#------------------------------------------------------------------------------ #$Date: 2019-10-09 11:48:58 +0300 (Wed, 09 Oct 2019) $ #$Revision: 219201 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234504.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_7234504 loop_ _publ_author_name 'Lisa M. Kozycz' 'Chang Guo' 'Joseph G. Manion' 'Andrew J. Tilley' 'Alan J. Lough' 'Yuning Li' 'Dwight S. Seferos' _publ_section_title ; Enhanced electron mobility in crystalline thionated naphthalene diimides ; _journal_name_full 'Journal of Materials Chemistry C' _journal_page_first 11505 _journal_page_last 11515 _journal_paper_doi 10.1039/C5TC02753E _journal_volume 3 _journal_year 2015 _chemical_formula_moiety 'C38 H54 N2 O4' _chemical_formula_sum 'C38 H54 N2 O4' _chemical_formula_weight 602.83 _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 _cell_angle_alpha 92.995(2) _cell_angle_beta 94.603(2) _cell_angle_gamma 104.495(2) _cell_formula_units_Z 1 _cell_length_a 4.6352(2) _cell_length_b 6.6073(2) _cell_length_c 27.9285(9) _cell_measurement_reflns_used 9910 _cell_measurement_temperature 147(2) _cell_measurement_theta_max 66.80 _cell_measurement_theta_min 3.18 _cell_volume 823.12(5) _computing_cell_refinement APEX2 _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT (Sheldrick, 2008)' _diffrn_ambient_temperature 147(2) _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'Bruker Kappa APEX-DUO CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_unetI/netI 0.0282 _diffrn_reflns_Laue_measured_fraction_full 0.980 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 29125 _diffrn_reflns_point_group_measured_fraction_full 0.980 _diffrn_reflns_point_group_measured_fraction_max 0.980 _diffrn_reflns_theta_full 67.391 _diffrn_reflns_theta_max 67.391 _diffrn_reflns_theta_min 1.591 _diffrn_source 'Bruker ImuS with multi-layer optics' _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_T_max 0.7529 _exptl_absorpt_correction_T_min 0.6574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.216 _exptl_crystal_description plate _exptl_crystal_F_000 328 _exptl_crystal_size_max 0.190 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.187 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.043 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 200 _refine_ls_number_reflns 2915 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.097 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0461 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.4910P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1213 _refine_ls_wR_factor_ref 0.1251 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2448 _reflns_number_total 2915 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file J-Mater-Chem-C-2015-3-11505.cif _cod_data_source_block d1548_a _cod_database_code 7234504 _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 0.893 _shelx_estimated_absorpt_t_max 0.976 _shelx_res_file ; d1548_a.res created by SHELXL-2014/7 TITL d1548_a.res in P-1 REM Old TITL d1548 in P-1 REM SHELXT solution in P-1 REM R1 0.128, Rweak 0.004, Alpha 0.030, Orientation as input REM Formula found by SHELXT: C19 N O2 CELL 1.54178 4.6352 6.6073 27.9285 92.995 94.603 104.495 ZERR 1.000 0.0002 0.0002 0.0009 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 38 54 2 4 TEMP -126.140 SIZE 0.04 0.16 0.19 ACTA L.S. 5 BOND $H HTAB CONF FMAP 2 PLAN 20 WGHT 0.045100 0.491000 FVAR 1.02912 O1 4 0.963877 0.123403 0.574056 11.00000 0.03935 0.02616 = 0.03166 0.00810 0.00319 0.01844 O2 4 0.571116 0.601819 0.650352 11.00000 0.04434 0.02843 = 0.02167 0.00140 0.00402 0.01420 N1 3 0.770508 0.364696 0.612431 11.00000 0.02396 0.02069 = 0.02121 0.00614 0.00187 0.00624 C1 1 0.498885 0.424252 0.434817 11.00000 0.01959 0.01380 = 0.02366 0.00348 0.00352 0.00070 C2 1 0.652239 0.270451 0.437176 11.00000 0.02748 0.01739 = 0.02343 0.00097 0.00548 0.00533 AFIX 43 H2A 2 0.687000 0.201300 0.408341 11.00000 -1.20000 AFIX 0 C3 1 0.757113 0.215647 0.481939 11.00000 0.02292 0.01406 = 0.03026 0.00373 0.00420 0.00638 AFIX 43 H3A 2 0.862406 0.109493 0.483158 11.00000 -1.20000 AFIX 0 C4 1 0.709084 0.313971 0.524053 11.00000 0.01792 0.01517 = 0.02483 0.00482 0.00347 0.00216 C5 1 0.552371 0.471899 0.522487 11.00000 0.01613 0.01394 = 0.02359 0.00385 0.00390 0.00101 C6 1 0.824603 0.257085 0.571209 11.00000 0.02218 0.01545 = 0.02797 0.00570 0.00406 0.00407 C7 1 0.612177 0.519095 0.612564 11.00000 0.02412 0.01764 = 0.02377 0.00356 0.00347 0.00301 C8 1 0.885895 0.309809 0.659655 11.00000 0.02629 0.02749 = 0.02199 0.00822 -0.00105 0.00755 AFIX 23 H8A 2 0.965617 0.439761 0.680952 11.00000 -1.20000 H8B 2 1.053470 0.245064 0.654987 11.00000 -1.20000 AFIX 0 C9 1 0.648188 0.159329 0.684289 11.00000 0.02543 0.02509 = 0.02490 0.00713 0.00142 0.00709 AFIX 23 H9A 2 0.516205 0.056695 0.659755 11.00000 -1.20000 H9B 2 0.523496 0.238869 0.700335 11.00000 -1.20000 AFIX 0 C10 1 0.789144 0.042826 0.721467 11.00000 0.02586 0.02272 = 0.02432 0.00594 0.00105 0.00627 AFIX 23 H10A 2 0.913827 -0.036120 0.705225 11.00000 -1.20000 H10B 2 0.922412 0.146290 0.745699 11.00000 -1.20000 AFIX 0 C11 1 0.558583 -0.108972 0.747131 11.00000 0.02758 0.02103 = 0.02393 0.00462 0.00331 0.00748 AFIX 23 H11A 2 0.460743 -0.027834 0.768474 11.00000 -1.20000 H11B 2 0.402367 -0.194690 0.722868 11.00000 -1.20000 AFIX 0 C12 1 0.695148 -0.253721 0.776932 11.00000 0.02755 0.02216 = 0.02684 0.00656 0.00305 0.00565 AFIX 23 H12A 2 0.848032 -0.167568 0.801615 11.00000 -1.20000 H12B 2 0.797961 -0.331450 0.755654 11.00000 -1.20000 AFIX 0 C13 1 0.468066 -0.410785 0.801952 11.00000 0.02932 0.02264 = 0.02821 0.00706 0.00361 0.00615 AFIX 23 H13A 2 0.312769 -0.495303 0.777389 11.00000 -1.20000 H13B 2 0.368366 -0.333343 0.823840 11.00000 -1.20000 AFIX 0 C14 1 0.607513 -0.557906 0.830858 11.00000 0.02927 0.02129 = 0.02877 0.00706 0.00423 0.00508 AFIX 23 H14A 2 0.701171 -0.638579 0.808698 11.00000 -1.20000 H14B 2 0.768053 -0.472820 0.854544 11.00000 -1.20000 AFIX 0 C15 1 0.385711 -0.710879 0.857517 11.00000 0.03083 0.02131 = 0.03054 0.00738 0.00516 0.00607 AFIX 23 H15A 2 0.224176 -0.795294 0.833897 11.00000 -1.20000 H15B 2 0.293443 -0.630372 0.879940 11.00000 -1.20000 AFIX 0 C16 1 0.526241 -0.858490 0.885925 11.00000 0.03015 0.02173 = 0.02974 0.00703 0.00425 0.00465 AFIX 23 H16A 2 0.616309 -0.940234 0.863433 11.00000 -1.20000 H16B 2 0.689485 -0.774008 0.909255 11.00000 -1.20000 AFIX 0 C17 1 0.305229 -1.009955 0.913126 11.00000 0.03203 0.02305 = 0.02974 0.00799 0.00451 0.00413 AFIX 23 H17A 2 0.135642 -1.088366 0.890099 11.00000 -1.20000 H17B 2 0.224494 -0.928414 0.937048 11.00000 -1.20000 AFIX 0 C18 1 0.442082 -1.165942 0.939058 11.00000 0.03906 0.02520 = 0.03234 0.00964 0.00349 0.00533 AFIX 23 H18A 2 0.608649 -1.087960 0.962671 11.00000 -1.20000 H18B 2 0.526474 -1.245790 0.915298 11.00000 -1.20000 AFIX 0 C19 1 0.216452 -1.319382 0.965228 11.00000 0.04819 0.02968 = 0.03990 0.01573 0.00437 0.00374 AFIX 137 H19A 2 0.315151 -1.417123 0.980783 11.00000 -1.50000 H19B 2 0.051492 -1.397892 0.942027 11.00000 -1.50000 H19C 2 0.137701 -1.241745 0.989693 11.00000 -1.50000 AFIX 0 HKLF 4 REM d1548_a.res in P-1 REM R1 = 0.0461 for 2448 Fo > 4sig(Fo) and 0.0535 for all 2915 data REM 200 parameters refined using 0 restraints END WGHT 0.0451 0.4914 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.187, deepest hole -0.246, 1-sigma level 0.043 Q1 1 0.7458 0.3016 0.5475 11.00000 0.05 0.19 Q2 1 0.4708 0.4596 0.4143 11.00000 0.05 0.17 Q3 1 0.4954 0.4842 0.4552 11.00000 0.05 0.16 Q4 1 0.6812 0.4224 0.5235 11.00000 0.05 0.15 Q5 1 0.7102 0.0963 0.7012 11.00000 0.05 0.14 Q6 1 0.6140 0.3724 0.4369 11.00000 0.05 0.14 Q7 1 0.2367 -0.4417 0.7965 11.00000 0.05 0.14 Q8 1 0.9947 0.1118 0.3681 11.00000 0.05 0.13 Q9 1 0.0348 -1.0765 0.9037 11.00000 0.05 0.13 Q10 1 1.0226 -0.0125 0.4693 11.00000 0.05 0.13 Q11 1 1.2024 0.1900 0.7177 11.00000 0.05 0.13 Q12 1 0.0647 -0.6612 0.9260 11.00000 0.05 0.13 Q13 1 0.1517 -0.7467 0.8500 11.00000 0.05 0.13 Q14 1 0.8075 0.2716 0.7330 11.00000 0.05 0.13 Q15 1 1.0272 -0.1339 0.6519 11.00000 0.05 0.13 Q16 1 0.7031 -1.0942 1.0121 11.00000 0.05 0.13 Q17 1 0.8038 0.2943 0.7605 11.00000 0.05 0.13 Q18 1 1.0417 0.2726 0.7430 11.00000 0.05 0.12 Q19 1 0.4490 0.1393 0.6786 11.00000 0.05 0.12 Q20 1 0.4037 -1.0646 0.9303 11.00000 0.05 0.12 ; _shelx_res_checksum 54048 _shelx_hkl_file ; -1 0 0 6565.64 409.66 -1 0 0 6553.84 409.36 -1 0 0 6534.55 409.66 1 0 0 6161.18 409.36 1 0 0 6135.09 409.56 1 0 0 6150.88 409.26 -2 0 0 6.00 1.10 -2 0 0 5.00 1.20 2 0 0 5.10 1.20 2 0 0 5.30 1.70 2 0 0 3.70 0.90 2 0 0 4.00 0.90 -3 0 0 15.20 3.90 -3 0 0 16.20 3.40 -3 0 0 10.70 3.60 -3 0 0 12.70 3.70 -3 0 0 16.20 2.10 -3 0 0 11.20 2.90 -3 0 0 19.20 5.50 -3 0 0 14.20 4.10 3 0 0 13.60 2.20 3 0 0 13.40 2.30 3 0 0 14.40 2.10 -4 0 0 18.20 7.00 -4 0 0 26.60 5.00 -4 0 0 32.80 6.70 -4 0 0 40.50 7.90 -4 0 0 32.20 6.40 -4 0 0 25.60 4.80 4 0 0 25.20 3.60 4 0 0 23.80 3.30 4 0 0 31.80 2.50 -5 0 0 2.60 3.40 -5 0 0 12.90 7.10 -5 0 0 3.60 3.70 -5 0 0 7.20 3.50 -5 0 0 7.90 5.90 -5 1 0 13.40 6.60 -5 1 0 21.20 4.80 -5 1 0 13.70 4.70 -5 1 0 23.60 4.90 -5 1 0 10.00 3.80 4 -1 0 16.90 2.90 -4 1 0 23.50 5.50 -4 1 0 18.30 4.10 -4 1 0 35.60 6.20 -4 1 0 14.00 4.10 -4 1 0 18.00 6.70 -4 1 0 19.40 5.60 3 -1 0 151.08 9.60 3 -1 0 144.79 10.40 -3 1 0 153.08 11.00 -3 1 0 145.69 12.90 -3 1 0 119.69 11.20 -3 1 0 126.79 9.60 -3 1 0 107.59 12.40 -3 1 0 144.39 11.40 2 -1 0 247.68 18.00 -2 1 0 278.97 17.90 -2 1 0 294.57 18.00 1 -1 0 525.85 34.20 -1 1 0 517.35 34.10 -1 1 0 523.05 34.10 -1 1 0 535.35 34.20 0 -1 0 524.75 33.80 0 -1 0 480.75 33.80 0 -1 0 527.15 33.80 0 -1 0 549.25 33.80 0 1 0 549.85 33.80 0 1 0 486.65 33.80 0 1 0 544.05 33.70 0 1 0 512.45 33.70 -1 -1 0 6611.64 439.06 -1 -1 0 6953.30 439.46 -1 -1 0 7005.80 439.06 -1 -1 0 7043.60 439.56 -1 -1 0 6755.12 439.36 1 1 0 6876.51 439.36 1 1 0 6364.86 439.16 1 1 0 6997.70 440.16 1 1 0 6700.23 439.36 -2 -1 0 15.30 1.90 -2 -1 0 20.40 2.30 -2 -1 0 23.50 2.10 -2 -1 0 23.20 2.30 2 1 0 21.20 2.80 2 1 0 23.10 2.20 2 1 0 14.00 2.00 2 1 0 23.50 2.30 -3 -1 0 -0.90 2.90 -3 -1 0 -0.10 3.30 -3 -1 0 0.00 3.30 -3 -1 0 1.60 3.30 -3 -1 0 2.30 4.20 -3 -1 0 -0.40 3.30 -3 -1 0 3.10 2.90 -3 -1 0 0.70 2.90 3 1 0 2.60 1.70 3 1 0 0.50 1.80 3 1 0 2.10 1.40 3 1 0 2.50 0.90 -4 -1 0 4.60 4.60 -4 -1 0 4.00 3.60 -4 -1 0 1.10 5.10 -4 -1 0 0.50 4.40 -4 -1 0 -1.50 3.90 -4 -1 0 6.30 4.30 -4 -1 0 6.80 7.30 4 1 0 2.50 1.10 4 1 0 2.20 2.00 4 1 0 4.50 1.40 -5 -1 0 -0.50 2.50 -5 -1 0 -1.40 5.30 -5 -1 0 -10.00 8.00 -5 -1 0 2.90 3.50 5 1 0 1.00 1.10 -5 2 0 15.90 3.80 -5 2 0 25.20 5.50 -5 2 0 4.10 5.10 -5 2 0 13.10 4.60 -4 2 0 -1.30 5.30 -4 2 0 0.80 3.70 -4 2 0 3.80 4.60 -4 2 0 1.50 5.20 -4 2 0 3.40 3.30 -4 2 0 3.10 4.00 3 -2 0 295.57 19.70 -3 2 0 316.87 22.10 -3 2 0 268.67 21.00 -3 2 0 288.97 20.20 -3 2 0 287.17 21.00 2 -2 0 1194.58 75.89 2 -2 0 1136.49 75.79 -2 2 0 1180.68 75.79 1 -2 0 173.48 11.00 1 -2 0 138.39 10.80 1 -2 0 178.48 11.00 1 -2 0 171.48 11.00 -1 2 0 178.88 11.00 -1 2 0 155.78 11.00 -1 2 0 149.49 10.90 -1 2 0 171.88 11.00 0 -2 0 273.47 17.90 0 -2 0 272.67 18.40 0 -2 0 270.97 18.00 0 -2 0 286.47 18.10 0 -2 0 279.87 18.00 0 2 0 266.57 18.00 0 2 0 289.97 17.90 0 2 0 259.77 18.00 0 2 0 281.07 17.90 0 2 0 278.07 18.10 -1 -2 0 407.46 28.00 -1 -2 0 458.75 28.10 -1 -2 0 425.16 28.00 -1 -2 0 449.95 28.10 -1 -2 0 425.26 28.00 -1 -2 0 421.26 28.10 1 2 0 437.56 28.40 1 2 0 438.66 28.10 1 2 0 434.56 28.00 1 2 0 418.96 28.10 1 2 0 404.66 27.90 1 2 0 447.66 28.10 -2 -2 0 269.27 17.30 -2 -2 0 233.78 17.20 -2 -2 0 258.27 17.20 -2 -2 0 262.47 17.20 2 2 0 253.47 17.20 2 2 0 246.48 16.90 2 2 0 287.17 17.20 2 2 0 229.28 17.70 2 2 0 270.17 17.30 2 2 0 272.67 17.20 -3 -2 0 34.90 6.20 -3 -2 0 21.00 4.90 -3 -2 0 24.20 3.60 -3 -2 0 25.30 5.70 -3 -2 0 24.40 5.50 -3 -2 0 22.00 4.10 -3 -2 0 28.40 6.30 -3 -2 0 27.00 5.90 -3 -2 0 25.80 6.70 3 2 0 25.60 3.30 3 2 0 28.40 4.10 3 2 0 29.80 2.50 3 2 0 34.30 5.10 3 2 0 34.60 3.20 3 2 0 24.70 3.40 -4 -2 0 24.30 5.40 -4 -2 0 13.60 6.70 -4 -2 0 34.30 7.70 -4 -2 0 27.40 5.50 -4 -2 0 25.40 4.70 -4 -2 0 29.30 6.20 4 2 0 39.90 3.40 4 2 0 40.60 3.30 -5 3 0 34.30 6.50 -4 3 0 16.60 7.50 -4 3 0 3.90 5.00 -4 3 0 11.20 3.70 -4 3 0 7.10 5.00 -4 3 0 4.90 5.30 -4 3 0 8.60 6.40 3 -3 0 11.80 2.20 -3 3 0 4.10 3.80 -3 3 0 4.80 4.80 -3 3 0 7.10 4.00 -3 3 0 6.80 2.90 -3 3 0 6.90 3.30 -3 3 0 9.30 4.70 2 -3 0 1071.89 65.09 2 -3 0 956.10 65.09 2 -3 0 1010.40 65.09 -2 3 0 973.60 65.09 1 -3 0 320.37 21.20 1 -3 0 346.67 21.30 1 -3 0 323.97 21.30 1 -3 0 343.17 21.30 1 -3 0 312.77 21.20 -1 3 0 314.17 21.10 -1 3 0 315.57 21.20 -1 3 0 304.67 21.20 -1 3 0 324.47 21.20 -1 3 0 331.87 21.30 0 -3 0 4.00 1.20 0 -3 0 5.20 1.10 0 -3 0 4.40 0.80 0 -3 0 4.10 1.20 0 -3 0 4.00 1.30 0 -3 0 5.20 1.30 0 -3 0 4.70 1.20 0 3 0 4.10 1.20 0 3 0 3.70 1.10 0 3 0 4.10 1.00 0 3 0 4.00 0.80 0 3 0 3.70 0.90 0 3 0 3.80 1.10 -1 -3 0 161.48 10.90 -1 -3 0 169.88 11.10 -1 -3 0 167.88 10.90 -1 -3 0 159.98 10.90 -1 -3 0 155.58 10.90 1 3 0 161.18 11.00 1 3 0 168.98 10.90 1 3 0 160.88 10.90 1 3 0 155.38 11.20 1 3 0 166.58 10.80 1 3 0 148.39 10.70 -2 -3 0 638.04 38.30 -2 -3 0 491.15 39.40 -2 -3 0 604.24 39.80 -2 -3 0 527.25 39.80 -2 -3 0 618.54 39.50 -2 -3 0 613.94 38.90 -2 -3 0 589.74 38.70 -2 -3 0 621.24 38.10 -2 -3 0 542.45 38.00 2 3 0 608.84 37.70 2 3 0 570.84 38.20 2 3 0 551.74 37.90 2 3 0 560.34 37.80 2 3 0 584.34 38.60 2 3 0 569.34 38.00 2 3 0 579.54 38.00 -3 -3 0 14.30 3.70 -3 -3 0 18.60 6.60 -3 -3 0 23.20 5.50 -3 -3 0 18.20 3.20 -3 -3 0 21.70 5.30 3 3 0 18.30 3.70 3 3 0 11.50 2.50 3 3 0 11.50 2.40 -4 -3 0 6.30 3.00 -4 -3 0 6.00 3.70 -4 -3 0 10.80 6.00 4 3 0 6.70 1.50 4 3 0 4.00 2.50 -5 4 0 9.70 5.10 -4 4 0 145.19 16.70 -4 4 0 94.69 14.50 -4 4 0 123.99 14.50 -4 4 0 144.59 10.90 -4 4 0 136.09 13.70 3 -4 0 286.17 19.10 -3 4 0 275.87 23.60 -3 4 0 267.47 20.80 -3 4 0 295.67 20.50 -3 4 0 290.57 19.90 -3 4 0 289.57 21.80 2 -4 0 1424.76 84.19 2 -4 0 1350.96 84.19 2 -4 0 1420.26 84.19 2 -4 0 1325.27 83.69 -2 4 0 1146.09 84.99 -2 4 0 1281.07 85.99 -2 4 0 1313.87 85.39 -2 4 0 1329.17 86.19 -2 4 0 1279.37 84.49 -2 4 0 1301.27 85.29 -2 4 0 1162.88 86.29 -2 4 0 1213.58 84.89 1 -4 0 52.59 4.30 1 -4 0 60.79 4.40 1 -4 0 61.49 5.30 1 -4 0 60.19 4.50 1 -4 0 58.49 4.10 1 -4 0 55.29 4.40 1 -4 0 54.99 4.50 -1 4 0 59.09 4.40 -1 4 0 50.79 4.20 -1 4 0 60.59 4.50 -1 4 0 58.69 4.40 -1 4 0 53.79 4.50 0 -4 0 8.70 1.80 0 -4 0 6.80 1.30 0 -4 0 6.30 1.60 0 -4 0 8.20 1.90 0 -4 0 13.50 1.90 0 -4 0 11.80 1.70 0 -4 0 9.10 1.50 0 4 0 11.80 1.80 0 4 0 12.20 1.70 0 4 0 9.60 1.40 0 4 0 10.60 1.70 -1 -4 0 36.20 3.90 -1 -4 0 42.60 3.60 -1 -4 0 35.40 3.40 -1 -4 0 40.70 5.10 -1 -4 0 49.40 3.70 -1 -4 0 42.90 3.60 -1 -4 0 41.50 3.90 -1 -4 0 34.70 4.70 -1 -4 0 40.40 5.20 1 4 0 35.40 5.40 1 4 0 41.60 3.40 1 4 0 42.40 3.90 1 4 0 39.50 3.90 1 4 0 46.30 3.80 1 4 0 49.90 5.80 1 4 0 36.20 4.60 1 4 0 39.90 4.30 1 4 0 43.10 3.80 -2 -4 0 20.70 3.20 -2 -4 0 12.60 4.60 -2 -4 0 10.90 6.40 -2 -4 0 15.00 2.70 -2 -4 0 17.60 3.80 -2 -4 0 27.90 4.60 2 4 0 25.40 4.10 2 4 0 21.40 3.90 2 4 0 17.10 2.70 2 4 0 19.70 4.40 2 4 0 19.50 2.70 2 4 0 22.40 2.90 2 4 0 21.40 3.30 2 4 0 23.70 2.40 2 4 0 21.40 3.10 -3 -4 0 8.80 6.50 -3 -4 0 4.80 4.10 -3 -4 0 4.90 4.10 -3 -4 0 4.50 2.60 -3 -4 0 4.60 3.50 3 4 0 5.90 3.50 3 4 0 5.40 3.20 3 4 0 5.50 3.30 3 4 0 3.80 1.70 4 -5 0 196.18 14.10 -4 5 0 189.78 17.90 -4 5 0 216.08 18.60 -4 5 0 256.67 18.50 -4 5 0 228.38 15.70 3 -5 0 28.20 3.40 3 -5 0 26.30 4.50 3 -5 0 29.80 2.70 3 -5 0 41.20 5.20 -3 5 0 18.60 5.60 -3 5 0 27.80 7.80 -3 5 0 29.60 5.20 -3 5 0 34.20 7.30 -3 5 0 18.40 3.70 -3 5 0 40.20 8.20 -3 5 0 32.30 6.40 2 -5 0 11.90 1.80 2 -5 0 16.00 1.80 2 -5 0 10.00 3.10 2 -5 0 15.70 2.40 2 -5 0 15.30 2.50 -2 5 0 14.30 4.60 -2 5 0 9.70 3.60 -2 5 0 13.50 5.30 -2 5 0 19.90 5.80 -2 5 0 13.90 4.00 -2 5 0 9.30 4.50 -2 5 0 7.20 3.40 -2 5 0 12.30 2.40 -2 5 0 10.40 2.70 1 -5 0 33.60 4.30 1 -5 0 19.90 3.50 1 -5 0 23.80 3.70 1 -5 0 28.30 2.80 1 -5 0 30.00 3.20 1 -5 0 33.70 2.90 1 -5 0 26.00 3.10 1 -5 0 28.20 2.90 1 -5 0 32.20 4.50 1 -5 0 28.70 3.10 -1 5 0 32.90 3.50 -1 5 0 31.70 6.10 -1 5 0 34.30 5.00 -1 5 0 31.50 4.60 -1 5 0 28.50 4.20 -1 5 0 29.60 3.30 -1 5 0 35.20 4.90 -1 5 0 36.00 4.30 0 -5 0 32.60 3.30 0 -5 0 27.20 4.00 0 -5 0 27.60 3.60 0 -5 0 33.40 3.50 0 -5 0 40.20 5.40 0 -5 0 37.20 4.20 0 -5 0 30.00 3.20 0 -5 0 23.20 3.60 0 5 0 29.80 3.20 0 5 0 32.30 4.40 0 5 0 29.60 3.40 0 5 0 28.10 4.80 0 5 0 30.30 3.50 0 5 0 41.40 5.60 0 5 0 32.50 4.30 0 5 0 30.90 3.40 -1 -5 0 47.90 4.70 -1 -5 0 51.19 6.20 -1 -5 0 37.30 4.10 -1 -5 0 48.30 5.60 -1 -5 0 55.79 4.80 -1 -5 0 44.60 6.70 -1 -5 0 41.70 4.20 1 5 0 51.19 4.50 1 5 0 49.40 4.70 1 5 0 51.39 4.60 1 5 0 43.60 5.90 1 5 0 40.00 4.20 1 5 0 44.00 5.30 1 5 0 48.50 5.70 -2 -5 0 0.60 2.80 -2 -5 0 2.60 3.30 -2 -5 0 2.30 5.70 -2 -5 0 1.00 2.20 -2 -5 0 1.80 2.70 2 5 0 4.30 2.30 2 5 0 -0.70 1.80 2 5 0 2.30 3.80 2 5 0 1.20 3.00 2 5 0 1.30 2.70 -3 -5 0 11.90 2.90 -3 -5 0 14.20 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245.88 16.10 1 -4 6 247.78 16.10 -2 4 -6 19.30 3.20 -2 4 -6 15.40 3.60 -2 4 -6 19.60 4.10 -2 4 -6 13.30 2.70 -2 4 -6 19.70 2.60 -2 4 -6 15.20 2.60 -2 4 -6 23.10 5.40 -2 4 -6 17.20 4.50 -2 4 -6 20.00 4.70 -2 4 -6 23.50 4.10 -2 4 -6 27.10 3.90 2 -4 6 23.30 2.50 2 -4 6 19.10 2.00 2 -4 6 18.40 2.40 2 -4 6 24.80 3.60 2 -4 6 21.50 2.40 2 -4 6 36.60 4.30 2 -4 6 24.40 3.10 2 -4 6 23.70 3.40 -3 4 -6 69.89 9.20 -3 4 -6 98.09 8.40 -3 4 -6 88.69 10.20 -3 4 -6 66.09 9.20 -3 4 -6 103.79 11.20 -3 4 -6 63.69 10.30 3 -4 6 91.89 8.00 3 -4 6 95.49 6.00 3 -4 6 91.09 8.20 -4 4 -6 31.00 7.00 -4 4 -6 21.90 6.90 -4 4 -6 33.40 8.60 -4 4 -6 43.70 5.80 -4 4 -6 14.00 5.50 4 -4 6 25.60 2.40 -5 4 -6 6.80 4.30 -5 4 -6 3.50 4.80 -5 4 -6 5.90 3.10 4 3 -6 52.39 4.20 4 3 -6 44.20 5.30 -4 -3 6 70.49 10.10 -4 -3 6 49.50 7.10 3 3 -6 109.09 8.30 3 3 -6 92.99 8.20 3 3 -6 111.79 7.70 3 3 -6 94.69 9.60 3 3 -6 125.99 8.70 3 3 -6 114.69 9.20 3 3 -6 94.09 7.80 -3 -3 6 76.29 14.00 -3 -3 6 109.39 9.00 -3 -3 6 98.99 9.50 -3 -3 6 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23.50 4.40 0 -1 28 25.00 4.10 0 -1 28 44.20 5.00 0 -1 28 38.90 4.00 0 -1 28 33.20 4.20 0 -1 28 32.00 3.40 0 -1 28 32.10 4.50 -1 1 -28 3.90 2.40 -1 1 -28 7.30 2.60 -1 1 -28 6.30 3.90 -1 1 -28 5.10 4.30 1 -1 28 7.00 3.10 1 -1 28 4.70 2.50 1 -1 28 4.70 2.30 1 -1 28 4.30 2.90 -2 1 -28 3.10 3.10 -2 1 -28 2.10 2.00 -2 1 -28 5.80 1.70 -2 1 -28 5.00 3.90 2 -1 28 1.20 2.40 2 -1 28 4.60 1.90 2 -1 28 1.90 1.70 2 -1 28 2.70 2.90 3 0 -28 2.30 0.80 3 0 -28 3.40 2.50 3 0 -28 0.00 2.50 3 0 -28 -1.80 2.70 -3 0 28 1.70 2.30 -3 0 28 1.90 1.70 2 0 -28 10.90 3.50 2 0 -28 12.50 2.70 2 0 -28 11.20 4.00 -2 0 28 11.80 2.80 -2 0 28 12.20 2.10 -2 0 28 9.90 2.80 -2 0 28 14.20 2.50 -2 0 28 7.40 4.20 1 0 -28 39.80 6.10 1 0 -28 37.80 5.20 1 0 -28 46.70 5.20 1 0 -28 34.30 4.30 -1 0 28 40.60 4.20 -1 0 28 43.20 5.90 -1 0 28 60.69 6.00 -1 0 28 49.90 6.20 -1 0 28 40.70 4.00 -1 0 28 39.00 4.70 0 0 -28 34.70 3.90 0 0 -28 22.80 4.50 0 0 -28 27.70 3.60 0 0 -28 33.60 5.60 0 0 -28 22.80 4.70 0 0 28 29.80 3.90 0 0 28 36.40 3.60 0 0 28 34.80 4.50 0 0 28 30.80 3.40 0 0 28 24.20 4.60 -1 0 -28 31.80 3.70 -1 0 -28 23.40 4.70 -1 0 -28 29.20 3.10 1 0 28 36.90 3.50 1 0 28 21.10 3.90 1 0 28 36.40 5.00 1 0 28 28.30 3.10 1 0 28 34.40 3.90 1 0 28 30.70 4.60 -2 0 -28 -1.20 3.10 -2 0 -28 -2.00 1.60 -2 0 -28 -0.40 3.60 -2 0 -28 2.10 2.40 -2 0 -28 0.30 1.70 2 0 28 0.00 2.20 2 0 28 -0.50 2.40 2 0 28 1.30 1.50 2 0 28 0.60 2.00 3 -1 -28 1.40 2.20 3 -1 -28 4.70 2.90 3 -1 -28 3.10 0.90 -3 1 28 6.00 3.20 -3 1 28 3.10 1.50 -3 1 28 5.00 2.70 2 -1 -28 2.60 3.30 2 -1 -28 -1.60 2.40 2 -1 -28 0.70 3.50 2 -1 -28 -0.10 2.30 -2 1 28 -0.90 1.70 -2 1 28 -0.90 3.60 -2 1 28 0.30 3.60 -2 1 28 1.80 2.30 -2 1 28 0.90 2.10 1 -1 -28 0.70 2.30 1 -1 -28 -2.40 2.50 1 -1 -28 1.40 3.40 1 -1 -28 -4.50 3.60 -1 1 28 -0.30 3.00 -1 1 28 -0.10 1.90 -1 1 28 -1.00 3.50 -1 1 28 0.40 2.40 0 -1 -28 5.50 2.80 0 -1 -28 2.10 3.40 0 -1 -28 1.00 3.10 0 -1 -28 6.30 2.50 0 1 28 4.90 3.40 0 1 28 7.40 2.50 0 1 28 5.10 1.90 0 1 28 5.60 2.20 -1 -1 -28 8.30 2.40 -1 -1 -28 9.80 2.10 -1 -1 -28 6.20 3.60 1 1 28 9.80 3.30 1 1 28 8.60 2.60 1 1 28 6.50 2.70 1 1 28 7.10 2.00 1 1 28 7.50 2.00 -2 -1 -28 167.78 12.40 -2 -1 -28 200.88 12.20 -2 -1 -28 200.08 14.50 -2 -1 -28 172.78 13.10 2 1 28 185.78 12.50 2 1 28 162.68 12.80 3 -2 -28 33.50 3.00 -3 2 28 44.50 3.40 2 -2 -28 21.10 3.10 2 -2 -28 11.70 2.60 2 -2 -28 17.80 4.20 2 -2 -28 17.20 3.70 -2 2 28 12.70 2.90 -2 2 28 10.30 2.30 -2 2 28 17.70 4.10 -2 2 28 14.90 4.50 1 -2 -28 15.90 5.10 1 -2 -28 9.60 2.70 1 -2 -28 10.00 2.70 1 -2 -28 8.00 4.00 -1 2 28 6.40 2.30 -1 2 28 10.40 3.40 -1 2 28 12.80 2.40 -1 2 28 17.50 4.90 -1 2 28 11.70 3.00 0 -2 -28 6.50 3.30 0 -2 -28 4.60 3.50 0 -2 -28 14.30 3.00 0 -2 -28 14.60 2.60 0 -2 -28 10.20 2.00 0 2 28 11.50 3.50 0 2 28 11.70 2.60 0 2 28 9.50 2.20 -1 -2 -28 25.30 4.10 -1 -2 -28 20.70 2.70 -1 -2 -28 32.10 2.90 1 2 28 32.30 3.50 1 2 28 28.80 3.10 1 2 28 31.30 4.20 2 -3 -28 18.10 3.30 2 -3 -28 19.30 2.70 2 -3 -28 18.40 2.60 2 -3 -28 16.10 3.50 -2 3 28 14.00 2.80 -2 3 28 21.60 2.40 -2 3 28 29.10 4.90 1 -3 -28 30.60 3.20 1 -3 -28 23.00 3.00 1 -3 -28 19.40 4.00 -1 3 28 20.40 3.20 -1 3 28 23.10 3.60 -1 3 28 34.00 5.50 -1 3 28 25.80 2.80 0 -3 -28 -1.70 2.30 0 -3 -28 1.10 1.70 0 -3 -28 1.30 2.10 0 3 28 1.10 2.50 0 3 28 0.70 1.40 0 4 -29 2.30 2.60 0 4 -29 5.10 2.40 0 4 -29 3.00 2.60 0 -4 29 3.50 2.80 0 -4 29 4.80 2.40 -1 4 -29 2.00 3.40 -1 4 -29 0.10 2.40 1 -4 29 2.30 2.60 1 3 -29 10.60 2.90 1 3 -29 12.40 2.10 -1 -3 29 13.60 3.20 -1 -3 29 16.30 2.20 -1 -3 29 12.90 2.30 -1 -3 29 15.40 3.10 0 3 -29 3.00 2.20 0 3 -29 2.00 3.10 0 3 -29 3.80 3.10 0 -3 29 2.50 3.10 0 -3 29 2.60 1.80 0 -3 29 2.60 2.90 -1 3 -29 4.10 2.20 -1 3 -29 3.50 2.20 -1 3 -29 5.10 2.70 -1 3 -29 4.10 2.60 1 -3 29 6.60 3.10 1 -3 29 2.30 1.60 1 -3 29 3.70 2.10 2 -3 29 3.50 2.70 2 -3 29 4.90 3.80 2 2 -29 14.30 2.90 2 2 -29 12.30 3.30 2 2 -29 9.20 2.60 -2 -2 29 13.90 2.30 -2 -2 29 12.40 3.10 -2 -2 29 12.50 3.00 -2 -2 29 10.50 1.90 -2 -2 29 11.80 2.40 -2 -2 29 12.40 3.00 1 2 -29 0.90 3.00 1 2 -29 0.10 2.50 1 2 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2.10 -1 -1 -30 8.90 2.00 -1 -1 -30 4.50 1.60 -1 -1 -30 8.70 3.30 1 1 30 6.30 2.60 1 1 30 6.60 1.90 1 1 30 9.50 2.10 1 1 30 7.60 1.70 2 -2 -30 47.70 4.20 2 -2 -30 39.50 4.80 2 -2 -30 40.40 4.00 2 -2 -30 38.60 4.90 -2 2 30 31.10 3.60 -2 2 30 40.90 5.50 1 -2 -30 30.30 3.20 1 -2 -30 27.70 3.20 1 -2 -30 24.90 4.40 -1 2 30 32.30 5.10 -1 2 30 23.40 3.60 -1 2 30 27.30 4.20 -1 2 30 19.20 2.70 0 -2 -30 7.90 2.50 0 -2 -30 10.20 2.10 0 2 30 15.40 3.70 0 2 30 12.60 2.00 0 2 30 10.40 2.20 0 2 30 9.60 2.90 1 -3 -30 2.30 2.80 0 3 -31 14.10 3.70 0 3 -31 20.20 2.80 0 3 -31 24.50 4.00 0 -3 31 25.30 3.50 0 -3 31 22.30 2.50 0 -3 31 20.10 3.60 -1 3 -31 0.30 2.10 1 2 -31 23.30 3.70 1 2 -31 21.70 2.60 -1 -2 31 12.60 2.10 -1 -2 31 15.30 3.40 -1 -2 31 17.90 3.10 -1 -2 31 18.50 2.50 -1 -2 31 12.40 2.90 0 2 -31 3.90 2.90 0 2 -31 5.00 3.20 0 2 -31 2.00 1.80 0 2 -31 2.80 2.10 0 -2 31 1.80 2.60 0 -2 31 4.20 1.70 0 -2 31 1.90 2.90 0 -2 31 3.20 1.90 -1 2 -31 10.20 2.30 -1 2 -31 15.30 2.50 1 -2 31 14.30 3.20 1 -2 31 6.30 2.10 1 -2 31 11.00 2.90 1 -2 31 12.10 1.80 2 1 -31 -0.80 2.00 2 1 -31 -1.10 2.20 -2 -1 31 0.60 1.60 -2 -1 31 1.10 2.50 1 1 -31 24.90 3.70 1 1 -31 26.00 3.00 1 1 -31 13.20 3.10 1 1 -31 24.10 3.90 -1 -1 31 20.90 4.40 -1 -1 31 13.90 2.30 -1 -1 31 17.30 3.50 -1 -1 31 17.50 2.80 -1 -1 31 20.70 2.90 0 1 -31 66.59 5.70 0 1 -31 53.29 6.60 0 1 -31 70.79 5.80 0 1 -31 65.09 6.30 0 -1 31 65.39 6.30 0 -1 31 69.69 5.70 0 -1 31 55.49 6.40 0 -1 31 72.99 5.30 -1 1 -31 2.70 1.90 -1 1 -31 0.90 2.20 -1 1 -31 1.90 3.10 1 -1 31 2.90 1.80 1 -1 31 2.40 1.60 1 -1 31 -1.10 2.40 1 -1 31 0.20 1.70 2 0 -31 4.00 2.40 2 0 -31 5.50 2.60 2 0 -31 6.30 1.90 -2 0 31 5.70 3.00 -2 0 31 6.40 1.60 -2 0 31 8.60 2.00 -2 0 31 6.00 2.60 1 0 -31 20.70 2.80 1 0 -31 21.30 3.90 1 0 -31 25.80 3.80 1 0 -31 31.40 3.30 -1 0 31 21.80 3.80 -1 0 31 19.90 2.50 -1 0 31 19.50 3.00 -1 0 31 22.60 2.70 0 0 -31 11.70 2.40 0 0 -31 4.10 3.10 0 0 -31 16.10 2.60 0 0 31 17.40 3.70 0 0 31 20.40 3.00 0 0 31 12.80 2.10 0 0 31 14.50 2.20 -1 0 -31 3.00 1.70 -1 0 -31 4.70 3.10 -1 0 -31 4.80 2.90 1 0 31 0.40 2.10 1 0 31 1.60 1.70 1 0 31 1.70 3.80 1 0 31 1.70 1.50 2 -1 -31 6.70 2.50 2 -1 -31 5.10 2.10 2 -1 -31 7.00 2.80 -2 1 31 7.90 1.60 -2 1 31 4.80 2.90 1 -1 -31 3.20 2.90 1 -1 -31 11.00 2.40 1 -1 -31 6.70 2.70 1 -1 -31 3.90 2.20 -1 1 31 4.20 2.70 -1 1 31 7.50 2.20 -1 1 31 6.60 3.00 -1 1 31 4.70 5.00 -1 1 31 5.70 1.80 0 -1 -31 -1.80 2.70 0 -1 -31 -1.90 2.20 0 -1 -31 1.30 1.90 0 -1 -31 0.50 1.90 0 1 31 -2.60 2.50 0 1 31 -1.20 1.40 0 1 31 -1.30 1.80 -1 -1 -31 1.10 3.10 1 1 31 -1.40 1.80 2 -2 -31 4.80 3.30 1 -2 -31 0.70 2.50 1 -2 -31 3.00 1.90 1 -2 -31 1.10 2.00 -1 2 31 1.20 2.90 -1 2 31 3.30 2.30 -1 2 31 2.10 1.40 0 2 31 8.20 1.60 0 2 31 10.40 2.60 1 2 -32 56.29 6.50 -1 -2 32 52.59 4.90 0 2 -32 -0.50 2.40 0 2 -32 2.90 1.90 0 -2 32 1.50 2.70 0 -2 32 -0.50 2.20 0 -2 32 0.20 2.10 0 -2 32 0.40 1.50 1 1 -32 27.70 3.70 1 1 -32 22.50 2.80 -1 -1 32 22.70 3.50 -1 -1 32 26.30 4.30 -1 -1 32 20.10 2.80 -1 -1 32 19.00 2.40 0 1 -32 121.19 8.10 0 1 -32 117.49 8.10 0 -1 32 109.39 7.80 0 -1 32 85.99 8.50 0 -1 32 112.19 8.10 -1 1 -32 1.90 2.60 -1 1 -32 0.70 3.30 1 -1 32 1.20 1.60 2 0 -32 119.29 9.60 1 0 -32 5.10 2.10 1 0 -32 4.30 2.10 1 0 -32 5.90 2.60 1 0 -32 3.90 2.60 -1 0 32 2.10 2.50 -1 0 32 4.60 2.10 -1 0 32 6.60 1.60 -1 0 32 6.10 1.90 -1 0 32 6.50 3.10 0 0 -32 4.90 3.00 0 0 -32 11.80 2.30 0 0 -32 9.90 2.20 0 0 32 7.70 2.80 0 0 32 3.20 2.00 0 0 32 7.90 1.60 0 0 32 9.50 1.70 1 -1 -32 65.39 4.80 1 -1 -32 58.69 4.90 -1 1 32 51.49 5.00 -1 1 32 49.50 5.40 -1 1 32 43.20 4.60 -1 1 32 48.40 4.20 0 -1 -32 1.00 1.70 0 1 32 3.10 1.40 0 1 32 3.60 1.90 0 1 32 1.40 2.70 -1 -1 33 -1.70 2.70 0 -1 33 124.39 9.80 1 0 -33 62.49 7.60 -1 0 33 82.19 6.60 0 0 -33 9.00 2.60 0 0 33 10.10 3.10 0 0 33 12.80 2.80 ; _shelx_hkl_checksum 22917 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.9639(3) 0.12340(18) 0.57406(4) 0.0304(3) Uani 1 1 d . . . . . O2 O 0.5711(3) 0.60182(18) 0.65035(4) 0.0306(3) Uani 1 1 d . . . . . N1 N 0.7705(3) 0.3647(2) 0.61243(5) 0.0217(3) Uani 1 1 d . . . . . C1 C 0.4989(4) 0.4243(2) 0.43482(6) 0.0195(4) Uani 1 1 d . . . . . C2 C 0.6522(4) 0.2705(2) 0.43718(6) 0.0227(4) Uani 1 1 d . . . . . H2A H 0.6870 0.2013 0.4083 0.027 Uiso 1 1 calc R U . . . C3 C 0.7571(4) 0.2156(2) 0.48194(6) 0.0220(4) Uani 1 1 d . . . . . H3A H 0.8624 0.1095 0.4832 0.026 Uiso 1 1 calc R U . . . C4 C 0.7091(4) 0.3140(2) 0.52405(6) 0.0195(4) Uani 1 1 d . . . . . C5 C 0.5524(3) 0.4719(2) 0.52249(5) 0.0182(3) Uani 1 1 d . . . . . C6 C 0.8246(4) 0.2571(2) 0.57121(6) 0.0218(4) Uani 1 1 d . . . . . C7 C 0.6122(4) 0.5191(2) 0.61256(6) 0.0221(4) Uani 1 1 d . . . . . C8 C 0.8859(4) 0.3098(3) 0.65966(6) 0.0251(4) Uani 1 1 d . . . . . H8A H 0.9656 0.4398 0.6810 0.030 Uiso 1 1 calc R U . . . H8B H 1.0535 0.2451 0.6550 0.030 Uiso 1 1 calc R U . . . C9 C 0.6482(4) 0.1593(3) 0.68429(6) 0.0249(4) Uani 1 1 d . . . . . H9A H 0.5162 0.0567 0.6598 0.030 Uiso 1 1 calc R U . . . H9B H 0.5235 0.2389 0.7003 0.030 Uiso 1 1 calc R U . . . C10 C 0.7891(4) 0.0428(3) 0.72147(6) 0.0242(4) Uani 1 1 d . . . . . H10A H 0.9138 -0.0361 0.7052 0.029 Uiso 1 1 calc R U . . . H10B H 0.9224 0.1463 0.7457 0.029 Uiso 1 1 calc R U . . . C11 C 0.5586(4) -0.1090(3) 0.74713(6) 0.0238(4) Uani 1 1 d . . . . . H11A H 0.4607 -0.0278 0.7685 0.029 Uiso 1 1 calc R U . . . H11B H 0.4024 -0.1947 0.7229 0.029 Uiso 1 1 calc R U . . . C12 C 0.6951(4) -0.2537(3) 0.77693(6) 0.0254(4) Uani 1 1 d . . . . . H12A H 0.8480 -0.1676 0.8016 0.031 Uiso 1 1 calc R U . . . H12B H 0.7980 -0.3314 0.7557 0.031 Uiso 1 1 calc R U . . . C13 C 0.4681(4) -0.4108(3) 0.80195(6) 0.0266(4) Uani 1 1 d . . . . . H13A H 0.3128 -0.4953 0.7774 0.032 Uiso 1 1 calc R U . . . H13B H 0.3684 -0.3333 0.8238 0.032 Uiso 1 1 calc R U . . . C14 C 0.6075(4) -0.5579(3) 0.83086(6) 0.0264(4) Uani 1 1 d . . . . . H14A H 0.7012 -0.6386 0.8087 0.032 Uiso 1 1 calc R U . . . H14B H 0.7681 -0.4728 0.8545 0.032 Uiso 1 1 calc R U . . . C15 C 0.3857(4) -0.7109(3) 0.85752(6) 0.0273(4) Uani 1 1 d . . . . . H15A H 0.2242 -0.7953 0.8339 0.033 Uiso 1 1 calc R U . . . H15B H 0.2934 -0.6304 0.8799 0.033 Uiso 1 1 calc R U . . . C16 C 0.5262(4) -0.8585(3) 0.88592(6) 0.0273(4) Uani 1 1 d . . . . . H16A H 0.6163 -0.9402 0.8634 0.033 Uiso 1 1 calc R U . . . H16B H 0.6895 -0.7740 0.9093 0.033 Uiso 1 1 calc R U . . . C17 C 0.3052(4) -1.0100(3) 0.91313(6) 0.0285(4) Uani 1 1 d . . . . . H17A H 0.1356 -1.0884 0.8901 0.034 Uiso 1 1 calc R U . . . H17B H 0.2245 -0.9284 0.9370 0.034 Uiso 1 1 calc R U . . . C18 C 0.4421(4) -1.1659(3) 0.93906(7) 0.0324(4) Uani 1 1 d . . . . . H18A H 0.6086 -1.0880 0.9627 0.039 Uiso 1 1 calc R U . . . H18B H 0.5265 -1.2458 0.9153 0.039 Uiso 1 1 calc R U . . . C19 C 0.2165(5) -1.3194(3) 0.96523(7) 0.0399(5) Uani 1 1 d . . . . . H19A H 0.3152 -1.4171 0.9808 0.060 Uiso 1 1 calc R U . . . H19B H 0.0515 -1.3979 0.9420 0.060 Uiso 1 1 calc R U . . . H19C H 0.1377 -1.2417 0.9897 0.060 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 O1 0.0394(8) 0.0262(7) 0.0317(7) 0.0081(5) 0.0032(5) 0.0184(6) O2 0.0443(8) 0.0284(7) 0.0217(6) 0.0014(5) 0.0040(5) 0.0142(6) N1 0.0240(8) 0.0207(7) 0.0212(7) 0.0061(5) 0.0019(5) 0.0062(6) C1 0.0196(9) 0.0138(8) 0.0237(8) 0.0035(6) 0.0035(6) 0.0007(6) C2 0.0275(10) 0.0174(8) 0.0234(8) 0.0010(6) 0.0055(7) 0.0053(7) C3 0.0229(9) 0.0141(8) 0.0303(9) 0.0037(6) 0.0042(7) 0.0064(7) C4 0.0179(9) 0.0152(8) 0.0248(8) 0.0048(6) 0.0035(6) 0.0022(6) C5 0.0161(8) 0.0139(7) 0.0236(8) 0.0038(6) 0.0039(6) 0.0010(6) C6 0.0222(9) 0.0154(8) 0.0280(9) 0.0057(6) 0.0041(7) 0.0041(7) C7 0.0241(9) 0.0176(8) 0.0238(8) 0.0036(6) 0.0035(7) 0.0030(7) C8 0.0263(10) 0.0275(9) 0.0220(8) 0.0082(7) -0.0011(7) 0.0076(7) C9 0.0254(9) 0.0251(9) 0.0249(8) 0.0071(7) 0.0014(7) 0.0071(7) C10 0.0259(9) 0.0227(8) 0.0243(8) 0.0059(7) 0.0011(7) 0.0063(7) C11 0.0276(10) 0.0210(8) 0.0239(8) 0.0046(7) 0.0033(7) 0.0075(7) C12 0.0275(10) 0.0222(9) 0.0268(9) 0.0066(7) 0.0030(7) 0.0057(7) C13 0.0293(10) 0.0226(9) 0.0282(9) 0.0071(7) 0.0036(7) 0.0062(7) C14 0.0293(10) 0.0213(8) 0.0288(9) 0.0071(7) 0.0042(7) 0.0051(7) C15 0.0308(10) 0.0213(9) 0.0305(9) 0.0074(7) 0.0052(7) 0.0061(7) C16 0.0301(10) 0.0217(9) 0.0297(9) 0.0070(7) 0.0042(7) 0.0046(7) C17 0.0320(10) 0.0231(9) 0.0297(9) 0.0080(7) 0.0045(7) 0.0041(8) C18 0.0391(12) 0.0252(9) 0.0323(10) 0.0096(7) 0.0035(8) 0.0053(8) C19 0.0482(13) 0.0297(10) 0.0399(11) 0.0157(8) 0.0044(9) 0.0037(9) 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 C6 N1 C7 124.88(13) . . C6 N1 C8 117.67(14) . . C7 N1 C8 117.44(14) . . C2 C1 C5 120.09(15) . 2_666 C2 C1 C7 120.08(15) . 2_666 C5 C1 C7 119.84(15) 2_666 2_666 C1 C2 C3 120.34(15) . . C1 C2 H2A 119.8 . . C3 C2 H2A 119.8 . . C4 C3 C2 120.68(15) . . C4 C3 H3A 119.7 . . C2 C3 H3A 119.7 . . C3 C4 C5 119.94(15) . . C3 C4 C6 120.30(15) . . C5 C4 C6 119.76(14) . . C1 C5 C5 119.40(19) 2_666 2_666 C1 C5 C4 121.04(15) 2_666 . C5 C5 C4 119.55(18) 2_666 . O1 C6 N1 121.03(15) . . O1 C6 C4 121.74(15) . . N1 C6 C4 117.23(14) . . O2 C7 N1 120.30(15) . . O2 C7 C1 122.46(16) . 2_666 N1 C7 C1 117.23(14) . 2_666 N1 C8 C9 112.98(14) . . N1 C8 H8A 109.0 . . C9 C8 H8A 109.0 . . N1 C8 H8B 109.0 . . C9 C8 H8B 109.0 . . H8A C8 H8B 107.8 . . C8 C9 C10 111.40(14) . . C8 C9 H9A 109.3 . . C10 C9 H9A 109.3 . . C8 C9 H9B 109.3 . . C10 C9 H9B 109.3 . . H9A C9 H9B 108.0 . . C11 C10 C9 113.08(14) . . C11 C10 H10A 109.0 . . C9 C10 H10A 109.0 . . C11 C10 H10B 109.0 . . C9 C10 H10B 109.0 . . H10A C10 H10B 107.8 . . C12 C11 C10 112.78(14) . . C12 C11 H11A 109.0 . . C10 C11 H11A 109.0 . . C12 C11 H11B 109.0 . . C10 C11 H11B 109.0 . . H11A C11 H11B 107.8 . . C11 C12 C13 113.83(15) . . C11 C12 H12A 108.8 . . C13 C12 H12A 108.8 . . C11 C12 H12B 108.8 . . C13 C12 H12B 108.8 . . H12A C12 H12B 107.7 . . C12 C13 C14 113.20(15) . . C12 C13 H13A 108.9 . . C14 C13 H13A 108.9 . . C12 C13 H13B 108.9 . . C14 C13 H13B 108.9 . . H13A C13 H13B 107.8 . . C15 C14 C13 113.92(15) . . C15 C14 H14A 108.8 . . C13 C14 H14A 108.8 . . C15 C14 H14B 108.8 . . C13 C14 H14B 108.8 . . H14A C14 H14B 107.7 . . C14 C15 C16 113.58(15) . . C14 C15 H15A 108.9 . . C16 C15 H15A 108.9 . . C14 C15 H15B 108.9 . . C16 C15 H15B 108.9 . . H15A C15 H15B 107.7 . . C17 C16 C15 113.64(15) . . C17 C16 H16A 108.8 . . C15 C16 H16A 108.8 . . C17 C16 H16B 108.8 . . C15 C16 H16B 108.8 . . H16A C16 H16B 107.7 . . C16 C17 C18 113.53(15) . . C16 C17 H17A 108.9 . . C18 C17 H17A 108.9 . . C16 C17 H17B 108.9 . . C18 C17 H17B 108.9 . . H17A C17 H17B 107.7 . . C17 C18 C19 112.88(17) . . C17 C18 H18A 109.0 . . C19 C18 H18A 109.0 . . C17 C18 H18B 109.0 . . C19 C18 H18B 109.0 . . H18A C18 H18B 107.8 . . C18 C19 H19A 109.5 . . C18 C19 H19B 109.5 . . H19A C19 H19B 109.5 . . C18 C19 H19C 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O1 C6 1.220(2) . O2 C7 1.214(2) . N1 C6 1.394(2) . N1 C7 1.398(2) . N1 C8 1.480(2) . C1 C2 1.380(2) . C1 C5 1.411(2) 2_666 C1 C7 1.482(2) 2_666 C2 C3 1.403(2) . C2 H2A 0.9500 . C3 C4 1.375(2) . C3 H3A 0.9500 . C4 C5 1.413(2) . C4 C6 1.484(2) . C5 C1 1.411(2) 2_666 C5 C5 1.411(3) 2_666 C7 C1 1.482(2) 2_666 C8 C9 1.523(2) . C8 H8A 0.9900 . C8 H8B 0.9900 . C9 C10 1.524(2) . C9 H9A 0.9900 . C9 H9B 0.9900 . C10 C11 1.524(2) . C10 H10A 0.9900 . C10 H10B 0.9900 . C11 C12 1.520(2) . C11 H11A 0.9900 . C11 H11B 0.9900 . C12 C13 1.523(2) . C12 H12A 0.9900 . C12 H12B 0.9900 . C13 C14 1.526(2) . C13 H13A 0.9900 . C13 H13B 0.9900 . C14 C15 1.521(2) . C14 H14A 0.9900 . C14 H14B 0.9900 . C15 C16 1.523(2) . C15 H15A 0.9900 . C15 H15B 0.9900 . C16 C17 1.523(2) . C16 H16A 0.9900 . C16 H16B 0.9900 . C17 C18 1.523(2) . C17 H17A 0.9900 . C17 H17B 0.9900 . C18 C19 1.525(3) . C18 H18A 0.9900 . C18 H18B 0.9900 . C19 H19A 0.9800 . C19 H19B 0.9800 . C19 H19C 0.9800 . 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 C5 C1 C2 C3 0.3(2) 2_666 . . . C7 C1 C2 C3 -179.79(15) 2_666 . . . C1 C2 C3 C4 0.0(2) . . . . C2 C3 C4 C5 0.1(2) . . . . C2 C3 C4 C6 -179.13(15) . . . . C3 C4 C5 C1 -179.76(15) . . . 2_666 C6 C4 C5 C1 -0.6(2) . . . 2_666 C3 C4 C5 C5 -0.3(3) . . . 2_666 C6 C4 C5 C5 178.86(17) . . . 2_666 C7 N1 C6 O1 -179.67(15) . . . . C8 N1 C6 O1 -0.5(2) . . . . C7 N1 C6 C4 1.0(2) . . . . C8 N1 C6 C4 -179.75(13) . . . . C3 C4 C6 O1 0.0(2) . . . . C5 C4 C6 O1 -179.14(15) . . . . C3 C4 C6 N1 179.32(14) . . . . C5 C4 C6 N1 0.1(2) . . . . C6 N1 C7 O2 178.60(15) . . . . C8 N1 C7 O2 -0.6(2) . . . . C6 N1 C7 C1 -1.7(2) . . . 2_666 C8 N1 C7 C1 179.10(14) . . . 2_666 C6 N1 C8 C9 -98.63(18) . . . . C7 N1 C8 C9 80.64(18) . . . . N1 C8 C9 C10 158.37(14) . . . . C8 C9 C10 C11 179.77(14) . . . . C9 C10 C11 C12 169.09(14) . . . . C10 C11 C12 C13 -178.54(14) . . . . C11 C12 C13 C14 178.80(14) . . . . C12 C13 C14 C15 177.98(14) . . . . C13 C14 C15 C16 179.48(15) . . . . C14 C15 C16 C17 179.30(14) . . . . C15 C16 C17 C18 176.55(15) . . . . C16 C17 C18 C19 -178.78(15) . . . .