 0.9853 0.4818 11.00000 0.05 0.18 Q20 1 0.4825 0.9856 0.4676 11.00000 0.05 0.17 ; _shelx_res_checksum 83428 _shelx_hkl_file ; 0 0 126847.38 707.64 0 0 127335.62 713.70 0 0 126978.65 711.29 0 0 127136.60 673.60 0 0 126718.32 688.21 0 0 128977.52 740.45 0 0 126888.86 692.44 0 0 128007.96 726.65 0 0 -128809.81 768.18 0 0 -128685.94 758.79 0 0 -127640.23 703.01 0 0 -128828.62 759.23 0 0 -127068.86 693.83 0 0 -128876.59 776.45 0 0 -127152.77 698.31 0 0 -129434.82 761.86 0 0 257171.52 1914.26 0 0 253801.37 1858.92 0 0 255383.87 1776.33 0 0 255574.37 1893.55 0 0 253293.66 1792.62 0 0 252943.00 1774.63 0 0 253540.59 1844.91 0 0 -258392.29 1967.26 0 0 -258475.26 2026.41 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629810.28 931.45 0 0 628448.08 940.25 0 0 -630754.43 999.33 0 0 -631396.63 1043.28 0 0 -632370.56 1107.07 0 0 -631239.14 946.51 0 0 -632162.76 1125.81 0 0 -632159.81 1061.98 0 0 -631700.68 1028.52 0 0 719857.04 636.88 0 0 719294.84 528.15 0 0 717922.13 524.65 0 0 719197.30 606.96 0 0 720140.94 582.13 0 0 720307.34 652.39 0 0 -720810.06 734.73 0 0 -720910.66 658.62 0 0 -721281.48 605.84 0 0 -721733.65 756.08 0 0 -721159.13 718.59 0 0 -721168.45 684.13 0 0 -721850.19 701.70 0 0 8 101.16 33.77 0 0 8 86.87 20.97 0 0 8 105.63 21.01 0 0 8 68.16 18.09 0 0 8 101.63 39.47 0 0 -8 86.24 65.57 0 0 -8 132.82 17.88 0 0 -8 128.69 42.97 0 0 -8 89.11 45.43 0 0 -8 117.83 54.44 0 0 -8 112.93 60.15 0 0 -8 108.65 40.83 0 0 -8 115.22 35.34 0 0 9 7334.15 203.19 0 0 9 7994.10 253.40 0 0 9 7290.13 203.17 0 0 9 8151.98 276.98 0 0 -9 8429.93 302.26 0 0 -9 8648.10 297.74 0 0 -9 8433.20 271.67 0 0 -9 8264.13 264.87 0 0 -9 8841.92 338.70 0 0 -9 8625.21 288.14 0 0 10 2511.51 132.27 0 0 -10 2678.34 137.35 0 0 -10 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-6 -1 -5 169.47 56.36 6 1 6 22.61 41.21 6 1 6 5.42 69.51 -6 -1 -6 22.13 56.72 6 1 7 3.65 32.32 6 1 7 -17.13 34.57 -6 -1 -7 -12.63 26.60 6 2 -10 753.86 130.24 6 2 -10 542.67 64.62 -6 -2 10 677.76 77.76 6 2 -9 38.29 61.22 6 2 -9 -12.37 21.98 -6 -2 9 -3.04 30.83 6 2 -8 1065.99 181.99 6 2 -8 976.37 77.72 -6 -2 8 1015.42 100.16 6 2 -7 -4.48 96.84 6 2 -7 80.99 41.12 -6 -2 7 44.12 45.08 6 2 -6 4153.13 242.35 6 2 -6 4296.07 195.24 -6 -2 6 4581.85 208.73 6 2 -5 73.51 66.28 6 2 -5 108.38 82.21 -6 -2 5 105.03 47.87 6 2 -4 1564.65 152.37 6 2 -4 1668.57 202.52 -6 -2 4 1519.96 100.28 6 2 -3 351.30 98.47 6 2 -3 496.29 87.19 -6 -2 3 448.76 55.99 6 2 -2 1138.39 136.21 6 2 -2 1308.52 125.75 -6 -2 2 1110.92 68.23 6 2 -1 2068.05 171.85 6 2 -1 2225.38 165.13 6 2 0 1010.07 126.83 6 2 0 1159.98 127.38 6 2 1 -7.80 37.02 6 2 1 -3.32 42.64 6 2 2 67.84 58.79 6 2 2 28.57 100.32 -6 -2 -2 44.15 44.57 6 2 3 3596.19 222.32 6 2 3 3335.87 162.09 -6 -2 -3 3501.21 170.55 6 2 4 851.58 119.33 6 2 4 935.75 88.64 -6 -2 -4 982.35 83.56 6 2 5 1655.59 144.78 6 2 5 1708.92 120.44 -6 -2 -5 1683.16 94.67 6 2 6 779.40 100.03 6 2 6 744.49 85.73 6 2 7 1058.78 91.87 -6 -3 10 14.20 30.93 6 3 -9 55.65 82.16 -6 -3 9 107.98 47.08 6 3 -8 -20.07 72.41 6 3 -8 -18.21 16.61 -6 -3 8 -20.79 35.42 6 3 -7 2866.85 178.50 6 3 -7 2436.76 106.93 -6 -3 7 3050.72 150.87 6 3 -6 3048.97 187.83 6 3 -6 2687.93 123.53 -6 -3 6 3286.12 151.92 6 3 -5 248.45 80.19 6 3 -5 332.35 53.86 -6 -3 5 408.61 55.87 6 3 -4 24.54 45.63 6 3 -4 18.77 33.31 -6 -3 4 22.07 25.30 6 3 -3 136.68 68.66 6 3 -3 203.40 54.60 -6 -3 3 91.87 28.04 6 3 -2 2981.63 188.68 6 3 -2 3070.08 164.71 6 3 -1 2278.96 158.21 6 3 -1 2330.33 145.61 6 3 0 721.25 150.39 6 3 1 223.28 114.01 -6 -3 -1 -29.49 32.49 6 3 2 48.51 36.26 6 3 2 -9.98 18.50 -6 -3 -2 3.64 23.84 6 3 3 258.91 79.61 6 3 3 396.97 48.83 -6 -3 -3 433.96 47.23 6 3 4 171.80 72.53 6 3 4 330.34 48.56 6 3 5 2723.17 169.13 6 3 5 2750.76 126.18 6 4 -8 26.80 37.10 -6 -4 8 22.58 29.00 6 4 -7 501.34 75.13 -6 -4 7 649.85 60.01 6 4 -6 12.26 34.56 -6 -4 6 1.85 18.38 6 4 -5 194.99 56.57 6 4 -4 18.28 55.50 6 4 -4 810.09 68.11 6 4 -3 20.16 49.89 6 4 -3 176.31 45.92 6 4 -2 -2.96 21.13 6 4 -1 52.38 34.43 -6 -4 1 0.20 16.64 6 4 0 8.42 26.61 6 4 1 1453.58 102.46 6 4 2 11.00 28.96 6 4 3 20.23 31.93 7 -2 -4 -0.18 19.49 7 -2 -4 0.09 19.89 -7 2 4 27.74 34.53 7 -2 -3 48.01 36.12 7 -2 -3 58.03 33.72 -7 2 3 54.60 37.57 7 -2 -2 0.54 23.99 -7 2 2 6.82 26.61 7 -2 -1 2483.42 130.74 -7 2 1 2590.86 172.08 7 -2 0 809.72 52.84 7 -2 0 893.30 82.99 -7 2 0 512.30 36.18 7 -2 1 1.34 30.61 7 -2 1 167.44 40.74 -7 2 -1 37.69 32.23 7 -2 2 45.11 31.14 7 -2 2 26.21 59.57 7 -1 -6 33.16 61.61 -7 1 6 16.67 32.97 7 -1 -5 123.22 86.63 -7 1 5 98.51 45.36 7 -1 -4 11.18 19.37 7 -1 -4 13.94 36.10 -7 1 4 6.47 14.93 -7 1 4 -26.50 26.05 7 -1 -3 140.12 34.62 7 -1 -3 197.48 56.24 -7 1 3 77.92 31.66 -7 1 3 159.42 43.05 7 -1 -2 1457.39 84.19 7 -1 -2 1826.81 117.94 -7 1 2 1570.08 89.88 -7 1 2 1774.56 95.88 7 -1 -1 2165.34 105.65 7 -1 -1 2559.94 136.58 -7 1 1 2075.18 106.52 7 -1 0 -4.84 20.88 7 -1 0 86.90 29.01 7 -1 0 107.15 37.14 -7 1 0 66.24 36.42 7 -1 1 -1.07 30.81 7 -1 1 171.85 54.54 7 -1 1 182.33 41.16 -7 1 -1 154.06 44.81 7 -1 2 416.33 50.44 7 -1 2 424.87 48.11 -7 1 -2 395.96 58.16 7 -1 3 58.87 33.71 -7 1 -3 29.74 53.07 7 0 -6 20.54 65.01 -7 0 6 -24.22 33.29 7 0 -5 -5.95 59.35 -7 0 5 12.76 31.22 7 0 -4 -7.64 38.31 -7 0 4 -8.36 27.41 7 0 -3 25.60 44.25 -7 0 3 18.07 29.09 -7 0 3 3.37 26.13 7 0 -2 166.66 63.83 -7 0 2 -40.02 38.14 7 0 -1 521.48 83.88 -7 0 1 482.02 70.26 7 0 0 -5.65 34.58 -7 0 0 7.97 32.09 7 0 1 0.03 16.17 7 0 1 42.20 34.77 -7 0 -1 34.04 38.52 7 0 2 70.80 50.26 7 0 2 -5.63 19.64 -7 0 -2 153.34 51.36 7 0 3 20.40 34.37 7 0 3 44.23 41.42 -7 0 -3 36.32 36.62 7 1 -6 2.51 28.66 7 1 -6 -12.46 30.17 -7 -1 6 1.53 39.28 7 1 -5 -12.55 37.01 7 1 -5 55.96 39.96 -7 -1 5 33.68 31.02 7 1 -4 -0.25 28.21 -7 -1 4 -11.25 24.32 7 1 -3 49.74 48.41 7 1 -2 2012.60 139.76 -7 -1 2 -12.79 35.30 7 1 -1 158.92 61.22 -7 -1 1 121.44 52.26 7 1 0 270.79 68.96 -7 -1 0 106.52 50.78 7 1 1 -41.99 75.93 -7 -1 -1 -15.55 34.89 7 1 2 121.95 55.55 -7 -1 -2 401.31 63.74 7 2 -5 67.36 36.28 7 2 -4 -6.74 28.84 7 2 -3 189.39 53.70 7 2 -2 991.01 92.45 -7 -2 2 0.44 25.30 7 2 -1 5079.46 313.19 -7 -2 1 5395.61 216.84 7 2 0 66.06 78.46 -7 -2 0 67.22 40.47 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 41714 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 _atom_site_refinement_flags_adp C1 C 0.8620(3) 0.6640(2) 0.37244(11) 0.0413(4) Uani 1 1 d . . H1 H 0.9898 0.6223 0.4018 0.050 Uiso 1 1 calc R U C2 C 0.8491(3) 0.6429(2) 0.27512(11) 0.0428(4) Uani 1 1 d . . H2 H 0.9689 0.5883 0.2490 0.051 Uiso 1 1 calc R U C3 C 0.6843(3) 0.6910(2) 0.21091(11) 0.0422(4) Uani 1 1 d . . C4 C 0.6824(3) 0.6658(3) 0.11310(12) 0.0545(5) Uani 1 1 d . . H4 H 0.7916 0.6113 0.0794 0.065 Uiso 1 1 calc R U C5 C 0.4903(4) 0.7358(3) 0.07443(13) 0.0620(5) Uani 1 1 d . . H5 H 0.4513 0.7358 0.0105 0.074 Uiso 1 1 calc R U C6 C 0.3649(3) 0.8060(3) 0.14590(12) 0.0550(5) Uani 1 1 d . . H6 H 0.2296 0.8600 0.1376 0.066 Uiso 1 1 calc R U C7 C 0.4766(3) 0.7814(2) 0.23201(11) 0.0421(4) Uani 1 1 d . . C8 C 0.4053(3) 0.8305(2) 0.31967(11) 0.0414(4) Uani 1 1 d . . H8 H 0.2693 0.8848 0.3196 0.050 Uiso 1 1 calc R U C9 C 0.5068(2) 0.8104(2) 0.40763(11) 0.0394(4) Uani 1 1 d . . H9 H 0.4266 0.8510 0.4576 0.047 Uiso 1 1 calc R U C10 C 0.7115(2) 0.73867(19) 0.43350(11) 0.0367(4) Uani 1 1 d . . C11 C 0.7742(2) 0.74425(19) 0.53692(11) 0.0367(4) Uani 1 1 d . . C12 C 0.9851(3) 0.8170(2) 0.57209(11) 0.0403(4) Uani 1 1 d . . H12 H 1.0708 0.8492 0.5268 0.048 Uiso 1 1 calc R U C13 C 1.0852(3) 0.8483(2) 0.66338(12) 0.0426(4) Uani 1 1 d . . H13 H 1.2248 0.9030 0.6704 0.051 Uiso 1 1 calc R U C14 C 1.0081(3) 0.8101(2) 0.74571(11) 0.0415(4) Uani 1 1 d . . C15 C 1.1186(3) 0.8438(3) 0.83618(13) 0.0549(5) Uani 1 1 d . . H15 H 1.2576 0.8987 0.8520 0.066 Uiso 1 1 calc R U C16 C 0.9855(3) 0.7813(3) 0.89855(13) 0.0600(5) Uani 1 1 d . . H16 H 1.0222 0.7884 0.9631 0.072 Uiso 1 1 calc R U C17 C 0.7904(3) 0.7069(3) 0.85044(12) 0.0533(5) Uani 1 1 d . . H17 H 0.6766 0.6554 0.8772 0.064 Uiso 1 1 calc R U C18 C 0.7928(3) 0.7220(2) 0.75528(11) 0.0413(4) Uani 1 1 d . . C19 C 0.6258(3) 0.6686(2) 0.68482(11) 0.0420(4) Uani 1 1 d . . H19 H 0.5015 0.6167 0.7041 0.050 Uiso 1 1 calc R U C20 C 0.6158(3) 0.6810(2) 0.58932(11) 0.0402(4) Uani 1 1 d . . H20 H 0.4830 0.6409 0.5548 0.048 Uiso 1 1 calc R U 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 0.0367(8) 0.0423(9) 0.0463(9) 0.0082(7) 0.0073(7) 0.0073(7) C2 0.0410(9) 0.0411(9) 0.0480(9) 0.0049(7) 0.0148(7) 0.0068(7) C3 0.0447(9) 0.0406(9) 0.0421(9) 0.0049(7) 0.0096(7) 0.0023(7) C4 0.0601(11) 0.0602(11) 0.0438(10) 0.0034(8) 0.0132(8) 0.0080(9) C5 0.0703(13) 0.0742(13) 0.0405(10) 0.0063(9) 0.0028(9) 0.0063(10) C6 0.0540(11) 0.0616(11) 0.0478(10) 0.0065(8) -0.0019(8) 0.0093(9) C7 0.0411(9) 0.0408(9) 0.0439(9) 0.0052(7) 0.0028(7) 0.0009(7) C8 0.0345(8) 0.0403(9) 0.0487(9) 0.0038(7) 0.0039(7) 0.0040(6) C9 0.0347(8) 0.0412(9) 0.0425(9) 0.0025(6) 0.0094(6) 0.0026(6) C10 0.0358(8) 0.0337(8) 0.0417(9) 0.0063(6) 0.0079(6) 0.0001(6) C11 0.0350(8) 0.0340(8) 0.0416(8) 0.0056(6) 0.0060(6) 0.0025(6) C12 0.0342(8) 0.0435(9) 0.0456(9) 0.0121(7) 0.0079(6) 0.0019(7) C13 0.0332(8) 0.0412(9) 0.0540(10) 0.0108(7) 0.0020(7) 0.0014(6) C14 0.0394(9) 0.0387(8) 0.0459(9) 0.0075(7) 0.0002(7) 0.0044(7) C15 0.0523(11) 0.0572(11) 0.0530(11) 0.0082(8) -0.0058(8) 0.0007(8) C16 0.0658(12) 0.0703(13) 0.0437(10) 0.0100(9) 0.0002(9) 0.0075(10) C17 0.0563(11) 0.0608(11) 0.0453(10) 0.0117(8) 0.0108(8) 0.0048(9) C18 0.0439(9) 0.0407(9) 0.0411(9) 0.0084(7) 0.0084(7) 0.0063(7) C19 0.0397(9) 0.0419(9) 0.0465(9) 0.0084(7) 0.0125(7) 0.0004(7) C20 0.0360(8) 0.0410(9) 0.0435(9) 0.0046(7) 0.0058(6) -0.0020(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 C1 C10 129.86(15) C2 C1 H1 115.1 C10 C1 H1 115.1 C3 C2 C1 129.67(14) C3 C2 H2 115.2 C1 C2 H2 115.2 C2 C3 C4 126.64(15) C2 C3 C7 127.09(14) C4 C3 C7 106.26(14) C5 C4 C3 108.74(16) C5 C4 H4 125.6 C3 C4 H4 125.6 C4 C5 C6 109.79(16) C4 C5 H5 125.1 C6 C5 H5 125.1 C5 C6 C7 108.45(16) C5 C6 H6 125.8 C7 C6 H6 125.8 C8 C7 C6 126.29(16) C8 C7 C3 126.96(15) C6 C7 C3 106.75(14) C7 C8 C9 129.42(15) C7 C8 H8 115.3 C9 C8 H8 115.3 C8 C9 C10 130.40(14) C8 C9 H9 114.8 C10 C9 H9 114.8 C1 C10 C9 126.57(15) C1 C10 C11 117.31(13) C9 C10 C11 116.12(13) C20 C11 C12 126.44(15) C20 C11 C10 116.96(14) C12 C11 C10 116.59(13) C13 C12 C11 130.25(15) C13 C12 H12 114.9 C11 C12 H12 114.9 C14 C13 C12 129.55(16) C14 C13 H13 115.2 C12 C13 H13 115.2 C13 C14 C15 126.84(17) C13 C14 C18 126.80(15) C15 C14 C18 106.35(15) C16 C15 C14 108.45(17) C16 C15 H15 125.8 C14 C15 H15 125.8 C17 C16 C15 110.07(17) C17 C16 H16 125.0 C15 C16 H16 125.0 C16 C17 C18 108.69(17) C16 C17 H17 125.7 C18 C17 H17 125.7 C19 C18 C17 126.39(17) C19 C18 C14 127.16(15) C17 C18 C14 106.44(15) C18 C19 C20 129.54(15) C18 C19 H19 115.2 C20 C19 H19 115.2 C19 C20 C11 130.12(15) C19 C20 H20 114.9 C11 C20 H20 114.9 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.386(2) C1 C10 1.404(2) C1 H1 0.9300 C2 C3 1.386(2) C2 H2 0.9300 C3 C4 1.397(2) C3 C7 1.485(2) C4 C5 1.391(3) C4 H4 0.9300 C5 C6 1.394(3) C5 H5 0.9300 C6 C7 1.394(2) C6 H6 0.9300 C7 C8 1.381(2) C8 C9 1.385(2) C8 H8 0.9300 C9 C10 1.405(2) C9 H9 0.9300 C10 C11 1.498(2) C11 C20 1.399(2) C11 C12 1.408(2) C12 C13 1.384(2) C12 H12 0.9300 C13 C14 1.383(2) C13 H13 0.9300 C14 C15 1.397(2) C14 C18 1.488(2) C15 C16 1.392(3) C15 H15 0.9300 C16 C17 1.385(3) C16 H16 0.9300 C17 C18 1.395(2) C17 H17 0.9300 C18 C19 1.379(2) C19 C20 1.390(2) C19 H19 0.9300 C20 H20 0.9300 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 C10 C1 C2 C3 0.5(3) C1 C2 C3 C4 179.85(18) C1 C2 C3 C7 0.8(3) C2 C3 C4 C5 -178.73(18) C7 C3 C4 C5 0.5(2) C3 C4 C5 C6 -0.3(2) C4 C5 C6 C7 0.0(2) C5 C6 C7 C8 -179.04(18) C5 C6 C7 C3 0.3(2) C2 C3 C7 C8 -1.9(3) C4 C3 C7 C8 178.85(17) C2 C3 C7 C6 178.73(17) C4 C3 C7 C6 -0.5(2) C6 C7 C8 C9 180.00(18) C3 C7 C8 C9 0.8(3) C7 C8 C9 C10 1.5(3) C2 C1 C10 C9 0.2(3) C2 C1 C10 C11 -179.37(16) C8 C9 C10 C1 -1.8(3) C8 C9 C10 C11 177.75(15) C1 C10 C11 C20 -131.05(15) C9 C10 C11 C20 49.32(19) C1 C10 C11 C12 50.50(19) C9 C10 C11 C12 -129.13(15) C20 C11 C12 C13 -1.8(3) C10 C11 C12 C13 176.45(15) C11 C12 C13 C14 2.8(3) C12 C13 C14 C15 179.38(16) C12 C13 C14 C18 0.6(3) C13 C14 C15 C16 -178.62(16) C18 C14 C15 C16 0.34(19) C14 C15 C16 C17 0.2(2) C15 C16 C17 C18 -0.7(2) C16 C17 C18 C19 -177.92(16) C16 C17 C18 C14 0.85(19) C13 C14 C18 C19 -3.0(3) C15 C14 C18 C19 178.02(16) C13 C14 C18 C17 178.23(15) C15 C14 C18 C17 -0.73(18) C17 C18 C19 C20 179.28(16) C14 C18 C19 C20 0.8(3) C18 C19 C20 C11 2.8(3) C12 C11 C20 C19 -2.0(3) C10 C11 C20 C19 179.68(15)