#------------------------------------------------------------------------------ #$Date: 2021-06-09 08:19:57 +0300 (Wed, 09 Jun 2021) $ #$Revision: 266288 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243851.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_2243851 loop_ _publ_author_name 'Ordinartsev, Artem A.' 'Petrov, Andrey A.' 'Lyssenko, Konstantin A.' 'Petrov, Andrey V.' 'Goodilin, Eugene A.' 'Tarasov, Alexey B.' _publ_section_title ; Crystal structure of new formamidinium triiodide jointly refined by single-crystal XRD, Raman scattering spectroscopy and DFT assessment of hydrogen-bond network features ; _journal_coeditor_code DX2037 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 692 _journal_page_last 695 _journal_paper_doi 10.1107/S2056989021005673 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C H5 N2 +, I3 -' _chemical_formula_moiety 'C H5 N2 +, I3 -' _chemical_formula_sum 'C H5 I3 N2' _chemical_formula_weight 425.77 _chemical_name_systematic ; Formamidinium triiodide ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 97.512(6) _cell_angle_beta 100.345(6) _cell_angle_gamma 99.437(6) _cell_formula_units_Z 2 _cell_length_a 6.0767(10) _cell_length_b 6.1886(11) _cell_length_c 11.727(2) _cell_measurement_reflns_used 899 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 29.12 _cell_measurement_theta_min 3.45 _cell_volume 422.10(13) _computing_cell_refinement ; SAINT (Bruker, 2019) ; _computing_data_collection ; APEX3 (Bruker, 2019) ; _computing_data_reduction ; SAINT (Bruker, 2019) ; _computing_molecular_graphics ; SHELXTL (Sheldrick, 2008) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 110(2) _diffrn_detector_area_resol_mean 7.31 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker D8 Quest with Photon III detector' _diffrn_measurement_method '\f and \w shutterless scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.1221 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4015 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.998 _diffrn_reflns_theta_min 1.790 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 11.014 _exptl_absorpt_correction_T_max 0.092177 _exptl_absorpt_correction_T_min 0.043680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (TWINABS; Bruker, 2019) ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 3.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 368 _exptl_crystal_size_max 0.257 _exptl_crystal_size_mid 0.187 _exptl_crystal_size_min 0.080 _refine_diff_density_max 2.452 _refine_diff_density_min -2.520 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 60 _refine_ls_number_reflns 4015 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 0.979 _refine_ls_R_factor_all 0.1522 _refine_ls_R_factor_gt 0.0844 _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^)+(0.0803P)^2^+4.4757P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1674 _refine_ls_wR_factor_ref 0.2004 _reflns_number_gt 2217 _reflns_number_total 4015 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file dx2037sup1.cif _cod_data_source_block I _cod_database_code 2243851 _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 0.164 _shelx_estimated_absorpt_t_max 0.473 _shelx_hkl_file ; 0 0 2 1481.59 16.5454 -2 1 0 0 1481.59 16.5454 1 0 0 4 652.843 23.9119 -2 2 0 0 652.843 23.9119 1 3 0 0 156.053 15.3059 2 0 -4 3 1956.91 54.8796 -3 4 0 0 1956.91 54.8796 1 4 0 0 569.800 21.5827 2 5 0 0 164.745 21.4448 1 5 0 0 55.0775 10.7612 2 6 0 0 20.9128 13.7321 2 6 0 0 0.19976 14.1890 1 7 0 0 23.1527 16.6781 2 0 -7 5 123.589 42.2377 -3 7 0 0 123.589 42.2377 1 8 0 0 5.06548 18.9205 2 8 0 0 58.6452 26.4838 1 -8 1 0 11.7047 19.3278 2 1 -8 5 89.5200 45.6764 -3 -8 1 0 89.5200 45.6764 1 -7 1 0 9.22358 11.6283 2 -7 1 0 17.9235 16.9809 1 -6 1 0 99.1736 22.2089 2 -6 1 0 292.868 29.7742 1 -5 1 0 24.3182 7.71316 2 1 -5 3 57.6767 21.9996 -3 -5 1 0 57.6767 21.9996 1 1 -4 2 443.905 28.1515 -3 -4 1 0 443.905 28.1515 1 -4 1 0 175.973 10.6240 2 -3 1 0 13.1473 7.84377 1 -3 1 0 12.6732 4.31618 2 -2 1 0 63.7997 4.33113 2 -2 1 0 150.049 8.13378 1 -1 1 0 3.78312 1.58676 2 -1 1 0 8.34841 3.15385 -3 -1 1 0 8.34841 3.15385 1 0 1 0 11.1824 1.62856 2 0 1 0 35.4168 3.10623 1 -1 0 1 24.3140 9.01837 -3 0 1 0 24.3140 9.01837 1 1 1 0 78.8878 5.09905 1 1 1 0 35.6906 5.61250 2 -1 -2 2 734.009 17.7340 -3 2 1 0 734.009 17.7340 1 2 1 0 115.979 12.4750 2 2 1 0 321.524 11.5717 1 -1 -3 3 205.545 22.0254 -3 3 1 0 205.545 22.0254 1 3 1 0 70.9679 13.3273 2 4 1 0 393.014 28.0556 1 4 1 0 127.577 18.5470 2 5 1 0 51.4189 18.2510 2 -1 -6 5 321.806 45.3252 -3 0 -1 12 321.806 45.3252 -2 6 1 0 321.806 45.3252 1 6 1 0 94.9739 21.3173 2 -7 2 0 6.20630 15.6658 1 2 -6 3 191.518 19.6755 -3 -6 2 0 191.518 19.6755 1 -6 2 0 137.580 26.5018 2 -5 2 0 305.272 29.3850 2 2 -5 2 898.955 26.6420 -3 -5 2 0 898.955 26.6420 1 -4 2 0 4.97375 7.95999 1 -4 2 0 3.71372 5.18935 2 -3 2 0 29.1927 7.02606 2 2 -3 1 72.3233 16.8278 -3 -3 2 0 72.3233 16.8278 1 -3 2 0 57.5346 14.9131 1 -2 2 0 1140.28 23.4505 2 -2 2 0 3387.07 39.1842 -3 -2 2 0 3387.07 39.1842 1 -1 2 0 2497.78 31.9820 2 -1 2 0 7494.01 54.8555 1 0 2 0 23.4776 3.48906 2 0 2 0 64.5505 6.81589 1 1 2 0 61.7694 13.4593 2 -2 -1 2 214.124 14.4873 -3 1 2 0 214.124 14.4873 1 -2 -2 3 2082.05 35.8647 -3 2 2 0 2082.05 35.8647 1 2 2 0 513.568 28.2265 2 2 2 0 1945.21 54.0424 1 3 2 0 1253.18 21.1207 1 3 2 0 432.703 30.2048 2 4 2 0 17.7681 11.7498 1 4 2 0 13.4746 13.7109 2 5 2 0 37.8396 16.9531 2 -2 -5 5 -2.1700 33.1552 -3 5 2 0 -2.1700 33.1552 1 6 2 0 17.5064 17.8359 2 -2 -6 6 202.937 43.7924 -3 6 2 0 202.937 43.7924 1 7 2 0 30.5885 21.3179 1 7 2 0 7.29340 21.7699 2 -8 3 0 -19.665 20.5290 2 3 -7 3 168.912 38.0429 -3 -1 3 12 168.912 38.0429 -2 -7 3 0 168.912 38.0429 1 -7 3 0 35.9545 22.2692 2 3 -4 1 80.1754 17.4171 -3 -1 3 6 80.1754 17.4171 -2 -4 3 0 80.1754 17.4171 1 -3 3 0 71.1955 12.6937 -3 -1 3 4 71.1955 12.6937 -2 -3 3 0 71.1955 12.6937 1 -1 3 0 50.6334 13.5279 -2 -1 3 0 50.6334 13.5279 1 -3 0 2 962.701 28.0604 -3 0 3 0 962.701 28.0604 1 0 3 0 2.36804 4.67620 2 -3 -1 3 541.619 33.4304 -3 1 3 0 541.619 33.4304 1 1 3 0 163.596 27.0038 2 1 3 0 443.406 28.6704 1 2 3 0 28.9102 15.7083 2 2 3 0 46.3415 9.15153 1 3 3 0 376.791 18.5566 1 3 3 0 98.0441 20.0355 2 4 3 0 -8.1341 13.0674 2 4 3 0 3.81160 9.95937 1 5 3 0 71.8440 22.7598 2 -3 -5 6 295.281 46.4418 -3 5 3 0 295.281 46.4418 1 6 3 0 3.82526 19.3566 1 6 3 0 1.93774 16.5486 2 7 3 0 42.3812 26.5098 1 7 3 0 9.50541 22.8699 2 -8 4 0 -24.042 16.6968 2 4 -8 3 97.2262 36.3741 -3 -8 4 0 97.2262 36.3741 1 4 -7 2 259.388 30.2016 -3 -7 4 0 259.388 30.2016 1 -7 4 0 116.595 17.3257 2 -6 4 0 52.5763 11.6621 2 4 -6 1 132.698 39.2863 -3 -6 4 0 132.698 39.2863 1 -6 4 0 136.266 24.4516 1 -5 4 0 31.5307 9.98429 2 4 -5 1 102.354 21.4082 -3 -5 4 0 102.354 21.4082 1 -4 4 0 195.040 16.4701 -3 -4 4 0 195.040 16.4701 1 -4 4 0 53.2528 11.0788 2 -4 3 1 2846.18 50.5794 -3 -3 4 0 2846.18 50.5794 1 -3 4 0 841.695 26.3483 2 -2 4 0 255.074 15.0909 2 -2 4 0 697.643 23.9038 1 -4 1 2 230.056 16.9512 -3 -1 4 0 230.056 16.9512 1 -1 4 0 104.005 12.7711 2 0 4 0 0.46674 15.2276 2 0 4 0 167.485 28.7355 1 -4 0 3 246.698 20.8279 -3 0 4 0 246.698 20.8279 1 1 4 0 1929.11 39.0735 1 -4 -3 5 115.844 33.2417 -3 1 -4 8 115.844 33.2417 -2 3 4 0 115.844 33.2417 1 1 -4 10 73.1253 23.7587 -2 4 4 0 73.1253 23.7587 1 -4 -4 6 134.817 40.9881 -3 1 -4 10 134.817 40.9881 -2 4 4 0 134.817 40.9881 1 -4 -6 7 152.354 73.4461 -3 1 -4 14 152.354 73.4461 -2 6 4 0 152.354 73.4461 1 6 4 0 7.47233 21.6275 2 -7 5 0 20.1247 20.9725 2 5 -6 1 58.7237 25.8130 -3 -6 5 0 58.7237 25.8130 1 -6 5 0 4.32759 19.6793 2 -5 5 0 21.4636 9.69497 2 -5 5 0 36.7981 22.9270 -3 -5 5 0 36.7981 22.9270 1 -4 5 0 -3.4690 8.05264 2 -3 5 0 11.8257 8.36749 1 -3 5 0 4.27198 9.67179 2 -2 5 0 20.9859 8.63064 2 -5 2 2 333.701 21.8888 -3 -2 5 0 333.701 21.8888 1 -5 1 3 367.046 21.9457 -3 -1 5 0 367.046 21.9457 1 -1 5 0 95.6560 12.6245 2 0 5 0 22.1353 7.05177 2 0 5 0 133.242 16.6398 1 -5 -1 4 329.938 29.6763 -3 1 5 0 329.938 29.6763 1 1 5 0 276.165 32.8854 1 1 5 0 66.6939 10.7158 2 -5 -2 5 44.6260 38.1151 -3 2 5 0 44.6260 38.1151 1 2 5 0 13.7399 21.3419 2 2 5 0 63.2526 22.0496 1 3 5 0 88.1772 23.4308 1 -5 -3 6 192.545 44.2670 -3 3 5 0 192.545 44.2670 1 3 5 0 50.0656 28.5527 2 4 5 0 85.4599 16.7784 1 5 5 0 14.6245 24.3230 2 6 -7 1 -13.440 36.9215 -3 -2 6 10 -13.440 36.9215 -2 -7 6 0 -13.440 36.9215 1 -6 6 0 128.755 49.9392 -3 -2 6 8 128.755 49.9392 -2 -6 6 0 128.755 49.9392 1 -6 5 1 505.333 36.6297 -3 -2 6 6 505.333 36.6297 -2 -5 6 0 505.333 36.6297 1 -4 6 0 597.196 50.6488 1 -6 3 2 35.9239 33.5162 -3 -3 6 0 35.9239 33.5162 1 -3 6 0 -1.5648 19.7233 2 -2 6 0 18.9820 9.62547 2 -6 2 3 35.9995 19.8984 -3 -2 6 0 35.9995 19.8984 1 -1 6 0 420.056 23.7642 1 -1 6 0 123.788 13.4738 2 -6 0 4 941.241 43.7881 -3 0 6 0 941.241 43.7881 1 0 6 0 686.430 52.4269 1 0 6 0 211.377 15.6659 2 1 6 0 4.24017 7.60514 2 1 6 0 38.9246 19.4735 1 -6 -1 5 46.6344 24.8408 -3 1 6 0 46.6344 24.8408 1 2 6 0 -1.4288 23.4992 2 2 6 0 17.3647 11.8276 1 3 6 0 6.50200 29.7253 2 3 6 0 57.8631 19.2658 1 4 6 0 64.2234 25.4916 1 4 6 0 60.3361 31.9829 2 -6 7 0 -0.5079 27.1312 2 -7 2 11 -28.309 36.8010 -3 -6 7 0 -28.309 36.8010 2 -7 6 1 -9.0194 49.5726 -3 -6 7 0 -9.0194 49.5726 1 -5 7 0 -6.6163 11.7724 2 -5 7 0 -29.171 27.1508 1 -7 4 2 99.2621 34.8756 -3 -2 7 4 99.2621 34.8756 -2 -4 7 0 99.2621 34.8756 1 -7 2 5 -52.399 43.9877 -3 -3 7 0 -52.399 43.9877 2 -7 3 3 166.319 45.1059 -3 -3 7 0 166.319 45.1059 1 -7 3 3 111.135 35.6110 -3 -2 7 2 111.135 35.6110 -2 -3 7 0 111.135 35.6110 1 -2 7 0 69.5998 20.9761 -2 -2 7 0 69.5998 20.9761 1 -7 1 4 -29.814 26.4048 -3 2 -7 2 -29.814 26.4048 -2 -1 7 0 -29.814 26.4048 1 -7 0 5 234.757 31.8631 -3 2 -7 4 234.757 31.8631 -2 0 7 0 234.757 31.8631 1 2 -7 6 0.78169 20.8076 -2 1 7 0 0.78169 20.8076 1 2 -7 8 43.2461 41.2314 -2 2 7 0 43.2461 41.2314 1 -7 -3 7 -56.576 52.5785 -3 2 -7 10 -56.576 52.5785 -2 3 7 0 -56.576 52.5785 1 3 7 0 17.4043 30.5006 2 2 -7 10 25.8774 45.8658 -2 3 7 0 25.8774 45.8658 1 -4 8 0 11.4083 13.9530 2 -8 4 3 45.6265 29.1709 -3 -4 8 0 45.6265 29.1709 1 -3 8 0 4.82996 12.6358 2 -3 8 0 29.5805 14.7971 1 -2 8 0 67.5731 17.8488 2 -2 8 0 273.340 44.2703 1 -1 8 0 24.9235 13.0356 2 -1 8 0 99.9559 30.9858 1 0 8 0 -4.5480 13.6018 1 0 8 0 -0.6575 11.0143 2 1 8 0 21.1721 30.3309 2 1 8 0 33.6591 18.3332 1 -2 -8 1 -8.7909 16.4141 1 -2 -8 1 -0.1235 27.8967 2 -1 -8 1 83.2394 19.3047 1 -1 -8 1 12.4265 29.0294 2 0 -8 1 7.00086 15.9197 1 0 -8 1 3.52962 11.9587 2 1 -8 1 35.0682 13.2780 2 1 -8 1 123.987 38.2239 1 2 -8 1 24.3837 28.3951 2 2 -8 1 12.9835 29.4040 1 -2 8 1 44.4312 59.1196 -2 3 -8 1 44.4312 59.1196 1 -8 4 2 59.5334 31.2725 -3 -2 8 3 59.5334 31.2725 -2 4 -8 1 59.5334 31.2725 1 -7 -3 6 55.1683 39.0653 -3 -3 -7 1 55.1683 39.0653 1 -3 -7 1 42.7259 30.8503 2 -3 -7 1 -11.375 25.5090 1 -2 -7 1 11.6372 12.3245 1 -2 -7 1 -36.302 24.8868 2 -1 -7 1 245.288 22.8392 1 -1 -7 1 80.3736 32.2453 2 0 -7 1 60.8028 12.4957 2 0 -7 1 275.864 43.8566 1 -7 0 4 301.176 32.4057 -3 0 -7 1 301.176 32.4057 1 1 -7 1 -4.5562 8.44777 2 -7 1 3 1.63330 26.3435 -3 1 -7 1 1.63330 26.3435 1 1 -7 1 -18.727 20.4200 1 2 -7 1 -3.2931 9.69759 2 2 -7 1 -1.2257 10.1294 1 -7 3 2 574.261 33.2103 -3 3 -7 1 574.261 33.2103 1 3 -7 1 177.300 19.4838 2 -7 4 1 331.995 31.4330 -3 4 -7 1 331.995 31.4330 1 4 -7 1 132.315 20.6593 2 5 -7 1 -13.258 28.2434 1 5 -7 1 -4.6986 22.1141 2 6 -7 1 14.4355 28.0521 2 -7 6 0 95.9196 65.9910 -3 -2 7 8 95.9196 65.9910 -2 6 -7 1 95.9196 65.9910 1 -6 -5 7 50.1454 68.3539 -3 1 -6 13 50.1454 68.3539 -2 -5 -6 1 50.1454 68.3539 1 1 -6 11 37.2026 40.9679 -2 -4 -6 1 37.2026 40.9679 1 1 -6 9 80.4810 40.5659 -2 -3 -6 1 80.4810 40.5659 1 -3 -6 1 -4.7391 22.6358 2 6 -1 4 103.425 54.1947 -3 -2 -6 1 103.425 54.1947 2 -2 -6 1 245.824 37.0066 1 1 -6 7 245.167 35.2068 -2 -2 -6 1 245.167 35.2068 1 -1 -6 1 26.6091 9.02146 2 -1 -6 1 49.2255 22.3324 1 6 -1 2 80.9214 48.3595 -3 -1 -6 1 80.9214 48.3595 2 -6 -1 4 112.595 30.9357 -3 1 -6 5 112.595 30.9357 -2 -1 -6 1 112.595 30.9357 1 0 -6 1 178.721 36.2242 1 -6 1 0 149.979 47.2076 -3 0 -6 1 149.979 47.2076 2 -6 0 3 271.642 28.8700 -3 0 -6 1 271.642 28.8700 1 1 -6 1 16.5229 20.4503 1 1 -6 1 9.12343 9.27641 2 2 -6 1 34.8608 11.1746 2 -6 2 2 58.5311 40.0781 -3 2 -6 1 58.5311 40.0781 1 -6 3 1 14.2080 18.4862 -3 3 -6 1 14.2080 18.4862 1 3 -6 1 3.98247 8.85887 2 4 -6 1 -12.826 18.7839 1 4 -6 1 -0.7143 9.15880 2 -6 4 0 82.4659 34.3797 -3 4 -6 1 82.4659 34.3797 1 5 -6 1 -3.8183 9.81277 2 -6 5 0 -17.051 26.3317 -3 5 -6 1 -17.051 26.3317 1 6 -6 1 20.1262 32.1132 -3 6 -6 1 20.1262 32.1132 1 6 -6 1 13.5921 11.3917 2 6 -7 2 -6.0152 34.3663 -3 7 -6 1 -6.0152 34.3663 1 7 -6 1 9.64975 12.9426 2 -6 -5 1 23.9945 25.8913 2 -6 -5 1 22.5834 27.8026 1 -5 -5 1 19.9055 26.4891 2 -5 -5 1 46.2479 26.2183 1 -4 -5 1 17.9821 14.1261 1 -4 -5 1 29.3770 23.1037 2 -5 -3 5 167.181 42.1151 -3 -3 -5 1 167.181 42.1151 1 -3 -5 1 137.882 25.8396 1 -3 -5 1 53.7892 28.1518 2 -2 -5 1 151.951 33.0087 2 -2 -5 1 601.378 40.5442 1 -1 -5 1 34.2984 8.22075 2 -5 -1 3 213.781 25.8775 -3 -1 -5 1 213.781 25.8775 1 1 -5 5 191.551 37.3438 -2 -1 -5 1 191.551 37.3438 1 1 -5 3 40.7724 15.8555 -2 0 -5 1 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13 339.253 35.0880 -3 -7 1 1 339.253 35.0880 -2 -1 1 13 339.253 35.0880 1 -1 0 14 72.8984 43.0049 -3 7 -1 1 72.8984 43.0049 -2 0 1 13 72.8984 43.0049 1 -1 -3 16 -74.364 52.0512 -3 7 -1 7 -74.364 52.0512 -2 3 1 13 -74.364 52.0512 1 -6 2 13 1.16302 23.7301 2 -2 5 11 166.366 43.4157 -3 -5 2 13 166.366 43.4157 1 -5 2 13 -11.226 17.6447 2 -4 2 13 -17.351 16.1658 2 -4 2 13 21.8367 16.0553 1 -3 2 13 12.8737 16.2349 2 -2 3 12 38.0703 39.5645 -3 -3 2 13 38.0703 39.5645 1 -2 2 13 68.5217 25.7903 -3 -2 2 13 68.5217 25.7903 1 -2 2 13 1.63648 15.3497 2 -1 2 13 12.3160 16.9214 2 -2 -1 15 162.443 31.4735 -3 7 -2 4 162.443 31.4735 -2 1 2 13 162.443 31.4735 1 -2 -2 16 76.8451 37.6994 -3 7 -2 6 76.8451 37.6994 -2 2 2 13 76.8451 37.6994 1 7 -2 6 77.2936 40.5534 -2 2 2 13 77.2936 40.5534 1 -5 3 13 44.9913 19.1804 1 -3 8 4 -3.1993 40.1944 -3 -5 3 13 -3.1993 40.1944 2 -3 4 12 217.223 32.2312 -3 -4 3 13 217.223 32.2312 1 -3 8 2 43.0163 38.5341 -3 -4 3 13 43.0163 38.5341 2 -3 3 13 356.613 26.5684 -3 -3 3 13 356.613 26.5684 1 -3 3 13 91.6213 22.4806 2 -3 2 14 2.44672 42.4060 -3 -2 3 13 2.44672 42.4060 1 -2 3 13 34.3235 18.2129 2 -1 3 13 19.6261 20.0419 2 -1 3 13 -14.205 21.4945 1 -3 0 15 54.6820 24.2898 -3 0 3 13 54.6820 24.2898 1 0 3 13 14.8286 23.9761 2 1 3 13 50.6903 30.9620 2 -3 -1 16 81.5250 28.1058 -3 1 3 13 81.5250 28.1058 1 -4 4 13 -34.153 30.6823 -3 -8 4 5 -34.153 30.6823 -2 -4 4 13 -34.153 30.6823 1 -4 3 14 127.602 56.9420 -3 -8 4 3 127.602 56.9420 -2 -3 4 13 127.602 56.9420 1 -4 1 15 25.5944 43.2505 -3 -1 4 13 25.5944 43.2505 1 0 4 13 -18.393 20.1631 1 0 4 13 5.81190 26.6460 2 -3 -5 14 42.9414 48.3096 1 -3 -5 14 48.8328 37.1369 2 -2 -5 14 12.3528 39.4127 1 -1 -5 14 -3.1697 33.5790 1 -1 -5 14 -7.1832 27.5810 2 0 -5 14 -5.1176 27.9638 2 0 -5 14 13.8752 34.7880 1 5 -1 11 134.688 70.8642 -3 1 -5 14 134.688 70.8642 1 1 -5 14 -9.6277 28.1319 2 -4 -4 14 135.390 50.5166 1 -3 -4 14 69.5050 38.8964 1 -2 -4 14 7.06276 28.7907 1 -2 -4 14 10.4637 34.0361 2 -1 -4 14 32.5439 30.6605 1 4 0 11 153.770 56.0487 -3 0 -4 14 153.770 56.0487 1 4 -1 12 89.9877 53.9598 -3 1 -4 14 89.9877 53.9598 1 -5 -3 14 -42.497 50.2357 1 -4 -3 14 -21.756 31.1398 2 -4 -3 14 22.4879 36.1248 1 -3 -3 14 -31.097 32.6021 1 -3 -3 14 -3.5025 26.9709 2 -2 -3 14 -12.077 22.5342 2 -2 -3 14 -25.027 27.0682 1 -1 -3 14 -5.6361 22.5785 2 0 -3 14 -23.110 30.6765 2 1 -3 14 18.5183 24.3252 1 1 -3 14 -4.7098 24.5939 2 3 -3 14 50.6805 57.3309 -3 6 3 5 50.6805 57.3309 -2 3 -3 14 50.6805 57.3309 1 -5 -2 14 185.544 46.7496 1 -4 -2 14 -15.725 30.3314 1 -3 -2 14 11.1121 28.3276 1 2 2 11 228.227 49.0252 -3 -2 -2 14 228.227 49.0252 1 -2 -2 14 11.0095 21.9268 2 2 1 12 341.233 51.5382 -3 -1 -2 14 341.233 51.5382 1 -1 -2 14 98.5785 25.8294 2 0 -2 14 10.7262 21.9485 2 0 -2 14 15.7400 23.7860 1 1 -2 14 16.0126 25.3647 2 2 -2 14 68.5537 36.2164 -3 2 -2 14 68.5537 36.2164 1 2 -2 14 -11.688 26.6712 2 2 -3 15 180.998 54.3875 -3 3 -2 14 180.998 54.3875 1 3 -2 14 64.6620 36.3890 2 -5 -1 14 -9.6398 31.5804 1 -7 -1 8 32.5452 51.4869 -2 -4 -1 14 32.5452 51.4869 1 1 3 11 1.65935 51.3437 -3 -7 -1 6 1.65935 51.3437 -2 -3 -1 14 1.65935 51.3437 1 1 2 12 59.1049 48.0914 -3 -7 -1 4 59.1049 48.0914 -2 -2 -1 14 59.1049 48.0914 1 -7 -1 2 1.03646 35.3265 -2 -1 -1 14 1.03646 35.3265 1 2 -1 14 -24.080 25.9602 2 1 -2 15 -13.234 44.1718 -3 2 -1 14 -13.234 44.1718 1 3 -1 14 12.5619 35.9243 2 3 -1 14 7.35968 26.8079 1 -5 0 14 15.1098 23.4098 1 -5 0 14 28.1574 25.3582 2 0 4 11 41.7619 44.3253 -3 -4 0 14 41.7619 44.3253 1 -3 0 14 120.372 26.1670 2 0 3 12 367.826 48.5202 -3 -3 0 14 367.826 48.5202 1 -2 0 14 77.8054 24.1056 2 -2 0 14 142.109 31.3005 1 2 0 14 32.9494 26.3360 1 0 -3 16 43.3986 48.0231 -3 3 0 14 43.3986 48.0231 1 -1 5 11 105.928 40.6102 -3 -5 1 14 105.928 40.6102 1 -5 1 14 32.3151 22.3079 2 -4 1 14 11.8077 19.0596 2 -1 4 12 88.7108 43.3561 -3 -4 1 14 88.7108 43.3561 1 -3 1 14 -2.7558 16.8170 1 -3 1 14 13.8004 19.0622 2 -1 1 14 20.5147 30.7396 -3 -1 1 14 20.5147 30.7396 1 -1 0 15 106.473 38.8759 -3 0 1 14 106.473 38.8759 1 1 1 14 16.2760 22.1191 1 1 1 14 23.8978 25.0906 2 2 1 14 71.0043 34.7671 2 -1 -2 16 156.864 40.2004 -3 2 1 14 156.864 40.2004 1 -2 5 12 117.361 49.8546 -3 -8 2 8 117.361 49.8546 -2 -5 2 14 117.361 49.8546 1 -2 2 14 -53.895 48.1146 -3 -8 2 2 -53.895 48.1146 -2 -2 2 14 -53.895 48.1146 1 -2 2 14 5.22635 23.4039 -3 -2 2 14 5.22635 23.4039 1 0 2 14 125.889 23.3497 1 -2 0 15 95.0798 44.8167 -3 0 2 14 95.0798 44.8167 1 -2 -1 16 134.164 36.8332 -3 1 2 14 134.164 36.8332 1 -4 3 14 4.78357 19.8915 2 -3 3 14 32.8366 23.7923 -3 -3 3 14 32.8366 23.7923 1 -3 3 14 15.9592 17.0870 2 -3 3 14 82.8130 40.7727 -3 -8 3 3 82.8130 40.7727 -2 -3 3 14 82.8130 40.7727 1 -3 2 15 -46.803 47.2726 -3 -8 3 1 -46.803 47.2726 -2 -2 3 14 -46.803 47.2726 1 -3 2 15 12.1768 44.0311 -3 -2 3 14 12.1768 44.0311 1 3 -8 2 98.2360 36.4440 -3 -2 3 14 98.2360 36.4440 2 -1 3 14 6.74157 26.9302 1 -3 0 16 77.6836 41.4947 -3 0 3 14 77.6836 41.4947 1 -3 -4 15 -30.190 39.7499 1 -3 -4 15 -55.879 33.9508 2 -2 -4 15 16.8037 30.2328 2 -2 -4 15 -26.032 29.5769 1 -1 -4 15 11.4518 32.3291 1 -1 -4 15 -28.790 27.2373 2 0 -4 15 6.05097 25.7295 2 4 0 12 -15.521 58.2217 -3 0 -4 15 -15.521 58.2217 1 4 -1 13 -34.182 58.3268 -3 1 -4 15 -34.182 58.3268 1 1 -4 15 -1.4293 29.5086 2 -7 -3 9 93.9390 57.5152 -2 -4 -3 15 93.9390 57.5152 1 -7 -3 7 41.0219 52.4603 -2 -3 -3 15 41.0219 52.4603 1 -7 -3 5 246.736 51.1378 -2 -2 -3 15 246.736 51.1378 1 3 1 12 18.6123 60.4573 -3 -7 -3 3 18.6123 60.4573 -2 -1 -3 15 18.6123 60.4573 1 -3 -7 6 29.1769 52.2556 -3 0 -3 15 29.1769 52.2556 2 1 -3 15 6.79725 28.8551 1 -3 -7 8 44.4116 60.3169 -3 1 -3 15 44.4116 60.3169 2 3 -2 14 22.2108 60.7792 -3 2 -3 15 22.2108 60.7792 1 2 -3 15 65.6163 33.2871 2 -4 -2 15 -38.647 29.8139 2 -4 -2 15 -4.6997 35.9057 1 -3 -2 15 17.4382 25.7384 2 -3 -2 15 -11.320 28.7978 1 -2 -2 15 -43.680 23.6727 2 2 1 13 -22.367 46.0724 -3 -1 -2 15 -22.367 46.0724 1 -1 -2 15 15.7585 24.6311 2 0 -2 15 56.9375 26.7618 1 0 -2 15 16.3453 23.6986 2 2 -1 14 -28.164 49.2749 -3 1 -2 15 -28.164 49.2749 1 1 -2 15 -32.134 26.9559 2 2 -2 15 56.5382 39.4550 -3 2 -2 15 56.5382 39.4550 1 -5 -1 15 1.73924 31.3697 2 -5 -1 15 37.8052 37.1445 1 -4 -1 15 181.184 44.7827 1 -4 -1 15 61.9643 28.1435 2 -3 -1 15 71.2875 27.2943 2 -2 -1 15 59.1720 25.0729 2 1 2 13 78.6279 47.6019 -3 -2 -1 15 78.6279 47.6019 1 -1 -1 15 -22.329 22.5839 2 -1 -1 15 20.6619 25.6301 1 1 0 14 141.736 52.0131 -3 0 -1 15 141.736 52.0131 1 0 -1 15 34.4313 27.3265 2 1 -1 15 87.8799 30.3868 -3 1 -1 15 87.8799 30.3868 1 1 -1 15 39.7230 27.6330 2 2 -1 15 1.89250 32.5168 2 2 -1 15 18.3268 27.2653 1 -5 0 15 22.3561 36.5585 1 0 8 3 94.3997 57.9422 -3 -5 0 15 94.3997 57.9422 2 0 4 12 22.8520 55.1546 -3 -8 0 7 22.8520 55.1546 -2 -4 0 15 22.8520 55.1546 1 0 3 13 59.5720 45.5804 -3 -3 0 15 59.5720 45.5804 1 -2 0 15 4.54960 23.1507 1 -2 0 15 21.0567 23.1083 2 0 1 14 125.333 42.1026 -3 -1 0 15 125.333 42.1026 1 -1 0 15 38.0957 23.6562 2 0 0 15 -2.6477 22.7379 -3 0 0 15 -2.6477 22.7379 1 1 0 15 56.5270 31.2705 2 0 -1 16 -41.380 45.9061 -3 1 0 15 -41.380 45.9061 1 -1 4 13 278.093 60.3518 -3 -8 1 6 278.093 60.3518 -2 -4 1 15 278.093 60.3518 1 -1 4 13 70.7183 46.6676 -3 -4 1 15 70.7183 46.6676 1 -4 1 15 37.8326 20.3698 2 -3 1 15 18.4647 21.3905 2 -3 1 15 -23.873 23.2439 1 -1 2 14 54.2112 42.0056 -3 -2 1 15 54.2112 42.0056 1 -1 1 15 138.447 29.5057 -3 -1 1 15 138.447 29.5057 1 -1 0 16 61.7452 44.9191 -3 0 1 15 61.7452 44.9191 1 8 -1 3 -29.821 41.5565 -2 1 1 15 -29.821 41.5565 1 -4 2 15 10.6922 17.4855 1 -4 2 15 44.2218 23.0069 2 -2 3 14 112.814 49.6125 -3 -3 2 15 112.814 49.6125 1 -3 2 15 2.15315 20.0425 2 -2 2 15 16.2222 20.7773 2 -2 2 15 18.8841 18.0022 -3 -2 2 15 18.8841 18.0022 1 -2 1 16 106.777 48.2249 -3 -1 2 15 106.777 48.2249 1 -1 2 15 15.2191 23.5849 2 0 2 15 11.5582 19.1345 1 -2 -3 16 -14.183 33.9626 1 -2 -3 16 -0.3078 29.8921 2 -1 -3 16 30.9647 30.8558 2 3 1 13 104.255 61.5284 -3 -1 -3 16 104.255 61.5284 1 0 -3 16 14.5490 31.1674 2 3 0 14 86.5626 54.2322 -3 0 -3 16 86.5626 54.2322 1 -2 -8 1 -10.989 57.1344 -3 -3 -2 16 -10.989 57.1344 2 -3 -2 16 -24.191 36.4442 1 -2 -8 3 41.9634 57.3091 -3 -2 -2 16 41.9634 57.3091 2 2 1 14 14.6182 54.5330 -3 -1 -2 16 14.6182 54.5330 1 -1 -2 16 11.4934 27.7945 2 0 -2 16 21.1917 29.2917 2 0 -2 16 56.9143 32.3238 1 1 3 13 1.35488 57.7666 -3 -3 -1 16 1.35488 57.7666 1 1 2 14 16.4875 53.0443 -3 -2 -1 16 16.4875 53.0443 1 -8 -1 2 57.7947 46.2145 -2 -1 -1 16 57.7947 46.2145 1 -3 0 16 9.48136 25.3326 2 0 3 14 -10.904 51.3264 -3 -3 0 16 -10.904 51.3264 1 -2 0 16 25.4579 25.6274 2 -2 0 16 196.261 40.3581 1 0 0 16 -46.995 47.7778 -3 8 0 1 -46.995 47.7778 -2 0 0 16 -46.995 47.7778 1 -3 1 16 4.13732 22.6885 2 -3 1 16 -45.677 25.7509 1 -2 1 16 12.4325 24.0043 2 -1 2 15 96.7248 47.8242 -3 -2 1 16 96.7248 47.8242 1 -1 1 16 23.6610 26.2813 -3 -1 1 16 23.6610 26.2813 1 -1 1 16 -11.948 25.1047 2 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 35131 _shelx_res_file ; TITL a_a.res in P-1 twin5.res created by SHELXL-2016/6 at 23:43:18 on 30-Apr-2021 CELL 0.71073 6.0767 6.1886 11.7269 97.5115 100.3445 99.4368 ZERR 2.000 0.0010 0.0011 0.0020 0.0060 0.0058 0.0061 LATT 1 SFAC C H N I UNIT 2 10 4 6 TEMP -163.150 L.S. 10 BOND $h conf htab isor 0.005 c1 omit -4 58 size 0.257 0.187 0.08 acta LIST 4 FMAP 2 PLAN 20 WGHT 0.080300 4.475700 BASF 0.21100 0.15788 FVAR 0.43101 I1 4 1.000000 0.000000 0.500000 10.50000 0.02678 0.02392 = 0.02695 0.00010 0.00488 0.00692 C1 1 0.514796 0.307465 0.216222 11.00000 0.01953 0.02269 = 0.02645 -0.00190 0.00589 0.00912 AFIX 43 H1A 2 0.481532 0.352625 0.141658 11.00000 -1.20000 AFIX 0 N1 3 0.371611 0.157013 0.238491 11.00000 0.04732 0.02899 = 0.06962 -0.00331 0.00366 0.00492 AFIX 93 H1B 2 0.396378 0.110694 0.306643 11.00000 -1.20000 H1C 2 0.246338 0.097725 0.185971 11.00000 -1.20000 AFIX 0 I2 4 0.721353 0.299874 0.586924 11.00000 0.03244 0.02974 = 0.03382 -0.00124 0.00838 0.01131 N2 3 0.704624 0.406499 0.286655 11.00000 0.03596 0.05498 = 0.02477 0.01093 0.01513 0.00925 AFIX 93 H2A 2 0.741417 0.369243 0.356493 11.00000 -1.20000 H2B 2 0.796631 0.510952 0.264606 11.00000 -1.20000 AFIX 0 I3 4 1.000000 0.500000 1.000000 10.50000 0.02972 0.02101 = 0.02756 0.00330 0.00666 0.00713 I4 4 0.782543 0.840725 1.105145 11.00000 0.03765 0.02619 = 0.03281 0.00179 0.01068 0.01284 HKLF 5 REM a_a.res in P-1 REM R1 = 0.0844 for 2217 Fo > 4sig(Fo) and 0.1522 for all 4015 data REM 60 parameters refined using 6 restraints END WGHT 0.0960 0.0000 REM Instructions for potential hydrogen bonds EQIV $3 -x+1, -y+1, -z+1 HTAB C1 I4_$3 EQIV $4 -x+1, -y, -z+1 HTAB N1 I2_$4 EQIV $5 x-1, y-1, z-1 HTAB N1 I4_$5 HTAB N2 I2 EQIV $6 -x+2, -y+1, -z+1 HTAB N2 I2_$6 EQIV $7 x, y, z-1 HTAB N2 I4_$7 REM Highest difference peak 2.452, deepest hole -2.520, 1-sigma level 0.553 Q1 1 0.9921 0.4315 1.0813 11.00000 0.05 2.45 Q2 1 0.6391 0.8220 1.0440 11.00000 0.05 2.37 Q3 1 1.0689 0.6628 1.0029 11.00000 0.05 2.25 Q4 1 0.8104 0.4077 0.5534 11.00000 0.05 2.23 Q5 1 0.8177 0.9007 1.0608 11.00000 0.05 2.16 Q6 1 0.3526 0.3607 0.0759 11.00000 0.05 2.11 Q7 1 0.6925 0.7282 0.9973 11.00000 0.05 2.01 Q8 1 1.1707 0.5522 1.0383 11.00000 0.05 1.94 Q9 1 0.7034 0.2228 0.6617 11.00000 0.05 1.93 Q10 1 0.4373 0.1878 0.3141 11.00000 0.05 1.85 Q11 1 0.7165 0.2302 0.0368 11.00000 0.05 1.84 Q12 1 0.7083 0.3767 0.1317 11.00000 0.05 1.78 Q13 1 0.9967 -0.0783 0.5797 11.00000 0.05 1.78 Q14 1 0.5466 -0.0226 0.3851 11.00000 0.05 1.74 Q15 1 0.1876 0.3921 0.1146 11.00000 0.05 1.73 Q16 1 0.5738 0.5998 0.3203 11.00000 0.05 1.71 Q17 1 0.8865 0.2808 0.6957 11.00000 0.05 1.65 Q18 1 1.0006 0.4310 0.2468 11.00000 0.05 1.65 Q19 1 0.6171 0.3128 0.5404 11.00000 0.05 1.60 Q20 1 0.5765 0.9749 1.0294 11.00000 0.05 1.59 ; _shelx_res_checksum 32747 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I I1 1.000000 0.000000 0.500000 0.0261(5) Uani d 1 . . C C1 0.515(3) 0.307(3) 0.216(2) 0.023(4) Uani d 1 . . H H1A 0.481532 0.352625 0.141658 0.027 Uiso calc 1 . . N N1 0.372(4) 0.157(3) 0.238(2) 0.051(7) Uani d 1 . . H H1B 0.396378 0.110694 0.306643 0.061 Uiso calc 1 . . H H1C 0.246338 0.097725 0.185971 0.061 Uiso calc 1 . . I I2 0.7214(3) 0.2999(2) 0.58692(14) 0.0318(5) Uani d 1 . . N N2 0.705(3) 0.406(4) 0.2867(17) 0.037(5) Uani d 1 . . H H2A 0.741417 0.369243 0.356493 0.044 Uiso calc 1 . . H H2B 0.796631 0.510952 0.264606 0.044 Uiso calc 1 . . I I3 1.000000 0.500000 1.000000 0.0258(5) Uani d 1 . . I I4 0.7825(3) 0.8407(2) 1.10514(14) 0.0313(4) Uani d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I1 0.0268(11) 0.0239(9) 0.0270(11) 0.0069(8) 0.0049(8) 0.0001(9) C1 0.020(6) 0.023(6) 0.026(7) 0.009(5) 0.006(5) -0.002(5) N1 0.047(14) 0.029(11) 0.070(18) 0.005(10) 0.004(12) -0.003(12) I2 0.0324(8) 0.0297(8) 0.0338(10) 0.0113(6) 0.0084(7) -0.0012(7) N2 0.036(12) 0.055(13) 0.025(11) 0.009(10) 0.015(9) 0.011(10) I3 0.0297(11) 0.0210(9) 0.0276(11) 0.0071(8) 0.0067(8) 0.0033(8) I4 0.0377(9) 0.0262(7) 0.0328(9) 0.0128(6) 0.0107(7) 0.0018(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' I I -0.4742 1.8119 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag I2 I1 I2 . 2_756 180.0 ? N1 C1 N2 . . 125(3) ? N1 C1 H1A . . 117.3 ? N2 C1 H1A . . 117.3 ? C1 N1 H1B . . 120.0 ? C1 N1 H1C . . 120.0 ? H1B N1 H1C . . 120.0 ? C1 N2 H2A . . 120.0 ? C1 N2 H2B . . 120.0 ? H2A N2 H2B . . 120.0 ? I4 I3 I4 . 2_767 180.0 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag I1 I2 . 2.9165(14) ? I1 I2 2_756 2.9165(14) ? C1 N1 . 1.25(3) ? C1 N2 . 1.30(3) ? C1 H1A . 0.9500 ? N1 H1B . 0.8800 ? N1 H1C . 0.8800 ? N2 H2A . 0.8800 ? N2 H2B . 0.8800 ? I3 I4 . 2.9209(14) ? I3 I4 2_767 2.9209(14) ? _cod_database_fobs_code 2243851