#------------------------------------------------------------------------------ #$Date: 2019-10-11 12:05:36 +0300 (Fri, 11 Oct 2019) $ #$Revision: 219291 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234558.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_7234558 loop_ _publ_author_name 'Takahiro Kamata' 'Hisahiro Sasabe' 'Yuichirio Watanabe' 'Daisuke Yokoyama' 'Hiroshi Katagiri' 'Junji Kido' _publ_section_title ; A series of fluorinated phenylpyridine-based electron-transporters for blue phosphorescent OLEDs ; _journal_name_full 'Journal of Materials Chemistry C' _journal_page_first 1104 _journal_page_last 1110 _journal_paper_doi 10.1039/C5TC03879K _journal_volume 4 _journal_year 2016 _chemical_formula_moiety 'C38 H25 F N4' _chemical_formula_sum 'C38 H25 F N4' _chemical_formula_weight 556.62 _chemical_name_systematic B4PyMFB _space_group_crystal_system orthorhombic _space_group_IT_number 31 _space_group_name_Hall 'P 2ac -2' _space_group_name_H-M_alt 'P m n 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 33.005(12) _cell_length_b 3.7442(13) _cell_length_c 10.782(4) _cell_measurement_reflns_used 3496 _cell_measurement_temperature 93 _cell_measurement_theta_max 30.4 _cell_measurement_theta_min 2.3 _cell_volume 1332.4(8) _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)' _computing_data_collection 'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012)' _computing_publication_material 'Yadokari-XG (Wakita, Nemoto et al., 2009)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 93 _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Rigaku Saturn 70 CCD area detector' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_unetI/netI 0.0187 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 15232 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.499 _diffrn_reflns_theta_min 1.987 _diffrn_source 'Rotating Anode' _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.906 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(REQAB; Jacobson, 1998)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.387 _exptl_crystal_description Prism _exptl_crystal_F_000 580 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.317 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.077 _refine_ls_abs_structure_details ; Flack x determined using 1230 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 199 _refine_ls_number_reflns 2817 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.107 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0335 _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^)+(0.0801P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.1054 _reflns_Friedel_coverage 0.898 _reflns_Friedel_fraction_full 0.997 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 2708 _reflns_number_total 2817 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file J-Mater-Chem-C-2016-4-1104.cif _cod_data_source_block ydkr2 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the built-in table derived from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated on 2014-11-21. Automatic conversion script Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas ; _cod_database_code 7234558 _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 0.991 _shelx_estimated_absorpt_t_max 0.996 _shelx_res_file ; ydkr2.res created by SHELXL-2014/7 TITL REM Yadorkari-X generated CELL 0.71075 33.0050 3.7442 10.7820 90.0000 90.0000 90.0000 ZERR 2.0 0.0120 0.0013 0.0040 0.0000 0.0000 0.0000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, +Y, +Z SYMM 1/2+X, -Y, 1/2+Z REM SPGR Pmn21 orthorhombic SFAC C H F N UNIT 76 50 2 8 SIZE 0.10 0.05 0.05 TEMP -180.0 L.S. 20 FMAP 2 PLAN -20 ACTA CONF LIST 4 BOND $H MERG 2 OMIT -10.000000 53.000000 WGHT 0.080100 FVAR 6.20320 F1 3 0.500000 -0.429907 0.480373 10.50000 0.01858 0.03157 = 0.01612 0.00707 0.00000 0.00000 N1 4 0.243493 0.393207 0.331237 11.00000 0.01567 0.02368 = 0.01891 -0.00164 0.00178 0.00099 N2 4 0.385608 -0.079634 -0.466717 11.00000 0.02237 0.02557 = 0.01532 0.00011 -0.00003 0.00041 C1 1 0.500000 -0.284011 0.364846 10.50000 0.01874 0.01958 = 0.01257 -0.00122 0.00000 0.00000 C2 1 0.463121 -0.216546 0.309275 11.00000 0.01394 0.01882 = 0.01740 -0.00211 0.00278 -0.00107 AFIX 43 H2 2 0.438455 -0.269041 0.350865 11.00000 -1.20000 AFIX 0 C3 1 0.463007 -0.069089 0.190303 11.00000 0.01390 0.01563 = 0.01569 -0.00339 0.00046 0.00097 C4 1 0.500000 0.007459 0.132644 10.50000 0.01805 0.01679 = 0.01305 -0.00128 0.00000 0.00000 AFIX 43 H4 2 0.499999 0.113689 0.052629 10.50000 -1.20000 AFIX 0 C5 1 0.389539 0.105981 0.188346 11.00000 0.01630 0.01676 = 0.01367 0.00000 -0.00027 0.00017 AFIX 43 H5 2 0.390594 0.129719 0.276010 11.00000 -1.20000 AFIX 0 C6 1 0.352917 0.171291 0.125672 11.00000 0.01495 0.01492 = 0.01754 -0.00013 0.00136 0.00076 C7 1 0.351988 0.139722 -0.003802 11.00000 0.01270 0.01869 = 0.01756 0.00018 -0.00215 0.00001 AFIX 43 H7 2 0.327454 0.184043 -0.047233 11.00000 -1.20000 AFIX 0 C8 1 0.386705 0.043929 -0.069518 11.00000 0.01791 0.01528 = 0.01268 0.00073 -0.00084 -0.00109 C9 1 0.422542 -0.023395 -0.005067 11.00000 0.01197 0.01823 = 0.01625 -0.00090 0.00238 -0.00095 AFIX 43 H9 2 0.446155 -0.091070 -0.049637 11.00000 -1.20000 AFIX 0 C10 1 0.424274 0.006995 0.123637 11.00000 0.01456 0.01466 = 0.01723 0.00021 -0.00069 -0.00007 C11 1 0.275313 0.227215 0.382152 11.00000 0.01927 0.02447 = 0.01546 -0.00201 0.00088 -0.00073 AFIX 43 H11 2 0.273059 0.152325 0.466053 11.00000 -1.20000 AFIX 0 C12 1 0.248071 0.495090 0.212544 11.00000 0.01492 0.02097 = 0.02038 -0.00009 -0.00128 0.00094 AFIX 43 H12 2 0.226193 0.617174 0.174063 11.00000 -1.20000 AFIX 0 C13 1 0.282714 0.433611 0.142348 11.00000 0.01619 0.02001 = 0.01631 -0.00002 -0.00030 -0.00044 AFIX 43 H13 2 0.284005 0.510325 0.058456 11.00000 -1.20000 AFIX 0 C14 1 0.315524 0.258296 0.196320 11.00000 0.01570 0.01620 = 0.01649 -0.00128 -0.00124 -0.00136 C15 1 0.311440 0.156979 0.320558 11.00000 0.01481 0.02172 = 0.01902 -0.00069 -0.00108 0.00153 AFIX 43 H15 2 0.333120 0.041434 0.362382 11.00000 -1.20000 AFIX 0 C16 1 0.385990 0.005036 -0.207037 11.00000 0.01571 0.01693 = 0.01455 -0.00043 -0.00027 0.00303 C17 1 0.352636 -0.141083 -0.268227 11.00000 0.01603 0.02058 = 0.01734 0.00050 0.00047 0.00028 AFIX 43 H17 2 0.329286 -0.212887 -0.223142 11.00000 -1.20000 AFIX 0 C18 1 0.354188 -0.179598 -0.396059 11.00000 0.01777 0.02427 = 0.01676 0.00001 -0.00359 -0.00053 AFIX 43 H18 2 0.331460 -0.283808 -0.436224 11.00000 -1.20000 AFIX 0 C19 1 0.417324 0.065250 -0.406967 11.00000 0.01834 0.02406 = 0.01813 0.00178 0.00141 0.00050 AFIX 43 H19 2 0.439931 0.141073 -0.454724 11.00000 -1.20000 AFIX 0 C20 1 0.418859 0.110119 -0.279483 11.00000 0.01694 0.02008 = 0.01837 0.00011 0.00090 -0.00143 AFIX 43 H20 2 0.442164 0.211844 -0.241722 11.00000 -1.20000 AFIX 0 HKLF 4 1 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 REM REM R1 = 0.0335 for 2708 Fo > 4sig(Fo) and 0.0373 for all 2817 data REM 199 parameters refined using 1 restraints END WGHT 0.0801 0.0000 REM Highest difference peak 0.317, deepest hole -0.270, 1-sigma level 0.077 Q1 1 0.3679 -0.0538 -0.2369 11.00000 0.05 0.32 Q2 1 0.3877 -0.0032 -0.1559 11.00000 0.05 0.31 Q3 1 0.4015 0.0436 -0.2376 11.00000 0.05 0.30 Q4 1 0.3590 -0.2193 -0.3251 11.00000 0.05 0.25 Q5 1 0.4221 0.0609 -0.3532 11.00000 0.05 0.25 Q6 1 0.3518 -0.1407 -0.3378 11.00000 0.05 0.23 Q7 1 0.4060 0.0131 -0.4211 11.00000 0.05 0.22 Q8 1 0.4014 0.0079 -0.0362 11.00000 0.05 0.22 Q9 1 0.5000 0.1171 -0.4045 10.50000 0.05 0.21 Q10 1 0.2638 0.4097 0.1776 11.00000 0.05 0.20 Q11 1 0.5000 0.0855 -0.2831 10.50000 0.05 0.19 Q12 1 0.3713 0.1329 0.1515 11.00000 0.05 0.19 Q13 1 0.4676 0.3260 -0.3265 11.00000 0.05 0.18 Q14 1 0.4812 -0.2036 -0.2802 11.00000 0.05 0.18 Q15 1 0.4802 0.0625 -0.3368 11.00000 0.05 0.18 Q16 1 0.4615 0.1108 -0.1893 11.00000 0.05 0.18 Q17 1 0.4777 0.4885 -0.2969 11.00000 0.05 0.18 Q18 1 0.4429 -0.0099 -0.4394 11.00000 0.05 0.18 Q19 1 0.4502 -0.1492 -0.3396 11.00000 0.05 0.17 Q20 1 0.4810 -0.1804 -0.3736 11.00000 0.05 0.17 ; _shelx_res_checksum 34360 _shelx_hkl_file ; 0 0 -3 -42.90 34.79 0 0 -3 -16.26 40.05 0 0 3 -14.47 29.56 0 0 3 -22.32 62.74 0 0 5 -133.22 182.92 0 0 -5 100.39 266.47 0 0 -5 238.95 137.37 0 0 5 80.18 85.15 0 0 -5 -149.47 70.52 0 0 5 23.64 38.07 0 0 5 20.96 259.66 0 0 -5 3.68 32.24 0 0 683197.97 506.69 0 0 -683714.40 504.02 0 0 685792.08 483.60 0 0 -682708.55 499.71 0 0 683383.08 502.75 0 0 683765.75 471.09 0 0 -683083.65 468.23 0 0 7 120.05 720.69 0 0 -7 94.03 390.46 0 0 7 22.34 350.06 0 0 -7 72.21 541.41 0 0 7 33.52 62.08 0 0 7 27.10 377.58 0 0 -7 -29.50 291.08 0 0 -8183903.7 944.17 0 0 -8178540.3 937.11 0 0 8180907.9 899.11 0 0 -9 -27.72 113.08 0 0 -9 -11.11 160.21 0 0 9 -54.97 83.11 0 0 10 1145.54 334.51 0 0 -10 1010.95 110.96 0 0 -10 994.94 126.79 0 0 10 938.57 110.18 0 0 11 49.68 166.08 0 0 -11 41.68 471.60 0 0 -11 48.36 417.93 0 0 11 -59.19 87.43 0 0 1266260.09 557.12 0 0 -1269309.72 559.22 0 0 -1266258.72 543.47 0 0 1265797.57 505.44 0 0 13 73.60 116.67 0 0 -13 -25.64 109.43 0 0 -13 11.60 122.96 0 0 13 140.01 149.52 0 0 14 6578.91 227.69 0 0 -14 6148.20 206.69 0 0 -14 6324.81 204.59 0 0 14 6606.12 220.20 0 0 15 -74.32 127.22 0 0 -15 93.71 66.03 0 0 15 30.12 108.10 0 0 16 7796.16 251.09 0 0 -16 7145.17 240.86 0 0 -16 7629.47 379.00 0 0 16 7763.60 245.99 0 0 17 165.17 185.76 0 0 -17 65.92 56.52 0 0 -17 79.80 159.65 0 0 17 93.62 140.97 0 0 18 1678.21 190.88 0 0 -18 1789.90 171.80 0 0 -18 2090.62 547.77 0 0 18 1971.73 149.64 0 0 -19 -16.38 96.20 0 0 -19 -23.72 179.69 0 0 19 13.44 39.73 0 0 -20 8070.54 287.56 0 0 -20 8567.56 324.82 0 0 20 8477.74 273.72 0 0 -21 -1.43 57.22 0 0 -21 14.90 172.80 0 0 21 187.30 124.28 0 0 -22 -30.18 123.00 0 0 -22 91.64 88.90 0 0 22 85.14 92.16 0 0 -23 143.23 122.48 0 0 -23 -37.97 139.17 0 0 23 1.31 85.94 0 0 -24 913.25 147.89 0 0 -24 1027.06 232.56 0 0 24 1134.87 147.06 0 0 -25 72.76 638.93 0 0 -25 80.29 865.80 0 0 25 10.58 110.96 0 0 -26242299.7 4745.03 0 0 26220491.3 4285.09 0 0 -27 808.11 688.26 0 0 -28205140.3 4032.14 0 0 -28208571.6 4128.18 0 0 -29 1461.59 1401.45 0 0 -30110647.9 1019.52 0 0 30106565.2 2495.11 0 0 -31 474.37 558.38 0 0 31 314.05 167.43 0 0 -32 294.77 176.09 0 0 -32 145.13 161.73 0 0 32 55.03 109.76 0 0 -33 -4.41 127.24 0 0 -33 58.34 72.03 0 0 33 118.07 160.11 0 0 34 9496.07 446.09 0 0 -34 8972.14 353.85 0 0 -34 9029.22 753.47 0 0 34 8914.39 340.25 0 0 35 -12.42 221.12 0 0 -35 202.39 150.30 0 0 -35 -16.35 184.52 0 0 35 154.14 172.44 0 0 3643793.71 751.95 0 0 -3640129.23 1231.12 0 0 -3642425.11 747.03 0 0 3641059.01 1240.76 0 0 37 -25.32 155.50 0 0 -37 174.59 73.22 0 0 -37 33.24 162.13 0 0 37 204.30 151.12 0 0 38 2159.91 274.51 0 0 -38 1956.45 215.27 0 0 -38 1859.00 255.61 0 0 39 282.74 166.31 0 0 -39 93.01 62.29 0 0 -39 -33.49 142.41 0 0 40 253.77 167.47 0 0 -40 105.28 114.38 0 0 -40 207.48 153.03 0 0 41 212.82 170.72 0 0 -41 79.43 132.51 0 0 -41 86.18 141.22 0 0 42 105.11 164.01 0 0 -42 -43.54 156.37 0 0 43 16.55 156.87 0 0 -43 46.89 145.21 0 0 44 1291.45 226.58 0 0 -44 1425.50 248.40 0 0 45 27.87 143.55 0 0 -45 64.72 59.38 0 0 -46 214.32 201.12 0 -1 0 2.38 14.41 0 1 0 -20.40 17.46 0 -1 0 -32.01 30.99 0 1 0 -13.38 20.19 0 -1 0 -2.22 27.15 0 -1 0 0.37 21.35 0 -1 1 -15.26 30.99 0 -1 -1 -6.09 28.99 0 1 1 -32.80 33.19 0 -1 -2 64.59 27.77 0 -1 2 -47.47 36.54 0 1 -2 26.25 32.50 0 -1 -2 62.10 49.01 0 1 2 -9.59 20.62 0 -1 -2 -21.46 45.79 0 1 2 15.69 44.42 0 -1 2 72.73 68.38 0 -1 -2 67.71 59.50 0 1 -4 46.40 57.38 0 1 4 -58.69 40.22 0 -1 -4 1.69 44.52 0 -1 4 2.90 29.64 0 1 -4 17.37 35.93 0 -1 -4 91.82 30.80 0 1 4 10.18 35.47 0 1 4 77.66 70.28 0 -1 -4 -116.22 79.89 0 1 -4 -93.20 50.32 0 -1 4 23.51 54.50 0 1 4 -39.61 1866.09 0 -1 -4 17.63 41.66 0 1 -6 38.24 87.21 0 -1 6 65.48 700.29 0 1 6 196.16 137.44 0 -1 -6 125.00 109.44 0 -1 6 54.13 95.25 0 1 -6 -42.38 72.44 0 1 6 53.80 87.45 0 -1 -6 111.56 121.53 0 1 -6 -1.72 99.62 0 -1 6 0.67 75.70 0 -1 6 -13.57 234.52 0 1 6 34.23 86.86 0 -1 -6 -55.23 927.31 0 -1 727942.60 308.02 0 1 727541.27 284.13 0 -1 -727267.09 272.96 0 -1 727857.25 298.04 0 -1 -726984.16 248.32 0 1 727961.02 263.38 0 -1 -728299.04 316.94 0 1 -728280.23 309.30 0 -1 727393.09 212.20 0 1 728596.04 325.14 0 -1 8 -98.38 126.12 0 1 8 -77.91 85.25 0 -1 -8 37.39 29.38 0 1 8 45.60 75.85 0 -1 -8 -50.02 105.46 0 1 -8 118.25 108.00 0 -1 8 -51.76 432.30 0 1 8 -24.63 179.50 0 1 -8 -4.38 76.12 0 -1 920714.84 291.95 0 1 920444.77 329.43 0 -1 -920454.03 232.98 0 1 -920175.98 280.18 0 -1 -920413.05 286.62 0 1 -920547.91 272.11 0 -1 920437.84 203.99 0 1 920337.31 280.58 0 1 -920382.45 208.32 0 -1 10 -161.45 104.19 0 1 10 -32.81 95.05 0 -1 -10 7.13 81.48 0 1 -10 -44.10 117.29 0 -1 -10 -29.80 101.67 0 1 -10 -41.92 104.57 0 -1 10 -15.93 97.87 0 1 10 21.04 119.16 0 -1 1111867.29 236.05 0 1 1111423.00 217.70 0 -1 -1111576.93 222.05 0 1 -1111687.06 254.20 0 -1 -1111440.66 219.33 0 1 -1111752.50 223.98 0 -1 1111981.47 184.68 0 1 1111343.98 224.81 0 -1 12 33.58 308.18 0 1 12 13.43 110.34 0 -1 -12 -9.59 169.70 0 1 -12 123.93 87.16 0 -1 -12 71.89 271.58 0 1 -12 42.96 98.09 0 -1 12 -33.68 185.67 0 1 12 35.75 114.23 0 -1 1380768.79 661.37 0 1 1378181.33 631.91 0 -1 -1376410.30 570.92 0 -1 -1378006.69 633.26 0 1 -1379015.97 635.81 0 -1 1378184.20 536.69 0 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6 -19 298.05 371.99 4 6 -19 345.13 201.03 4 -6 -19 408.80 298.30 4 6 19 459.68 192.36 -4 -6 20 2940.77 332.13 -4 6 20 2436.14 452.65 -4 -6 -20 2558.68 342.98 -4 6 -20 1133.21 868.70 4 6 -20 1961.48 701.29 4 -6 -20 2136.79 631.18 -4 -6 21 31.56 151.14 -4 6 21 117.12 160.21 -4 6 -21 -165.26 159.61 4 6 -21 161.46 163.82 -4 -6 22 4973.20 448.26 -4 6 22 4178.84 402.42 -4 6 -22 4148.08 545.26 4 6 -22 3948.46 498.68 -4 -6 23 234.77 226.21 -4 6 -23 174.45 255.74 4 6 -23 312.76 151.45 -4 -6 24 2820.81 330.45 -4 7 0 6919.35 613.09 -4 -7 0 7262.42 735.43 4 7 0 6117.30 408.00 4 -7 0 6525.89 559.49 4 7 0 6633.76 803.22 -4 7 1 1931.72 562.45 -4 7 -1 1727.38 733.56 -4 -7 -1 1823.07 397.57 -4 -7 1 2204.90 337.66 4 7 -1 1350.64 401.27 4 7 1 1275.48 645.54 4 -7 1 1541.47 808.98 4 -7 -1 1607.76 768.09 4 7 1 1797.04 262.38 4 7 -1 1305.49 669.01 -4 7 2 1354.05 460.65 -4 7 -2 940.50 631.35 -4 -7 -2 918.73 512.75 -4 -7 2 1758.90 284.02 4 7 -2 1205.70 213.21 4 7 2 1142.36 221.86 4 -7 2 927.02 497.86 4 -7 -2 1151.96 596.00 4 7 -2 734.64 594.03 4 7 2 1399.84 255.40 -4 7 3 8538.51 530.96 -4 7 -3 9060.23 543.70 -4 -7 3 8154.59 563.72 -4 -7 -3 8746.31 685.45 4 7 -3 8313.79 574.63 4 7 3 7892.79 518.05 4 -7 -3 7003.43 721.16 4 -7 3 8670.45 502.52 4 7 -3 8398.33 525.17 4 7 3 7152.28 1052.28 -4 7 4 5725.64 495.70 -4 7 -4 5570.64 673.20 -4 -7 4 4636.68 975.95 4 7 -4 5160.31 384.28 4 -7 -4 5112.13 773.60 4 -7 4 4970.69 373.86 4 7 -4 4833.17 723.16 4 7 4 5201.10 425.77 -4 7 5 574.50 297.80 -4 7 -5 1085.64 260.76 -4 -7 5 626.98 414.72 -4 -7 -5 909.31 307.60 4 7 -5 922.53 406.97 4 -7 -5 813.60 430.21 4 -7 5 936.20 220.87 4 7 -5 146.23 322.35 4 7 5 674.29 290.99 -4 7 6 1.71 215.62 -4 7 -6 115.52 156.53 -4 -7 6 244.20 178.00 -4 -7 -6 383.18 235.04 4 7 -6 232.78 146.49 4 -7 -6 79.64 133.96 4 -7 6 -6.44 148.21 4 7 6 133.78 207.74 -4 7 7 2009.50 962.32 -4 7 -7 2239.81 284.20 -4 -7 7 1859.24 283.85 -4 -7 -7 1639.33 818.60 4 7 -7 1878.42 499.83 4 -7 -7 1699.64 671.61 4 -7 7 1999.07 567.55 4 7 -7 2097.93 263.93 4 7 7 2679.05 319.16 -4 7 8 3135.69 474.34 -4 7 -8 2913.19 338.58 -4 -7 8 2878.86 515.76 -4 -7 -8 2444.36 575.91 4 7 -8 1980.70 432.32 4 -7 -8 2575.28 930.84 4 -7 8 2882.07 378.05 4 7 8 2237.49 698.76 -4 7 9 1047.64 416.02 -4 7 -9 1377.78 257.34 -4 -7 9 641.89 568.59 -4 -7 -9 787.65 446.48 4 7 -9 872.29 237.82 4 -7 -9 702.35 390.31 4 -7 9 814.08 197.20 4 7 -9 847.76 187.92 4 7 9 451.24 293.82 -4 7 10 930.11 345.49 -4 7 -10 452.65 235.30 -4 -7 10 687.16 316.31 -4 -7 -10 561.56 253.40 4 7 -10 485.14 196.18 4 -7 -10 442.58 252.80 4 -7 10 422.38 177.76 4 7 -10 715.78 175.40 4 7 10 418.45 234.00 -4 7 11 784.33 252.20 -4 7 -11 999.81 235.14 -4 -7 11 1479.55 291.26 -4 -7 -11 1139.94 428.12 4 7 -11 513.65 284.00 4 -7 -11 731.14 428.40 4 -7 11 534.75 141.32 4 7 11 865.10 263.14 -4 7 12 576.64 384.82 -4 7 -12 372.03 342.34 -4 -7 12 684.64 207.69 -4 -7 -12 417.52 293.24 4 7 -12 369.16 274.89 4 -7 -12 451.96 311.12 4 -7 12 488.30 132.74 4 7 12 633.55 194.33 -4 7 13 916.94 479.85 -4 7 -13 829.33 462.38 -4 -7 13 1617.67 245.55 -4 -7 -13 1010.11 413.06 4 7 -13 1261.21 274.71 4 -7 -13 808.83 361.38 4 7 13 680.24 360.40 -4 7 14 3882.59 307.10 -4 7 -14 4289.39 376.94 -4 -7 -14 3885.72 336.32 4 7 -14 4079.45 342.86 4 -7 -14 3536.18 544.01 4 7 14 3592.90 559.00 -4 7 15 629.74 206.98 -4 -7 -15 830.17 302.06 4 -7 -15 730.65 305.07 4 7 15 493.82 379.51 -4 7 16 495.21 359.74 -4 7 -16 710.88 370.58 -4 -7 16 450.32 149.92 -4 -7 -16 379.09 196.26 4 7 -16 1173.33 237.52 4 -7 -16 481.19 408.69 4 7 16 592.63 605.93 -4 7 17 115.95 99.28 -4 7 -17 170.86 206.42 -4 -7 17 210.29 146.91 4 7 -17 113.22 115.16 -4 7 18 2527.97 337.91 -4 -7 18 2120.75 245.99 -4 7 -18 1906.08 246.74 4 7 -18 2607.12 325.02 -4 7 19 104.76 220.12 -4 7 -19 180.32 160.76 4 7 -19 284.72 164.32 -4 7 20 107.20 165.80 -4 -7 20 18.90 130.00 4 7 -20 328.98 253.35 -4 -7 21 998.62 315.04 -4 8 0 2174.31 286.13 -4 -8 0 2182.44 381.90 4 8 0 1605.68 746.10 4 -8 0 2028.59 1027.49 4 8 0 2595.30 287.75 -4 8 1 3444.19 631.76 -4 8 -1 2871.19 315.60 -4 -8 1 2685.42 298.25 -4 -8 -1 2607.82 470.96 4 8 1 1606.38 791.81 4 8 -1 1960.12 520.86 4 -8 1 2368.75 644.06 4 -8 -1 2237.76 996.93 4 8 1 2634.48 290.99 4 8 -1 2699.98 429.82 -4 8 2 696.34 351.79 -4 8 -2 569.70 247.89 -4 -8 2 381.43 271.80 -4 -8 -2 321.36 289.76 4 8 2 775.79 200.06 4 8 -2 734.85 236.92 4 -8 2 362.69 322.59 4 -8 -2 507.36 300.29 4 8 -2 449.47 284.15 4 8 2 719.27 234.37 -4 8 3 1885.33 799.34 -4 8 -3 2449.36 345.19 -4 -8 3 1527.12 784.66 -4 -8 -3 2120.41 304.09 4 8 -3 2275.21 256.61 4 -8 3 1923.83 859.01 4 -8 -3 1410.89 752.20 4 8 -3 1465.51 495.85 4 8 3 2271.84 445.47 -4 8 4 3404.12 312.08 -4 8 -4 3453.48 660.64 -4 -8 4 3515.52 527.88 -4 -8 -4 2690.51 599.28 4 8 -4 3312.95 313.66 4 -8 4 2263.57 881.21 4 -8 -4 3100.03 689.18 4 8 4 3293.89 330.11 -4 8 5 382.71 341.25 -4 8 -5 770.11 269.66 -4 -8 5 1320.29 400.23 -4 -8 -5 513.32 306.95 4 8 -5 652.60 559.17 4 8 5 380.58 175.55 4 -8 -5 496.73 382.88 4 -8 5 605.77 403.01 4 8 -5 444.24 187.48 4 8 5 1004.86 255.12 -4 8 6 4594.14 585.51 -4 8 -6 5192.36 934.90 -4 -8 6 4895.49 986.54 -4 -8 -6 5779.47 413.12 4 8 -6 4941.78 324.99 4 -8 -6 6814.80 364.70 4 -8 6 4457.14 1120.05 4 8 -6 5662.01 371.48 4 8 6 5276.31 356.21 -4 8 7 138.41 144.30 -4 8 -7 307.29 223.71 -4 -8 7 93.63 153.83 4 8 -7 219.03 145.67 4 -8 -7 121.02 86.57 4 -8 7 165.25 108.51 4 8 -7 39.77 72.53 4 8 7 123.51 155.00 -4 8 8 429.49 354.05 -4 8 -8 305.70 175.90 -4 -8 8 393.17 150.07 -4 -8 -8 278.82 307.55 4 8 -8 689.07 203.76 4 -8 -8 292.24 207.71 4 -8 8 557.73 157.40 4 8 8 296.26 202.52 -4 8 9 2942.45 483.60 -4 8 -9 3066.53 360.39 -4 -8 9 3262.60 282.13 -4 -8 -9 3616.42 351.09 4 8 -9 3242.79 309.70 4 -8 -9 2777.63 641.15 4 8 9 2440.87 450.09 -4 8 10 3384.49 336.51 -4 8 -10 3024.91 1074.74 -4 -8 10 3781.89 339.42 -4 -8 -10 2605.07 1065.73 4 8 -10 2448.51 552.08 4 -8 -10 3385.63 597.72 4 8 10 2475.11 594.77 -4 8 11 745.40 225.27 -4 8 -11 584.10 378.26 -4 -8 11 428.54 208.48 4 8 -11 335.21 217.39 4 -8 -11 854.97 346.57 4 8 11 735.65 240.30 -4 8 12 1820.57 252.05 -4 8 -12 1790.58 291.74 -4 -8 12 2230.12 330.86 4 8 -12 1553.61 244.59 4 -8 -12 1673.87 560.04 4 8 12 1325.96 915.18 -4 8 13 3730.48 373.92 -4 8 -13 2674.89 778.33 -4 -8 13 3468.17 401.10 4 8 -13 2560.84 298.93 4 -8 -13 2828.53 836.15 4 8 13 2253.17 942.66 -4 8 14 1337.60 253.41 -4 -8 14 1720.64 293.58 4 8 -14 838.76 637.83 -4 -8 15 338.27 231.25 4 8 -15 96.22 197.02 -4 8 16 963.32 710.69 -4 -8 16 2099.35 305.48 4 8 -16 1067.39 576.35 -4 8 17 480.90 195.86 -4 -8 17 638.99 248.72 -4 -8 18 185.22 137.71 -4 9 0 8046.26 1035.88 4 -9 0 8140.12 579.01 -4 9 -1 5408.85 458.85 -4 9 1 5087.46 638.09 -4 -9 1 5065.54 498.05 4 9 -1 3377.48 853.14 4 -9 1 4857.38 418.38 4 -9 -1 3876.36 648.64 4 9 1 2652.32 1040.64 4 9 -1 4838.90 502.81 -4 9 2 1306.44 522.22 -4 9 -2 1474.04 256.74 -4 -9 2 1839.63 354.04 4 9 2 1062.82 387.11 4 9 -2 895.86 574.92 4 -9 2 927.26 468.19 4 -9 -2 1361.10 742.32 4 9 2 643.55 689.20 4 9 -2 534.46 660.05 -4 9 3 366.45 269.92 -4 9 -3 739.21 371.28 -4 -9 3 801.34 294.55 4 9 3 789.31 240.26 4 9 -3 656.03 216.37 4 -9 -3 368.57 229.30 4 9 -3 327.46 138.04 4 9 3 309.24 362.16 -4 9 4 4096.26 1180.79 -4 9 -4 5800.49 465.63 4 9 -4 4913.04 434.37 4 9 4 4862.49 406.88 4 -9 -4 4797.03 678.33 4 -9 4 5404.64 653.07 4 9 4 4442.93 396.66 -4 9 5 5179.03 432.76 -4 9 -5 4551.13 755.67 4 9 -5 5436.49 468.75 4 9 5 4173.72 566.30 4 -9 -5 5254.76 434.00 4 9 5 4581.92 411.37 -4 9 6 336.47 157.52 -4 9 -6 298.46 270.05 -4 -9 6 811.08 236.93 4 9 -6 233.01 234.28 4 9 6 192.24 181.66 -4 9 7 1029.45 430.12 -4 9 -7 1010.57 832.88 4 9 -7 1216.89 455.96 4 9 7 913.94 405.96 4 -9 -7 1066.02 737.55 4 9 7 1088.06 258.05 -4 9 8 531.66 217.19 -4 9 -8 359.54 248.24 4 9 -8 454.82 248.62 4 -9 -8 526.05 210.95 4 9 8 201.23 298.92 -4 9 9 4891.54 459.54 4 9 -9 4623.66 419.61 4 9 9 4284.67 425.05 -4 9 10 771.86 224.56 4 9 -10 209.21 268.83 -4 9 11 989.40 715.96 4 9 -11 808.39 541.98 -4 9 12 859.27 457.28 -4 9 13 782.50 237.94 -4 10 0 1821.72 706.32 4 10 1 713.13 247.52 4 10 -1 441.43 192.73 4 -10 -1 411.76 311.68 4 -10 -2 2502.40 683.56 4 10 2 1335.27 776.88 -4 10 3 1584.07 368.36 4 10 3 792.16 411.24 4 10 3 422.56 345.50 -4 10 4 215.12 218.84 4 10 4 346.76 231.57 4 -10 -4 383.52 260.69 4 10 4 461.47 227.83 4 10 5 377.17 212.62 4 10 5 273.20 154.95 -5 0 0 1665.93 284.59 5 0 0 2309.67 305.01 -5 0 -1 562.21 327.43 -5 0 1 346.74 363.40 5 0 -1 771.50 262.61 5 0 1 504.92 239.52 -5 0 2 -9.04 136.85 -5 0 -2 269.70 151.41 5 0 -2 87.41 169.74 -5 0 3 1823.24 262.10 -5 0 -3 1297.57 780.57 5 0 -3 1194.71 820.81 5 0 3 1188.83 637.50 -5 0 4 195.62 206.97 -5 0 -4 536.81 216.48 5 0 4 121.70 156.57 -5 0 5 98.59 204.48 -5 0 -5 22.72 109.81 5 0 5 70.38 167.81 -5 0 -6 -16.67 140.67 5 0 -6 91.61 189.32 5 0 6 133.34 149.31 -5 0 7 1213.25 250.12 -5 0 -7 735.47 459.88 -5 0 -7 1335.96 246.80 5 0 -7 816.15 379.32 -5 0 8 399.08 230.97 -5 0 -8 143.37 156.92 -5 0 -8 299.23 232.45 -5 0 -9 1452.62 327.13 -5 0 -9 1478.01 243.95 -5 0 -10 110.14 129.81 -5 0 -11 44.09 131.79 -5 0 -11 -22.71 132.73 -5 0 -12 132.51 126.77 -5 0 -13 121.97 58.96 -5 0 -14 2815.13 314.50 -5 1 0 2460.41 317.37 -5 -1 0 1976.05 261.41 5 -1 0 1779.70 757.82 5 1 0 1994.02 296.48 -5 1 1 860.43 483.50 -5 -1 -1 622.52 381.55 -5 -1 1 1007.45 286.42 -5 1 -1 734.74 661.55 5 -1 1 1245.65 302.63 5 -1 -1 629.51 386.38 5 1 1 1016.46 312.65 5 1 -1 1452.11 285.33 -5 -1 -2 720.93 479.58 -5 1 2 605.83 484.83 -5 -1 2 1460.83 353.78 -5 1 -2 1331.41 487.85 5 -1 -2 1461.18 271.86 5 -1 2 917.54 189.60 5 1 2 655.92 667.17 5 1 -2 1269.28 304.73 -5 -1 -3 320.01 189.54 -5 1 3 440.84 229.16 -5 -1 3 259.01 190.49 -5 1 -3 42.07 170.22 -5 -1 -3 384.76 162.70 5 1 -3 439.80 218.23 5 -1 3 166.90 163.58 -5 1 4 1823.81 454.05 -5 -1 4 2205.67 289.35 -5 -1 -4 1608.58 312.04 -5 1 -4 1110.94 615.71 -5 -1 -4 1038.81 609.88 5 -1 -4 1769.24 279.60 5 1 -4 2312.34 341.62 5 1 4 1168.71 456.58 5 -1 4 1573.18 269.51 -5 -1 5 895.20 562.13 -5 1 5 1441.77 444.35 -5 -1 -5 1093.82 477.55 -5 1 -5 1783.53 272.36 -5 -1 -5 2334.04 298.51 5 1 -5 1504.33 415.81 5 1 5 1851.94 367.17 5 -1 5 1235.22 603.19 -5 -1 6 481.75 195.23 -5 1 6 918.42 288.70 -5 -1 -6 787.28 225.80 -5 1 -6 650.97 299.88 -5 -1 -6 1084.15 259.20 5 1 -6 1057.72 308.49 -5 -1 7 2353.93 573.85 -5 -1 -7 2481.08 301.80 -5 1 -7 1935.80 973.92 5 1 -7 2435.42 361.97 -5 -1 8 1010.63 315.65 -5 1 -8 758.46 237.26 -5 -1 -8 845.79 289.79 -5 -1 -8 819.03 218.99 5 1 -8 753.36 292.35 5 -1 8 1148.93 295.31 -5 -1 9 746.09 450.78 -5 -1 -9 1403.66 300.24 -5 -1 -10 5772.47 1034.36 -5 -1 -10 6154.75 965.94 -5 1 -10 7032.47 528.59 -5 -1 -11 1048.06 247.75 -5 1 -11 880.44 213.45 -5 -1 -12 738.02 227.64 -5 -1 -12 1083.21 266.02 -5 1 -12 513.24 302.24 -5 -1 -13 3647.22 1132.07 -5 -1 -13 6390.97 534.41 -5 -1 -14 3363.75 360.61 -5 1 -15 861.47 253.64 -5 -2 0 1446.88 238.76 -5 2 0 1239.90 787.51 5 -2 0 888.25 587.68 5 2 0 871.57 424.94 -5 2 1 50.86 175.69 -5 -2 -1 200.63 211.19 -5 -2 1 252.32 143.80 -5 2 -1 227.00 249.06 -5 -2 -1 210.07 133.63 5 -2 1 241.46 222.64 5 -2 -1 124.16 152.95 5 2 1 315.56 218.43 5 2 -1 70.25 202.51 -5 2 2 314.23 292.99 -5 -2 -2 599.59 352.17 -5 -2 2 364.46 117.84 -5 -2 -2 994.35 263.44 5 -2 2 555.55 182.51 5 -2 -2 211.33 149.53 5 2 2 365.16 221.87 5 2 -2 334.72 325.52 -5 -2 3 833.68 666.14 -5 -2 -3 783.98 613.78 -5 2 -3 1119.37 576.38 -5 -2 -3 1504.36 475.12 5 -2 3 807.31 604.33 5 2 -3 1219.80 362.95 -5 -2 4 126.88 207.98 -5 -2 -4 -25.73 155.82 -5 2 -4 156.82 182.13 5 2 -4 39.51 191.78 -5 -2 5 1166.48 307.97 -5 -2 -5 1650.45 252.01 5 2 -5 2009.20 321.73 -5 -2 -6 2690.91 816.37 -5 -2 -6 3967.48 423.08 5 2 -6 3551.60 385.06 -5 -2 -7 1004.44 829.55 -5 -2 -7 1788.10 343.50 5 2 -7 1038.88 753.93 -5 -2 8 132.29 170.31 -5 -2 -8 215.02 156.38 -5 -2 -9 633.08 221.06 -5 -2 10 76.95 104.75 -5 -2 -10 -48.79 134.15 -5 -2 -10 8.35 148.88 -5 -2 -11 963.61 851.02 -5 -2 -11 1526.66 658.45 -5 -2 -12 2525.05 789.62 -5 -2 -12 3732.13 417.16 -5 -2 -13 2431.10 768.67 -5 -2 -1414938.57 921.35 -5 2 -15 3062.15 373.21 -5 -3 0 864.72 216.05 -5 -3 0 1096.77 201.53 -5 -3 1 112.04 209.66 -5 -3 -1 455.85 208.11 -5 -3 1 267.30 246.68 -5 -3 2 762.29 206.41 -5 -3 -2 904.58 312.08 -5 -3 3 238.31 154.20 -5 -3 -3 154.08 202.35 -5 -3 -3 49.03 89.90 -5 -3 4 860.39 275.35 -5 -3 -4 762.03 477.73 -5 -3 -4 611.49 215.37 -5 -3 5 115.32 150.81 -5 -3 -5 313.51 203.39 -5 -3 6 174.73 166.99 -5 -3 -6 -9.54 124.01 -5 -3 -6 134.26 130.62 -5 -3 -7 535.90 220.22 -5 -3 8 2104.08 466.71 -5 -3 -8 2708.39 289.28 -5 -3 -8 2732.37 539.75 -5 -3 9 1162.16 412.17 -5 -3 -9 806.90 541.14 -5 -3 10 522.87 406.83 -5 -4 -1 919.66 567.29 -5 -4 2 1106.37 395.04 -5 -4 -2 934.04 675.32 -5 -4 3 1518.03 825.70 -5 -4 -3 1713.90 900.48 -5 -4 4 58.91 127.54 -5 -4 -4 52.15 150.23 -5 -4 -5 627.69 231.11 -5 -4 6 787.15 209.10 -5 -4 -6 522.86 445.30 -5 -4 7 1339.56 746.68 -5 -4 8 434.49 276.74 -5 -4 9 712.03 372.60 -5 -4 10 2816.55 545.58 -5 -5 1 281.34 343.78 -5 -5 2 428.98 311.29 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 71831 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y, z' 'x+1/2, -y, 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 F1 F 0.5000 -0.4299(5) 0.48037(17) 0.0221(4) Uani 1 2 d S T P . . N1 N 0.24349(5) 0.3932(5) 0.33124(18) 0.0194(4) Uani 1 1 d . . . . . N2 N 0.38561(6) -0.0796(5) -0.46672(17) 0.0211(4) Uani 1 1 d . . . . . C1 C 0.5000 -0.2840(8) 0.3648(3) 0.0170(6) Uani 1 2 d S T P . . C2 C 0.46312(6) -0.2165(6) 0.3093(2) 0.0167(4) Uani 1 1 d . . . . . H2 H 0.4385 -0.2690 0.3509 0.020 Uiso 1 1 calc R U . . . C3 C 0.46301(6) -0.0691(5) 0.1903(2) 0.0151(4) Uani 1 1 d . . . . . C4 C 0.5000 0.0075(8) 0.1326(3) 0.0160(6) Uani 1 2 d S T P . . H4 H 0.5000 0.1137 0.0526 0.019 Uiso 1 2 calc R U P . . C5 C 0.38954(6) 0.1060(6) 0.1883(2) 0.0156(4) Uani 1 1 d . . . . . H5 H 0.3906 0.1297 0.2760 0.019 Uiso 1 1 calc R U . . . C6 C 0.35292(6) 0.1713(6) 0.12567(19) 0.0158(5) Uani 1 1 d . . . . . C7 C 0.35199(6) 0.1397(6) -0.0038(2) 0.0163(4) Uani 1 1 d . . . . . H7 H 0.3275 0.1840 -0.0472 0.020 Uiso 1 1 calc R U . . . C8 C 0.38670(7) 0.0439(6) -0.06952(19) 0.0153(5) Uani 1 1 d . . . . . C9 C 0.42254(6) -0.0234(5) -0.0051(2) 0.0155(4) Uani 1 1 d . . . . . H9 H 0.4462 -0.0911 -0.0496 0.019 Uiso 1 1 calc R U . . . C10 C 0.42427(6) 0.0070(6) 0.12364(19) 0.0155(4) Uani 1 1 d . . . . . C11 C 0.27531(6) 0.2272(6) 0.3822(2) 0.0197(5) Uani 1 1 d . . . . . H11 H 0.2731 0.1523 0.4661 0.024 Uiso 1 1 calc R U . . . C12 C 0.24807(7) 0.4951(6) 0.2125(2) 0.0188(5) Uani 1 1 d . . . . . H12 H 0.2262 0.6172 0.1741 0.023 Uiso 1 1 calc R U . . . C13 C 0.28271(6) 0.4336(6) 0.1423(2) 0.0175(5) Uani 1 1 d . . . . . H13 H 0.2840 0.5103 0.0585 0.021 Uiso 1 1 calc R U . . . C14 C 0.31552(6) 0.2583(6) 0.19632(19) 0.0161(4) Uani 1 1 d . . . . . C15 C 0.31144(6) 0.1570(6) 0.3206(2) 0.0185(5) Uani 1 1 d . . . . . H15 H 0.3331 0.0414 0.3624 0.022 Uiso 1 1 calc R U . . . C16 C 0.38599(6) 0.0050(6) -0.20704(19) 0.0157(5) Uani 1 1 d . . . . . C17 C 0.35264(6) -0.1411(6) -0.2682(2) 0.0180(5) Uani 1 1 d . . . . . H17 H 0.3293 -0.2129 -0.2231 0.022 Uiso 1 1 calc R U . . . C18 C 0.35419(6) -0.1796(6) -0.3961(2) 0.0196(5) Uani 1 1 d . . . . . H18 H 0.3315 -0.2838 -0.4362 0.024 Uiso 1 1 calc R U . . . C19 C 0.41732(7) 0.0653(6) -0.4070(2) 0.0202(5) Uani 1 1 d . . . . . H19 H 0.4399 0.1411 -0.4547 0.024 Uiso 1 1 calc R U . . . C20 C 0.41886(6) 0.1101(6) -0.2795(2) 0.0185(5) Uani 1 1 d . . . . . H20 H 0.4422 0.2118 -0.2417 0.022 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 F1 0.0186(9) 0.0316(10) 0.0161(9) 0.0071(8) 0.000 0.000 N1 0.0157(9) 0.0237(10) 0.0189(9) -0.0016(8) 0.0018(7) 0.0010(7) N2 0.0224(10) 0.0256(10) 0.0153(9) 0.0001(8) 0.0000(7) 0.0004(8) C1 0.0187(14) 0.0196(14) 0.0126(14) -0.0012(12) 0.000 0.000 C2 0.0139(10) 0.0188(10) 0.0174(10) -0.0021(9) 0.0028(8) -0.0011(8) C3 0.0139(10) 0.0156(10) 0.0157(10) -0.0034(8) 0.0005(8) 0.0010(8) C4 0.0180(14) 0.0168(14) 0.0130(14) -0.0013(11) 0.000 0.000 C5 0.0163(10) 0.0168(10) 0.0137(10) 0.0000(8) -0.0003(8) 0.0002(8) C6 0.0150(10) 0.0149(10) 0.0175(11) -0.0001(8) 0.0014(8) 0.0008(8) C7 0.0127(9) 0.0187(10) 0.0176(11) 0.0002(8) -0.0022(8) 0.0000(8) C8 0.0179(11) 0.0153(10) 0.0127(11) 0.0007(8) -0.0008(8) -0.0011(8) C9 0.0120(9) 0.0182(10) 0.0163(11) -0.0009(8) 0.0024(8) -0.0010(7) C10 0.0146(10) 0.0147(10) 0.0172(11) 0.0002(8) -0.0007(8) -0.0001(8) C11 0.0193(10) 0.0245(11) 0.0155(9) -0.0020(9) 0.0009(8) -0.0007(9) C12 0.0149(10) 0.0210(10) 0.0204(12) -0.0001(9) -0.0013(8) 0.0009(8) C13 0.0162(10) 0.0200(10) 0.0163(10) 0.0000(8) -0.0003(8) -0.0004(8) C14 0.0157(10) 0.0162(9) 0.0165(10) -0.0013(8) -0.0012(8) -0.0014(8) C15 0.0148(10) 0.0217(11) 0.0190(11) -0.0007(9) -0.0011(9) 0.0015(8) C16 0.0157(11) 0.0169(10) 0.0146(12) -0.0004(8) -0.0003(8) 0.0030(8) C17 0.0160(10) 0.0206(10) 0.0173(11) 0.0005(9) 0.0005(9) 0.0003(9) C18 0.0178(10) 0.0243(11) 0.0168(11) 0.0000(9) -0.0036(8) -0.0005(9) C19 0.0183(11) 0.0241(11) 0.0181(12) 0.0018(9) 0.0014(9) 0.0005(8) C20 0.0169(10) 0.0201(11) 0.0184(11) 0.0001(9) 0.0009(9) -0.0014(8) 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 C11 N1 C12 115.74(18) . . C18 N2 C19 116.3(2) . . F1 C1 C2 118.11(13) . . F1 C1 C2 118.11(13) . 3_655 C2 C1 C2 123.8(3) . 3_655 C1 C2 C3 118.27(19) . . C1 C2 H2 120.9 . . C3 C2 H2 120.9 . . C2 C3 C4 119.1(2) . . C2 C3 C10 121.31(18) . . C4 C3 C10 119.6(2) . . C3 C4 C3 121.4(3) . 3_655 C3 C4 H4 119.3 . . C3 C4 H4 119.3 3_655 . C10 C5 C6 120.88(19) . . C10 C5 H5 119.6 . . C6 C5 H5 119.6 . . C7 C6 C5 118.87(19) . . C7 C6 C14 120.72(18) . . C5 C6 C14 120.37(18) . . C8 C7 C6 120.67(18) . . C8 C7 H7 119.7 . . C6 C7 H7 119.7 . . C7 C8 C9 119.36(19) . . C7 C8 C16 121.19(19) . . C9 C8 C16 119.44(19) . . C10 C9 C8 121.07(19) . . C10 C9 H9 119.5 . . C8 C9 H9 119.5 . . C5 C10 C9 119.1(2) . . C5 C10 C3 120.95(19) . . C9 C10 C3 119.91(19) . . N1 C11 C15 124.4(2) . . N1 C11 H11 117.8 . . C15 C11 H11 117.8 . . N1 C12 C13 124.3(2) . . N1 C12 H12 117.8 . . C13 C12 H12 117.8 . . C12 C13 C14 119.3(2) . . C12 C13 H13 120.3 . . C14 C13 H13 120.3 . . C13 C14 C15 116.92(18) . . C13 C14 C6 122.30(19) . . C15 C14 C6 120.75(18) . . C11 C15 C14 119.27(19) . . C11 C15 H15 120.4 . . C14 C15 H15 120.4 . . C20 C16 C17 117.38(19) . . C20 C16 C8 121.2(2) . . C17 C16 C8 121.42(19) . . C18 C17 C16 118.79(19) . . C18 C17 H17 120.6 . . C16 C17 H17 120.6 . . N2 C18 C17 124.4(2) . . N2 C18 H18 117.8 . . C17 C18 H18 117.8 . . N2 C19 C20 123.6(2) . . N2 C19 H19 118.2 . . C20 C19 H19 118.2 . . C19 C20 C16 119.6(2) . . C19 C20 H20 120.2 . . C16 C20 H20 120.2 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 F1 C1 1.360(3) . N1 C11 1.338(3) . N1 C12 1.344(3) . N2 C18 1.340(3) . N2 C19 1.344(3) . C1 C2 1.380(2) . C1 C2 1.380(2) 3_655 C2 C3 1.397(3) . C2 H2 0.9500 . C3 C4 1.400(2) . C3 C10 1.494(3) . C4 C3 1.400(2) 3_655 C4 H4 0.9500 . C5 C10 1.392(3) . C5 C6 1.406(3) . C5 H5 0.9500 . C6 C7 1.401(3) . C6 C14 1.486(3) . C7 C8 1.394(3) . C7 H7 0.9500 . C8 C9 1.395(3) . C8 C16 1.490(3) . C9 C10 1.394(3) . C9 H9 0.9500 . C11 C15 1.390(3) . C11 H11 0.9500 . C12 C13 1.390(3) . C12 H12 0.9500 . C13 C14 1.394(3) . C13 H13 0.9500 . C14 C15 1.399(3) . C15 H15 0.9500 . C16 C20 1.393(3) . C16 C17 1.395(3) . C17 C18 1.387(3) . C17 H17 0.9500 . C18 H18 0.9500 . C19 C20 1.386(3) . C19 H19 0.9500 . C20 H20 0.9500 . 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 F1 C1 C2 C3 -179.6(2) . . . . C2 C1 C2 C3 -0.5(4) 3_655 . . . C1 C2 C3 C4 -0.6(3) . . . . C1 C2 C3 C10 179.2(2) . . . . C2 C3 C4 C3 1.7(4) . . . 3_655 C10 C3 C4 C3 -178.14(18) . . . 3_655 C10 C5 C6 C7 -0.8(3) . . . . C10 C5 C6 C14 176.8(2) . . . . C5 C6 C7 C8 0.2(3) . . . . C14 C6 C7 C8 -177.39(19) . . . . C6 C7 C8 C9 0.5(3) . . . . C6 C7 C8 C16 179.2(2) . . . . C7 C8 C9 C10 -0.6(3) . . . . C16 C8 C9 C10 -179.41(19) . . . . C6 C5 C10 C9 0.7(3) . . . . C6 C5 C10 C3 -178.85(19) . . . . C8 C9 C10 C5 0.1(3) . . . . C8 C9 C10 C3 179.60(19) . . . . C2 C3 C10 C5 32.2(3) . . . . C4 C3 C10 C5 -148.0(2) . . . . C2 C3 C10 C9 -147.3(2) . . . . C4 C3 C10 C9 32.5(3) . . . . C12 N1 C11 C15 -0.2(3) . . . . C11 N1 C12 C13 1.0(3) . . . . N1 C12 C13 C14 -0.6(3) . . . . C12 C13 C14 C15 -0.6(3) . . . . C12 C13 C14 C6 177.6(2) . . . . C7 C6 C14 C13 -23.5(3) . . . . C5 C6 C14 C13 158.9(2) . . . . C7 C6 C14 C15 154.7(2) . . . . C5 C6 C14 C15 -22.9(3) . . . . N1 C11 C15 C14 -1.1(4) . . . . C13 C14 C15 C11 1.4(3) . . . . C6 C14 C15 C11 -176.9(2) . . . . C7 C8 C16 C20 142.9(2) . . . . C9 C8 C16 C20 -38.3(3) . . . . C7 C8 C16 C17 -37.7(3) . . . . C9 C8 C16 C17 141.0(2) . . . . C20 C16 C17 C18 1.1(3) . . . . C8 C16 C17 C18 -178.2(2) . . . . C19 N2 C18 C17 0.3(3) . . . . C16 C17 C18 N2 -1.2(4) . . . . C18 N2 C19 C20 0.7(3) . . . . N2 C19 C20 C16 -0.7(4) . . . . C17 C16 C20 C19 -0.3(3) . . . . C8 C16 C20 C19 179.1(2) . . . .