#------------------------------------------------------------------------------ #$Date: 2024-12-07 19:04:45 +0200 (Sat, 07 Dec 2024) $ #$Revision: 296757 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312709.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2312709 loop_ _publ_author_name 'Kanthapazham, Rajakumar' 'Osipov, Artyom A.' 'Zherebtsov, Dmitry A.' 'Efremov, Andrey N.' 'Nayfert, Sergey A.' 'Adonin, Sergey A.' 'Spiridonova, Dar'ya V.' 'Atapin, Sergey V.' _publ_section_title ; Structures of hexamethyl-[1,1'-biphenyl]-4,4'-diammonium salts. ; _journal_coeditor_code AW5097 _journal_issue 6 _journal_name_full 'Acta crystallographica Section B, Structural science, crystal engineering and materials' _journal_page_first 751 _journal_page_last 759 _journal_paper_doi 10.1107/S2052520624009818 _journal_volume 80 _journal_year 2024 _chemical_formula_moiety 'I, C17 H23 N2' _chemical_formula_sum 'C17 H23 I N2' _chemical_formula_weight 382.27 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2024-03-15 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 97.412(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 5.76000(10) _cell_length_b 7.90630(10) _cell_length_c 17.6186(3) _cell_measurement_reflns_used 3398 _cell_measurement_temperature 99.8(6) _cell_measurement_theta_max 71.7390 _cell_measurement_theta_min 2.5300 _cell_volume 795.65(2) _computing_cell_refinement 'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 99.8(6) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix3000 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -100.00 -73.00 0.50 0.25 -- -41.10 -38.00 -60.00 54 2 \w 0.00 52.00 0.50 0.25 -- 41.10 -38.00 -60.00 104 3 \w 52.00 87.00 0.50 0.25 -- 41.10 38.00 94.00 70 4 \w 125.00 157.00 0.50 1.00 -- 100.00 38.00 94.00 64 5 \w 49.00 112.00 0.50 1.00 -- 100.00 -38.00 -60.00 126 6 \w 87.00 112.00 0.50 1.00 -- 100.00 38.00 94.00 50 7 \w -16.00 13.00 0.50 0.25 -- -41.10 65.00-180.00 58 8 \w -56.00 -25.00 0.50 0.25 -- -41.10 -54.00 150.00 62 9 \w -104.00 -64.00 0.50 0.25 -- -41.10 -54.00 150.00 80 10 \w -16.00 13.00 0.50 0.25 -- -41.10 38.00 94.00 58 11 \w -51.00 -26.00 0.50 0.25 -- -41.10 65.00-180.00 50 12 \w 17.00 72.00 0.50 0.25 -- 41.10-138.00 90.00 110 13 \w -7.00 50.00 0.50 0.25 -- 41.10 -43.00-180.00 114 14 \w 80.00 106.00 0.50 0.25 -- 41.10 32.00 -30.00 52 15 \w 39.00 69.00 0.50 0.25 -- 41.10 32.00 -30.00 60 16 \w 62.00 97.00 0.50 0.25 -- 41.10 32.00 -90.00 70 17 \w 59.00 85.00 0.50 1.00 -- 100.00-133.00 -60.00 52 18 \w 45.00 97.00 0.50 1.00 -- 100.00 -25.00-120.00 104 19 \w 106.00 131.00 0.50 1.00 -- 100.00 68.00-180.00 50 20 \w 40.00 101.00 0.50 1.00 -- 100.00 -93.00 90.00 122 21 \w 98.00 152.00 0.50 1.00 -- 100.00 33.00 30.00 108 22 \w 36.00 107.00 0.50 1.00 -- 100.00 -33.00-180.00 142 23 \w 104.00 134.00 0.50 1.00 -- 100.00 133.00 -30.00 60 24 \w 62.00 108.00 0.50 1.00 -- 100.00-111.00-120.00 92 25 \w 40.00 84.00 0.50 1.00 -- 100.00-111.00 -30.00 88 26 \w 113.00 149.00 0.50 1.00 -- 100.00 33.00 -90.00 72 27 \w 124.00 150.00 0.50 1.00 -- 100.00 33.00-180.00 52 28 \w 104.00 136.00 0.50 1.00 -- 100.00 33.00 60.00 64 29 \w 86.00 148.00 0.50 1.00 -- 100.00 17.00 0.00 124 30 \w 41.00 108.00 0.50 1.00 -- 100.00-111.00 -60.00 134 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, HyPix3000' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0524861000 _diffrn_orient_matrix_UB_12 0.0910533000 _diffrn_orient_matrix_UB_13 -0.0775579000 _diffrn_orient_matrix_UB_21 0.2641942000 _diffrn_orient_matrix_UB_22 0.0276065000 _diffrn_orient_matrix_UB_23 -0.0014970000 _diffrn_orient_matrix_UB_31 0.0147648000 _diffrn_orient_matrix_UB_32 -0.1698943000 _diffrn_orient_matrix_UB_33 -0.0419968000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_unetI/netI 0.0441 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 3876 _diffrn_reflns_point_group_measured_fraction_full 0.741 _diffrn_reflns_point_group_measured_fraction_max 0.735 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 69.987 _diffrn_reflns_theta_min 2.529 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 15.733 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.73254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.596 _exptl_crystal_description prism _exptl_crystal_F_000 384 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.915 _refine_diff_density_min -1.318 _refine_diff_density_rms 0.112 _refine_ls_abs_structure_details ; Classical Flack method preferred over Parsons because s.u. lower. ; _refine_ls_abs_structure_Flack -0.018(12) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 186 _refine_ls_number_reflns 2199 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0285 _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^)+(0.0445P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.0707 _reflns_Friedel_coverage 0.365 _reflns_Friedel_fraction_full 0.440 _reflns_Friedel_fraction_max 0.426 _reflns_number_gt 2120 _reflns_number_total 2199 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file aw5097sup1.cif _cod_data_source_block hmbi-sni4 _cod_depositor_comments 'Adding full bibliography for 2312709--2312717.cif.' _cod_database_code 2312709 _cod_database_fobs_code 2312709 _shelx_shelxl_version_number 2019/3 _chemical_oxdiff_formula 'C18 H26 N2 Sn I4' _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_max 0.650 _shelx_estimated_absorpt_t_min 0.254 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C3(H3), C7(H7), C16(H16), C2(H2), C6(H6), C12(H12), C13(H13), C15(H15) 2.b Idealised Me refined as rotating group: C19(H19A,H19B,H19C), C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C) ; _shelx_res_file ; TITL hmbi-sni4_a.res in P2(1) hmbi-sni4.res created by SHELXL-2019/3 at 12:23:07 on 15-Mar-2024 REM Old TITL HMBI-SnI4 in P2(1) REM SHELXT solution in P2(1): R1 0.061, Rweak 0.014, Alpha 0.031 REM 0.365 for 5 systematic absences, Orientation as input REM Flack x = 0.093 ( 0.020 ) from 557 Parsons' quotients REM Formula found by SHELXT: C15 N3 I CELL 1.54184 5.76 7.9063 17.6186 90 97.412 90 ZERR 2 0.0001 0.0001 0.0003 0 0.002 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H I N UNIT 34 46 2 4 L.S. 15 PLAN 1 SIZE 0.12 0.05 0.03 TEMP -173 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT -4 140 REM REM REM WGHT 0.044500 FVAR 0.54090 I1 3 -0.159478 0.794944 0.897329 11.00000 0.01880 0.01189 = 0.01571 0.00154 0.00421 0.00163 C19 1 0.282702 0.459760 0.897282 11.00000 0.01986 0.01126 = 0.01508 -0.00082 0.00188 0.00388 AFIX 137 H19A 2 0.245298 0.450714 0.949838 11.00000 -1.50000 H19B 2 0.137523 0.458498 0.861522 11.00000 -1.50000 H19C 2 0.366744 0.565782 0.891446 11.00000 -1.50000 AFIX 0 N2 4 0.433342 0.313443 0.880528 11.00000 0.01248 0.00855 = 0.01206 0.00116 0.00326 0.00157 C3 1 0.564335 0.403111 0.513102 11.00000 0.01280 0.01315 = 0.01780 -0.00113 0.00157 0.00170 AFIX 43 H3 2 0.427971 0.462971 0.522564 11.00000 -1.20000 AFIX 0 N1 4 0.899469 0.320996 0.350851 11.00000 0.02197 0.01502 = 0.01560 0.00213 0.00364 0.00496 C7 1 0.962626 0.231243 0.484188 11.00000 0.01514 0.01585 = 0.01986 0.00205 0.00304 0.00443 AFIX 43 H7 2 1.098264 0.170170 0.474987 11.00000 -1.20000 AFIX 0 C16 1 0.661392 0.199860 0.781320 11.00000 0.01470 0.01545 = 0.01672 0.00601 0.00037 -0.00057 AFIX 43 H16 2 0.727320 0.118844 0.817699 11.00000 -1.20000 AFIX 0 C14 1 0.628926 0.319256 0.652385 11.00000 0.00991 0.00767 = 0.01718 0.00277 0.00317 0.00018 C2 1 0.628207 0.404050 0.440020 11.00000 0.01686 0.01418 = 0.01589 -0.00180 0.00071 0.00081 AFIX 43 H2 2 0.533945 0.462919 0.400329 11.00000 -1.20000 AFIX 0 C8 1 0.746191 0.394579 0.287534 11.00000 0.02525 0.01589 = 0.01560 0.00044 0.00376 0.00177 AFIX 137 H8A 2 0.594833 0.336237 0.281956 11.00000 -1.50000 H8B 2 0.817528 0.382316 0.240255 11.00000 -1.50000 H8C 2 0.722761 0.514848 0.297654 11.00000 -1.50000 AFIX 0 C4 1 0.694427 0.316800 0.573266 11.00000 0.01360 0.01452 = 0.01426 -0.00380 0.00044 -0.00028 C18 1 0.646648 0.312246 0.940409 11.00000 0.01403 0.02246 = 0.01548 -0.00020 -0.00158 0.00255 AFIX 137 H18A 2 0.739277 0.414617 0.935275 11.00000 -1.50000 H18B 2 0.742007 0.212272 0.933228 11.00000 -1.50000 H18C 2 0.596851 0.309072 0.991518 11.00000 -1.50000 AFIX 0 C6 1 0.896593 0.233027 0.556900 11.00000 0.01675 0.01537 = 0.01881 -0.00095 0.00236 0.00168 AFIX 43 H6 2 0.991190 0.175690 0.597013 11.00000 -1.20000 AFIX 0 C1 1 0.831156 0.318931 0.423544 11.00000 0.01452 0.01189 = 0.01431 0.00123 0.00381 0.00063 C11 1 0.503569 0.319930 0.801484 11.00000 0.01609 0.01044 = 0.01436 0.00085 0.00384 -0.00172 C9 1 1.082776 0.207010 0.333772 11.00000 0.01805 0.02287 = 0.01796 -0.00228 0.00286 0.00183 AFIX 137 H9A 2 1.039804 0.090525 0.344901 11.00000 -1.50000 H9B 2 1.229875 0.236640 0.365331 11.00000 -1.50000 H9C 2 1.102627 0.216770 0.279534 11.00000 -1.50000 AFIX 0 C12 1 0.409218 0.439057 0.748517 11.00000 0.01921 0.01597 = 0.01765 0.00145 0.00472 0.00454 AFIX 43 H12 2 0.303365 0.522223 0.762408 11.00000 -1.20000 AFIX 0 C13 1 0.471444 0.435416 0.674638 11.00000 0.01753 0.02035 = 0.01691 0.00068 0.00304 0.00071 AFIX 43 H13 2 0.403170 0.515647 0.638274 11.00000 -1.20000 AFIX 0 C15 1 0.721906 0.199688 0.707001 11.00000 0.01549 0.01262 = 0.01384 -0.00074 0.00428 0.00297 AFIX 43 H15 2 0.828268 0.116878 0.693117 11.00000 -1.20000 AFIX 0 C17 1 0.297367 0.153914 0.888514 11.00000 0.02026 0.01817 = 0.01598 0.00238 0.00546 0.00284 AFIX 137 H17A 2 0.242125 0.151812 0.938837 11.00000 -1.50000 H17B 2 0.398390 0.055863 0.883539 11.00000 -1.50000 H17C 2 0.162798 0.149897 0.848380 11.00000 -1.50000 AFIX 0 HKLF 4 REM hmbi-sni4_a.res in P2(1) REM wR2 = 0.0707, GooF = S = 1.040, Restrained GooF = 1.040 for all data REM R1 = 0.0285 for 2120 Fo > 4sig(Fo) and 0.0293 for all 2199 data REM 186 parameters refined using 1 restraints END WGHT 0.0449 0.0000 REM Highest difference peak 0.915, deepest hole -1.318, 1-sigma level 0.112 Q1 1 -0.3570 0.7977 0.8785 11.00000 0.05 0.91 ; _shelx_res_checksum 84899 _shelx_hkl_file ; 0 -9 0 -0.72 1.67 0 -9 1 221.79 10.88 0 -9 -1 228.67 10.91 0 -9 -2 348.90 14.38 0 -9 2 354.74 14.51 0 -9 -3 412.20 15.87 0 -9 3 393.38 15.66 0 -9 4 99.97 6.62 0 -9 -4 107.23 6.80 0 -9 -5 4.42 1.81 0 -9 -6 232.07 10.35 0 -9 -7 345.06 13.07 0 -8 0 850.98 30.07 0 -8 1 373.27 17.15 0 -8 -1 406.81 17.67 0 -8 -2 63.63 6.26 0 -8 -3 83.56 7.10 0 -8 -4 442.10 18.76 0 -8 -5 576.94 22.37 0 -8 -6 317.24 14.86 0 -8 -7 21.72 3.70 0 -8 -8 111.96 7.79 0 -8 -8 107.33 6.92 0 -8 -9 375.68 15.57 0 -8 -9 364.59 14.41 0 -8 -10 391.21 15.33 0 -8 -10 375.25 14.23 0 -8 -11 151.47 7.29 0 -7 0 1.46 1.76 0 -7 -1 189.03 11.65 0 -7 -2 577.66 23.84 0 -7 -2 579.41 23.57 0 -7 -3 529.14 22.35 0 -7 3 581.92 22.98 0 -7 -3 549.61 22.53 0 -7 -4 84.74 7.47 0 -7 4 93.92 7.99 0 -7 -4 85.71 7.61 0 -7 5 2.59 2.15 0 -7 -5 4.37 2.39 0 -7 6 248.10 13.83 0 -7 -6 248.85 13.14 0 -7 -6 253.75 13.84 0 -7 7 589.09 23.86 0 -7 -7 586.10 22.96 0 -7 -7 599.88 23.99 0 -7 -8 363.11 16.47 0 -7 8 361.38 17.26 0 -7 -8 360.37 17.24 0 -7 -9 200.50 11.15 0 -7 -9 196.67 11.99 0 -7 9 186.27 11.45 0 -7 -10 13.34 3.47 0 -7 -10 13.61 2.87 0 -7 -11 283.48 13.94 0 -7 -11 264.22 12.59 0 -7 -12 460.15 17.34 0 -7 -13 127.93 7.13 0 -6 0 1282.17 40.57 0 -6 0 1262.22 40.41 0 -6 -1 1058.34 35.28 0 -6 1 1075.20 35.29 0 -6 1 1035.57 35.01 0 -6 -1 1101.89 34.57 0 -6 2 119.24 8.41 0 -6 2 120.16 8.42 0 -6 -2 120.24 8.11 0 -6 -2 125.91 8.68 0 -6 -3 122.68 8.67 0 -6 -3 128.63 8.90 0 -6 3 138.18 9.00 0 -6 -3 127.40 8.47 0 -6 3 133.65 9.06 0 -6 -4 1349.83 41.33 0 -6 4 1314.73 42.00 0 -6 -4 1279.74 41.88 0 -6 -4 1278.99 41.43 0 -6 5 924.75 32.39 0 -6 -5 925.70 31.91 0 -6 -5 932.26 32.49 0 -6 -6 683.63 25.92 0 -6 -6 674.59 25.30 0 -6 6 654.91 25.73 0 -6 -6 667.13 24.73 0 -6 -7 40.07 5.08 0 -6 -7 58.94 6.37 0 -6 -7 53.63 5.75 0 -6 7 49.15 5.92 0 -6 -8 202.69 12.53 0 -6 -8 215.09 12.16 0 -6 8 201.25 12.52 0 -6 -8 207.89 11.91 0 -6 -9 787.51 28.49 0 -6 9 771.05 29.31 0 -6 -9 772.02 29.72 0 -6 -9 769.14 28.07 0 -6 10 591.42 24.19 0 -6 -10 578.54 23.11 0 -6 -10 584.47 24.58 0 -6 -10 586.29 22.87 0 -6 -11 310.50 15.00 0 -6 -11 308.05 16.21 0 -6 -12 43.26 5.54 0 -6 -12 43.38 5.01 0 -6 -13 301.89 13.78 0 -6 -14 614.80 21.63 0 -6 -15 321.88 12.80 0 -5 2 1114.56 34.32 0 -5 2 1085.07 34.36 0 -5 -3 851.53 27.59 0 -5 3 813.19 27.10 0 -5 3 804.86 27.40 0 -5 -3 857.48 27.15 0 -5 4 273.22 25.40 0 -5 4 267.65 25.35 0 -5 -4 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21.65 4 1 -11 0.50 2.39 4 1 -10 117.65 10.35 -4 1 10 168.32 22.11 4 1 -10 137.58 23.04 4 1 -9 1099.90 40.47 -4 1 9 1205.98 62.41 4 1 -9 1172.01 69.34 4 1 -8 723.91 29.67 -4 1 8 767.55 47.36 4 1 -8 781.85 53.50 4 1 -7 173.69 12.13 -4 1 7 193.15 22.12 4 1 -7 168.02 23.47 4 1 -6 31.61 10.57 4 1 -6 25.81 4.67 -4 1 6 32.08 8.83 4 1 -6 17.51 7.84 4 1 -5 410.62 35.02 4 1 -5 314.20 16.92 -4 1 5 371.08 29.56 4 1 -4 839.60 51.12 4 1 -4 669.93 27.76 -4 1 3 714.76 27.98 -4 1 2 175.55 11.50 4 1 -1 43.54 11.70 -4 1 1 27.08 4.46 4 1 0 859.11 55.34 -4 1 0 912.78 32.93 4 1 1 933.65 59.53 -4 1 -1 1019.63 35.85 4 1 2 439.38 39.74 4 1 3 182.47 13.07 4 1 3 222.91 28.48 4 1 4 128.37 10.87 4 1 4 124.93 22.01 -4 1 -4 144.67 9.69 -4 1 -5 644.95 24.97 -4 1 -6 794.43 29.68 -4 1 -6 980.34 61.18 -4 1 -7 335.53 16.80 -4 1 -7 428.46 40.60 -4 1 -8 81.78 7.63 -4 1 -9 40.10 6.37 -4 1 -9 33.62 4.99 -4 1 -10 367.37 19.48 -4 1 -10 373.97 17.95 -4 1 -11 430.36 21.19 -4 1 -12 239.19 15.01 4 1 12 287.90 18.82 4 1 13 17.56 4.98 -4 1 -13 17.96 4.19 -4 1 -14 32.99 4.95 -4 1 -15 210.66 11.58 4 2 -15 220.36 13.30 4 2 -14 22.32 4.28 4 2 -13 76.23 8.07 4 2 -12 401.24 20.28 4 2 -11 746.91 30.39 4 2 -10 39.65 5.92 4 2 -7 518.01 41.64 4 2 -6 646.42 47.05 4 2 -5 576.41 43.67 4 2 -4 38.29 11.10 4 2 -3 190.01 24.27 4 2 -2 726.10 48.88 4 2 -1 512.17 42.12 4 2 0 590.90 46.01 4 2 1 14.45 7.68 4 2 2 119.81 21.07 4 2 3 246.93 30.79 4 2 4 960.00 64.03 4 2 5 181.65 27.18 -4 2 -8 578.48 23.40 -4 2 -9 429.13 19.07 4 3 -8 570.41 46.03 4 3 -7 163.64 24.11 4 3 -6 34.39 11.51 4 3 -5 558.89 44.80 4 3 -4 807.59 54.24 4 3 -3 423.74 37.81 4 3 -2 44.81 12.06 4 3 -1 91.27 17.07 4 3 0 646.38 50.10 4 3 1 869.32 59.85 4 3 2 609.77 49.84 4 3 3 107.25 20.99 4 3 4 445.45 43.38 4 3 5 572.46 49.88 4 4 -4 24.66 10.20 4 4 -3 68.18 15.40 4 4 -2 372.55 36.05 4 4 0 394.92 39.91 4 4 1 -2.33 5.77 -5 -6 9 150.82 11.16 5 -6 -9 148.95 7.15 -5 -6 8 349.64 18.89 5 -6 -8 345.20 13.10 -5 -6 7 325.69 18.80 5 -6 -7 290.92 11.99 -5 -6 6 95.74 10.47 -5 -6 5 8.41 4.60 -5 -6 4 308.30 20.14 -5 -6 3 385.30 15.57 -5 -6 3 418.43 24.00 -5 -6 2 370.97 15.18 -5 -6 2 373.84 22.91 -5 -6 1 78.45 6.08 -5 -6 1 84.28 5.62 -5 -6 1 82.08 10.81 -5 -6 0 66.11 5.45 -5 -6 0 69.97 10.15 -5 -6 -1 227.41 10.90 -5 -6 -1 288.93 20.42 -5 -6 -2 241.69 11.04 -5 -6 -2 306.23 20.93 -5 -6 -3 324.08 13.04 -5 -6 -3 371.81 23.31 -5 -6 -4 84.78 5.37 -5 -6 -5 55.35 3.95 5 -5 -12 47.36 3.74 5 -5 -11 258.65 10.96 5 -5 -10 314.27 13.17 -5 -5 9 284.50 17.85 5 -5 -9 269.33 12.41 -5 -5 8 3.90 3.78 5 -5 -8 7.00 2.34 -5 -5 7 119.30 12.33 5 -5 -7 102.44 7.39 -5 -5 6 360.48 22.73 5 -5 -6 330.81 14.92 -5 -5 5 267.63 19.92 -5 -5 4 239.02 19.20 -5 -5 3 6.19 4.77 -5 -5 2 106.14 13.41 -5 -5 1 431.79 27.86 -5 -5 0 314.94 23.82 -5 -5 -1 183.11 18.20 -5 -5 -2 24.66 3.77 -5 -5 -2 30.90 8.67 -5 -5 -3 180.80 9.89 -5 -5 -3 194.64 19.30 -5 -5 -4 284.42 12.85 -5 -5 -4 360.50 26.13 -5 -5 -5 170.30 8.90 -5 -5 -5 230.11 20.83 -5 -5 -6 104.22 6.30 -5 -5 -6 160.18 17.68 -5 -5 -7 2.77 1.33 -5 -5 -8 108.12 5.63 -5 -4 14 110.93 6.79 5 -4 -14 128.05 6.19 -5 -4 13 316.80 13.92 5 -4 -13 326.40 12.74 -5 -4 12 353.55 15.78 5 -4 -12 360.04 14.49 -5 -4 11 115.18 8.57 5 -4 -11 109.21 7.45 -5 -4 10 39.80 5.40 5 -4 -10 40.23 4.76 -5 -4 9 182.96 11.82 5 -4 -9 187.59 10.97 -5 -4 8 565.95 24.31 5 -4 -8 599.50 23.24 -5 -4 7 338.15 17.58 -5 -4 7 376.41 23.66 5 -4 -7 352.54 16.61 -5 -4 6 138.72 14.81 5 -4 -6 132.35 9.35 -5 -4 5 75.14 11.68 -5 -4 4 566.47 32.36 -5 -4 3 711.51 37.59 -5 -4 2 510.91 31.54 -5 -4 1 11.49 6.21 -5 -4 0 59.44 11.37 -5 -4 -1 464.94 31.52 -5 -4 -2 566.07 35.94 -5 -4 -3 617.57 38.47 -5 -4 -4 13.98 3.16 -5 -4 -4 21.56 9.16 -5 -4 -5 178.02 20.79 -5 -4 -6 286.42 13.21 -5 -4 -6 350.90 29.31 -5 -4 -7 290.81 12.91 -5 -4 -7 345.21 28.80 -5 -4 -8 171.37 8.78 -5 -4 -8 194.44 21.10 -5 -4 -9 4.95 1.63 -5 -4 -10 65.50 4.30 -5 -3 15 318.04 13.40 5 -3 -15 306.75 11.56 -5 -3 14 325.33 14.63 5 -3 -14 310.52 12.71 5 -3 -13 14.75 2.78 -5 -3 13 15.42 3.47 -5 -3 12 52.87 6.23 5 -3 -12 61.74 5.65 -5 -3 11 314.21 16.72 5 -3 -11 330.69 15.36 -5 -3 10 427.42 20.63 5 -3 -10 444.84 19.21 -5 -3 9 271.26 15.84 5 -3 -9 266.52 14.29 -5 -3 8 61.08 7.28 5 -3 -8 54.86 6.23 -5 -3 7 82.34 8.62 5 -3 -7 108.06 8.60 -5 -3 6 376.64 19.57 5 -3 -6 370.11 17.70 -5 -3 5 282.08 16.65 -5 -3 4 467.56 29.17 -5 -3 3 22.03 7.35 -5 -3 2 159.07 17.34 -5 -3 1 517.22 32.84 -5 -3 0 468.14 31.54 -5 -3 -1 221.72 22.11 -5 -3 -2 2.61 6.27 -5 -3 -3 160.57 20.50 -5 -3 -4 240.05 25.05 -5 -3 -5 857.91 50.79 -5 -3 -6 117.68 19.41 -5 -3 -7 21.20 10.51 -5 -3 -8 114.82 19.29 -5 -3 -9 435.56 18.73 -5 -3 -9 445.90 16.86 -5 -3 -10 292.31 13.42 -5 -3 -10 288.92 11.82 -5 -3 -11 93.21 5.35 -5 -2 16 110.12 6.98 5 -2 -15 1.35 1.19 -5 -2 15 -0.29 1.47 -5 -2 14 155.17 10.06 -5 -2 14 145.68 9.65 5 -2 -14 163.27 8.86 -5 -2 13 285.79 15.09 -5 -2 13 268.85 14.55 -5 -2 12 287.06 15.78 -5 -2 12 275.97 15.32 -5 -2 11 173.26 12.22 -5 -2 11 157.91 11.47 -5 -2 10 33.03 5.74 -5 -2 10 36.02 5.71 -5 -2 10 30.54 5.71 -5 -2 9 159.14 11.93 -5 -2 9 130.80 10.85 -5 -2 8 859.05 33.90 -5 -2 8 855.15 33.40 -5 -2 7 423.88 21.29 -5 -2 7 424.06 20.95 -5 -2 6 80.96 8.73 -5 -2 6 95.92 9.07 -5 -2 5 72.71 8.18 -5 -2 5 72.20 7.87 -5 -2 4 441.83 21.92 -5 -2 4 451.98 21.50 -5 -2 3 775.09 30.80 -5 -2 2 446.55 21.31 5 -2 -1 74.16 9.75 -5 -2 1 67.56 12.32 5 -2 0 30.20 6.85 -5 -2 0 45.24 10.56 5 -2 1 593.87 30.19 -5 -2 -1 602.10 38.48 5 -2 2 827.41 37.16 -5 -2 -2 793.26 29.54 5 -2 3 410.50 23.78 -5 -2 -3 352.93 17.06 -5 -2 -4 110.30 8.49 -5 -2 -4 129.88 19.81 -5 -2 -5 140.83 9.68 -5 -2 -5 193.93 24.13 -5 -2 -6 289.71 14.65 -5 -2 -6 385.90 34.65 -5 -2 -7 399.02 17.77 -5 -2 -7 605.19 44.43 5 -2 8 201.54 15.30 -5 -2 -8 188.27 10.76 5 -2 9 5.08 3.57 -5 -2 -9 2.77 2.35 5 -2 10 76.48 8.48 -5 -2 -10 91.38 7.60 -5 -2 -10 72.37 5.52 5 -2 11 219.33 13.41 -5 -2 -11 202.31 11.21 -5 -2 -11 210.46 9.29 -5 -2 -12 202.97 10.31 5 -2 12 203.47 11.78 -5 -1 17 17.06 2.55 -5 -1 16 286.50 12.87 -5 -1 16 294.68 13.41 5 -1 -16 311.33 11.74 -5 -1 15 457.41 18.19 5 -1 -15 396.19 18.05 -5 -1 14 171.31 10.72 5 -1 -14 153.11 10.69 5 -1 -13 24.54 4.64 -5 -1 13 24.02 4.47 -5 -1 12 87.75 8.36 5 -1 -12 81.63 8.37 -5 -1 11 602.02 25.38 5 -1 -11 536.14 25.15 -5 -1 10 816.06 31.69 5 -1 -10 748.28 31.82 -5 -1 9 63.08 7.43 -5 -1 9 50.44 7.11 -5 -1 8 63.22 7.69 -5 -1 8 80.20 8.71 -5 -1 7 104.04 9.59 -5 -1 7 102.38 9.78 -5 -1 6 487.54 23.15 -5 -1 6 498.64 23.73 -5 -1 5 454.99 22.10 -5 -1 5 463.71 22.49 -5 -1 4 325.74 17.90 -5 -1 4 317.10 17.79 5 -1 -3 5.69 3.76 -5 -1 3 3.92 2.27 5 -1 -2 244.59 17.22 -5 -1 2 236.89 14.98 5 -1 -1 588.89 28.54 -5 -1 1 528.86 24.60 5 -1 0 369.00 21.95 5 -1 1 122.51 12.26 5 -1 2 0.68 3.13 -5 -1 -2 -4.40 9.08 5 -1 3 369.10 22.03 -5 -1 -3 339.94 17.05 5 -1 4 116.03 11.80 -5 -1 -4 115.87 9.08 5 -1 5 880.61 38.22 -5 -1 -5 925.18 33.11 -5 -1 -6 49.91 15.45 -5 -1 -6 26.95 4.42 -5 -1 -7 14.33 3.43 -5 -1 -7 27.92 12.59 -5 -1 -8 186.29 11.28 -5 -1 -8 253.98 30.21 -5 -1 -9 371.86 18.48 -5 -1 -10 355.01 17.36 5 -1 10 371.59 20.72 -5 -1 -11 49.12 5.69 5 -1 11 47.57 6.72 5 -1 12 27.79 4.73 -5 -1 -12 22.99 3.75 -5 -1 -13 44.95 4.45 5 -1 13 44.16 5.06 -5 0 17 380.72 14.81 5 0 -16 145.19 9.09 5 0 -15 1.07 1.77 5 0 -14 127.67 9.86 5 0 -13 301.41 16.67 5 0 -12 243.21 15.25 5 0 -11 207.81 14.22 5 0 -10 1.08 2.68 5 0 -9 93.17 9.44 -5 0 8 980.81 37.83 -5 0 7 531.61 25.00 -5 0 6 75.55 8.45 5 0 -5 16.51 4.91 -5 0 5 15.36 4.36 -5 0 4 402.99 20.17 5 0 -4 430.42 23.08 -5 0 4 415.25 21.07 5 0 -3 774.60 33.39 -5 0 3 735.12 30.69 5 0 -2 482.17 25.17 -5 0 2 492.09 23.25 5 0 -1 202.36 15.27 -5 0 1 184.48 13.06 5 0 0 3.81 3.24 5 0 1 602.06 28.94 5 0 2 906.03 37.97 5 0 3 285.34 18.62 -5 0 -3 278.51 15.01 5 0 4 196.84 15.14 -5 0 -4 205.92 12.49 5 0 5 69.66 8.90 -5 0 -5 74.49 7.40 -5 0 -5 90.36 19.29 5 0 6 328.35 19.84 -5 0 -6 349.05 17.06 -5 0 -7 509.06 21.71 -5 0 -7 599.53 47.17 -5 0 -8 164.91 10.75 -5 0 -9 49.09 6.24 -5 0 -9 37.51 4.92 -5 0 -10 38.98 5.45 -5 0 -11 239.20 13.12 5 0 11 261.72 15.99 -5 0 -12 271.29 13.36 5 0 12 294.52 15.70 -5 0 -13 104.30 6.95 5 0 13 113.54 8.16 -5 1 16 284.40 12.98 5 1 -15 411.82 18.12 5 1 -14 116.80 9.24 5 1 -13 16.39 3.86 5 1 -12 75.47 8.07 5 1 -11 478.47 23.22 5 1 -10 765.35 31.77 -5 1 9 0.52 2.51 -5 1 8 66.67 8.13 -5 1 7 95.87 9.52 -5 1 6 472.42 22.97 -5 1 5 467.49 22.71 -5 1 4 286.48 16.75 -5 1 3 6.45 2.68 -5 1 2 210.39 13.96 5 1 -1 555.07 27.33 -5 1 1 564.70 25.36 5 1 0 314.32 19.42 5 1 1 127.57 11.87 5 1 2 -1.81 3.17 5 1 3 385.27 21.59 -5 1 -3 381.16 17.98 5 1 4 98.30 10.17 -5 1 -4 96.51 8.17 -5 1 -5 852.12 31.06 -5 1 -6 26.56 4.50 -5 1 -7 11.80 3.30 -5 1 -8 213.54 12.11 5 1 11 73.17 8.15 5 1 12 29.09 4.73 5 2 1 536.89 26.10 5 2 2 721.88 31.41 -5 2 -2 722.23 27.04 5 2 3 335.17 19.26 -5 2 -3 327.39 15.94 -5 2 -4 173.07 10.80 -5 2 -5 175.66 10.96 -5 2 -6 326.13 15.59 -5 2 -7 366.75 16.62 -5 2 -8 143.70 9.12 -6 -5 4 25.73 2.81 -6 -5 4 26.53 6.21 -6 -5 3 194.95 8.74 -6 -5 3 223.90 16.12 -6 -5 2 252.50 10.39 -6 -5 2 289.66 18.80 -6 -5 1 252.60 10.26 -6 -5 1 265.33 18.56 -6 -5 0 33.35 3.15 -6 -5 0 34.46 7.11 -6 -4 3 120.02 13.49 -6 -4 2 -2.49 5.04 -6 -4 1 113.85 14.07 -6 -4 0 474.24 28.86 -6 -4 -1 195.94 9.21 -6 -4 -1 198.21 18.58 -6 -4 -2 133.36 15.27 -6 -4 -3 2.83 4.95 -6 -4 -4 82.40 12.43 -6 -4 -5 297.40 21.62 6 -3 -11 225.36 9.44 6 -3 -10 76.32 5.19 6 -3 -9 103.05 6.33 -6 -3 1 223.74 20.84 -6 -3 0 18.18 7.85 -6 -3 -1 30.11 8.98 -6 -3 -2 248.34 23.17 -6 -3 -3 450.16 31.51 -6 -3 -4 121.71 16.76 -6 -3 -5 3.31 6.96 -6 -3 -6 152.54 7.32 -6 -3 -6 198.83 19.43 -6 -3 -7 136.01 6.30 6 -2 -12 1.88 1.18 6 -2 -11 29.10 3.35 -6 -2 10 333.88 14.80 6 -2 -10 318.21 13.37 -6 -2 9 387.48 16.79 6 -2 -9 365.00 15.06 -6 -2 8 140.51 9.52 -6 -2 7 13.82 3.36 -6 -2 1 159.11 9.50 -6 -2 0 384.21 16.24 -6 -2 -1 331.17 14.63 -6 -2 -2 77.26 6.19 -6 -2 -2 104.37 16.82 -6 -2 -3 22.37 3.41 -6 -2 -3 27.85 10.64 -6 -2 -4 173.48 9.25 -6 -2 -4 221.80 23.95 -6 -2 -5 163.09 20.39 -6 -2 -6 503.92 34.39 -6 -2 -7 57.15 5.25 -6 -2 -8 20.06 2.98 -6 -2 -8 25.20 2.54 -6 -1 13 149.87 8.21 6 -1 -13 136.85 6.96 -6 -1 12 348.78 14.99 -6 -1 11 244.78 12.60 -6 -1 10 64.90 6.44 -6 -1 9 22.13 4.12 -6 -1 8 105.45 8.71 -6 -1 7 691.12 27.34 -6 -1 6 491.49 21.90 -6 -1 5 43.47 5.88 6 -1 -3 336.14 19.27 6 -1 -2 519.77 25.48 6 -1 -1 240.85 16.36 6 -1 0 79.99 9.38 -6 -1 0 63.82 6.14 6 -1 1 3.50 3.15 -6 -1 -1 2.16 1.99 6 -1 2 219.22 15.30 -6 -1 -2 235.18 12.14 -6 -1 -3 478.00 19.12 -6 -1 -4 172.44 9.79 -6 -1 -5 56.90 5.26 -6 -1 -5 50.78 12.67 -6 -1 -6 179.54 9.40 6 -1 7 216.10 13.08 -6 -1 -7 205.43 10.93 -6 -1 -8 214.66 10.71 6 -1 8 250.11 13.02 -6 0 13 116.68 7.40 -6 0 12 1.71 1.66 -6 0 11 34.86 4.68 -6 0 10 480.40 20.48 -6 0 9 467.12 20.64 -6 0 8 33.09 5.13 -6 0 7 14.43 3.73 -6 0 6 101.09 8.99 -6 0 5 375.87 18.93 6 0 -4 156.24 12.50 6 0 -3 194.68 14.40 6 0 -2 24.20 5.61 6 0 -1 261.98 17.04 6 0 0 305.23 18.52 6 0 1 330.42 19.37 -6 0 -1 332.57 15.52 6 0 2 60.40 7.86 -6 0 -2 63.15 6.07 6 0 3 20.59 4.88 -6 0 -3 24.58 3.93 6 0 4 369.40 19.22 -6 0 -4 343.44 15.44 -6 0 -5 33.52 4.24 -6 0 -6 425.45 16.77 -6 0 -7 40.14 4.15 6 0 8 4.85 2.45 6 0 9 88.87 7.14 -6 1 13 182.74 9.26 -6 1 12 293.37 13.35 -6 1 11 242.48 12.51 -6 1 10 60.29 6.15 -6 1 9 7.75 2.71 -6 1 8 186.55 11.91 -6 1 7 648.04 26.17 6 1 -6 442.73 21.68 -6 1 6 469.40 21.17 6 1 -5 51.69 7.32 -6 1 5 53.54 6.59 6 1 -4 0.53 2.80 6 1 -3 360.73 20.06 6 1 -2 506.24 24.68 6 1 -1 228.03 15.47 6 1 0 78.11 8.74 -6 1 0 61.44 6.09 6 1 1 7.95 3.54 -6 1 -1 9.39 2.61 6 1 2 267.10 16.26 -6 1 -2 248.98 12.76 6 1 3 438.22 21.75 -6 1 -3 467.89 18.69 6 1 4 163.85 11.83 -6 1 -4 182.47 10.13 -6 1 -5 70.97 5.95 -6 1 -6 175.29 9.25 6 2 -7 12.39 3.64 6 2 -6 101.23 9.35 6 2 -5 347.44 18.67 6 2 -4 177.11 12.89 6 2 -3 195.98 13.68 6 2 -2 4.08 2.90 6 2 -1 149.58 11.88 6 2 0 344.00 18.69 6 2 1 257.32 15.47 6 2 2 113.93 9.78 6 2 3 13.74 3.97 6 3 -9 75.53 6.57 6 3 -8 184.07 11.30 6 3 -7 442.59 19.91 6 3 -6 293.89 15.85 6 3 -5 65.83 7.38 6 3 -4 48.86 6.46 6 3 -3 299.11 16.51 6 3 -2 319.25 17.13 6 3 -1 187.52 12.47 6 3 0 18.45 4.24 6 3 1 20.10 4.08 6 4 -9 273.49 12.27 6 4 -8 56.04 5.50 6 4 -7 27.33 4.14 6 4 -6 118.90 8.70 6 4 -5 240.23 13.18 6 4 -4 182.61 11.32 6 4 -3 100.27 8.19 6 4 -2 1.39 1.83 6 4 -1 87.58 7.41 6 5 -5 81.32 6.06 6 5 -4 23.94 3.44 6 5 -3 131.57 7.88 -7 -1 4 258.47 10.19 -7 -1 3 112.10 5.98 -7 -1 2 106.41 5.76 -7 -1 1 7.76 1.73 -7 0 6 284.79 10.87 -7 0 5 247.39 10.06 -7 0 4 30.47 3.05 7 0 -3 3.14 1.78 -7 0 3 6.47 1.52 -7 0 2 243.63 10.09 -7 0 1 283.13 11.06 -7 0 0 149.23 7.14 -7 1 4 298.85 11.25 7 1 -3 72.00 6.11 -7 1 3 89.44 5.15 7 1 -2 96.03 7.10 -7 1 2 101.71 5.64 7 1 -1 4.24 2.18 -7 1 1 6.92 1.55 7 1 0 88.24 6.54 0 0 0 0.00 0.00 TITL HMBI-SnI4 in P2(1) REM P2(1) (#4 in standard setting) CELL 1.54184 5.760043 7.906325 17.618618 90.0000 97.4125 90.0000 ZERR 2.00 0.000097 0.000131 0.000275 0.0000 0.0015 0.0000 LATT -1 SYMM -x, y+1/2,-z SFAC C H N Sn I UNIT 36.00 52.00 4.00 2.00 8.00 REM CrysAlisPro recorded range (K): Min=99.4; max=100.3; aver:99.8 TEMP -173 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 38686 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 4.208 _oxdiff_exptl_absorpt_empirical_full_min 0.481 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I1 I -0.15948(5) 0.79494(12) 0.89733(2) 0.01529(12) Uani 1 1 d . . . . . C19 C 0.2827(17) 0.4598(11) 0.8973(4) 0.0154(16) Uani 1 1 d . . . . . H19A H 0.245298 0.450714 0.949838 0.023 Uiso 1 1 calc R U . . . H19B H 0.137523 0.458498 0.861522 0.023 Uiso 1 1 calc R U . . . H19C H 0.366744 0.565782 0.891446 0.023 Uiso 1 1 calc R U . . . N2 N 0.4333(8) 0.3134(9) 0.8805(2) 0.0109(13) Uani 1 1 d . . . . . C3 C 0.5643(11) 0.4031(8) 0.5131(3) 0.0146(12) Uani 1 1 d . . . . . H3 H 0.427971 0.462971 0.522564 0.018 Uiso 1 1 calc R U . . . N1 N 0.8995(9) 0.3210(7) 0.3509(3) 0.0174(16) Uani 1 1 d . . . . . C7 C 0.9626(10) 0.2312(8) 0.4842(3) 0.0169(12) Uani 1 1 d . . . . . H7 H 1.098264 0.170170 0.474987 0.020 Uiso 1 1 calc R U . . . C16 C 0.6614(11) 0.1999(8) 0.7813(3) 0.0158(12) Uani 1 1 d . . . . . H16 H 0.727320 0.118844 0.817699 0.019 Uiso 1 1 calc R U . . . C14 C 0.6289(9) 0.3193(8) 0.6524(3) 0.0115(16) Uani 1 1 d . . . . . C2 C 0.6282(11) 0.4040(8) 0.4400(3) 0.0158(12) Uani 1 1 d . . . . . H2 H 0.533945 0.462919 0.400329 0.019 Uiso 1 1 calc R U . . . C8 C 0.7462(12) 0.3946(8) 0.2875(3) 0.0188(13) Uani 1 1 d . . . . . H8A H 0.594833 0.336237 0.281956 0.028 Uiso 1 1 calc R U . . . H8B H 0.817528 0.382316 0.240255 0.028 Uiso 1 1 calc R U . . . H8C H 0.722761 0.514848 0.297654 0.028 Uiso 1 1 calc R U . . . C4 C 0.6944(10) 0.3168(9) 0.5733(3) 0.0142(16) Uani 1 1 d . . . . . C18 C 0.6466(10) 0.3122(11) 0.9404(3) 0.0176(15) Uani 1 1 d . . . . . H18A H 0.739277 0.414617 0.935275 0.026 Uiso 1 1 calc R U . . . H18B H 0.742007 0.212272 0.933228 0.026 Uiso 1 1 calc R U . . . H18C H 0.596851 0.309072 0.991518 0.026 Uiso 1 1 calc R U . . . C6 C 0.8966(11) 0.2330(8) 0.5569(3) 0.0170(12) Uani 1 1 d . . . . . H6 H 0.991190 0.175690 0.597013 0.020 Uiso 1 1 calc R U . . . C1 C 0.8312(10) 0.3189(8) 0.4235(3) 0.0134(17) Uani 1 1 d . . . . . C11 C 0.5036(10) 0.3199(7) 0.8015(3) 0.0135(17) Uani 1 1 d . . . . . C9 C 1.0828(11) 0.2070(9) 0.3338(3) 0.0196(13) Uani 1 1 d . . . . . H9A H 1.039804 0.090525 0.344901 0.029 Uiso 1 1 calc R U . . . H9B H 1.229875 0.236640 0.365331 0.029 Uiso 1 1 calc R U . . . H9C H 1.102627 0.216770 0.279534 0.029 Uiso 1 1 calc R U . . . C12 C 0.4092(11) 0.4391(8) 0.7485(3) 0.0174(13) Uani 1 1 d . . . . . H12 H 0.303365 0.522223 0.762408 0.021 Uiso 1 1 calc R U . . . C13 C 0.4714(11) 0.4354(8) 0.6746(3) 0.0182(13) Uani 1 1 d . . . . . H13 H 0.403170 0.515647 0.638274 0.022 Uiso 1 1 calc R U . . . C15 C 0.7219(10) 0.1997(8) 0.7070(3) 0.0138(12) Uani 1 1 d . . . . . H15 H 0.828268 0.116878 0.693117 0.017 Uiso 1 1 calc R U . . . C17 C 0.2974(17) 0.1539(12) 0.8885(5) 0.0179(19) Uani 1 1 d . . . . . H17A H 0.242125 0.151812 0.938837 0.027 Uiso 1 1 calc R U . . . H17B H 0.398390 0.055863 0.883539 0.027 Uiso 1 1 calc R U . . . H17C H 0.162798 0.149897 0.848380 0.027 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 I1 0.01880(19) 0.01189(18) 0.01571(17) 0.0015(2) 0.00421(11) 0.0016(2) C19 0.020(3) 0.011(4) 0.015(3) -0.001(2) 0.002(2) 0.004(3) N2 0.012(2) 0.009(4) 0.0121(18) 0.001(2) 0.0033(15) 0.002(2) C3 0.013(3) 0.013(3) 0.018(3) -0.001(2) 0.002(2) 0.002(2) N1 0.022(2) 0.015(5) 0.016(2) 0.002(2) 0.0036(18) 0.005(2) C7 0.015(3) 0.016(3) 0.020(3) 0.002(2) 0.003(2) 0.004(2) C16 0.015(3) 0.015(3) 0.017(3) 0.006(2) 0.000(2) -0.001(3) C14 0.010(2) 0.008(5) 0.017(2) 0.003(2) 0.0032(19) 0.000(2) C2 0.017(3) 0.014(3) 0.016(3) -0.002(2) 0.001(2) 0.001(3) C8 0.025(3) 0.016(3) 0.016(3) 0.000(2) 0.004(2) 0.002(3) C4 0.014(2) 0.015(5) 0.014(2) -0.004(2) 0.0004(19) 0.000(2) C18 0.014(2) 0.022(5) 0.015(2) 0.000(3) -0.0016(18) 0.003(3) C6 0.017(3) 0.015(3) 0.019(3) -0.001(2) 0.002(2) 0.002(2) C1 0.015(2) 0.012(5) 0.014(2) 0.001(2) 0.0038(19) 0.001(2) C11 0.016(3) 0.010(5) 0.014(2) 0.001(2) 0.004(2) -0.002(2) C9 0.018(3) 0.023(3) 0.018(3) -0.002(3) 0.003(2) 0.002(3) C12 0.019(3) 0.016(3) 0.018(3) 0.001(2) 0.005(2) 0.005(3) C13 0.018(3) 0.020(3) 0.017(3) 0.001(2) 0.003(2) 0.001(3) C15 0.015(3) 0.013(3) 0.014(3) -0.001(2) 0.004(2) 0.003(3) C17 0.020(4) 0.018(5) 0.016(3) 0.002(3) 0.005(3) 0.003(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' I I -0.3257 6.8362 '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' 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 _geom_angle_publ_flag H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C19 H19A 109.5 . . ? N2 C19 H19B 109.5 . . ? N2 C19 H19C 109.5 . . ? C19 N2 C18 107.8(6) . . ? C19 N2 C11 112.9(5) . . ? C19 N2 C17 107.9(4) . . ? C11 N2 C18 110.8(4) . . ? C11 N2 C17 108.8(5) . . ? C17 N2 C18 108.4(6) . . ? C2 C3 H3 119.1 . . ? C2 C3 C4 121.9(6) . . ? C4 C3 H3 119.1 . . ? C1 N1 C8 119.8(5) . . ? C1 N1 C9 119.0(5) . . ? C9 N1 C8 118.5(5) . . ? C6 C7 H7 119.6 . . ? C6 C7 C1 120.8(6) . . ? C1 C7 H7 119.6 . . ? C11 C16 H16 120.3 . . ? C11 C16 C15 119.3(5) . . ? C15 C16 H16 120.3 . . ? C13 C14 C4 121.9(5) . . ? C13 C14 C15 117.3(5) . . ? C15 C14 C4 120.8(5) . . ? C3 C2 H2 119.5 . . ? C3 C2 C1 121.0(6) . . ? C1 C2 H2 119.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C4 C14 121.9(5) . . ? C3 C4 C6 117.0(5) . . ? C6 C4 C14 121.1(5) . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C7 C6 C4 122.0(6) . . ? C7 C6 H6 119.0 . . ? C4 C6 H6 119.0 . . ? N1 C1 C7 121.1(5) . . ? N1 C1 C2 121.7(5) . . ? C7 C1 C2 117.2(5) . . ? C16 C11 N2 118.5(5) . . ? C12 C11 N2 121.2(5) . . ? C12 C11 C16 120.2(5) . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C12 H12 120.4 . . ? C11 C12 C13 119.3(6) . . ? C13 C12 H12 120.4 . . ? C14 C13 C12 122.4(6) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C16 C15 C14 121.5(5) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19 N2 1.498(10) . ? N2 C18 1.513(6) . ? N2 C11 1.500(6) . ? N2 C17 1.501(10) . ? C3 H3 0.9500 . ? C3 C2 1.384(8) . ? C3 C4 1.395(9) . ? N1 C8 1.452(8) . ? N1 C1 1.388(7) . ? N1 C9 1.449(8) . ? C7 H7 0.9500 . ? C7 C6 1.383(8) . ? C7 C1 1.410(9) . ? C16 H16 0.9500 . ? C16 C11 1.392(9) . ? C16 C15 1.398(8) . ? C14 C4 1.490(7) . ? C14 C13 1.383(9) . ? C14 C15 1.405(9) . ? C2 H2 0.9500 . ? C2 C1 1.411(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C4 C6 1.402(9) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C6 H6 0.9500 . ? C11 C12 1.387(9) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C12 H12 0.9500 . ? C12 C13 1.394(8) . ? C13 H13 0.9500 . ? C15 H15 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 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 _geom_torsion_publ_flag C19 N2 C11 C16 174.1(6) . . . . ? C19 N2 C11 C12 -7.8(9) . . . . ? N2 C11 C12 C13 -177.1(6) . . . . ? C3 C2 C1 N1 -179.0(6) . . . . ? C3 C2 C1 C7 1.0(10) . . . . ? C3 C4 C6 C7 -1.7(10) . . . . ? C16 C11 C12 C13 1.0(9) . . . . ? C14 C4 C6 C7 -179.0(6) . . . . ? C2 C3 C4 C14 178.5(6) . . . . ? C2 C3 C4 C6 1.2(9) . . . . ? C8 N1 C1 C7 172.5(6) . . . . ? C8 N1 C1 C2 -7.5(9) . . . . ? C4 C3 C2 C1 -0.9(10) . . . . ? C4 C14 C13 C12 -179.9(6) . . . . ? C4 C14 C15 C16 -179.7(6) . . . . ? C18 N2 C11 C16 53.0(8) . . . . ? C18 N2 C11 C12 -128.9(7) . . . . ? C6 C7 C1 N1 178.5(6) . . . . ? C6 C7 C1 C2 -1.5(10) . . . . ? C1 C7 C6 C4 1.9(10) . . . . ? C11 C16 C15 C14 0.7(9) . . . . ? C11 C12 C13 C14 -1.5(10) . . . . ? C9 N1 C1 C7 11.3(9) . . . . ? C9 N1 C1 C2 -168.7(6) . . . . ? C13 C14 C4 C3 -15.0(9) . . . . ? C13 C14 C4 C6 162.2(6) . . . . ? C13 C14 C15 C16 -1.2(9) . . . . ? C15 C16 C11 N2 177.5(6) . . . . ? C15 C16 C11 C12 -0.6(9) . . . . ? C15 C14 C4 C3 163.5(6) . . . . ? C15 C14 C4 C6 -19.3(9) . . . . ? C15 C14 C13 C12 1.6(9) . . . . ? C17 N2 C11 C16 -66.1(7) . . . . ? C17 N2 C11 C12 112.0(7) . . . . ?