#------------------------------------------------------------------------------ #$Date: 2024-02-05 13:06:48 +0100 (Mon, 05 Feb 2024) $ #$Revision: 289689 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/29/2022990.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_2022990 loop_ _publ_author_name 'Neary, Michelle C.' 'Corfield, Peter W. R.' 'Parkin, Sean R.' 'Saba, Shahrokh' _publ_section_title ; Crystal structures of two formamidinium hexa-fluorido-phosphate salts, one with batch-dependent disorder. ; _journal_issue 'Pt 1' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 88 _journal_page_last 93 _journal_paper_doi 10.1107/S2056989023010848 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C5 H11 N2 +, P F6 -' _chemical_formula_moiety 'C5 H11 N2 +, F6 P -' _chemical_formula_sum 'C5 H11 F6 N2 P' _chemical_formula_weight 244.13 _chemical_name_systematic ; Pyrrolidinoformamidinium hexafluorophosphate ; _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_Hall 'C -2yc' _space_group_name_H-M_alt 'C 1 c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 105.4000(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 12.3588(3) _cell_length_b 12.7942(3) _cell_length_c 12.2759(3) _cell_measurement_reflns_used 9886 _cell_measurement_temperature 130(2) _cell_measurement_theta_max 74.50 _cell_measurement_theta_min 3.73 _cell_volume 1871.38(8) _computing_cell_refinement ; SAINT (Bruker, 2022) ; _computing_data_collection ; APEX4 (Bruker, 2022) ; _computing_data_reduction ; SAINT (Bruker, 2022) ; _computing_molecular_graphics ; XP in SHELXTL (Sheldrick, 2008) and WinGX (Farrugia, 2012) ; _computing_publication_material ; SHELX (Sheldrick, 2008) and publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 130(2) _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'Bruker D8 with PHOTON III area detector' _diffrn_measurement_method '\f and \w shutterless scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_unetI/netI 0.0348 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 17935 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 74.581 _diffrn_reflns_theta_min 5.072 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 3.279 _exptl_absorpt_correction_T_max 0.754 _exptl_absorpt_correction_T_min 0.639 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.733 _exptl_crystal_description block _exptl_crystal_F_000 992 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.366 _refine_diff_density_min -0.346 _refine_ls_abs_structure_details ; Refined as an inversion twin ; _refine_ls_abs_structure_Flack 0.49(4) _refine_ls_extinction_coef 0.0014(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL-2018/3 (Sheldrick 2015b) ; _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 257 _refine_ls_number_reflns 3467 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0488 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+2.0200P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1343 _refine_ls_wR_factor_ref 0.1345 _reflns_number_gt 3450 _reflns_number_total 3467 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5706sup1.cif _cod_data_source_block 2 _cod_depositor_comments 'Adding full bibliography for 2022988--2022990.cif.' _cod_original_sg_symbol_H-M 'C c' _cod_database_code 2022990 _cod_database_fobs_code 2022990 _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 0.546 _shelx_estimated_absorpt_t_max 0.714 _shelx_hkl_file ; -2 0 0 1918.31 80.69 -10 0 0 247.88 11.00 -12 0 0 46.10 3.00 -12 0 0 41.40 2.40 -12 0 0 44.30 2.00 -12 0 0 43.90 2.00 -12 0 0 44.50 2.00 -12 0 0 46.40 1.90 -12 0 0 48.20 2.50 -12 0 0 42.90 1.90 -12 0 0 45.10 1.90 -14 0 0 24.20 1.00 -14 0 0 25.40 1.10 -14 0 0 22.50 1.50 -14 0 0 24.80 1.10 -14 0 0 25.20 1.10 -1 -1 0 64.79 2.80 -1 1 0 58.09 3.00 -3 -1 0 404.86 17.30 -5 -1 0 78.09 3.70 -5 -1 0 85.59 4.70 -9 -1 0 259.47 11.70 -9 -1 0 259.87 11.20 -9 1 0 260.07 11.20 -9 1 0 281.27 11.30 -9 1 0 266.27 11.20 -11 -1 0 2.10 0.20 -11 -1 0 1.80 0.30 -11 -1 0 2.30 0.20 -11 -1 0 1.80 0.40 -11 -1 0 2.20 0.20 -11 -1 0 1.70 0.70 -11 -1 0 2.30 0.20 -11 -1 0 2.40 0.50 -11 -1 0 2.10 0.20 -11 1 0 2.50 0.50 -11 1 0 1.90 0.70 -11 1 0 1.70 0.10 -11 1 0 2.00 0.40 -11 1 0 2.30 0.20 -11 1 0 1.70 0.20 -13 -1 0 24.10 1.10 -13 -1 0 22.50 1.00 -13 -1 0 23.70 1.10 -13 -1 0 23.60 1.00 -13 -1 0 23.60 1.10 -13 -1 0 21.10 2.00 -13 -1 0 23.60 1.00 -13 1 0 22.80 1.40 -13 1 0 23.70 1.10 -13 1 0 20.90 1.60 -13 1 0 23.10 1.00 -13 1 0 23.30 1.00 0 2 0 1415.56 60.49 -4 -2 0 422.06 18.70 -4 -2 0 453.55 20.30 -6 -2 0 1720.23 73.59 -10 -2 0 15.50 0.70 -10 -2 0 13.90 0.70 -10 -2 0 15.20 0.70 -10 -2 0 15.10 1.00 -10 -2 0 16.10 0.70 -10 -2 0 16.60 0.80 -10 2 0 15.30 0.70 -10 2 0 17.00 0.80 -10 2 0 16.20 0.80 10 2 0 15.30 0.90 -10 2 0 16.30 1.00 -10 2 0 16.20 0.80 -12 -2 0 33.30 1.50 -12 -2 0 34.40 1.50 -12 -2 0 34.10 1.60 -12 -2 0 35.10 1.60 -12 -2 0 34.20 1.50 -12 -2 0 34.10 1.50 -12 -2 0 33.70 2.60 12 2 0 23.50 1.20 -12 2 0 34.20 2.00 -12 2 0 34.60 1.50 -12 2 0 33.70 1.50 -12 2 0 34.10 2.00 -12 2 0 33.90 1.50 -12 2 0 33.30 1.50 -14 -2 0 5.80 0.30 -14 -2 0 6.20 0.30 -14 -2 0 5.80 0.30 -14 -2 0 5.80 0.30 -14 -2 0 5.80 0.30 -14 -2 0 6.50 0.80 -14 2 0 5.30 0.30 -14 2 0 5.70 0.30 -14 2 0 5.80 0.30 -1 -3 0 3.30 0.20 -1 -3 0 3.80 0.50 1 -3 0 2.70 0.30 -1 -3 0 3.00 0.30 -1 -3 0 3.10 0.40 -1 3 0 3.40 0.40 1 3 0 3.90 2.00 1 3 0 2.80 0.30 -1 3 0 2.10 1.20 -1 3 0 2.90 0.20 -3 -3 0 34.30 1.40 -3 -3 0 32.20 1.50 3 -3 0 32.50 1.70 -3 -3 0 32.10 1.90 -3 3 0 29.60 1.70 3 3 0 33.00 1.50 -3 3 0 31.60 1.60 -3 3 0 32.20 2.50 3 3 0 34.60 1.90 -5 -3 0 21.60 1.00 -5 -3 0 17.40 1.50 -5 -3 0 13.20 4.20 -5 -3 0 18.80 1.30 5 3 0 15.30 1.40 -5 3 0 21.90 1.00 5 3 0 17.30 1.40 -7 -3 0 50.59 2.40 -7 -3 0 52.79 3.00 -7 -3 0 53.39 4.50 7 3 0 32.80 1.50 -9 -3 0 232.08 10.60 9 3 0 212.98 9.20 -9 3 0 232.38 9.90 -9 3 0 236.98 10.40 -9 3 0 238.38 10.60 -11 -3 0 40.40 1.90 -11 -3 0 43.50 1.90 -11 -3 0 43.10 1.90 -11 -3 0 45.20 2.00 -11 -3 0 44.40 2.00 -11 3 0 43.40 1.90 -11 3 0 45.20 2.40 -11 3 0 43.10 1.90 -11 3 0 43.40 1.90 11 3 0 37.30 1.80 -11 3 0 42.80 2.00 11 3 0 37.50 1.60 -13 -3 0 5.70 0.30 -13 -3 0 5.80 0.30 -13 -3 0 6.00 0.40 -13 -3 0 6.20 0.30 -13 -3 0 5.60 0.30 -13 3 0 6.30 0.30 -13 3 0 5.50 0.30 -13 3 0 6.60 0.30 -13 3 0 5.70 0.30 0 4 0 2097.49 89.99 -2 -4 0 678.93 28.80 -2 4 0 663.53 29.80 -4 -4 0 102.89 4.90 -4 -4 0 102.39 4.90 4 -4 0 94.99 4.30 4 4 0 85.69 4.50 -4 4 0 89.09 4.60 -6 -4 0 175.28 13.90 -6 -4 0 207.88 9.10 -6 -4 0 198.88 9.10 6 4 0 167.08 7.10 6 4 0 159.18 7.00 6 4 0 170.68 7.90 -8 -4 0 618.64 29.00 -8 -4 0 625.74 26.70 -10 -4 0 45.40 2.00 -10 -4 0 47.20 2.00 -10 -4 0 43.50 1.90 -10 -4 0 47.50 1.90 -10 -4 0 40.00 3.20 -10 -4 0 43.70 2.20 -10 -4 0 47.30 2.00 -10 -4 0 45.90 1.90 -10 -4 0 39.90 2.50 -10 4 0 43.90 1.90 -10 4 0 43.40 2.00 -10 4 0 41.50 1.90 -10 4 0 42.50 1.90 10 4 0 39.50 1.90 10 4 0 39.00 1.70 -10 4 0 44.20 1.90 -10 4 0 45.30 1.90 -10 4 0 42.80 2.50 -12 -4 0 12.50 1.40 -12 -4 0 11.20 0.60 -12 -4 0 12.20 0.50 -12 -4 0 10.90 0.60 -12 -4 0 10.90 0.60 -12 -4 0 11.70 0.50 -12 -4 0 12.30 0.50 -12 4 0 10.10 1.20 -12 4 0 12.60 1.00 12 4 0 7.10 0.50 -12 4 0 11.40 0.50 -12 4 0 10.40 0.90 -12 4 0 11.40 0.50 12 4 0 7.90 0.40 -12 4 0 10.80 0.60 -12 4 0 11.40 0.50 -14 -4 0 15.20 0.70 -14 -4 0 15.40 0.70 -14 -4 0 14.70 1.50 -14 -4 0 14.70 0.60 -1 -5 0 1109.29 49.00 1 5 0 1165.98 53.09 -1 5 0 1191.08 50.69 -3 -5 0 56.89 3.00 3 -5 0 47.90 2.50 3 -5 0 47.60 2.60 -3 -5 0 48.10 2.90 3 5 0 44.10 2.70 -3 5 0 42.50 4.50 5 -5 0 1.80 0.20 -5 -5 0 1.10 0.60 5 5 0 1.70 0.10 -5 5 0 1.30 0.80 -5 5 0 0.90 0.40 5 5 0 1.20 0.50 -7 -5 0 92.39 3.80 -7 -5 0 93.39 4.10 -7 -5 0 94.89 5.10 -7 -5 0 89.59 3.80 -7 -5 0 85.99 3.90 -7 -5 0 91.49 3.80 -7 -5 0 91.69 3.90 -7 -5 0 93.29 4.40 7 5 0 78.39 3.70 -7 5 0 90.59 3.80 -7 5 0 92.29 3.90 -7 5 0 86.69 4.50 -7 5 0 82.19 3.90 7 5 0 83.19 4.10 -7 5 0 92.69 4.50 -7 5 0 87.89 3.80 -7 5 0 89.69 3.80 -7 5 0 83.89 4.30 7 5 0 86.39 3.60 -9 -5 0 121.29 5.00 -9 -5 0 120.29 5.00 -9 -5 0 119.69 5.30 -9 -5 0 118.89 5.00 -9 -5 0 117.19 5.10 -9 -5 0 119.89 5.60 -9 -5 0 121.99 5.10 -9 -5 0 113.79 5.00 -9 -5 0 117.49 5.00 -9 5 0 114.39 5.00 -9 5 0 110.29 5.00 -9 5 0 118.59 5.70 9 5 0 97.19 4.50 -9 5 0 117.89 5.50 -9 5 0 118.29 5.00 -9 5 0 112.09 5.00 9 5 0 103.09 4.30 -9 5 0 117.99 5.00 -9 5 0 117.49 5.00 -11 -5 0 72.09 3.20 -11 -5 0 71.29 3.10 -11 -5 0 74.09 3.10 -11 -5 0 71.59 3.10 -11 -5 0 74.19 3.20 -11 -5 0 71.29 4.50 -11 -5 0 73.59 3.20 -11 -5 0 74.39 3.10 -11 5 0 70.59 3.10 -11 5 0 70.49 3.10 11 5 0 57.99 2.80 -11 5 0 74.99 3.80 -11 5 0 76.49 3.80 -11 5 0 74.39 3.10 -11 5 0 73.29 3.10 -11 5 0 73.59 3.20 11 5 0 62.89 2.60 -11 5 0 75.09 3.60 -11 5 0 70.09 3.40 -13 -5 0 29.60 1.30 -13 -5 0 30.50 1.30 -13 -5 0 31.50 1.30 -13 -5 0 28.80 1.40 -13 -5 0 30.20 1.30 -13 -5 0 28.90 2.00 -13 -5 0 29.20 1.30 -13 5 0 29.80 1.30 13 5 0 19.40 0.90 -13 5 0 29.90 1.30 -13 5 0 28.60 1.60 -13 5 0 31.30 1.60 0 -6 0 1524.85 64.29 0 6 0 1498.25 66.69 -2 -6 0 251.57 9.60 -2 -6 0 213.48 10.40 2 6 0 211.68 13.50 2 6 0 197.58 9.50 -2 6 0 207.28 12.50 -4 -6 0 316.77 14.40 4 6 0 305.77 14.10 -4 6 0 314.37 15.70 -6 -6 0 567.24 25.00 -8 -6 0 28.00 1.30 8 -6 0 26.20 1.20 -8 -6 0 27.60 1.20 -8 -6 0 28.40 1.30 -8 -6 0 26.00 1.20 -8 -6 0 26.90 1.20 8 -6 0 23.30 1.10 -8 6 0 26.30 1.20 -8 6 0 29.30 1.80 8 6 0 26.00 1.30 8 6 0 21.90 1.70 8 6 0 25.00 1.10 -8 6 0 25.10 1.20 -8 6 0 24.10 1.20 -8 6 0 25.70 1.20 -8 6 0 26.20 1.20 -10 -6 0 16.40 0.80 -10 -6 0 14.60 0.70 -10 -6 0 16.60 0.80 -10 -6 0 15.90 0.70 -10 -6 0 15.70 0.80 -10 6 0 15.00 0.70 10 6 0 13.20 0.60 -10 6 0 14.30 1.40 -10 6 0 15.10 0.80 10 6 0 14.40 0.90 -10 6 0 15.90 0.70 -12 -6 0 6.70 0.30 -12 -6 0 6.70 0.30 -12 -6 0 5.90 1.00 -12 -6 0 6.60 0.40 -12 -6 0 6.40 0.40 -12 -6 0 6.40 0.30 -12 -6 0 6.80 0.40 -12 -6 0 5.90 0.30 12 6 0 5.00 0.40 -12 6 0 6.40 0.30 -12 6 0 6.80 0.60 12 6 0 5.00 0.30 -12 6 0 6.90 0.70 -12 6 0 6.50 0.30 -12 6 0 6.10 0.50 -12 6 0 6.50 0.70 -1 -7 0 11.00 0.50 1 -7 0 11.20 0.60 1 -7 0 11.10 0.50 -1 -7 0 11.40 0.60 1 7 0 10.80 0.50 1 7 0 21.40 6.60 -1 7 0 18.10 5.20 -3 -7 0 653.63 28.80 -3 7 0 658.33 30.90 3 7 0 586.84 31.60 -5 -7 0 10.60 0.50 -5 -7 0 11.70 1.60 5 -7 0 10.30 0.50 5 -7 0 11.20 0.50 -5 -7 0 10.10 0.70 -5 -7 0 10.70 0.60 -5 -7 0 10.50 0.70 -5 -7 0 9.20 0.50 5 7 0 10.30 0.50 5 7 0 10.10 1.20 -5 7 0 11.10 1.40 -5 7 0 9.80 0.50 5 7 0 10.50 0.70 -5 7 0 10.50 0.90 -5 7 0 10.30 0.50 -5 7 0 9.50 0.90 -5 7 0 10.80 1.00 -7 -7 0 110.59 4.70 -7 -7 0 120.29 4.60 7 -7 0 97.59 4.30 -7 -7 0 102.39 5.80 -7 -7 0 112.99 5.90 -7 -7 0 106.99 4.90 -7 -7 0 103.59 4.60 -7 -7 0 111.69 4.60 7 -7 0 101.99 4.40 7 7 0 105.09 5.10 -7 7 0 99.49 5.40 7 7 0 99.39 4.50 -7 7 0 101.29 4.60 -7 7 0 104.29 4.60 -7 7 0 109.09 4.60 -7 7 0 110.99 5.20 7 7 0 101.29 4.30 9 -7 0 160.38 7.40 9 -7 0 191.28 7.50 -9 -7 0 207.88 9.60 -9 7 0 211.68 9.50 9 7 0 179.18 7.40 9 7 0 173.88 7.60 -9 7 0 201.08 9.20 9 7 0 167.28 8.30 -9 7 0 205.38 9.20 -9 7 0 194.08 8.60 -11 -7 0 11.10 0.50 -11 -7 0 10.90 0.50 -11 -7 0 11.10 0.60 -11 -7 0 9.70 1.20 -11 -7 0 10.60 0.50 -11 -7 0 10.40 0.50 -11 -7 0 11.00 0.60 -11 -7 0 10.70 0.50 11 7 0 9.00 0.60 -11 7 0 11.30 0.50 -11 7 0 9.90 0.70 -11 7 0 10.60 0.90 -11 7 0 11.00 0.50 -11 7 0 11.60 1.00 -11 7 0 11.20 0.90 -11 7 0 11.10 0.50 11 7 0 9.10 0.40 -13 -7 0 10.00 0.50 -13 -7 0 9.40 0.50 -13 -7 0 10.10 0.50 -13 7 0 10.10 0.40 -13 7 0 10.80 0.70 13 7 0 7.20 0.30 -13 7 0 9.20 0.60 -2 -8 0 389.76 18.90 -2 -8 0 381.36 16.60 -2 -8 0 399.06 18.30 2 8 0 390.26 18.20 -2 8 0 407.06 21.00 -4 -8 0 406.16 18.60 6 -8 0 130.49 5.50 -6 -8 0 142.99 6.20 -6 -8 0 157.78 7.80 -6 -8 0 148.09 7.40 -6 -8 0 146.19 6.20 -6 -8 0 147.89 6.50 -6 -8 0 140.09 6.30 6 -8 0 131.19 5.60 -6 8 0 140.89 6.20 6 8 0 128.49 5.50 -6 8 0 142.89 6.90 6 8 0 127.69 5.70 8 -8 0 101.49 4.40 -8 -8 0 120.69 5.10 -8 -8 0 115.89 5.40 -8 -8 0 121.19 5.10 8 -8 0 97.79 4.40 -8 -8 0 116.99 5.10 -8 -8 0 118.69 5.20 -8 -8 0 120.39 6.40 8 -8 0 106.39 4.70 8 8 0 107.09 5.30 -8 8 0 119.69 5.10 8 8 0 107.49 4.90 -8 8 0 117.99 5.60 -8 8 0 120.69 5.70 -8 8 0 123.09 5.10 -8 8 0 119.69 5.90 8 8 0 103.69 4.40 -10 -8 0 3.20 0.30 -10 -8 0 2.80 0.20 -10 -8 0 2.70 0.20 -10 -8 0 2.80 0.20 -10 -8 0 2.60 0.30 10 -8 0 2.50 0.30 -10 8 0 3.20 0.50 -10 8 0 3.00 0.20 -10 8 0 2.80 0.50 10 8 0 2.30 0.20 -10 8 0 3.10 0.70 10 8 0 2.20 0.40 -10 8 0 3.00 0.20 -10 8 0 2.60 0.20 -10 8 0 2.50 0.40 -12 -8 0 1.40 0.20 -12 -8 0 1.30 0.10 -12 -8 0 1.20 0.40 -12 -8 0 1.30 0.20 -12 -8 0 1.30 0.10 -12 -8 0 1.20 0.10 -12 8 0 1.30 0.10 -12 8 0 1.30 0.10 -12 8 0 1.20 0.30 12 8 0 1.10 0.10 -12 8 0 1.40 0.40 -12 8 0 1.30 0.30 1 -9 0 139.79 6.30 -1 -9 0 145.69 6.10 -1 9 0 137.29 6.00 -1 9 0 139.49 6.60 1 9 0 165.98 14.30 -1 9 0 134.39 5.90 -1 9 0 152.98 12.30 -3 -9 0 25.70 1.40 -3 -9 0 23.30 1.10 3 -9 0 22.20 1.10 -3 -9 0 23.90 1.40 3 -9 0 22.50 1.20 -3 -9 0 24.20 1.10 3 -9 0 23.70 1.00 3 -9 0 24.10 1.10 3 -9 0 24.10 1.80 -3 -9 0 27.80 2.90 3 9 0 25.70 1.60 3 9 0 22.60 1.20 -3 9 0 24.70 1.70 3 9 0 22.70 1.00 -3 9 0 23.20 1.30 -3 9 0 23.60 1.10 -3 9 0 23.90 1.70 -3 9 0 22.60 1.30 -3 9 0 30.10 6.50 -3 9 0 24.60 1.10 5 -9 0 2.80 0.30 -5 -9 0 3.80 0.50 -5 -9 0 3.70 0.40 -5 -9 0 3.00 0.30 -5 -9 0 3.80 0.20 5 -9 0 2.20 0.30 5 -9 0 2.90 0.20 5 9 0 2.60 0.20 -5 9 0 2.90 0.70 5 9 0 2.20 0.40 -5 9 0 3.40 0.20 -7 -9 0 120.79 5.10 7 -9 0 102.69 4.60 -7 -9 0 120.99 5.20 -7 -9 0 120.69 5.20 7 -9 0 101.29 4.90 -7 -9 0 121.69 6.20 -7 -9 0 120.89 5.10 7 -9 0 109.69 4.50 -7 -9 0 119.89 5.50 -7 -9 0 129.79 6.80 -7 9 0 120.19 5.10 7 9 0 104.39 4.60 -7 9 0 119.09 5.80 7 9 0 118.29 5.50 -7 9 0 116.59 5.90 -7 9 0 114.19 5.70 -7 9 0 120.99 5.10 7 9 0 108.29 5.00 -9 -9 0 26.40 1.20 9 -9 0 24.80 1.00 -9 -9 0 23.30 1.30 -9 -9 0 26.10 1.20 -9 -9 0 27.10 1.20 -9 -9 0 26.70 1.10 -9 -9 0 24.50 1.20 9 -9 0 24.50 1.20 -9 9 0 27.40 1.80 -9 9 0 28.20 1.60 9 9 0 21.40 1.10 -9 9 0 22.80 1.70 -9 9 0 24.20 1.20 -9 9 0 25.30 1.10 -9 9 0 25.90 1.10 9 9 0 24.90 1.30 -9 9 0 27.60 1.60 -11 -9 0 9.80 0.50 -11 -9 0 9.50 0.50 -11 -9 0 9.40 0.50 -11 -9 0 10.10 0.50 -11 -9 0 10.30 0.50 -11 9 0 8.90 0.80 -11 9 0 9.50 0.50 -11 9 0 10.40 0.70 -11 9 0 10.60 0.90 -11 9 0 9.50 0.40 -11 9 0 9.50 0.40 11 9 0 8.80 0.40 11 9 0 9.20 0.60 0 -10 0 1.90 0.20 0 -10 0 2.20 0.60 0 10 0 2.50 0.60 -2 -10 0 155.78 7.20 -2 -10 0 154.08 6.80 -2 -10 0 153.98 6.70 2 -10 0 156.58 6.60 -2 10 0 155.28 6.70 -2 10 0 177.58 13.40 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0.70 -6 -4 13 23.00 1.40 6 -4 -13 19.20 1.20 6 4 -13 19.90 1.20 -6 4 13 22.60 1.30 -4 -4 13 2.50 0.20 4 -4 -13 1.10 0.30 4 4 -13 0.90 0.30 -2 -4 13 1.60 0.10 2 -4 -13 1.40 0.30 2 4 -13 1.40 0.10 2 4 -13 1.40 0.50 2 4 -13 1.40 0.30 2 4 -13 1.30 0.30 0 -4 13 5.60 0.30 0 -4 -13 5.40 0.30 0 -4 13 5.60 0.50 0 -4 -13 6.00 0.60 0 -4 -13 5.00 0.40 0 -4 -13 5.00 0.70 0 4 -13 5.50 0.70 0 4 -13 5.10 0.30 0 4 13 5.40 0.30 0 4 -13 5.30 0.30 0 4 -13 4.90 0.50 2 -4 13 5.90 0.30 -2 -4 -13 6.40 0.30 -2 -4 -13 6.00 0.30 -2 -4 -13 5.70 0.50 -2 4 -13 6.20 0.30 2 4 13 5.70 0.30 -2 4 -13 5.60 0.60 -2 4 -13 5.40 0.60 -2 4 -13 6.20 0.30 -2 4 -13 6.60 0.50 -9 -5 13 51.29 2.70 -9 -5 13 50.69 2.30 -9 5 13 48.60 2.10 -9 5 13 45.40 2.10 -7 -5 13 30.50 1.60 7 -5 -13 25.80 1.40 -7 5 13 30.80 1.60 7 5 -13 24.60 1.40 -7 5 13 31.00 1.30 7 5 -13 26.20 1.40 5 -5 -13 2.40 0.30 -5 -5 13 3.00 0.20 -5 5 13 2.70 0.40 5 5 -13 2.30 0.30 5 5 -13 2.20 0.30 3 -5 -13 14.70 0.90 -3 -5 13 15.40 0.70 3 5 -13 14.70 0.90 3 5 -13 14.40 0.90 3 5 -13 13.00 1.10 -1 -5 13 9.60 0.50 1 -5 -13 10.70 0.70 -1 -5 13 9.50 0.40 1 5 -13 11.00 0.70 1 5 -13 9.40 0.50 1 5 -13 10.90 0.60 1 5 -13 9.10 0.50 1 -5 13 34.80 1.50 -1 -5 -13 30.80 1.70 1 -5 13 34.30 1.50 -1 -5 -13 35.60 1.50 -1 5 -13 36.10 1.50 -1 5 -13 34.20 1.50 -8 -6 13 10.70 0.90 -8 -6 13 11.40 0.70 8 6 -13 8.70 0.60 -8 6 13 11.80 0.50 6 -6 -13 2.20 0.30 -6 -6 13 2.60 0.40 -6 6 13 2.60 0.40 6 6 -13 2.30 0.30 6 6 -13 2.30 0.30 4 -6 -13 6.70 0.50 4 6 -13 7.00 0.60 4 6 -13 7.20 0.50 -2 -6 13 7.50 0.40 2 -6 -13 6.10 0.50 2 6 -13 5.90 0.50 2 6 -13 6.00 0.40 2 6 -13 6.40 0.70 2 6 -13 6.30 0.30 0 -6 13 1.50 0.10 0 -6 -13 1.90 0.10 0 -6 13 1.60 0.10 0 6 -13 1.70 0.10 2 -6 13 2.70 0.20 -2 -6 -13 2.40 0.10 -7 -7 13 8.10 0.60 -7 7 13 9.30 0.60 7 7 -13 7.20 0.50 -7 7 13 9.00 0.40 5 -7 -13 27.10 1.40 5 7 -13 25.00 1.30 5 7 -13 27.00 1.40 -5 7 13 32.60 1.60 -3 -7 13 15.90 0.70 3 -7 -13 15.80 0.90 3 7 -13 15.00 0.80 -3 7 13 16.90 1.00 3 7 -13 13.00 1.00 -1 -7 13 27.10 1.20 1 -7 -13 29.40 1.30 1 7 -13 29.70 1.60 1 7 -13 24.10 1.60 1 7 -13 24.60 1.20 1 -7 13 28.50 1.20 -1 -7 -13 27.90 1.10 -1 7 -13 24.10 1.40 -6 8 13 10.60 0.50 6 8 -13 8.20 0.50 -6 8 13 10.60 0.60 4 -8 -13 0.80 0.20 4 8 -13 0.70 0.20 -2 -8 13 4.10 0.20 8 0 -14 1.80 0.30 -8 0 14 2.50 0.30 6 0 -14 4.10 0.40 -6 0 14 5.60 0.30 -6 0 14 5.10 0.50 2 0 -14 77.89 3.30 2 0 -14 63.79 3.00 0 0 -14 4.90 0.60 0 0 14 7.30 0.30 -2 0 -14 32.40 1.40 -9 -1 14 67.69 3.00 -9 1 14 67.79 3.00 -9 1 14 59.79 2.80 -7 -1 14 18.90 1.10 7 -1 -14 15.00 0.90 -7 1 14 19.00 1.10 -7 1 14 18.20 0.80 -5 -1 14 21.90 1.30 5 -1 -14 18.40 1.10 5 1 -14 17.50 1.10 3 -1 -14 134.19 5.70 3 1 -14 134.49 5.70 1 -1 -14 65.09 3.50 1 -1 -14 68.59 3.10 1 -1 -14 78.99 3.30 -1 -1 14 65.29 2.80 1 -1 -14 76.19 3.30 1 1 -14 69.49 3.10 1 1 -14 74.39 3.20 1 1 -14 76.59 3.40 1 -1 14 79.99 3.40 -1 -1 -14 85.39 3.50 -1 1 -14 76.49 3.80 -1 1 -14 86.89 3.60 -1 1 -14 81.99 3.50 -8 -2 14 3.20 0.40 -8 2 14 3.00 0.50 -8 2 14 3.70 0.20 8 2 -14 2.40 0.30 6 -2 -14 4.50 0.40 -6 -2 14 5.50 0.50 -6 2 14 5.50 0.50 6 2 -14 4.60 0.50 -4 -2 14 21.70 1.00 4 -2 -14 23.20 1.30 4 -2 -14 20.10 1.00 4 2 -14 23.70 1.30 2 -2 -14 5.80 0.30 2 -2 -14 5.30 0.50 2 2 -14 5.10 0.40 2 2 -14 5.00 0.50 2 2 -14 5.70 0.30 0 -2 14 37.00 1.60 -2 -2 -14 10.20 0.40 -2 2 -14 10.20 0.40 -9 -3 14 26.40 1.30 -9 3 14 26.70 1.20 -9 3 14 23.60 1.10 7 -3 -14 90.19 4.10 -7 -3 14 112.49 5.00 7 3 -14 89.89 4.10 5 -3 -14 73.29 3.20 5 -3 -14 77.59 3.50 5 3 -14 76.09 3.50 -5 3 14 89.49 4.10 3 -3 -14 16.90 0.70 3 -3 -14 16.90 1.00 -3 -3 14 17.90 0.80 3 3 -14 16.20 0.90 3 3 -14 15.90 1.20 3 3 -14 15.90 1.00 1 -3 -14 136.19 6.30 1 3 -14 143.49 6.50 1 3 -14 150.18 6.00 -1 -3 -14 24.00 1.00 -1 3 -14 24.00 1.10 -1 3 -14 21.70 1.30 -1 3 -14 23.00 1.00 -8 -4 14 6.10 0.50 -8 4 14 6.10 0.40 8 4 -14 4.30 0.40 6 -4 -14 2.70 0.30 -6 -4 14 3.00 0.40 -6 4 14 3.20 0.40 6 4 -14 2.60 0.30 4 -4 -14 2.60 0.30 4 -4 -14 2.90 0.10 -4 -4 14 3.50 0.20 4 4 -14 2.50 0.30 -4 4 14 2.90 0.40 4 4 -14 2.20 0.30 -2 -4 14 19.10 0.90 2 -4 -14 26.10 1.30 2 4 -14 26.40 1.30 2 4 -14 27.20 1.40 0 -4 14 2.00 0.10 0 -4 -14 2.50 0.10 -7 -5 14 28.40 1.50 7 5 -14 24.00 1.20 -7 5 14 28.30 1.40 5 -5 -14 21.40 1.00 5 -5 -14 24.10 1.20 -5 5 14 27.00 1.40 5 5 -14 22.70 1.20 -5 5 14 29.60 1.20 5 5 -14 24.10 1.20 5 5 -14 20.80 1.30 -3 -5 14 128.79 5.50 3 5 -14 108.59 5.10 3 5 -14 111.29 4.60 1 -5 -14 24.90 1.10 1 -5 -14 23.80 1.00 -1 -5 14 25.00 1.10 1 5 -14 22.60 1.30 1 5 -14 22.60 1.20 6 6 -14 3.00 0.30 -6 6 14 3.80 0.40 4 -6 -14 2.00 0.30 4 -6 -14 2.10 0.10 4 6 -14 1.90 0.20 4 6 -14 2.20 0.10 -2 -6 14 6.50 0.30 2 -6 -14 8.80 0.50 2 6 -14 8.30 0.50 6 0 -15 0.00 0.10 4 0 -15 0.00 0.10 2 0 -15 0.10 0.10 2 0 -15 0.00 0.10 5 -1 -15 21.50 1.10 5 1 -15 21.20 1.10 3 -1 -15 3.20 0.30 3 -1 -15 3.30 0.30 3 -1 -15 3.40 0.40 3 1 -15 3.30 0.50 3 1 -15 3.30 0.30 3 1 -15 3.10 0.30 1 -1 -15 5.30 0.30 1 1 -15 6.40 0.50 6 -2 -15 1.90 0.20 6 2 -15 1.70 0.20 6 2 -15 1.90 0.20 4 -2 -15 1.90 0.20 4 2 -15 1.80 0.20 4 2 -15 1.70 0.40 4 2 -15 1.90 0.30 2 -2 -15 1.90 0.10 2 -2 -15 2.00 0.20 -2 -2 15 2.00 0.10 2 2 -15 1.70 0.40 2 2 -15 2.30 0.20 5 -3 -15 5.40 0.40 5 3 -15 5.30 0.40 5 3 -15 5.20 0.40 3 -3 -15 23.20 1.10 3 3 -15 22.80 1.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 35765 _shelx_res_file ; TITL saba2low_a.res in Cc fulldata.res created by SHELXL-2018/3 at 17:51:38 on 09-Oct-2023 REM Old TITL Saba2 Low Temp Data Iminium Cation REM SHELXT solution in Cc: R1 0.132, Rweak 0.016, Alpha 0.020 REM 1.936 for 85 systematic absences, Orientation as input REM Flack x = 0.494 ( 0.007 ) from 708 Parsons' quotients REM Formula found by SHELXT: N3 C11 P2 F12 CELL 1.54178 12.3588 12.7942 12.2759 90.000 105.400 90.000 ZERR 8.000 0.0003 0.0003 0.0003 0.000 0.001 0.000 LATT -7 SYMM X, -Y, 1/2+Z SFAC N C H P F UNIT 16 40 88 8 48 L.S. 10 SIZE 0.11 0.21 0.21 TEMP -143(2) EQIV $1 1/2+x,y-1/2,z, EQIV $2 x,y-1,z HTAB HTAB N7 F1 HTAB N7 F3a HTAB N7 F4a HTAB C16 F6_$1 HTAB N17 F2 HTAB N17 F4 HTAB N17 F6a_$2 ACTA BOND $H FMAP -2 PLAN 20 TWIN -1 0 0 0 -1 0 0 0 -1 EADP H7A H7B EADP H17A H17B WGHT 0.085000 2.020000 EXTI 0.001390 BASF 0.48657 FVAR 0.32845 N1 1 0.320624 0.727968 0.754979 11.00000 0.03257 0.03166 = 0.02753 -0.00011 0.00777 0.00258 C2 2 0.320465 0.841929 0.766553 11.00000 0.04438 0.02519 = 0.04103 0.00057 0.01665 -0.00095 AFIX 23 H2A 3 0.291759 0.876189 0.692152 11.00000 -1.50000 H2B 3 0.396755 0.868571 0.802754 11.00000 -1.50000 AFIX 0 C3 2 0.241448 0.860117 0.841953 11.00000 0.05126 0.03674 = 0.03851 0.00167 0.02516 0.00381 AFIX 23 H3A 3 0.283785 0.863514 0.922572 11.00000 -1.50000 H3B 3 0.198412 0.925707 0.821178 11.00000 -1.50000 AFIX 0 C4 2 0.164569 0.766139 0.819293 11.00000 0.03188 0.04283 = 0.03517 0.00339 0.01325 0.00385 AFIX 23 H4A 3 0.105798 0.773984 0.747162 11.00000 -1.50000 H4B 3 0.128245 0.755416 0.881246 11.00000 -1.50000 AFIX 0 C5 2 0.243471 0.676196 0.813197 11.00000 0.04009 0.03287 = 0.02918 0.00008 0.01122 -0.00126 AFIX 23 H5A 3 0.284091 0.651192 0.889404 11.00000 -1.50000 H5B 3 0.202882 0.617023 0.768457 11.00000 -1.50000 AFIX 0 C6 2 0.376983 0.677707 0.696507 11.00000 0.03633 0.03215 = 0.03667 0.00015 0.01162 0.00172 AFIX 43 H6 3 0.370295 0.603790 0.691284 11.00000 -1.20000 AFIX 0 N7 1 0.443904 0.725811 0.643488 11.00000 0.04564 0.03815 = 0.04788 -0.00081 0.02828 0.00199 AFIX 94 H7A 3 0.450907 0.792401 0.647310 11.00000 -1.20000 H7B 3 0.479947 0.690166 0.605559 11.00000 -1.20000 AFIX 0 N11 1 0.769838 0.230299 0.315927 11.00000 0.02618 0.02268 = 0.02685 -0.00275 0.00706 0.00012 C12 2 0.763260 0.344889 0.298452 11.00000 0.03732 0.02350 = 0.03731 0.00068 0.01302 -0.00150 AFIX 23 H12A 3 0.793006 0.382648 0.370603 11.00000 -1.50000 H12B 3 0.684995 0.367475 0.264147 11.00000 -1.50000 AFIX 0 C13 2 0.836169 0.363252 0.218414 11.00000 0.04295 0.02717 = 0.04301 0.00305 0.01284 -0.00296 AFIX 23 H13A 3 0.805789 0.420775 0.165124 11.00000 -1.50000 H13B 3 0.914031 0.380689 0.260727 11.00000 -1.50000 AFIX 0 C14 2 0.832159 0.258777 0.155238 11.00000 0.03479 0.04005 = 0.03225 -0.00269 0.01313 -0.00243 AFIX 23 H14A 3 0.761520 0.251673 0.094543 11.00000 -1.50000 H14B 3 0.896670 0.251823 0.122180 11.00000 -1.50000 AFIX 0 C15 2 0.838310 0.179681 0.247555 11.00000 0.03391 0.02667 = 0.04293 -0.00131 0.01281 0.00347 AFIX 23 H15A 3 0.805607 0.111878 0.216390 11.00000 -1.50000 H15B 3 0.916660 0.168610 0.292739 11.00000 -1.50000 AFIX 0 C16 2 0.717296 0.180339 0.377436 11.00000 0.03529 0.02623 = 0.03200 0.00405 0.00791 0.00093 AFIX 43 H16 3 0.722967 0.106294 0.380722 11.00000 -1.20000 AFIX 0 N17 1 0.656224 0.227023 0.435842 11.00000 0.04532 0.03479 = 0.04449 0.00473 0.02800 0.00295 AFIX 94 H17A 3 0.650457 0.288521 0.434225 11.00000 -1.20000 H17B 3 0.625297 0.193575 0.472553 11.00000 -1.20000 AFIX 0 P1 4 0.527483 0.480902 0.506746 11.00000 0.03048 0.02718 = 0.02968 -0.00023 0.01354 -0.00084 F1 5 0.559673 0.601979 0.503870 11.00000 0.06557 0.03242 = 0.06305 -0.01153 0.04113 -0.01440 F2 5 0.495210 0.360192 0.508903 11.00000 0.04477 0.02850 = 0.07537 0.00674 0.02796 0.00234 F3 5 0.547870 0.489588 0.638359 11.00000 0.12506 0.07284 = 0.03277 0.00070 0.02683 0.00220 F4 5 0.656128 0.448957 0.520920 11.00000 0.03591 0.05361 = 0.11177 -0.02141 0.02208 -0.00178 F5 5 0.508995 0.472849 0.374641 11.00000 0.13119 0.05490 = 0.03631 -0.00838 0.02794 -0.01020 F6 5 0.400846 0.513177 0.488611 11.00000 0.03314 0.04427 = 0.12437 -0.00207 0.01801 0.00707 P2 4 0.553350 0.979315 0.550599 11.00000 0.03162 0.02910 = 0.03100 0.00054 0.01438 0.00355 F1A 5 0.577385 0.956450 0.683038 11.00000 0.06620 0.06835 = 0.03656 0.01496 0.01596 -0.00448 F2A 5 0.529410 1.004853 0.419506 11.00000 0.09181 0.06159 = 0.02887 0.00071 0.01640 -0.00351 F3A 5 0.424201 0.956683 0.538238 11.00000 0.03099 0.05649 = 0.07186 -0.01272 0.01437 -0.00825 F4A 5 0.573510 0.859433 0.528683 11.00000 0.08939 0.03043 = 0.08666 -0.00055 0.06407 0.01031 F5A 5 0.683012 1.004674 0.564972 11.00000 0.03791 0.06084 = 0.07484 0.01897 0.02905 0.00701 F6A 5 0.534994 1.100213 0.574224 11.00000 0.05408 0.03093 = 0.05407 -0.00582 0.02694 0.00111 HKLF 4 REM saba2low_a.res in Cc REM wR2 = 0.1345, GooF = S = 1.074, Restrained GooF = 1.074 for all data REM R1 = 0.0488 for 3450 Fo > 4sig(Fo) and 0.0492 for all 3467 data REM 257 parameters refined using 2 restraints END WGHT 0.0849 2.0060 REM Instructions for potential hydrogen bonds EQIV $3 x-1/2, y+1/2, z HTAB C2 F4_$3 EQIV $4 x, -y+2, z+1/2 HTAB C2 F2A_$4 HTAB C3 F3_$3 EQIV $5 x-1/2, -y+3/2, z+1/2 HTAB C4 F4A_$5 EQIV $6 x, -y+1, z+1/2 HTAB C5 F2_$6 EQIV $7 x-1/2, y-1/2, z HTAB C5 F1A_$7 HTAB N7 F1A HTAB N7 F3A HTAB N7 F4A HTAB N7 F1 HTAB C12 F3A_$1 HTAB C13 F2A_$1 EQIV $8 x+1/2, -y+1/2, z-1/2 HTAB C14 F2_$8 EQIV $9 x, -y+1, z-1/2 HTAB C15 F5A_$9 HTAB C16 F6_$1 HTAB N17 F2 HTAB N17 F4 HTAB N17 F6A_$2 REM Highest difference peak 0.366, deepest hole -0.346, 1-sigma level 0.069 Q1 1 0.4020 0.8064 0.7100 11.00000 0.05 0.37 Q2 1 0.4970 1.0020 0.5207 11.00000 0.05 -0.35 Q3 1 0.3313 0.7810 0.7613 11.00000 0.05 0.34 Q4 1 0.4378 0.9260 0.4748 11.00000 0.05 0.34 Q5 1 0.4812 0.4765 0.5119 11.00000 0.05 -0.33 Q6 1 0.7547 0.2805 0.3053 11.00000 0.05 0.33 Q7 1 0.5622 0.4801 0.3579 11.00000 0.05 -0.31 Q8 1 0.6833 0.3096 0.3421 11.00000 0.05 0.31 Q9 1 0.6210 0.4663 0.4749 11.00000 0.05 0.31 Q10 1 0.5816 0.5044 0.5381 11.00000 0.05 -0.30 Q11 1 0.6452 0.4260 0.5877 11.00000 0.05 0.30 Q12 1 0.4656 0.9640 0.5803 11.00000 0.05 0.30 Q13 1 0.4618 0.5116 0.5966 11.00000 0.05 0.29 Q14 1 0.4226 0.4767 0.5476 11.00000 0.05 0.29 Q15 1 0.5993 0.4612 0.4444 11.00000 0.05 0.29 Q16 1 0.6022 0.9897 0.4531 11.00000 0.05 0.28 Q17 1 0.5949 0.9677 0.5249 11.00000 0.05 -0.27 Q18 1 0.2989 0.6487 0.7551 11.00000 0.05 0.27 Q19 1 0.4276 0.4932 0.4005 11.00000 0.05 0.27 Q20 1 0.5343 0.9724 0.7176 11.00000 0.05 -0.26 ; _shelx_res_checksum 73682 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' 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 N N1 0.3206(4) 0.7280(3) 0.7550(3) 0.0306(9) Uani d 1 . . C C2 0.3205(5) 0.8419(4) 0.7666(5) 0.0359(11) Uani d 1 . . H H2A 0.291759 0.876189 0.692152 0.054 Uiso calc 1 . . H H2B 0.396755 0.868571 0.802754 0.054 Uiso calc 1 . . C C3 0.2414(5) 0.8601(4) 0.8420(4) 0.0397(11) Uani d 1 . . H H3A 0.283785 0.863514 0.922572 0.059 Uiso calc 1 . . H H3B 0.198412 0.925707 0.821178 0.059 Uiso calc 1 . . C C4 0.1646(4) 0.7661(4) 0.8193(4) 0.0358(9) Uani d 1 . . H H4A 0.105798 0.773984 0.747162 0.054 Uiso calc 1 . . H H4B 0.128245 0.755416 0.881246 0.054 Uiso calc 1 . . C C5 0.2435(4) 0.6762(4) 0.8132(4) 0.0337(10) Uani d 1 . . H H5A 0.284091 0.651192 0.889404 0.050 Uiso calc 1 . . H H5B 0.202882 0.617023 0.768457 0.050 Uiso calc 1 . . C C6 0.3770(4) 0.6777(4) 0.6965(4) 0.0347(10) Uani d 1 . . H H6 0.370295 0.603790 0.691284 0.042 Uiso calc 1 . . N N7 0.4439(4) 0.7258(3) 0.6435(4) 0.0409(10) Uani d 1 . . H H7A 0.4509(6) 0.792(4) 0.6473(4) 0.049 Uiso calc 1 . . H H7B 0.480(2) 0.690(2) 0.606(2) 0.049 Uiso calc 1 . . N N11 0.7698(3) 0.2303(3) 0.3159(3) 0.0252(7) Uani d 1 . . C C12 0.7633(4) 0.3449(4) 0.2985(4) 0.0321(10) Uani d 1 . . H H12A 0.793006 0.382648 0.370603 0.048 Uiso calc 1 . . H H12B 0.684995 0.367475 0.264147 0.048 Uiso calc 1 . . C C13 0.8362(4) 0.3633(4) 0.2184(4) 0.0374(11) Uani d 1 . . H H13A 0.805789 0.420775 0.165124 0.056 Uiso calc 1 . . H H13B 0.914031 0.380689 0.260727 0.056 Uiso calc 1 . . C C14 0.8322(4) 0.2588(4) 0.1552(4) 0.0349(9) Uani d 1 . . H H14A 0.761520 0.251673 0.094543 0.052 Uiso calc 1 . . H H14B 0.896670 0.251823 0.122180 0.052 Uiso calc 1 . . C C15 0.8383(4) 0.1797(4) 0.2476(4) 0.0340(10) Uani d 1 . . H H15A 0.805607 0.111878 0.216390 0.051 Uiso calc 1 . . H H15B 0.916660 0.168610 0.292739 0.051 Uiso calc 1 . . C C16 0.7173(4) 0.1803(4) 0.3774(4) 0.0314(10) Uani d 1 . . H H16 0.722967 0.106294 0.380722 0.038 Uiso calc 1 . . N N17 0.6562(4) 0.2270(3) 0.4358(4) 0.0385(9) Uani d 1 . . H H17A 0.6505(5) 0.289(4) 0.4342(4) 0.046 Uiso calc 1 . . H H17B 0.6253(18) 0.194(2) 0.473(2) 0.046 Uiso calc 1 . . P P1 0.52748(8) 0.48090(9) 0.50675(8) 0.0281(3) Uani d 1 . . F F1 0.5597(3) 0.6020(2) 0.5039(3) 0.0491(8) Uani d 1 . . F F2 0.4952(3) 0.3602(2) 0.5089(3) 0.0473(8) Uani d 1 . . F F3 0.5479(6) 0.4896(4) 0.6384(4) 0.0758(15) Uani d 1 . . F F4 0.6561(3) 0.4490(3) 0.5209(4) 0.0666(11) Uani d 1 . . F F5 0.5090(5) 0.4728(3) 0.3746(4) 0.0730(14) Uani d 1 . . F F6 0.4008(3) 0.5132(3) 0.4886(5) 0.0678(13) Uani d 1 . . P P2 0.55335(8) 0.97931(9) 0.55060(8) 0.0294(3) Uani d 1 . . F F1A 0.5774(4) 0.9564(4) 0.6830(3) 0.0566(9) Uani d 1 . . F F2A 0.5294(5) 1.0049(3) 0.4195(3) 0.0607(11) Uani d 1 . . F F3A 0.4242(3) 0.9567(3) 0.5382(3) 0.0530(9) Uani d 1 . . F F4A 0.5735(4) 0.8594(3) 0.5287(4) 0.0611(11) Uani d 1 . . F F5A 0.6830(3) 1.0047(3) 0.5650(4) 0.0552(10) Uani d 1 . . F F6A 0.5350(3) 1.1002(2) 0.5742(3) 0.0440(7) 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 N1 0.0326(19) 0.032(2) 0.0275(17) 0.0026(15) 0.0078(14) -0.0001(14) C2 0.044(3) 0.025(2) 0.041(2) -0.0009(18) 0.017(2) 0.0006(18) C3 0.051(3) 0.037(2) 0.039(2) 0.004(2) 0.025(2) 0.002(2) C4 0.032(2) 0.043(2) 0.0352(19) 0.0038(18) 0.0133(16) 0.0034(18) C5 0.040(3) 0.033(2) 0.029(2) -0.001(2) 0.0112(19) 0.0001(18) C6 0.036(2) 0.032(2) 0.037(2) 0.0017(17) 0.0116(19) 0.0001(17) N7 0.046(2) 0.038(2) 0.048(2) 0.0020(17) 0.0283(18) -0.0008(17) N11 0.0262(17) 0.0227(19) 0.0269(15) 0.0001(13) 0.0071(13) -0.0027(13) C12 0.037(2) 0.023(2) 0.037(2) -0.0015(17) 0.013(2) 0.0007(17) C13 0.043(3) 0.027(2) 0.043(3) -0.003(2) 0.013(2) 0.003(2) C14 0.035(2) 0.040(2) 0.0323(19) -0.0024(17) 0.0131(16) -0.0027(17) C15 0.034(2) 0.027(2) 0.043(3) 0.0035(18) 0.013(2) -0.0013(19) C16 0.035(2) 0.0262(19) 0.032(2) 0.0009(17) 0.0079(17) 0.0040(16) N17 0.045(2) 0.035(2) 0.044(2) 0.0030(16) 0.0280(18) 0.0047(16) P1 0.0305(6) 0.0272(5) 0.0297(6) -0.0008(4) 0.0135(4) -0.0002(4) F1 0.066(2) 0.0324(14) 0.0631(19) -0.0144(15) 0.0411(17) -0.0115(15) F2 0.0448(16) 0.0285(14) 0.075(2) 0.0023(12) 0.0280(15) 0.0067(13) F3 0.125(5) 0.073(3) 0.033(2) 0.002(3) 0.027(2) 0.0007(15) F4 0.0359(18) 0.054(2) 0.112(3) -0.0018(17) 0.0221(19) -0.021(2) F5 0.131(4) 0.055(2) 0.036(2) -0.010(2) 0.028(2) -0.0084(15) F6 0.0331(19) 0.0443(19) 0.124(4) 0.0071(14) 0.018(2) -0.002(2) P2 0.0316(6) 0.0291(6) 0.0310(6) 0.0036(4) 0.0144(4) 0.0005(4) F1A 0.066(2) 0.068(2) 0.0366(17) -0.0045(19) 0.0160(15) 0.0150(16) F2A 0.092(3) 0.062(2) 0.0289(18) -0.004(2) 0.0164(18) 0.0007(14) F3A 0.0310(17) 0.0565(19) 0.072(2) -0.0083(15) 0.0144(15) -0.0127(17) F4A 0.089(3) 0.0304(15) 0.087(3) 0.0103(17) 0.064(2) -0.0006(16) F5A 0.0379(19) 0.061(2) 0.075(3) 0.0070(16) 0.0291(18) 0.0190(18) F6A 0.0541(18) 0.0309(13) 0.0541(17) 0.0011(13) 0.0269(13) -0.0058(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 '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 C6 N1 C5 . . 123.5(4) ? C6 N1 C2 . . 124.2(5) ? C5 N1 C2 . . 112.2(4) ? N1 C2 C3 . . 103.1(4) ? N1 C2 H2A . . 111.1 ? C3 C2 H2A . . 111.1 ? N1 C2 H2B . . 111.1 ? C3 C2 H2B . . 111.1 ? H2A C2 H2B . . 109.1 ? C4 C3 C2 . . 103.8(4) ? C4 C3 H3A . . 111.0 ? C2 C3 H3A . . 111.0 ? C4 C3 H3B . . 111.0 ? C2 C3 H3B . . 111.0 ? H3A C3 H3B . . 109.0 ? C3 C4 C5 . . 103.3(4) ? C3 C4 H4A . . 111.1 ? C5 C4 H4A . . 111.1 ? C3 C4 H4B . . 111.1 ? C5 C4 H4B . . 111.1 ? H4A C4 H4B . . 109.1 ? N1 C5 C4 . . 100.8(4) ? N1 C5 H5A . . 111.6 ? C4 C5 H5A . . 111.6 ? N1 C5 H5B . . 111.6 ? C4 C5 H5B . . 111.6 ? H5A C5 H5B . . 109.4 ? N1 C6 N7 . . 122.4(5) ? N1 C6 H6 . . 118.8 ? N7 C6 H6 . . 118.8 ? C6 N7 H7A . . 120.0 ? C6 N7 H7B . . 120.0 ? H7A N7 H7B . . 120.0 ? C16 N11 C12 . . 124.0(4) ? C16 N11 C15 . . 124.4(4) ? C12 N11 C15 . . 111.5(4) ? N11 C12 C13 . . 103.2(4) ? N11 C12 H12A . . 111.1 ? C13 C12 H12A . . 111.1 ? N11 C12 H12B . . 111.1 ? C13 C12 H12B . . 111.1 ? H12A C12 H12B . . 109.1 ? C14 C13 C12 . . 104.3(4) ? C14 C13 H13A . . 110.9 ? C12 C13 H13A . . 110.9 ? C14 C13 H13B . . 110.9 ? C12 C13 H13B . . 110.9 ? H13A C13 H13B . . 108.9 ? C15 C14 C13 . . 102.5(4) ? C15 C14 H14A . . 111.3 ? C13 C14 H14A . . 111.3 ? C15 C14 H14B . . 111.3 ? C13 C14 H14B . . 111.3 ? H14A C14 H14B . . 109.2 ? N11 C15 C14 . . 102.1(4) ? N11 C15 H15A . . 111.4 ? C14 C15 H15A . . 111.4 ? N11 C15 H15B . . 111.4 ? C14 C15 H15B . . 111.4 ? H15A C15 H15B . . 109.2 ? N11 C16 N17 . . 123.1(5) ? N11 C16 H16 . . 118.5 ? N17 C16 H16 . . 118.5 ? C16 N17 H17A . . 120.0 ? C16 N17 H17B . . 120.0 ? H17A N17 H17B . . 120.0 ? F5 P1 F3 . . 179.1(4) ? F5 P1 F6 . . 90.3(3) ? F3 P1 F6 . . 90.5(3) ? F5 P1 F2 . . 89.2(2) ? F3 P1 F2 . . 91.4(2) ? F6 P1 F2 . . 90.73(19) ? F5 P1 F4 . . 87.9(3) ? F3 P1 F4 . . 91.3(3) ? F6 P1 F4 . . 178.1(3) ? F2 P1 F4 . . 89.8(2) ? F5 P1 F1 . . 90.5(2) ? F3 P1 F1 . . 88.9(2) ? F6 P1 F1 . . 89.2(2) ? F2 P1 F1 . . 179.7(2) ? F4 P1 F1 . . 90.2(2) ? F3A P2 F2A . . 91.6(3) ? F3A P2 F5A . . 178.5(2) ? F2A P2 F5A . . 88.9(3) ? F3A P2 F1A . . 88.5(2) ? F2A P2 F1A . . 178.7(3) ? F5A P2 F1A . . 90.8(2) ? F3A P2 F4A . . 90.4(2) ? F2A P2 F4A . . 91.3(2) ? F5A P2 F4A . . 91.0(2) ? F1A P2 F4A . . 90.0(2) ? F3A P2 F6A . . 90.4(2) ? F2A P2 F6A . . 89.3(2) ? F5A P2 F6A . . 88.3(2) ? F1A P2 F6A . . 89.4(2) ? F4A P2 F6A . . 179.1(3) ? 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 C6 . 1.296(7) ? N1 C5 . 1.490(7) ? N1 C2 . 1.465(5) ? C2 C3 . 1.531(7) ? C2 H2A . 0.9900 ? C2 H2B . 0.9900 ? C3 C4 . 1.512(7) ? C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C4 C5 . 1.523(6) ? C4 H4A . 0.9900 ? C4 H4B . 0.9900 ? C5 H5A . 0.9900 ? C5 H5B . 0.9900 ? C6 N7 . 1.331(7) ? C6 H6 . 0.9500 ? N7 H7A . 0.86(5) ? N7 H7B . 0.86(5) ? N11 C16 . 1.289(6) ? N11 C12 . 1.481(5) ? N11 C15 . 1.489(6) ? C12 C13 . 1.517(7) ? C12 H12A . 0.9900 ? C12 H12B . 0.9900 ? C13 C14 . 1.540(7) ? C13 H13A . 0.9900 ? C13 H13B . 0.9900 ? C14 C15 . 1.506(7) ? C14 H14A . 0.9900 ? C14 H14B . 0.9900 ? C15 H15A . 0.9900 ? C15 H15B . 0.9900 ? C16 N17 . 1.315(6) ? C16 H16 . 0.9500 ? N17 H17A . 0.79(5) ? N17 H17B . 0.79(5) ? P1 F5 . 1.580(4) ? P1 F3 . 1.572(4) ? P1 F6 . 1.576(4) ? P1 F2 . 1.597(3) ? P1 F4 . 1.606(4) ? P1 F1 . 1.602(3) ? P2 F3A . 1.589(3) ? P2 F2A . 1.591(4) ? P2 F5A . 1.598(4) ? P2 F1A . 1.600(3) ? P2 F4A . 1.588(3) ? P2 F6A . 1.601(3) ? 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 _geom_hbond_publ_flag N7 H7B F1 . 0.86 2.11 2.966(5) 176.5 yes N7 H7A F3A . 0.86 2.47 3.207(6) 145.2 yes N7 H7A F4A . 0.86 2.51 2.945(6) 112.0 yes C16 H16 F6 3_545 0.95 2.54 3.153(6) 122.2 yes N17 H17A F2 . 0.79 2.51 2.935(5) 115.3 yes N17 H17A F4 . 0.79 2.30 3.026(6) 152.2 yes N17 H17B F6A 1_545 0.79 2.23 3.019(5) 179.0 yes