#------------------------------------------------------------------------------ #$Date: 2020-01-15 02:25:11 +0200 (Wed, 15 Jan 2020) $ #$Revision: 246845 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/78/4037817.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_4037817 loop_ _publ_author_name 'Wang, Rongkang' 'Ding, Tianqi' 'Jiang, Lvqi' 'He, Wujuan' 'Yi, Wenbin' _publ_section_title ; Fluoromethoxymethylation of Nitrogen Heterocyclic Compounds with Fluoromethyl Iodide. ; _journal_name_full 'The Journal of organic chemistry' _journal_paper_doi 10.1021/acs.joc.9b03193 _journal_year 2020 _chemical_formula_sum 'C13 H13 F N2 O2' _chemical_formula_weight 248.25 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.2319(3) _cell_length_b 14.2453(9) _cell_length_c 19.5737(12) _cell_measurement_reflns_used 4071 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.17 _cell_measurement_theta_min 2.52 _cell_volume 1179.99(13) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_unetI/netI 0.0361 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 7088 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.009 _diffrn_reflns_theta_max 25.009 _diffrn_reflns_theta_min 2.525 _exptl_absorpt_coefficient_mu 0.106 _exptl_crystal_density_diffrn 1.397 _exptl_crystal_description BLOCK _exptl_crystal_F_000 520 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.160 _refine_diff_density_max 0.122 _refine_diff_density_min -0.201 _refine_diff_density_rms 0.037 _refine_ls_abs_structure_details ; Flack x determined using 716 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.6(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 164 _refine_ls_number_reflns 2065 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0342 _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^)+(0.0512P)^2^+0.1488P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0886 _refine_ls_wR_factor_ref 0.0909 _reflns_Friedel_coverage 0.651 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 1900 _reflns_number_total 2065 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo9b03193_si_002.cif _cod_data_source_block 20190104LMF_0m_a _cod_database_code 4037817 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.977 _shelx_estimated_absorpt_t_max 0.983 _shelx_res_file ; TITL 20190104LMF_0m_a.res in P2(1)2(1)2(1) 20190104LMF_0m_a.res created by SHELXL-2018/3 at 19:58:47 on 04-Jan-2019 CELL 0.71073 4.2319 14.2453 19.5737 90.000 90.000 90.000 ZERR 4.000 0.0003 0.0009 0.0012 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H N O F UNIT 52 52 8 8 4 L.S. 10 OMIT -3 50.02 ACTA BOND $H FMAP 2 SIZE .22 .19 .16 PLAN 20 LIST 6 TEMP -100 WGHT 0.051200 0.148800 FVAR 1.52552 C1 1 0.534736 0.441237 0.503118 11.00000 0.02130 0.02518 = 0.02970 0.00422 -0.00424 0.00590 C2 1 0.364263 0.359052 0.491185 11.00000 0.02471 0.02729 = 0.03424 0.00936 -0.00169 0.00144 AFIX 43 H2 2 0.253012 0.328355 0.526933 11.00000 -1.20000 AFIX 0 C3 1 0.363464 0.324187 0.425680 11.00000 0.02697 0.02264 = 0.04300 0.00205 -0.00770 -0.00191 AFIX 43 H3 2 0.249655 0.268270 0.415980 11.00000 -1.20000 AFIX 0 C4 1 0.528023 0.369755 0.372735 11.00000 0.02583 0.02477 = 0.03192 -0.00088 -0.00486 0.00436 C5 1 0.698051 0.450516 0.384178 11.00000 0.02129 0.02564 = 0.02944 0.00318 -0.00137 0.00262 AFIX 43 H5 2 0.807743 0.481011 0.348114 11.00000 -1.20000 AFIX 0 C6 1 0.703971 0.486440 0.451159 11.00000 0.02054 0.02134 = 0.02989 0.00487 -0.00391 0.00450 C7 1 0.854808 0.566789 0.480945 11.00000 0.02058 0.02322 = 0.03153 0.00222 -0.00371 0.00529 C8 1 0.769181 0.568375 0.547931 11.00000 0.02544 0.02596 = 0.03062 0.00097 -0.00571 0.00342 AFIX 43 H8 2 0.834080 0.614495 0.580057 11.00000 -1.20000 AFIX 0 C9 1 1.067112 0.634844 0.444665 11.00000 0.02618 0.02506 = 0.03513 0.00161 -0.00449 0.00096 AFIX 23 H9A 2 1.202204 0.667155 0.478608 11.00000 -1.20000 H9B 2 1.207035 0.599896 0.413104 11.00000 -1.20000 AFIX 0 C10 1 0.888306 0.705038 0.405873 11.00000 0.02960 0.02520 = 0.03119 -0.00074 0.00188 -0.00231 C11 1 0.434142 0.473899 0.627092 11.00000 0.02793 0.03782 = 0.03124 0.00609 0.00053 0.00659 AFIX 23 H11A 2 0.223881 0.444802 0.620519 11.00000 -1.20000 H11B 2 0.405931 0.532981 0.653015 11.00000 -1.20000 AFIX 0 C12 1 0.480518 0.359379 0.713144 11.00000 0.04899 0.03002 = 0.03409 0.00201 0.00553 -0.00052 AFIX 23 H12A 2 0.622266 0.309606 0.730659 11.00000 -1.20000 H12B 2 0.293242 0.328834 0.692540 11.00000 -1.20000 AFIX 0 C13 1 0.667581 0.369951 0.254638 11.00000 0.04954 0.04099 = 0.03028 -0.00184 -0.00488 -0.00667 AFIX 137 H13A 2 0.588480 0.433838 0.247397 11.00000 -1.50000 H13B 2 0.636724 0.332967 0.212952 11.00000 -1.50000 H13C 2 0.893217 0.372296 0.265773 11.00000 -1.50000 AFIX 0 F1 5 0.385993 0.416822 0.766629 11.00000 0.07399 0.05351 = 0.03262 0.00020 0.00877 0.00694 N1 3 0.746094 0.760630 0.377369 11.00000 0.04814 0.03884 = 0.05124 0.01252 -0.00054 0.00725 N2 3 0.574462 0.493309 0.562447 11.00000 0.02753 0.03132 = 0.02661 0.00360 -0.00186 0.00233 O1 4 0.499173 0.327373 0.309655 11.00000 0.04084 0.03136 = 0.03469 -0.00447 -0.00224 -0.00428 O2 4 0.635851 0.411240 0.664327 11.00000 0.03149 0.04179 = 0.03481 0.01526 0.00130 0.00550 HKLF 4 REM 20190104LMF_0m_a.res in P2(1)2(1)2(1) REM wR2 = 0.0909, GooF = S = 1.055, Restrained GooF = 1.055 for all data REM R1 = 0.0342 for 1900 Fo > 4sig(Fo) and 0.0384 for all 2065 data REM 164 parameters refined using 0 restraints END WGHT 0.0397 0.2169 REM Highest difference peak 0.122, deepest hole -0.201, 1-sigma level 0.037 Q1 1 0.6109 0.4095 0.7668 11.00000 0.05 0.12 Q2 1 0.8603 0.5195 0.4616 11.00000 0.05 0.12 Q3 1 0.2040 0.3588 0.6937 11.00000 0.05 0.12 Q4 1 0.5041 0.3480 0.2108 11.00000 0.05 0.11 Q5 1 0.5253 0.4740 0.4741 11.00000 0.05 0.11 Q6 1 0.8344 0.4572 0.4208 11.00000 0.05 0.10 Q7 1 0.9557 0.5574 0.5159 11.00000 0.05 0.10 Q8 1 0.2936 0.4593 0.3830 11.00000 0.05 0.10 Q9 1 0.2807 0.4335 0.4917 11.00000 0.05 0.10 Q10 1 0.3381 0.4748 0.2661 11.00000 0.05 0.10 Q11 1 0.9293 0.5930 0.4603 11.00000 0.05 0.10 Q12 1 0.5747 0.5065 0.2398 11.00000 0.05 0.10 Q13 1 0.9729 0.6248 0.6233 11.00000 0.05 0.10 Q14 1 0.6066 0.4821 0.7635 11.00000 0.05 0.10 Q15 1 0.8135 0.5777 0.6458 11.00000 0.05 0.10 Q16 1 1.1738 0.6066 0.6002 11.00000 0.05 0.09 Q17 1 0.7992 0.3814 0.3776 11.00000 0.05 0.09 Q18 1 0.2456 0.4474 0.2381 11.00000 0.05 0.09 Q19 1 1.1005 0.5203 0.3966 11.00000 0.05 0.09 Q20 1 0.4489 0.3778 0.1592 11.00000 0.05 0.09 ; _shelx_res_checksum 71692 _shelx_hkl_file ; 1 0 0 -2.40 1.20 -1 0 0 -0.10 1.70 2 0 0 212.08 12.50 -3 0 0 5.10 6.00 -4 0 0 38.70 10.40 -5 0 0 -1.50 14.20 -1 -1 0 7996.90 334.67 1 -1 0 7955.40 334.47 -1 1 0 8271.37 334.47 -2 -1 0 17.40 4.10 2 -1 0 25.30 4.50 3 -1 0 218.08 16.00 -3 -1 0 205.58 16.10 -4 -1 0 56.09 11.90 -4 1 0 22.90 10.80 -5 -1 0 10.20 14.10 -5 1 0 -14.80 13.50 -2 -2 0 6.50 3.30 2 -2 0 2.60 3.00 3 -2 0 577.64 30.80 -3 -2 0 572.94 31.20 -4 -2 0 0.30 8.40 -5 -2 0 13.50 14.40 -5 2 0 9.00 16.20 0 -3 0 1.50 1.00 0 3 0 2.00 1.50 1 -3 0 6268.97 266.07 -1 -3 0 6200.18 266.07 -1 3 0 6314.77 265.77 1 3 0 6640.14 266.47 -1 3 0 6580.24 265.37 -2 -3 0 467.35 22.50 2 -3 0 411.16 22.10 -2 3 0 424.76 23.00 -3 -3 0 21.20 7.40 3 -3 0 26.20 7.40 -4 -3 0 327.37 24.50 4 -3 0 329.77 25.20 -5 -3 0 -21.10 12.70 -5 3 0 -27.50 17.00 0 -4 0 5036.90 212.58 0 4 0 5196.98 212.58 -1 -4 0 260.07 13.90 1 -4 0 271.57 13.90 1 4 0 257.17 14.40 -1 4 0 283.97 12.60 -1 4 0 269.57 13.70 2 -4 0 1527.85 67.89 -2 -4 0 1550.54 67.89 -2 4 0 1518.05 67.29 -3 -4 0 712.63 36.70 3 -4 0 720.13 37.00 -4 -4 0 106.99 15.40 4 -4 0 115.49 15.90 -5 -4 0 53.99 16.80 -5 4 0 42.70 16.90 0 -5 0 5.90 1.50 0 -5 0 6.00 2.10 0 5 0 1.10 2.20 1 -5 0 72.09 6.00 -1 -5 0 77.39 6.20 -1 5 0 82.59 4.10 2 -5 0 2450.75 105.79 -2 -5 0 2450.45 105.59 -2 5 0 2420.96 104.19 -3 -5 0 89.99 11.50 3 -5 0 87.29 11.10 4 -5 0 63.89 13.70 -4 -5 0 91.29 14.10 -5 -5 0 -3.80 12.70 5 -5 0 35.10 16.40 0 -6 0 177.68 9.90 0 -6 0 163.18 8.50 1 -6 0 16.80 3.70 -1 -6 0 18.90 3.60 -2 -6 0 2246.58 99.29 2 -6 0 2202.28 99.49 -2 6 0 2397.46 97.29 3 -6 0 254.17 19.30 -3 -6 0 275.97 19.20 4 -6 0 18.40 11.20 -4 -6 0 8.80 9.20 5 -6 0 -0.60 14.90 -5 -6 0 13.00 14.80 1 -7 0 614.54 29.30 -1 -7 0 611.04 29.20 -2 -7 0 3.20 5.30 2 -7 0 0.70 4.60 -2 7 0 6.20 3.20 3 -7 0 212.68 17.90 -3 -7 0 193.28 16.50 4 -7 0 27.50 12.40 -4 -7 0 -2.80 9.70 -5 -7 0 -6.10 16.00 5 -7 0 4.10 17.60 0 -8 0 46.80 4.20 0 -8 0 52.19 5.80 -1 -8 0 786.22 37.20 1 -8 0 797.32 37.40 -2 -8 0 39.30 6.80 2 -8 0 43.50 7.80 -2 8 0 42.00 4.10 -3 -8 0 219.98 17.70 3 -8 0 241.28 19.60 4 -8 0 50.79 13.10 -4 -8 0 83.19 14.30 0 -9 0 8.90 3.90 0 -9 0 2.60 2.00 -1 -9 0 0.40 4.60 1 -9 0 -0.80 4.20 -2 -9 0 350.26 21.60 2 -9 0 365.46 22.40 -3 -9 0 341.57 23.50 3 -9 0 328.57 24.50 -4 -9 0 56.29 13.40 4 -9 0 85.29 16.90 0 -10 0 589.14 25.60 0 -10 0 558.04 26.70 -1 -10 0 26.90 6.10 1 -10 0 16.10 5.60 2 -10 0 3.40 7.30 -2 -10 0 -5.20 5.40 3 -10 0 111.19 14.80 -3 -10 0 80.59 11.70 -3 10 0 107.49 8.80 4 -10 0 294.67 28.40 -4 -10 0 184.58 22.50 0 -11 0 8.10 4.70 0 -11 0 -3.80 4.40 0 -11 0 4.00 2.40 1 -11 0 28.30 7.50 -1 -11 0 28.20 6.60 -1 -11 0 35.70 6.00 -2 -11 0 70.49 10.30 2 -11 0 83.39 12.00 -3 -11 0 70.29 12.00 3 -11 0 47.20 12.90 -4 -11 0 4.60 12.90 4 -11 0 -8.00 12.80 0 -12 0 285.17 13.30 0 -12 0 250.17 15.30 0 -12 0 272.57 17.90 -1 -12 0 94.59 11.70 1 -12 0 85.19 11.00 -1 -12 0 95.69 10.50 -2 -12 0 79.89 12.10 2 -12 0 80.89 13.00 3 -12 0 -4.40 10.10 -3 -12 0 -2.60 8.80 4 -12 0 1.60 16.40 -4 -12 0 -7.60 13.20 0 -13 0 11.70 5.00 0 -13 0 8.20 2.80 0 -13 0 18.20 6.80 -1 -13 0 0.60 5.80 1 -13 0 11.00 7.50 -1 -13 0 0.80 7.00 2 -13 0 130.79 17.10 -2 -13 0 121.49 15.60 -2 -13 0 153.38 18.70 -3 -13 0 -10.50 10.00 3 -13 0 -11.00 12.00 0 -14 0 897.31 37.10 0 -14 0 827.32 43.70 1 -14 0 20.00 8.70 -1 -14 0 15.60 7.20 -1 -14 0 13.50 8.10 2 -14 0 1.10 9.90 -2 -14 0 27.30 11.30 -2 -14 0 3.40 9.40 -3 -14 0 9.60 11.10 3 -14 0 -10.20 13.90 -3 -14 0 5.40 16.30 0 -15 0 3.20 8.00 1 -15 0 547.45 32.70 -1 -15 0 507.55 30.80 -1 -15 0 485.55 27.40 2 -15 0 -9.80 10.40 -2 -15 0 10.00 12.20 -2 -15 0 3.90 9.10 -3 -15 0 29.20 19.20 3 -15 0 6.30 15.10 -3 -15 0 -5.80 10.80 0 -16 0 623.34 37.00 1 -16 0 334.17 25.50 -1 -16 0 321.17 23.70 -1 -16 0 294.27 20.00 2 -16 0 -10.40 14.00 -2 -16 0 -4.60 12.40 -2 -16 0 13.40 11.00 0 -17 0 27.70 12.20 -1 -17 0 26.80 13.10 1 -17 0 17.50 12.40 2 -17 0 3.40 13.90 -2 -17 0 9.90 13.90 -2 -17 0 -7.90 12.10 0 -18 0 85.09 18.40 -1 -18 0 218.78 26.30 1 -18 0 194.98 24.80 -5 0 1 457.75 37.00 -4 0 1 151.58 18.40 -3 0 1 63.79 9.60 2 0 -1 12.10 3.70 -1 0 1 2415.56 99.89 1 0 -1 2307.87 99.89 -1 0 1 2391.86 100.49 1 0 1 2262.97 98.39 -1 0 -1 2430.66 98.49 -3 0 -1 76.69 9.80 -4 0 -1 170.88 18.80 -5 0 -1 463.65 35.70 -5 -1 1 82.29 18.40 -5 1 1 60.59 18.90 -4 -1 1 8.30 9.80 -4 1 1 10.80 10.00 -3 -1 1 57.99 9.40 3 -1 -1 65.19 10.10 2 -1 -1 1359.66 59.89 -2 -1 1 1330.67 59.99 -1 -1 1 7657.83 327.87 -1 -1 1 8176.48 327.87 1 -1 -1 7381.26 327.67 -1 1 1 8086.89 327.77 -1 1 1 8231.68 328.17 -1 -1 -1 7859.31 331.07 1 -1 1 7621.04 330.87 1 1 1 8227.38 331.27 -1 1 -1 8265.57 330.97 2 -1 1 1368.16 59.69 -2 -1 -1 1336.67 59.79 3 -1 1 54.39 8.40 -3 -1 -1 72.19 9.70 -4 -1 -1 -1.80 9.20 -4 1 -1 -0.80 8.90 -5 -1 -1 72.89 17.20 -5 1 -1 104.59 18.20 -5 -2 1 283.47 28.90 -5 2 1 223.28 26.40 -4 -2 1 258.87 21.10 -3 -2 1 95.49 12.20 3 -2 -1 73.09 10.00 -2 -2 1 1557.04 67.49 2 -2 -1 1485.85 67.09 1 -2 -1 4131.99 178.48 -1 -2 1 4073.29 178.58 -1 2 1 4399.36 178.38 -1 2 1 4383.06 178.28 1 2 -1 4391.36 178.88 0 -2 1 57.89 3.00 0 -2 -1 51.59 3.00 0 -2 -1 53.39 3.20 0 -2 1 55.49 3.30 0 2 1 56.99 3.10 0 2 1 59.59 3.30 0 2 -1 60.49 3.30 0 2 -1 46.20 3.00 -1 -2 -1 4110.59 174.98 1 -2 1 3992.30 174.78 1 2 1 4497.95 175.38 -1 2 -1 4191.08 174.68 2 -2 1 1562.84 69.89 -2 -2 -1 1636.74 70.29 -3 -2 -1 93.19 11.70 3 -2 1 100.99 11.40 -4 -2 -1 274.27 21.90 -4 2 -1 229.28 21.80 -5 -2 -1 295.97 28.50 -5 2 -1 285.27 29.80 -5 -3 1 36.00 16.10 -5 3 1 39.10 18.00 4 -3 -1 19.30 11.00 -4 -3 1 42.10 10.90 3 -3 -1 15.70 6.50 -3 -3 1 19.00 6.40 2 -3 -1 186.58 12.60 -2 -3 1 214.58 13.00 1 -3 -1 6430.16 272.77 1 -3 -1 6113.89 271.97 -1 -3 1 6339.37 272.87 -1 3 1 6918.71 271.97 1 3 -1 6810.32 273.27 -1 3 1 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5.80 12.90 -3 3 20 21.30 15.40 3 3 -20 48.60 20.90 2 -3 -20 33.70 14.40 -2 -3 20 17.80 10.50 2 3 -20 0.90 13.10 1 -3 -20 33.90 10.80 -1 -3 20 28.70 8.40 1 3 -20 35.70 12.90 0 -3 20 68.39 8.00 0 -3 -20 103.59 13.40 0 3 20 88.29 9.20 0 3 -20 66.09 13.60 -1 -3 -20 20.70 8.00 -1 3 -20 45.20 10.20 -2 -3 -20 16.10 9.10 -2 3 -20 19.80 9.20 -3 -3 -20 17.50 12.00 -3 3 -20 26.50 11.40 -3 -4 20 20.70 13.90 3 -4 -20 6.80 18.00 3 4 -20 52.09 21.80 -2 -4 20 69.59 13.20 2 -4 -20 85.69 16.00 2 -4 -20 82.99 17.10 2 4 -20 79.99 17.50 -1 -4 20 59.19 9.50 1 -4 -20 65.39 13.30 1 -4 -20 53.79 11.80 1 4 -20 51.09 13.90 0 -4 -20 16.30 9.30 0 -4 20 12.80 4.40 0 -4 -20 23.30 7.40 0 4 -20 17.50 10.40 -1 -4 -20 60.59 10.80 -1 4 -20 36.30 10.40 -2 -4 -20 110.59 14.90 -2 4 -20 101.29 13.60 -3 -4 -20 32.30 13.60 -3 4 -20 43.60 12.00 3 -5 -20 47.80 18.40 3 -5 -20 60.09 18.40 -3 -5 20 55.59 16.60 3 5 -20 17.10 21.10 2 -5 -20 39.70 14.50 2 -5 -20 41.20 14.50 -2 -5 20 18.60 10.70 2 5 -20 -14.80 14.50 -1 -5 20 94.59 11.20 1 -5 -20 63.49 13.50 1 -5 -20 99.89 14.60 1 5 -20 69.59 15.10 0 -5 -20 -5.50 7.90 0 -5 20 3.50 4.50 0 -5 -20 -3.80 8.10 0 5 -20 1.20 9.70 -1 -5 -20 83.39 12.20 -1 5 -20 97.49 13.80 -2 -5 -20 20.50 10.00 -2 5 -20 11.80 9.30 -3 -5 -20 36.60 14.80 -3 5 -20 35.90 11.90 2 -6 -20 62.89 16.60 -2 -6 20 68.79 13.60 2 -6 -20 59.89 15.50 2 6 -20 49.30 17.40 1 -6 -20 96.89 15.20 -1 -6 20 115.39 12.70 1 -6 -20 101.29 15.00 1 6 -20 97.89 18.60 0 -6 20 56.49 7.10 0 -6 -20 58.59 11.60 0 -6 -20 68.49 11.90 0 6 -20 51.19 12.70 -1 -6 -20 125.69 15.90 -1 6 -20 121.49 15.50 -2 -6 -20 74.29 14.30 -2 6 -20 51.49 11.20 -2 -7 20 39.00 12.00 2 -7 -20 46.80 15.60 2 -7 -20 54.89 15.70 2 7 -20 77.49 19.90 1 -7 -20 11.90 12.90 -1 -7 20 13.80 8.20 1 -7 -20 7.10 11.30 1 7 -20 19.30 13.30 0 -7 20 0.80 5.70 0 -7 -20 4.90 9.70 0 -7 -20 18.80 9.50 0 7 -20 -5.60 11.10 -1 -7 -20 -1.20 8.90 -1 7 -20 0.70 10.30 -2 -7 -20 45.90 12.70 -2 7 -20 71.69 12.60 -2 -8 20 69.39 14.20 2 -8 -20 38.10 15.10 2 -8 -20 58.49 17.50 2 8 -20 46.20 20.90 1 -8 -20 158.48 19.00 -1 -8 20 162.48 16.90 1 -8 -20 162.48 20.30 1 8 -20 106.49 19.80 0 -8 -20 8.90 11.10 0 -8 -20 11.00 8.90 0 -8 20 8.70 7.10 0 8 -20 19.90 12.90 -1 -8 -20 150.28 17.70 -1 8 -20 175.68 20.70 -2 -8 -20 72.29 14.40 -2 8 -20 58.09 13.00 2 -9 -20 92.09 20.20 2 -9 -20 115.49 19.80 -2 -9 20 67.99 15.70 2 9 -20 59.69 23.50 -1 -9 20 41.90 10.70 1 -9 -20 45.00 13.30 1 -9 -20 33.70 15.00 1 9 -20 36.00 17.00 0 -9 20 122.29 13.80 0 -9 -20 145.69 18.70 0 -9 -20 135.79 17.10 0 9 -20 113.49 18.40 -1 -9 -20 45.90 11.00 -1 9 -20 33.00 13.20 -2 -9 -20 109.79 16.30 -2 9 -20 98.69 15.40 1 -10 -20 52.19 16.30 -1 -10 20 44.50 11.70 1 -10 -20 45.80 14.00 1 10 -20 26.70 20.50 0 -10 -20 -4.30 12.80 0 -10 20 19.90 8.50 0 -10 -20 -0.80 9.90 0 10 -20 33.50 15.60 -1 -10 -20 53.09 12.40 -1 10 -20 50.29 14.20 0 -11 -20 171.38 21.00 0 -11 -20 247.28 27.20 0 -11 20 161.78 17.70 0 11 -20 132.79 21.40 3 0 -21 27.00 19.20 -3 0 21 60.69 17.20 2 0 -21 16.30 14.00 -2 0 21 34.60 12.00 1 0 -21 29.80 12.20 -1 0 21 50.69 9.70 0 0 -21 0.10 9.10 0 0 21 3.00 5.40 -1 0 -21 30.00 9.50 -2 0 -21 29.70 9.90 -3 0 -21 70.19 14.80 -3 -1 21 -7.50 14.90 3 -1 -21 35.30 18.10 -3 1 21 -9.90 14.80 3 1 -21 40.00 21.00 -2 -1 21 104.79 15.50 2 -1 -21 117.69 20.00 -2 1 21 95.09 15.70 2 1 -21 111.49 20.40 1 -1 -21 60.29 14.50 -1 -1 21 49.20 9.60 1 1 -21 66.49 14.00 -1 1 21 59.89 10.50 0 -1 -21 120.59 15.90 0 -1 21 84.49 8.30 0 1 -21 86.59 14.60 0 1 21 74.29 8.20 -1 -1 -21 49.70 10.60 -1 1 -21 71.59 12.10 -2 -1 -21 121.39 14.70 -2 1 -21 119.19 15.40 -3 -1 -21 37.00 13.10 -3 1 -21 6.40 11.60 -3 -2 21 46.50 15.80 3 -2 -21 40.80 21.60 -3 2 21 64.59 17.30 3 2 -21 34.40 21.00 -2 -2 21 66.09 13.40 2 -2 -21 82.59 17.40 -2 2 21 80.09 15.40 2 2 -21 61.39 18.70 -1 -2 21 -1.40 7.90 1 -2 -21 0.30 11.70 -1 2 21 1.90 8.80 1 2 -21 5.30 11.60 0 -2 21 7.10 4.50 0 -2 -21 -0.70 8.50 0 2 -21 2.90 9.40 0 2 21 14.60 6.20 -1 -2 -21 3.90 8.90 -1 2 -21 -6.00 8.30 -2 -2 -21 99.09 13.80 -2 2 -21 90.19 13.10 -3 -2 -21 62.79 14.70 -3 2 -21 68.69 13.80 -2 -3 21 119.19 16.10 2 -3 -21 93.59 19.00 2 3 -21 96.49 18.20 -2 3 21 110.99 17.60 1 -3 -21 53.99 14.50 -1 -3 21 43.30 9.40 -1 3 21 35.90 11.00 1 3 -21 29.00 14.20 0 -3 -21 186.88 18.20 0 -3 21 198.48 12.60 0 3 -21 224.78 21.60 0 3 21 204.78 15.40 -1 -3 -21 58.89 11.50 -1 3 -21 41.50 11.50 -2 -3 -21 98.89 13.90 -2 3 -21 112.49 14.70 -2 -4 21 5.20 11.80 2 -4 -21 0.50 12.40 2 -4 -21 34.60 14.10 2 4 -21 11.60 15.50 1 -4 -21 3.50 10.00 1 -4 -21 3.00 10.20 -1 -4 21 17.90 8.10 1 4 -21 19.30 13.40 0 -4 -21 8.90 9.70 0 -4 21 6.70 5.00 0 4 -21 18.60 10.80 -1 -4 -21 -7.40 8.40 -1 4 -21 2.70 9.90 -2 -4 -21 0.40 9.90 -2 4 -21 18.00 11.10 2 -5 -21 54.19 15.80 2 -5 -21 46.70 14.60 -2 -5 21 52.59 13.60 2 5 -21 48.80 19.10 1 -5 -21 -3.00 10.90 -1 -5 21 -0.60 7.90 1 -5 -21 -3.90 11.70 1 5 -21 0.30 14.90 0 -5 21 6.00 5.70 0 -5 -21 19.50 9.00 0 -5 -21 5.30 8.60 0 5 -21 19.60 11.70 -1 -5 -21 1.10 9.00 -1 5 -21 12.70 10.20 -2 -5 -21 89.29 14.80 -2 5 -21 89.89 13.80 -2 -6 21 -7.50 10.50 2 -6 -21 33.70 14.90 2 -6 -21 27.20 16.60 2 6 -21 25.70 18.80 -1 -6 21 24.70 9.30 1 -6 -21 50.69 13.60 1 -6 -21 18.50 11.70 1 6 -21 43.90 16.40 0 -6 -21 24.80 11.10 0 -6 -21 26.90 10.90 0 -6 21 6.30 6.10 0 6 -21 15.30 12.40 -1 -6 -21 29.90 10.20 -1 6 -21 37.30 11.80 -2 -6 -21 35.60 11.80 -2 6 -21 47.10 12.50 -2 -7 21 64.39 13.90 2 -7 -21 58.69 18.00 2 -7 -21 64.69 18.50 2 7 -21 43.60 20.30 -1 -7 21 11.00 9.00 1 -7 -21 -1.70 10.90 1 -7 -21 13.00 13.10 1 7 -21 -2.10 14.30 0 -7 -21 15.30 10.10 0 -7 -21 3.00 9.50 0 7 -21 -0.70 12.20 -1 -7 -21 -2.10 10.00 -1 7 -21 3.30 11.30 -2 -7 -21 83.79 15.40 -2 7 -21 58.39 13.40 2 -8 -21 32.50 16.90 -2 -8 21 42.40 14.00 2 -8 -21 21.80 16.20 2 8 -21 32.30 20.30 -1 -8 21 81.59 11.90 1 -8 -21 88.89 16.00 1 -8 -21 79.89 15.80 1 8 -21 55.39 18.40 0 -8 -21 15.70 11.60 0 -8 -21 -14.70 10.00 0 8 -21 10.90 13.50 -1 -8 -21 70.89 13.90 -1 8 -21 72.69 14.60 -2 -8 -21 39.40 13.80 -2 8 -21 30.00 12.60 -1 -9 21 83.19 12.00 1 -9 -21 93.49 17.50 1 -9 -21 95.29 17.00 1 9 -21 64.89 20.20 0 -9 -21 74.89 16.00 0 -9 -21 65.79 13.80 0 9 -21 77.89 17.20 -1 -9 -21 92.59 15.40 -1 9 -21 74.89 16.20 0 -10 -21 13.50 14.70 0 -10 -21 4.80 11.60 0 10 -21 14.90 16.30 -2 0 22 28.40 13.60 2 0 -22 56.99 17.10 1 0 -22 33.10 12.90 -1 0 22 59.79 10.10 0 0 -22 18.60 10.40 -1 0 -22 45.50 11.90 -2 0 -22 45.80 11.20 -2 -1 22 -15.90 11.00 2 -1 -22 -1.70 14.90 2 1 -22 4.60 16.10 -2 1 22 18.50 13.60 -1 -1 22 180.48 17.40 1 -1 -22 177.38 21.60 -1 1 22 169.88 18.80 1 1 -22 181.08 22.60 0 -1 -22 198.98 20.70 0 1 -22 185.88 22.30 -1 -1 -22 218.68 20.20 -1 1 -22 184.58 20.50 -2 -1 -22 -8.10 10.20 -2 1 -22 9.00 10.10 -2 -2 22 29.50 12.40 2 -2 -22 21.10 15.70 2 2 -22 21.30 16.60 -2 2 22 31.00 13.50 -1 -2 22 22.70 9.00 1 -2 -22 7.90 11.60 1 2 -22 27.30 13.10 -1 2 22 11.70 10.20 0 -2 -22 -4.40 10.30 0 2 -22 -14.00 10.70 -1 -2 -22 -1.30 8.60 -1 2 -22 30.60 10.60 -2 -2 -22 7.50 9.50 -2 2 -22 27.00 11.10 -2 -3 22 210.18 23.10 2 -3 -22 160.58 22.90 -2 3 22 240.48 25.20 2 3 -22 194.88 25.40 1 -3 -22 43.50 13.60 -1 -3 22 81.29 11.00 1 3 -22 36.40 14.00 -1 3 22 83.49 13.10 0 -3 -22 185.98 19.90 0 3 -22 137.59 19.40 -1 -3 -22 65.79 12.10 -1 3 -22 85.69 15.50 -2 -3 -22 213.38 22.10 -2 3 -22 255.47 21.90 2 -4 -22 51.49 16.70 -2 -4 22 29.80 12.40 2 4 -22 25.50 18.80 1 -4 -22 1.10 11.50 -1 -4 22 -2.40 8.00 1 4 -22 -2.30 13.50 0 -4 -22 9.40 9.20 0 4 -22 9.30 13.10 -1 -4 -22 -3.60 9.80 -1 4 -22 -7.50 10.90 -2 -4 -22 32.20 12.00 -2 4 -22 46.30 12.70 2 -5 -22 7.00 14.70 -2 -5 22 21.00 12.40 2 -5 -22 12.80 15.30 2 5 -22 16.50 18.50 1 -5 -22 129.49 18.80 1 -5 -22 164.98 18.00 -1 -5 22 123.49 15.70 1 5 -22 114.39 19.70 0 -5 -22 29.60 11.10 0 5 -22 43.70 15.20 -1 -5 -22 163.28 19.70 -1 5 -22 167.08 20.60 -2 -5 -22 6.20 11.20 -2 5 -22 17.10 12.10 2 -6 -22 55.29 19.50 2 -6 -22 35.90 16.20 -2 -6 22 47.40 13.20 2 6 -22 17.70 18.90 1 -6 -22 60.69 15.20 1 -6 -22 48.40 14.00 -1 -6 22 36.80 9.90 1 6 -22 16.00 16.00 0 -6 -22 -18.60 9.30 0 6 -22 -1.80 13.20 -1 -6 -22 19.90 11.40 -1 6 -22 31.30 13.60 -2 -6 -22 48.50 13.00 -2 6 -22 36.80 12.90 1 -7 -22 -8.30 13.10 1 -7 -22 2.60 12.50 -1 -7 22 6.00 9.50 1 7 -22 17.40 16.30 0 -7 -22 5.10 11.70 0 7 -22 -9.80 13.50 -1 -7 -22 -13.90 9.50 -1 7 -22 19.30 14.10 1 -8 -22 22.80 14.80 1 -8 -22 16.30 13.90 -1 -8 22 28.90 10.40 1 8 -22 9.00 17.50 0 -8 -22 1.30 11.60 0 8 -22 11.20 16.10 -1 -8 -22 25.00 11.20 -1 8 -22 49.60 16.00 0 -9 -22 -11.00 11.50 0 9 -22 -6.10 16.60 2 0 -23 68.29 19.50 -2 0 23 41.90 14.20 1 0 -23 56.69 16.10 -1 0 23 45.70 11.00 0 0 -23 -6.80 11.70 -1 0 -23 66.89 14.00 -2 0 -23 66.79 13.30 2 -1 -23 14.60 18.00 -2 -1 23 63.59 14.30 -2 1 23 25.50 14.80 2 1 -23 46.80 19.70 1 -1 -23 132.79 19.50 -1 -1 23 110.49 13.60 1 1 -23 78.09 16.80 -1 1 23 91.09 13.70 0 -1 -23 2.10 11.60 0 1 -23 6.30 11.70 -1 -1 -23 104.49 15.60 -1 1 -23 136.89 17.50 -2 -1 -23 28.50 11.80 -2 1 -23 45.80 12.20 -2 -2 23 -2.50 12.20 2 -2 -23 -9.90 16.60 2 2 -23 26.80 16.80 -2 2 23 2.10 13.70 1 -2 -23 46.10 15.40 -1 -2 23 24.30 10.20 1 2 -23 53.29 16.90 -1 2 23 33.00 11.90 0 -2 -23 31.40 12.70 0 2 -23 37.20 12.00 -1 -2 -23 25.30 11.50 -1 2 -23 30.00 12.10 -2 -2 -23 12.20 11.20 -2 2 -23 1.60 11.90 -2 -3 23 88.79 15.90 2 -3 -23 91.99 21.00 -2 3 23 76.39 17.20 2 3 -23 42.20 21.90 1 -3 -23 7.40 13.70 -1 -3 23 3.30 9.40 1 3 -23 -2.60 13.60 -1 3 23 17.60 11.60 0 -3 -23 262.47 24.10 0 3 -23 247.88 24.90 -1 -3 -23 -2.10 10.40 -1 3 -23 -11.80 10.70 -2 -3 -23 102.09 17.10 -2 3 -23 88.29 15.90 -2 -4 23 21.40 13.40 2 -4 -23 23.30 18.60 -2 4 23 2.70 14.60 2 4 -23 47.00 20.00 -1 -4 23 7.70 8.90 1 -4 -23 -3.20 12.70 1 4 -23 28.10 16.20 -1 4 23 -6.10 11.90 0 -4 -23 -9.00 11.30 0 4 -23 -3.10 12.40 -1 -4 -23 -17.20 9.30 -1 4 -23 19.00 11.40 -2 -4 -23 40.90 13.80 -2 4 -23 23.90 13.10 1 -5 -23 140.99 18.30 1 -5 -23 137.69 19.80 -1 -5 23 143.49 16.90 1 5 -23 159.58 25.20 0 -5 -23 21.20 12.50 0 5 -23 37.10 14.20 -1 -5 -23 170.28 20.30 -1 5 -23 112.59 17.70 1 -6 -23 15.70 12.40 1 -6 -23 22.50 14.70 -1 -6 23 -0.60 9.20 1 6 -23 5.40 17.60 0 -6 -23 29.90 13.40 0 6 -23 30.90 15.90 -1 -6 -23 19.10 11.50 -1 6 -23 35.10 14.00 -1 -7 23 17.10 10.20 1 -7 -23 27.00 15.40 1 -7 -23 51.99 17.00 1 7 -23 44.20 19.70 0 -7 -23 13.70 11.40 0 7 -23 -4.40 15.20 -1 -7 -23 27.30 13.20 -1 7 -23 37.20 14.70 1 0 -24 9.40 15.10 0 0 -24 140.29 20.20 -1 0 -24 -1.00 11.80 1 -1 -24 12.90 13.00 -1 1 24 1.00 16.00 1 1 -24 12.60 15.70 0 -1 -24 34.60 13.60 0 1 -24 77.59 16.50 -1 -1 -24 21.80 11.50 -1 1 -24 25.00 12.50 1 -2 -24 34.40 14.50 -1 2 24 7.20 12.50 1 2 -24 19.30 15.90 0 -2 -24 0.80 11.70 0 2 -24 14.00 13.50 -1 -2 -24 34.10 12.70 -1 2 -24 37.40 14.30 1 -3 -24 17.20 14.30 -1 3 24 38.30 13.90 1 3 -24 16.80 16.40 0 -3 -24 24.00 13.50 0 3 -24 17.20 13.70 -1 -3 -24 16.70 12.50 -1 3 -24 33.70 13.40 1 -4 -24 48.60 15.90 1 4 -24 34.90 17.20 -1 4 24 38.70 13.90 0 -4 -24 24.40 12.60 0 4 -24 32.60 15.00 -1 -4 -24 48.10 14.30 -1 4 -24 61.49 16.10 1 -5 -24 69.29 18.60 1 5 -24 87.89 21.60 0 -5 -24 45.30 13.60 0 5 -24 37.60 16.30 -1 -5 -24 65.39 16.20 -1 5 -24 95.59 19.10 0 -6 -24 44.30 15.40 0 6 -24 21.60 17.30 1 0 -25 30.40 18.70 0 0 -25 3.50 13.80 -1 0 -25 52.09 14.60 1 -1 -25 54.49 20.20 1 1 -25 37.30 18.30 0 -1 -25 83.99 18.10 0 1 -25 96.39 18.60 -1 -1 -25 56.29 15.50 -1 1 -25 49.60 16.00 0 -2 -25 -27.70 13.70 0 2 -25 11.50 14.80 0 -3 -25 181.68 22.80 0 3 -25 158.88 21.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 16213 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -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 0.5347(6) 0.44124(15) 0.50312(11) 0.0254(5) Uani 1 1 d . . C2 C 0.3643(6) 0.35905(16) 0.49118(12) 0.0287(5) Uani 1 1 d . . H2 H 0.253012 0.328355 0.526933 0.034 Uiso 1 1 calc R U C3 C 0.3635(6) 0.32419(16) 0.42568(12) 0.0309(6) Uani 1 1 d . . H3 H 0.249655 0.268270 0.415980 0.037 Uiso 1 1 calc R U C4 C 0.5280(6) 0.36976(16) 0.37273(11) 0.0275(6) Uani 1 1 d . . C5 C 0.6981(6) 0.45052(15) 0.38418(11) 0.0255(5) Uani 1 1 d . . H5 H 0.807743 0.481011 0.348114 0.031 Uiso 1 1 calc R U C6 C 0.7040(6) 0.48644(15) 0.45116(11) 0.0239(5) Uani 1 1 d . . C7 C 0.8548(6) 0.56679(15) 0.48095(11) 0.0251(5) Uani 1 1 d . . C8 C 0.7692(6) 0.56837(16) 0.54793(12) 0.0273(5) Uani 1 1 d . . H8 H 0.834080 0.614495 0.580057 0.033 Uiso 1 1 calc R U C9 C 1.0671(6) 0.63484(16) 0.44466(13) 0.0288(6) Uani 1 1 d . . H9A H 1.202204 0.667155 0.478608 0.035 Uiso 1 1 calc R U H9B H 1.207035 0.599896 0.413104 0.035 Uiso 1 1 calc R U C10 C 0.8883(6) 0.70504(16) 0.40587(11) 0.0287(6) Uani 1 1 d . . C11 C 0.4341(7) 0.47390(17) 0.62709(12) 0.0323(6) Uani 1 1 d . . H11A H 0.223881 0.444802 0.620519 0.039 Uiso 1 1 calc R U H11B H 0.405931 0.532981 0.653015 0.039 Uiso 1 1 calc R U C12 C 0.4805(8) 0.35938(17) 0.71314(12) 0.0377(7) Uani 1 1 d . . H12A H 0.622266 0.309606 0.730659 0.045 Uiso 1 1 calc R U H12B H 0.293242 0.328834 0.692540 0.045 Uiso 1 1 calc R U C13 C 0.6676(7) 0.36995(19) 0.25464(12) 0.0403(7) Uani 1 1 d . . H13A H 0.588480 0.433838 0.247397 0.060 Uiso 1 1 calc R U H13B H 0.636724 0.332967 0.212952 0.060 Uiso 1 1 calc R U H13C H 0.893217 0.372296 0.265773 0.060 Uiso 1 1 calc R U F1 F 0.3860(5) 0.41682(11) 0.76663(7) 0.0534(5) Uani 1 1 d . . N1 N 0.7461(6) 0.76063(16) 0.37737(12) 0.0461(6) Uani 1 1 d . . N2 N 0.5745(5) 0.49331(13) 0.56245(9) 0.0285(5) Uani 1 1 d . . O1 O 0.4992(5) 0.32737(11) 0.30965(8) 0.0356(5) Uani 1 1 d . . O2 O 0.6359(5) 0.41124(12) 0.66433(8) 0.0360(5) Uani 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0213(13) 0.0252(11) 0.0297(12) 0.0042(9) -0.0042(10) 0.0059(10) C2 0.0247(13) 0.0273(12) 0.0342(12) 0.0094(9) -0.0017(11) 0.0014(11) C3 0.0270(13) 0.0226(11) 0.0430(14) 0.0021(11) -0.0077(12) -0.0019(11) C4 0.0258(14) 0.0248(11) 0.0319(13) -0.0009(9) -0.0049(11) 0.0044(11) C5 0.0213(13) 0.0256(12) 0.0294(12) 0.0032(9) -0.0014(10) 0.0026(10) C6 0.0205(13) 0.0213(11) 0.0299(12) 0.0049(9) -0.0039(10) 0.0045(10) C7 0.0206(12) 0.0232(11) 0.0315(12) 0.0022(9) -0.0037(10) 0.0053(10) C8 0.0254(13) 0.0260(12) 0.0306(13) 0.0010(9) -0.0057(10) 0.0034(11) C9 0.0262(14) 0.0251(11) 0.0351(12) 0.0016(10) -0.0045(11) 0.0010(11) C10 0.0296(14) 0.0252(11) 0.0312(13) -0.0007(9) 0.0019(12) -0.0023(11) C11 0.0279(15) 0.0378(13) 0.0312(13) 0.0061(10) 0.0005(12) 0.0066(11) C12 0.0490(18) 0.0300(12) 0.0341(13) 0.0020(10) 0.0055(13) -0.0005(14) C13 0.0495(18) 0.0410(13) 0.0303(13) -0.0018(11) -0.0049(13) -0.0067(15) F1 0.0740(14) 0.0535(9) 0.0326(8) 0.0002(7) 0.0088(9) 0.0069(10) N1 0.0481(16) 0.0388(13) 0.0512(14) 0.0125(11) -0.0005(13) 0.0072(12) N2 0.0275(12) 0.0313(10) 0.0266(10) 0.0036(8) -0.0019(9) 0.0023(10) O1 0.0408(11) 0.0314(8) 0.0347(9) -0.0045(7) -0.0022(8) -0.0043(9) O2 0.0315(10) 0.0418(10) 0.0348(9) 0.0153(7) 0.0013(8) 0.0055(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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 N2 C1 C2 130.6(2) N2 C1 C6 107.4(2) C2 C1 C6 121.9(2) C3 C2 C1 117.4(2) C3 C2 H2 121.3 C1 C2 H2 121.3 C2 C3 C4 121.3(2) C2 C3 H3 119.4 C4 C3 H3 119.4 O1 C4 C5 123.9(2) O1 C4 C3 114.4(2) C5 C4 C3 121.7(2) C4 C5 C6 117.7(2) C4 C5 H5 121.1 C6 C5 H5 121.1 C1 C6 C5 120.0(2) C1 C6 C7 107.41(19) C5 C6 C7 132.6(2) C8 C7 C6 106.6(2) C8 C7 C9 127.2(2) C6 C7 C9 126.1(2) C7 C8 N2 110.2(2) C7 C8 H8 124.9 N2 C8 H8 124.9 C10 C9 C7 112.1(2) C10 C9 H9A 109.2 C7 C9 H9A 109.2 C10 C9 H9B 109.2 C7 C9 H9B 109.2 H9A C9 H9B 107.9 N1 C10 C9 178.1(3) N2 C11 O2 108.9(2) N2 C11 H11A 109.9 O2 C11 H11A 109.9 N2 C11 H11B 109.9 O2 C11 H11B 109.9 H11A C11 H11B 108.3 O2 C12 F1 110.20(19) O2 C12 H12A 109.6 F1 C12 H12A 109.6 O2 C12 H12B 109.6 F1 C12 H12B 109.6 H12A C12 H12B 108.1 O1 C13 H13A 109.5 O1 C13 H13B 109.5 H13A C13 H13B 109.5 O1 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C8 N2 C1 108.31(19) C8 N2 C11 125.6(2) C1 N2 C11 126.1(2) C4 O1 C13 116.44(19) C12 O2 C11 113.8(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N2 1.388(3) C1 C2 1.395(3) C1 C6 1.401(3) C2 C3 1.375(3) C2 H2 0.9500 C3 C4 1.407(3) C3 H3 0.9500 C4 O1 1.380(3) C4 C5 1.375(3) C5 C6 1.408(3) C5 H5 0.9500 C6 C7 1.434(3) C7 C8 1.361(3) C7 C9 1.500(3) C8 N2 1.380(3) C8 H8 0.9500 C9 C10 1.466(3) C9 H9A 0.9900 C9 H9B 0.9900 C10 N1 1.140(3) C11 N2 1.425(3) C11 O2 1.434(3) C11 H11A 0.9900 C11 H11B 0.9900 C12 O2 1.375(3) C12 F1 1.388(3) C12 H12A 0.9900 C12 H12B 0.9900 C13 O1 1.427(3) C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800