############################################################################## # # # This CIF contains the data in a paper accepted for publication in # # Acta Crystallographica Section E. It conforms to the requirements of # # Notes for Authors for Acta Crystallographica Section E, and has been # # peer reviewed under the auspices of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. # # # # Software is freely available for graphical display of the structure(s) # # in this CIF. For information consult the CIF software page # # http://www.iucr.org/resources/cif/software. # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_global _audit_creation_method 'from SHELXL97 CIF aIt is very nd IUCr SHELXL97-template' _journal_date_recd_electronic 2017-03-09 _journal_date_accepted 2017-03-16 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2017 _journal_volume 73 _journal_issue 4 _journal_page_first 569 _journal_page_last 572 _journal_paper_category GO _journal_paper_doi 10.1107/S205698901700425X _journal_coeditor_code LH5840 _publ_contact_author_name 'Alexey B. Tarasov' _publ_contact_author_address ; Faculty of Materials Science, Lomonosov Moscow State University, Lenin Hills, 119991 Moscow, Russia ; _publ_contact_author_email 'alexey.bor.tarasov@gmail.com' _publ_contact_author_fax '+7-495-4339588' _publ_contact_author_phone '+7-495-9550976' _publ_section_title ; Formamidinium iodide: crystal structure and phase transitions ; _publ_section_title_footnote . loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Andrey A. Petrov' . ; Department of Materials Science, Lomonosov Moscow State University, Lenin Hills, 119991 Moscow, Russian Federation ; 'Eugene A. Goodilin' . ; Department of Materials Science, Lomonosov Moscow State University, Lenin Hills, 119991 Moscow, Russian Federation Department of Chemistry, Lomonosov Moscow State University, Lenin Hills, 119991 Moscow, Russian Federation ; 'Alexey B. Tarasov' . ; Department of Materials Science, Lomonosov Moscow State University, Lenin Hills, 119991 Moscow, Russian Federation Department of Chemistry, Lomonosov Moscow State University, Lenin Hills, 119991 Moscow, Russian Federation ; 'Vladimir A. Lazarenko' . ; National Research Centre `Kurchatov Institute', 1 Acad. Kurchatov Sq., Moscow 123182, Russian Federation ; 'Pavel V. Dorovatovskii' . ; National Research Centre `Kurchatov Institute', 1 Acad. Kurchatov Sq., Moscow 123182, Russian Federation ; 'Victor N. Khrustalev' . ; Inorganic Chemistry Department, Peoples' Friendship University of Russia (RUDN University), 6 Miklukho-Maklay St., Moscow 117198, Russian Federation X-Ray Structural Centre, A.N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, 28 Vavilov St., B-334, Moscow 119991, Russian Federation ; _publ_section_synopsis ; Crystal structure, thermal behaviour and phase transitions of formamidinium iodide were studied by DTG, DSC, powder diffraction and X-ray crystallography. ; data_I _audit_creation_method SHELXL-2015 _chemical_name_systematic ; Formamidinium iodide ; _chemical_name_common ? _chemical_formula_moiety 'C H5 N2 +, I -' _chemical_formula_sum 'C H5 I N2' _chemical_formula_iupac 'C H5 N2 +, I -' _chemical_formula_weight 171.97 _chemical_melting_point ? _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. ; _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 4.8211(6) _cell_length_b 13.776(3) _cell_length_c 7.0113(10) _cell_angle_alpha 90 _cell_angle_beta 98.06(3) _cell_angle_gamma 90 _cell_volume 461.06(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 600 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 36.0 _cell_measurement_temperature 100(2) _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 2.477 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 312 _exptl_absorpt_coefficient_mu 15.384 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (Scala; Evans, 2006) ; _shelx_estimated_absorpt_T_min 0.442 _shelx_estimated_absorpt_T_max 0.641 _exptl_absorpt_correction_T_min 0.400 _exptl_absorpt_correction_T_max 0.600 _diffrn_ambient_temperature 100(2) _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.96990 _diffrn_measurement_device_type 'Rayonix SX165 CCD' _diffrn_measurement_method '\f scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5111 _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_theta_min 4.037 _diffrn_reflns_theta_max 38.506 _diffrn_reflns_theta_full 35.587 _diffrn_measured_fraction_theta_max 0.929 _diffrn_measured_fraction_theta_full 0.968 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _refine_special_details ? _reflns_number_total 949 _reflns_number_gt 894 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_gt 0.0920 _refine_ls_wR_factor_ref 0.0930 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_number_reflns 949 _refine_ls_number_parameters 38 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+0.7865P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.867 _refine_diff_density_min -0.913 _refine_ls_extinction_method ; SHELXL2014 (Sheldrick, 2015b) ; _refine_ls_extinction_coef 0.0064(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0070 0.0030 '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' 0.0130 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.0340 3.1360 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; Marccd (Doyle, 2011) ; _computing_cell_refinement ; iMosflm (Battye et al., 2011) ; _computing_data_reduction ; iMosflm (Battye et al., 2011) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015b) ; _computing_molecular_graphics ; SHELXTL (Sheldrick, 2008) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) ; 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 0.86658(6) 0.38577(2) 0.20022(5) 0.0218(2) Uani d 1 . . N N1 0.6120(9) 0.4171(3) 0.6569(7) 0.0250(10) Uani d 1 . . H H1A 0.7250 0.4174 0.5650 0.030 Uiso d 1 . . H H1B 0.6251 0.4648 0.7454 0.030 Uiso d 1 . . N N2 0.2540(9) 0.3389(3) 0.7860(7) 0.0254(11) Uani d 1 . . H H2A 0.1352 0.2882 0.7776 0.030 Uiso d 1 . . H H2B 0.2515 0.3832 0.8801 0.030 Uiso d 1 . . C C1 0.4296(11) 0.3478(4) 0.6606(8) 0.0227(11) Uani d 1 . . H H1 0.4233 0.2994 0.5637 0.027 Uiso calc 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 0.0230(3) 0.0215(3) 0.0217(4) 0.00012(9) 0.0054(2) -0.00041(10) N1 0.022(2) 0.030(2) 0.023(3) -0.0030(18) 0.0030(19) 0.000(2) N2 0.021(2) 0.022(2) 0.034(3) -0.0020(17) 0.008(2) 0.0011(19) C1 0.023(2) 0.026(3) 0.019(3) 0.002(2) 0.001(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N1 C1 . 1.301(7) ? N1 H1A . 0.9001 ? N1 H1B . 0.9001 ? N2 C1 . 1.309(8) ? N2 H2A . 0.8999 ? N2 H2B . 0.9000 ? C1 H1 . 0.9500 ? 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 C1 N1 H1A . . 119.7 ? C1 N1 H1B . . 120.3 ? H1A N1 H1B . . 120.0 ? C1 N2 H2A . . 119.7 ? C1 N2 H2B . . 120.3 ? H2A N2 H2B . . 120.0 ? N1 C1 N2 . . 125.8(5) ? N1 C1 H1 . . 117.1 ? N2 C1 H1 . . 117.1 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H1A I1 . 0.90 2.77 3.612(5) 156 N2 H2A I1 4_466 0.90 2.74 3.622(4) 166 _shelx_hkl_file ; 0 0 1 6.70 1.13 0 0 1 1.32 1.15 0 0 -1 1.41 1.15 0 0 3 0.57 0.85 0 0 3 0.19 1.22 0 0 3 1.87 2.02 0 0 -3 1.10 0.79 0 0 -3 11.35 3.68 0 0 4 405.66 59.10 0 0 4 406.07 59.10 0 0 4 370.22 79.13 0 0 -4 273.20 39.78 0 0 -4 399.51 85.37 0 0 5 -4.75 2.45 0 0 5 -0.44 1.55 0 0 5 -0.59 3.53 0 0 -5 1.37 1.65 0 0 -5 -0.98 3.33 0 0 6 385.09 56.50 0 0 6 400.50 58.44 0 0 6 388.81 83.92 0 0 -6 338.01 49.40 0 0 -6 578.21 123.66 0 0 7 1.41 3.91 0 0 -7 0.08 6.17 0 -1 0 1.12 0.35 0 -1 0 0.59 0.94 0 1 0 0.88 0.31 0 1 0 0.51 0.88 0 -1 1 266.18 38.65 0 -1 1 241.70 35.07 0 -1 1 222.37 47.46 0 -1 -1 283.37 41.18 0 -1 -1 344.70 73.39 0 1 1 234.88 34.17 0 1 1 307.86 65.54 0 1 -1 250.54 36.37 0 1 -1 272.67 39.57 0 1 -1 270.93 57.78 0 -1 2 2314.10 335.41 0 -1 2 1823.03 264.20 0 -1 2 1957.26 415.08 0 -1 -2 1961.81 284.31 0 -1 -2 2478.89 525.77 0 1 2 1972.95 286.05 0 1 2 2395.87 508.00 0 1 -2 1981.21 287.12 0 1 -2 2377.70 504.29 0 -1 3 1719.78 249.34 0 -1 3 1923.81 278.95 0 -1 3 1744.56 370.18 0 -1 -3 2290.97 486.11 0 -1 -3 2054.32 297.78 0 1 3 1811.88 262.84 0 1 3 1868.87 270.93 0 1 3 2119.99 449.77 0 1 -3 1913.48 277.33 0 1 -3 2327.73 493.96 0 -1 4 2042.34 296.17 0 -1 4 1866.40 270.68 0 -1 4 1886.63 400.41 0 -1 -4 1915.55 277.71 0 -1 -4 2408.27 511.31 0 1 4 2150.55 311.95 0 1 4 2178.22 315.91 0 1 4 2404.96 510.07 0 1 -4 1932.89 280.14 0 1 -4 2209.20 468.76 0 -1 5 2107.59 305.71 0 -1 5 2058.86 298.65 0 -1 5 1816.42 385.63 0 -1 -5 1874.65 271.84 0 -1 -5 2585.03 548.48 0 1 5 1879.20 272.58 0 1 5 2277.75 330.45 0 1 5 1979.15 420.03 0 1 -5 2307.49 334.50 0 1 -5 2328.97 494.37 0 -1 6 712.03 103.58 0 -1 6 628.19 91.65 0 -1 6 712.86 152.40 0 -1 -6 661.64 96.23 0 -1 -6 889.62 189.69 0 1 6 685.18 99.70 0 1 6 673.62 98.30 0 1 6 645.13 137.95 0 1 -6 800.41 116.35 0 1 -6 949.10 202.25 0 -1 7 809.92 118.04 0 -1 -7 1118.02 238.31 0 1 7 695.51 101.39 0 1 -7 999.49 213.16 0 -2 0 132.41 19.31 0 -2 0 100.98 21.86 0 2 0 139.85 20.39 0 2 0 126.05 27.18 0 -2 1 3578.33 758.70 0 -2 -1 4324.22 626.95 0 2 1 3971.11 575.32 0 -2 2 59.43 8.78 0 -2 2 53.82 7.90 0 -2 2 69.43 15.37 0 -2 -2 49.19 7.40 0 -2 -2 99.70 21.85 0 2 2 57.37 8.58 0 2 2 67.49 14.83 0 2 -2 53.28 7.83 0 2 -2 50.39 7.46 0 2 -2 62.65 13.99 0 -2 3 2039.86 295.80 0 -2 3 2136.51 309.68 0 -2 3 2145.60 455.13 0 -2 -3 2073.72 300.67 0 -2 -3 3463.51 734.75 0 2 3 1953.55 283.28 0 2 3 2497.06 529.90 0 2 -3 2096.03 303.89 0 2 -3 2149.73 455.96 0 -2 4 0.76 1.34 0 -2 4 0.11 0.98 0 -2 4 3.19 3.18 0 -2 -4 4.72 3.21 0 -2 -4 0.60 1.28 0 2 4 2.01 1.39 0 2 4 1.69 2.02 0 2 4 0.40 2.71 0 2 -4 0.00 0.86 0 2 -4 0.61 2.27 0 -2 5 31.47 5.08 0 -2 5 35.81 6.05 0 -2 5 63.31 15.05 0 -2 -5 33.45 5.55 0 -2 -5 47.79 11.96 0 2 5 36.99 6.06 0 2 5 43.86 7.50 0 2 5 37.71 9.80 0 2 -5 32.26 5.08 0 2 -5 37.14 9.28 0 -2 6 14.30 4.49 0 -2 6 10.90 3.09 0 -2 6 8.31 8.48 0 -2 -6 5.76 3.09 0 -2 -6 14.89 7.13 0 2 6 16.83 5.96 0 2 6 13.16 3.22 0 2 6 7.64 8.18 0 2 -6 8.93 3.01 0 2 -6 13.18 4.99 0 -2 7 403.76 59.27 0 -2 -7 508.83 109.66 0 2 7 390.29 57.20 0 2 -7 481.16 103.29 0 -3 0 1.74 0.83 0 -3 0 0.11 2.15 0 3 0 4.00 1.00 0 3 0 0.18 2.16 0 -3 1 189.28 27.55 0 -3 1 234.14 34.02 0 -3 1 169.70 36.55 0 -3 -1 164.21 35.44 0 -3 -1 156.65 22.91 0 3 1 238.85 51.13 0 3 1 254.08 37.04 0 3 -1 217.78 31.69 0 3 -1 129.98 28.22 0 3 -1 210.80 45.27 0 -3 2 3287.56 476.61 0 -3 2 3157.06 669.49 0 -3 -2 2905.94 421.27 0 -3 -2 3330.52 706.66 0 3 2 2519.37 365.22 0 3 2 3891.39 825.20 0 3 -2 3107.08 450.19 0 3 -2 3191.75 462.57 0 3 -2 2716.79 576.56 0 -3 3 1242.75 180.28 0 -3 3 1218.80 176.68 0 -3 3 1119.67 237.82 0 -3 -3 1507.08 320.09 0 -3 -3 1780.07 258.21 0 3 3 1822.21 386.62 0 3 3 1194.84 173.38 0 3 -3 1006.92 146.00 0 3 -3 1197.73 173.67 0 3 -3 1523.19 323.43 0 -3 4 3452.36 500.57 0 -3 4 3586.17 519.98 0 -3 4 3346.63 709.97 0 -3 -4 3975.65 843.37 0 -3 -4 3102.12 449.77 0 3 4 4287.06 909.04 0 3 4 3514.72 509.66 0 3 -4 3660.52 530.72 0 3 -4 4295.31 910.69 0 -3 5 1291.90 187.46 0 -3 5 1315.03 190.81 0 -3 5 1049.47 223.32 0 -3 -5 951.17 138.16 0 -3 -5 1462.06 310.96 0 3 5 1437.69 208.78 0 3 5 1429.85 303.89 0 3 5 1008.57 146.54 0 3 -5 1264.64 183.38 0 3 -5 1472.38 312.86 0 -3 6 1241.93 180.32 0 -3 6 1204.75 174.99 0 -3 -6 1735.47 369.06 0 3 6 1211.36 175.98 0 3 6 1063.91 226.66 0 3 -6 1351.79 196.10 0 3 -6 1442.24 306.58 0 -3 7 360.10 52.87 0 -3 -7 596.80 128.45 0 3 7 443.58 64.93 0 3 -7 572.02 122.50 0 -4 0 7838.95 1661.55 0 -4 1 884.67 128.37 0 -4 -1 602.58 87.56 0 -4 -1 645.54 137.50 0 4 1 1027.99 149.10 0 4 1 1125.87 239.22 0 4 -1 977.59 141.83 0 4 -1 1115.13 236.99 0 4 -1 773.98 164.75 0 -4 2 5530.22 801.24 0 -4 2 5369.15 1138.26 0 -4 -2 4452.26 645.13 0 -4 -2 5815.19 1233.67 0 4 2 4728.98 685.60 0 4 2 8830.18 1872.17 0 4 -2 6013.44 871.45 0 4 -2 5439.36 1153.13 0 4 -2 4505.95 955.71 0 -4 3 275.31 40.02 0 -4 3 294.97 42.91 0 -4 3 320.46 68.85 0 -4 -3 307.49 44.85 0 -4 -3 353.86 75.91 0 4 3 296.25 43.28 0 4 3 367.04 78.43 0 4 -3 262.67 38.19 0 4 -3 273.66 58.69 0 -4 4 330.70 48.12 0 -4 4 308.97 44.94 0 -4 4 245.83 52.91 0 -4 -4 305.05 44.52 0 -4 -4 351.31 75.46 0 4 4 323.97 47.33 0 4 4 335.57 71.82 0 4 -4 305.46 44.40 0 4 -4 239.47 51.50 0 -4 5 11.33 2.63 0 -4 5 7.69 1.99 0 -4 5 16.83 7.83 0 -4 -5 13.29 5.94 0 -4 -5 9.90 2.99 0 4 5 4.59 4.27 0 4 5 10.04 2.58 0 4 5 15.09 6.54 0 4 -5 8.45 1.88 0 4 -5 14.21 4.87 0 -4 6 236.12 34.56 0 -4 6 242.81 35.65 0 -4 -6 385.79 83.22 0 4 6 242.32 35.67 0 4 -6 338.71 72.86 0 -4 -7 68.77 19.66 0 4 7 40.41 7.11 0 4 -7 51.38 13.32 0 -5 0 0.81 0.88 0 -5 0 -0.53 2.51 0 5 0 -1.05 0.93 0 5 0 2.38 3.47 0 -5 1 354.52 51.59 0 -5 -1 277.91 40.55 0 -5 -1 349.04 74.88 0 5 1 595.15 86.53 0 5 1 442.34 94.58 0 5 -1 454.72 66.08 0 5 -1 271.14 58.40 0 5 -1 426.64 91.23 0 -5 2 397.07 57.70 0 -5 2 351.35 51.05 0 -5 -2 361.75 52.74 0 -5 -2 243.35 52.53 0 5 2 347.97 50.76 0 5 2 404.63 86.57 0 5 -2 362.54 52.74 0 5 -2 285.14 61.58 0 5 -2 326.74 69.96 0 -5 3 2080.75 301.70 0 -5 3 1993.60 288.94 0 -5 3 1717.71 364.68 0 -5 -3 3147.56 667.84 0 -5 -3 2291.38 332.23 0 5 3 3084.78 654.63 0 5 3 1970.88 285.88 0 5 -3 2041.52 296.05 0 5 -3 1939.09 411.94 0 5 -3 2525.56 536.09 0 -5 4 547.24 79.50 0 -5 4 567.89 82.44 0 -5 4 413.84 88.67 0 -5 -4 601.34 87.48 0 -5 -4 574.08 122.63 0 5 4 568.30 121.22 0 5 4 485.70 70.79 0 5 -4 615.80 131.30 0 5 -4 597.21 128.04 0 -5 5 1906.87 276.59 0 -5 5 2159.23 313.23 0 -5 5 1735.47 369.23 0 -5 -5 2550.76 541.87 0 -5 -5 2082.40 302.20 0 5 5 2128.25 308.89 0 5 5 1926.28 279.52 0 5 5 2401.66 510.07 0 5 -5 2336.82 496.03 0 5 -5 2269.50 482.81 0 -5 -6 329.79 71.49 0 5 6 235.38 34.70 0 5 -6 281.26 60.71 0 -5 -7 804.13 172.64 0 5 7 945.39 137.54 0 5 -7 684.77 146.33 0 -6 0 864.43 125.52 0 -6 0 807.02 171.93 0 6 0 694.27 100.86 0 6 0 557.15 119.03 0 -6 1 4122.26 597.63 0 -6 -1 5179.16 750.45 0 -6 -1 3694.79 783.89 0 6 1 4386.18 635.63 0 6 1 3585.76 760.76 0 6 -1 5067.65 734.34 0 6 -1 5555.00 1177.90 0 6 -1 4898.31 1039.14 0 -6 2 310.83 45.22 0 -6 2 314.88 45.84 0 -6 -2 459.26 66.83 0 -6 -2 284.60 61.37 0 6 2 363.07 77.94 0 6 2 379.27 55.30 0 6 -2 399.79 58.15 0 6 -2 316.74 67.90 0 6 -2 250.33 54.31 0 -6 3 1336.09 193.74 0 -6 3 1583.07 229.47 0 -6 -3 2014.67 427.88 0 -6 -3 1274.96 185.07 0 6 3 1582.24 229.60 0 6 3 1977.08 419.62 0 6 -3 1398.45 202.91 0 6 -3 1092.41 232.65 0 6 -3 1141.98 242.81 0 -6 4 12.67 2.49 0 -6 4 19.75 3.19 0 -6 4 8.44 6.19 0 -6 -4 21.86 7.23 0 -6 -4 12.96 3.64 0 6 4 18.59 7.06 0 6 4 7.10 2.25 0 6 -4 7.13 1.78 0 6 -4 9.47 3.84 0 6 -4 8.21 8.45 0 -6 5 5.26 1.66 0 -6 5 6.81 1.62 0 -6 5 11.81 10.26 0 -6 -5 6.44 3.99 0 -6 -5 14.04 7.12 0 6 5 9.49 7.48 0 6 5 7.90 2.51 0 6 -5 9.43 4.32 0 6 -5 17.00 14.16 0 -6 -6 70.13 17.64 0 6 6 43.78 7.14 0 6 -6 78.31 17.99 0 -7 0 0.75 1.44 0 -7 0 0.11 2.63 0 7 0 3.25 1.41 0 7 0 -1.33 3.46 0 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4 8 -3 78.72 13.09 4 8 -3 180.57 39.75 -4 8 3 80.78 12.68 4 -8 -2 1064.33 154.50 4 -8 -2 773.98 165.12 4 8 -2 1018.90 148.15 4 8 -2 880.54 187.75 -4 8 2 708.73 103.25 4 -8 -1 251.78 36.85 4 -8 -1 194.32 42.87 4 8 -1 261.43 38.49 4 8 -1 409.75 88.18 -4 8 1 216.01 31.84 4 -8 0 944.56 137.16 4 -8 0 819.83 175.03 4 8 0 1058.55 153.84 4 8 0 1111.83 236.87 -4 8 0 1014.36 147.37 4 -8 1 247.44 36.14 4 -8 1 212.37 47.33 4 8 1 243.72 35.80 -4 8 -1 255.07 37.42 4 -8 2 378.23 55.14 4 8 2 354.73 51.92 -4 8 -2 414.66 60.67 4 -8 3 62.16 9.75 4 8 3 46.26 7.62 -4 8 -3 57.74 9.62 4 8 4 18.40 4.75 -4 8 -4 24.77 7.45 4 -9 -5 920.60 133.90 4 -9 -5 1027.16 219.64 4 9 -5 800.83 171.23 4 -9 -4 8.82 2.97 4 -9 -4 17.28 7.88 4 9 -4 8.78 6.16 -4 9 4 11.71 4.19 4 -9 -3 463.39 67.44 4 -9 -3 536.09 114.82 4 9 -3 906.97 193.45 -4 9 3 494.37 72.24 4 -9 -2 4.08 1.48 4 -9 -2 9.64 7.08 4 9 -2 2.18 5.06 4 9 -2 11.13 7.26 -4 9 2 7.19 2.54 4 -9 -1 34.19 5.41 4 -9 -1 34.19 10.18 4 9 -1 36.11 6.89 4 9 -1 50.18 14.01 -4 9 1 36.35 6.35 4 -9 0 1.93 1.60 4 -9 0 3.75 8.88 4 9 0 -0.28 2.93 4 9 0 2.84 9.42 -4 9 0 -0.68 2.51 4 -9 1 359.98 52.49 4 -9 1 271.01 59.68 4 9 1 263.99 38.82 -4 9 -1 313.56 45.97 4 -9 2 7.72 2.57 4 9 2 7.39 2.86 -4 9 -2 6.72 3.28 4 -9 3 972.22 141.25 4 9 3 1246.06 180.98 -4 9 -3 841.72 122.63 4 9 4 28.63 5.84 4 -10 -5 8.65 4.57 4 -10 -5 6.84 10.82 4 10 -5 11.78 7.51 4 -10 -4 143.15 21.36 4 -10 -4 139.52 32.00 4 10 -4 275.19 60.46 -4 10 4 134.56 20.63 4 -10 -3 224.14 32.93 4 -10 -3 302.32 65.88 4 10 -3 283.12 61.70 -4 10 3 262.01 38.72 4 -10 -2 400.08 58.32 4 -10 -2 445.64 95.82 4 10 -2 461.74 67.90 4 10 -2 626.95 134.36 -4 10 2 716.16 104.24 4 -10 -1 762.41 110.81 4 -10 -1 583.17 125.19 4 10 -1 822.31 119.82 4 10 -1 772.74 165.32 -4 10 1 984.20 143.11 4 -10 0 597.63 86.86 4 -10 0 463.81 100.16 4 10 0 543.53 79.42 4 10 0 576.97 124.36 -4 10 0 529.90 77.23 4 -10 1 578.21 84.13 4 -10 1 522.46 112.84 4 10 1 604.24 88.18 4 10 1 289.23 64.59 -4 10 -1 567.47 82.73 4 -10 2 151.37 22.46 4 10 2 271.55 40.03 -4 10 -2 179.20 26.81 4 10 3 59.89 9.72 -4 10 -3 60.30 11.04 4 -11 -4 661.23 96.23 4 -11 -4 357.66 77.65 4 11 -4 392.28 85.04 -4 11 4 513.79 75.17 4 -11 -3 7.21 2.66 4 -11 -3 6.11 8.76 4 11 -3 -1.24 8.12 -4 11 3 7.03 3.42 4 -11 -2 107.30 16.11 4 -11 -2 149.31 34.23 4 11 -2 118.25 27.68 -4 11 2 105.98 16.13 4 -11 -1 0.16 1.92 4 -11 -1 2.76 10.05 4 11 -1 -4.53 6.00 4 11 -1 6.18 10.30 -4 11 1 -2.22 2.55 4 -11 0 77.15 11.73 4 -11 0 60.22 16.82 4 11 0 81.65 13.30 4 11 0 75.09 21.15 -4 11 0 71.24 11.33 4 -11 1 10.48 3.07 4 -11 1 8.94 11.44 4 11 1 11.95 4.82 -4 11 -1 13.39 4.75 4 -11 2 340.94 49.85 4 11 2 379.31 55.67 -4 11 -2 390.21 57.45 4 -12 -3 240.87 35.30 4 -12 -3 176.97 40.13 4 12 -3 167.39 38.10 -4 12 3 220.84 32.90 4 -12 -2 360.14 52.58 4 -12 -2 383.89 84.09 4 12 -2 340.12 74.14 -4 12 2 368.24 54.06 4 -12 -1 465.87 67.90 4 -12 -1 383.23 83.72 4 12 -1 398.31 87.10 -4 12 1 398.93 58.48 4 -12 0 372.53 54.39 4 -12 0 312.36 68.64 4 12 0 394.80 58.32 -4 12 0 496.85 72.73 4 -12 1 257.22 37.73 4 12 1 303.69 44.94 -4 12 -1 237.57 35.25 4 -13 -2 0.72 3.12 4 -13 -2 5.93 9.11 -4 13 2 7.24 5.05 4 -13 -1 15.85 4.05 4 -13 -1 17.51 13.37 -4 13 1 30.03 6.57 4 -13 0 1.34 2.61 -4 13 0 2.27 5.01 5 0 -6 442.75 96.07 5 0 -5 4.75 8.21 5 0 -4 1414.15 205.60 5 0 -4 1236.97 263.54 5 0 -3 2.57 3.35 5 0 -3 17.81 9.13 5 0 -2 1311.72 190.36 5 0 -2 1485.60 316.29 -5 0 2 1139.50 165.78 5 0 -1 -0.83 2.20 5 0 -1 1.66 8.68 -5 0 1 -3.40 3.27 5 0 0 315.21 46.17 -5 0 0 282.91 41.71 5 0 1 0.77 2.17 -5 0 -1 -3.51 3.46 5 0 2 42.66 6.66 -5 0 -2 30.19 5.36 5 0 3 2.74 2.41 -5 0 -3 -0.44 3.16 5 0 4 244.84 35.96 5 -1 -6 271.30 59.93 5 1 -6 317.85 69.80 5 -1 -5 160.16 36.71 5 1 -5 226.79 50.43 5 -1 -4 12.89 5.21 5 -1 -4 20.28 10.07 5 1 -4 5.45 6.27 5 1 -4 11.21 9.54 5 -1 -3 3.54 3.40 5 -1 -3 -2.14 7.97 5 1 -3 5.55 3.59 5 1 -3 9.57 8.81 -5 1 3 0.76 4.63 5 -1 -2 296.62 64.88 5 1 -2 294.64 43.28 5 1 -2 254.74 55.96 -5 1 2 265.77 39.36 5 -1 -1 202.58 29.75 -5 -1 1 220.47 32.74 5 1 -1 190.19 27.94 -5 1 1 191.84 28.51 5 -1 0 705.84 102.63 -5 -1 0 1109.35 161.28 5 1 0 598.45 87.06 -5 1 0 769.85 112.13 5 -1 1 539.40 78.43 -5 -1 -1 531.55 77.60 5 1 1 796.28 115.73 -5 1 -1 704.60 102.63 5 -1 2 473.72 69.06 -5 -1 -2 444.40 65.01 5 1 2 676.10 98.34 -5 1 -2 513.79 75.00 5 -1 3 508.42 74.18 5 1 3 410.58 60.01 -5 1 -3 379.72 55.76 5 -1 4 116.84 17.71 5 1 4 111.64 17.16 5 -2 -6 18.08 12.13 5 2 -6 31.94 13.22 5 -2 -5 775.63 166.19 5 2 -5 916.47 195.77 5 -2 -4 33.60 6.89 5 -2 -4 51.09 15.27 5 2 -4 35.33 8.71 5 2 -4 50.14 13.53 5 -2 -3 949.10 138.03 5 -2 -3 1286.11 273.91 5 2 -3 1256.80 182.63 5 2 -3 1516.99 322.89 -5 2 3 1455.87 211.71 5 -2 -2 32.18 5.49 5 -2 -2 27.47 10.69 -5 -2 2 28.26 6.56 5 2 -2 20.27 4.51 5 2 -2 32.95 11.29 -5 2 2 19.99 5.01 5 -2 -1 759.52 110.40 -5 -2 1 1080.85 157.23 5 2 -1 861.54 125.27 -5 2 1 1070.52 155.74 5 -2 0 8.49 2.41 5 -2 0 -3.06 14.64 -5 -2 0 -0.10 2.99 5 2 0 2.99 2.13 5 2 0 1.03 13.56 -5 2 0 2.76 2.93 5 -2 1 111.35 16.59 -5 -2 -1 105.86 16.18 5 2 1 96.69 14.50 -5 2 -1 120.97 18.21 5 -2 2 1.30 1.99 5 2 2 2.08 2.17 -5 2 -2 1.31 2.91 5 -2 3 200.23 29.57 5 2 3 132.37 19.84 -5 2 -3 166.81 25.06 5 -2 4 -0.32 3.32 5 2 4 4.52 3.77 5 -3 -5 101.35 25.78 5 3 -5 103.38 25.32 5 -3 -4 19.25 5.30 5 -3 -4 43.45 13.75 5 3 -4 23.00 7.87 5 3 -4 44.61 13.71 5 -3 -3 -0.18 2.73 5 -3 -3 0.72 7.20 5 3 -3 2.38 4.38 5 3 -3 -1.68 7.65 -5 3 3 -1.27 4.37 5 -3 -2 248.27 36.40 5 -3 -2 260.85 57.33 -5 -3 2 227.74 34.02 5 3 -2 272.21 40.14 5 3 -2 324.50 70.62 -5 3 2 229.35 33.97 5 -3 -1 118.08 17.65 5 -3 -1 49.97 14.84 -5 -3 1 74.67 12.09 5 3 -1 116.22 17.41 -5 3 1 109.74 16.76 5 -3 0 669.49 97.35 -5 -3 0 990.81 144.15 5 3 0 721.53 104.95 -5 3 0 789.68 114.90 5 3 1 290.63 42.66 -5 3 -1 237.98 35.16 5 -3 2 530.31 77.19 5 3 2 709.14 103.13 -5 3 -2 797.52 115.93 5 -3 3 206.88 30.50 5 3 3 205.35 30.26 -5 3 -3 149.27 22.39 5 3 4 187.18 27.70 5 -4 -5 32.41 13.75 5 4 -5 24.77 11.78 5 -4 -4 915.23 133.28 5 -4 -4 1336.09 284.69 5 4 -4 1731.34 368.65 5 -4 -3 95.94 14.75 5 -4 -3 82.97 20.39 5 4 -3 85.95 14.35 5 4 -3 91.11 22.27 -5 4 3 94.62 14.94 5 -4 -2 918.95 133.53 5 -4 -2 1049.47 223.98 5 4 -2 1013.12 147.33 5 4 -2 1158.50 247.11 -5 4 2 907.39 132.08 5 -4 -1 68.27 10.36 5 -4 -1 40.17 13.70 5 4 -1 87.31 13.62 5 4 -1 24.43 13.74 -5 4 1 69.88 10.99 5 4 0 289.68 42.50 -5 4 0 258.38 38.10 5 -4 1 11.68 2.58 5 -4 1 6.85 14.13 5 4 1 9.28 2.70 -5 4 -1 9.77 3.23 5 -4 2 23.59 4.45 5 4 2 15.36 3.63 -5 4 -2 31.18 6.07 5 -4 3 11.27 3.53 5 4 3 12.59 3.76 -5 4 -3 8.27 4.94 5 -5 -5 186.84 42.83 5 5 -5 152.02 35.32 5 -5 -4 1.83 4.14 5 -5 -4 1.40 6.88 5 5 -4 7.47 8.92 5 -5 -3 15.45 3.99 5 -5 -3 12.96 9.16 5 5 -3 7.53 7.10 5 5 -3 15.49 8.95 -5 5 3 9.30 4.46 5 -5 -2 86.32 12.99 5 -5 -2 103.50 25.37 5 5 -2 101.64 16.01 5 5 -2 104.62 25.70 -5 5 2 83.51 13.09 5 -5 -1 333.34 48.74 5 -5 -1 297.99 65.59 5 5 -1 358.70 52.66 5 5 -1 297.49 66.33 -5 5 1 384.14 56.33 5 5 0 303.03 44.48 -5 5 0 214.64 31.79 5 -5 1 902.02 131.05 5 5 1 996.59 144.89 -5 5 -1 812.81 118.29 5 -5 2 171.19 25.39 5 -5 3 576.97 84.05 5 5 3 641.00 93.38 -5 5 -3 538.98 78.93 5 -6 -5 472.48 102.26 5 6 -5 436.56 94.87 5 -6 -4 152.27 22.89 5 -6 -4 201.01 45.27 5 6 -4 202.05 45.18 5 -6 -3 989.99 143.86 5 -6 -3 1006.09 214.89 5 6 -3 944.15 201.63 -5 6 3 991.64 144.31 5 -6 -2 127.04 19.02 5 -6 -2 137.25 32.24 5 6 -2 134.19 20.93 5 6 -2 176.52 40.50 -5 6 2 161.81 24.31 5 -6 -1 450.60 65.71 5 -6 -1 389.22 84.83 5 6 -1 525.35 76.82 5 6 -1 532.79 115.31 -5 6 1 626.54 91.36 5 -6 0 50.72 7.94 5 -6 0 0.22 12.70 5 6 0 46.34 8.21 -5 6 0 32.98 6.22 5 -6 1 47.83 7.75 5 6 1 42.42 7.32 -5 6 -1 55.30 9.31 5 -6 2 13.95 3.70 5 6 2 2.38 3.14 -5 6 -2 8.74 4.54 5 -6 3 87.56 13.51 5 6 3 104.20 15.97 -5 6 -3 56.62 9.91 5 -7 -4 52.20 8.84 5 -7 -4 49.19 14.84 5 7 -4 55.43 16.91 5 -7 -3 -0.03 2.98 5 -7 -3 0.62 10.65 5 7 -3 4.44 9.87 -5 7 3 2.91 3.77 5 -7 -2 134.07 19.96 5 -7 -2 129.36 30.76 5 7 -2 114.69 18.68 5 7 -2 117.26 28.64 -5 7 2 92.89 14.63 5 -7 -1 31.82 5.74 5 -7 -1 26.16 13.25 5 7 -1 24.65 6.29 5 7 -1 37.23 17.08 -5 7 1 28.27 5.82 5 7 0 570.78 83.39 -5 7 0 574.91 83.88 5 -7 1 40.43 6.55 5 7 1 48.82 8.88 -5 7 -1 50.14 8.49 5 -7 2 584.41 85.12 5 7 2 501.40 73.31 -5 7 -2 576.15 84.13 5 -8 -4 384.92 83.92 5 -8 -3 180.57 26.80 5 -8 -3 231.95 52.37 5 8 -3 206.22 46.67 -5 8 3 158.14 24.19 5 -8 -2 566.23 82.52 5 -8 -2 479.92 104.00 5 8 -2 590.19 127.62 -5 8 2 582.34 85.12 5 -8 -1 141.09 21.01 5 -8 -1 114.41 28.83 5 8 -1 151.04 23.57 -5 8 1 198.12 29.62 5 8 0 232.57 34.70 -5 8 0 159.67 24.19 5 -8 1 12.94 3.56 5 8 1 22.69 6.17 -5 8 -1 23.93 6.27 5 -8 2 11.83 3.87 5 8 2 3.26 4.65 -5 8 -2 20.08 6.21 5 -9 -3 42.21 7.53 5 -9 -3 25.26 13.02 -5 9 3 44.23 9.07 5 -9 -2 3.65 2.62 5 -9 -2 3.16 10.68 -5 9 2 6.43 4.34 5 -9 -1 473.72 69.06 5 -9 -1 364.64 80.83 -5 9 1 441.93 64.80 5 -9 0 27.75 4.89 -5 9 0 39.28 7.31 5 -9 1 736.40 107.14 -5 9 -1 845.02 123.20 5 -10 -2 206.96 30.61 -5 10 2 215.84 32.40 5 -10 -1 171.40 25.45 -5 10 1 226.29 33.87 5 -10 0 71.82 11.28 -5 10 0 53.40 9.31 6 0 -1 3.93 4.20 6 0 0 21.95 5.19 6 -1 -1 505.11 73.76 6 1 -1 362.29 53.32 6 -1 0 191.97 28.56 6 1 0 151.21 22.93 -6 1 0 198.91 30.09 6 -2 -1 8.10 3.82 6 -2 0 4.88 3.62 -6 2 0 8.74 6.12 6 -3 -1 243.85 36.04 -6 3 0 254.70 37.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 48725 _shelx_res_file ; TITL I in P2(1)/c CELL 0.96990 4.8211 13.7762 7.0113 90.000 98.055 90.000 ZERR 4.00 0.0006 0.0030 0.0010 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N I DISP C 0.007 0.003 25.571 DISP H -0 0 0.636 DISP N 0.013 0.007 47.42 DISP I -0.034 3.136 18629.286 UNIT 4 20 8 4 TEMP -173.0 SIZE 0.03 0.05 0.06 L.S. 12 BOND $H ACTA CONF HTAB N1 I1 EQIV $1 x-1, -y+1/2, z+1/2 HTAB N2 I1_$1 WGHT 0.000000 0.786500 EXTI 0.006373 FVAR 0.56555 I1 4 0.866581 0.385767 0.200218 11.00000 0.02295 0.02152 = 0.02168 -0.00041 0.00545 0.00012 N1 3 0.611971 0.417143 0.656877 11.00000 0.02198 0.03005 = 0.02306 0.00035 0.00305 -0.00303 AFIX 3 H1A 2 0.724991 0.417383 0.565007 11.00000 -1.20000 H1B 2 0.625071 0.464843 0.745417 11.00000 -1.20000 AFIX 0 N2 3 0.254044 0.338906 0.785981 11.00000 0.02137 0.02216 = 0.03367 0.00114 0.00787 -0.00201 AFIX 3 H2A 2 0.135214 0.288216 0.777582 11.00000 -1.20000 H2B 2 0.251544 0.383176 0.880131 11.00000 -1.20000 AFIX 0 C1 1 0.429609 0.347845 0.660619 11.00000 0.02266 0.02553 = 0.01929 -0.00028 0.00092 0.00221 AFIX 43 H1 2 0.423285 0.299391 0.563696 11.00000 -1.20000 AFIX 0 HKLF 4 REM I in P2(1)/c REM R1 = 0.0388 for 894 Fo > 4sig(Fo) and 0.0402 for all 949 data REM 38 parameters refined using 0 restraints END WGHT 0.0000 0.7865 REM Highest difference peak 0.867, deepest hole -0.913, 1-sigma level 0.254 Q1 1 0.1196 0.3849 1.0612 11.00000 0.05 0.87 Q2 1 0.9559 0.4518 0.1432 11.00000 0.05 0.85 Q3 1 0.7056 0.3925 0.0982 11.00000 0.05 0.83 Q4 1 0.7869 0.3179 0.0669 11.00000 0.05 0.82 Q5 1 0.8751 0.4430 0.1837 11.00000 0.05 0.79 Q6 1 0.7016 0.4480 0.2328 11.00000 0.05 0.79 Q7 1 1.1331 0.4278 0.2930 11.00000 0.05 0.78 Q8 1 -0.1001 0.3149 0.8280 11.00000 0.05 0.77 Q9 1 0.8218 0.4602 0.0685 11.00000 0.05 0.76 Q10 1 0.9428 0.5037 0.1196 11.00000 0.05 0.76 Q11 1 0.8549 0.3317 0.2110 11.00000 0.05 0.75 Q12 1 0.1692 0.3201 0.9586 11.00000 0.05 0.75 Q13 1 0.1303 0.3133 0.7710 11.00000 0.05 0.74 Q14 1 0.1692 0.4483 0.9473 11.00000 0.05 0.74 Q15 1 0.8730 0.3522 0.4468 11.00000 0.05 0.73 Q16 1 0.8503 0.4565 0.3294 11.00000 0.05 0.72 Q17 1 0.1021 0.4539 0.7737 11.00000 0.05 0.72 Q18 1 0.1527 0.2686 0.9210 11.00000 0.05 0.71 Q19 1 0.0475 0.2753 0.6198 11.00000 0.05 0.70 Q20 1 1.0102 0.3142 0.1604 11.00000 0.05 0.68 ; _shelx_res_checksum 20789 _shelxl_version_number 2014/6