data_9827-10660_ca263 _audit_creation_date 2018-10-25 _audit_creation_method ; Olex2 1.2-ac3 (compiled 2017.01.05 svn.r3372 for Rigaku Oxford Diffraction, GUI svn.r5289) ; _shelx_SHELXL_version_number '2014/7' _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_id_orcid ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C18 H17 F N2 O' _chemical_formula_sum 'C18 H17 F N2 O' _chemical_formula_weight 296.33 _chemical_melting_point ? _chemical_oxdiff_formula 'C17 F N2 O' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5047(3) _cell_length_b 9.2211(4) _cell_length_c 11.4499(6) _cell_angle_alpha 90.884(4) _cell_angle_beta 103.956(4) _cell_angle_gamma 95.264(4) _cell_volume 765.14(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4475 _cell_measurement_temperature 114(2) _cell_measurement_theta_max 72.1620 _cell_measurement_theta_min 3.9530 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91261 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 312 _exptl_crystal_preparation ? _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_unetI/netI 0.0312 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 9305 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.520 _diffrn_reflns_theta_min 3.981 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 114(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean ? _diffrn_detector_type HyPix3000 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -13.00 37.00 0.50 0.53 -- 38.95 -79.00 139.00 100 2 \w 82.00 110.00 0.50 2.12 -- 104.29 79.00 -96.00 56 3 \w 118.00 152.00 0.50 2.12 -- 104.29 79.00 -96.00 68 4 \w 60.00 129.00 0.50 2.12 -- 104.29 -79.00 139.00 138 5 \w -48.00 -16.00 0.50 0.53 -- -38.95 -65.00-120.00 64 6 \w -51.00 -22.00 0.50 0.53 -- -38.95 32.00-120.00 58 7 \w -35.00 6.00 0.50 0.53 -- -38.95 104.00 0.00 82 8 \w -100.00 -57.00 0.50 0.53 -- -38.95 -65.00-120.00 86 9 \w -77.00 -40.00 0.50 0.53 -- -38.95 104.00 0.00 74 10 \w -41.00 27.00 0.50 0.53 -- -38.95 79.00 -96.00 136 11 \w -2.00 24.00 0.50 0.53 -- -38.95 32.00-120.00 52 12 \w -101.00 -23.00 0.50 0.53 -- -38.95 -43.00 30.00 156 13 \w -58.00 -21.00 0.50 0.53 -- -38.95 54.00 30.00 74 14 \w 41.00 97.00 0.50 0.53 -- 38.95-138.00 -90.00 112 15 \w 11.00 38.00 0.50 0.53 -- 38.95-138.00 -90.00 54 16 \w 67.00 105.00 0.50 0.53 -- 38.95 43.00 0.00 76 17 \w -31.00 5.00 0.50 0.53 -- 38.95 -89.00 120.00 72 18 \w 27.00 52.00 0.50 0.53 -- 38.95 43.00 0.00 50 19 \w 1.00 51.00 0.50 0.53 -- 38.95 -65.00 60.00 100 20 \w 83.00 108.00 0.50 0.53 -- 38.95 32.00 -60.00 50 21 \w 14.00 39.00 0.50 0.53 -- 38.95 -32.00 -60.00 50 22 \w -26.00 11.00 0.50 0.53 -- 38.95 -43.00 120.00 74 23 \w 13.00 54.00 0.50 0.53 -- 38.95 -89.00 120.00 82 24 \w 49.00 79.00 0.50 0.53 -- 38.95 32.00 -60.00 60 25 \w -22.00 8.00 0.50 0.53 -- 38.95 -32.00 -60.00 60 26 \w 28.00 58.00 0.50 0.53 -- 38.95 -54.00 120.00 60 27 \w 11.00 37.00 0.50 0.53 -- 38.95 -54.00 0.00 52 28 \w 40.00 117.00 0.50 2.12 -- 104.29-133.00 -30.00 154 29 \w 82.00 157.00 0.50 2.12 -- 104.29 61.00 -60.00 150 30 \w 47.00 103.00 0.50 2.12 -- 104.29 -53.00-120.00 112 31 \w 67.00 110.00 0.50 2.12 -- 104.29-111.00 0.00 86 32 \w 45.00 124.00 0.50 2.12 -- 104.29 -53.00 120.00 158 33 \w 91.00 155.00 0.50 2.12 -- 104.29 30.00-150.00 128 34 \w 93.00 119.00 0.50 2.12 -- 104.29 15.00 0.00 52 35 \w 115.00 149.00 0.50 2.12 -- 104.29 37.00 90.00 68 36 \w 87.00 117.00 0.50 2.12 -- 104.29 -30.00 30.00 60 37 \w 66.00 105.00 0.50 2.12 -- 104.29 -37.00 120.00 78 38 \w 95.00 154.00 0.50 2.12 -- 104.29 37.00 -30.00 118 39 \w 82.00 107.00 0.50 2.12 -- 104.29 93.00 0.00 50 40 \w 35.00 77.00 0.50 2.12 -- 104.29-111.00 90.00 84 41 \w 35.00 68.00 0.50 2.12 -- 104.29 -30.00 30.00 66 42 \w 69.00 121.00 0.50 2.12 -- 104.29-133.00 150.00 104 43 \w 76.00 105.00 0.50 2.12 -- 104.29 -86.00 0.00 58 44 \w 38.00 64.00 0.50 2.12 -- 104.29 -37.00 120.00 52 45 \w 41.00 103.00 0.50 2.12 -- 104.29 -30.00 -90.00 124 46 \w 55.00 91.00 0.50 2.12 -- 104.29-111.00 -30.00 72 47 \w 39.00 73.00 0.50 2.12 -- 104.29 -86.00 0.00 68 48 \w 80.00 111.00 0.50 2.12 -- 104.29-111.00-180.00 62 49 \w 37.00 69.00 0.50 2.12 -- 104.29-111.00-180.00 64 50 \w 35.00 86.00 0.50 2.12 -- 104.29-111.00 150.00 102 51 \w 132.00 157.00 0.50 2.12 -- 104.29 93.00 0.00 50 52 \w 83.00 109.00 0.50 2.12 -- 104.29-111.00 -90.00 52 53 \w 85.00 121.00 0.50 2.12 -- 104.29 53.00 -90.00 72 54 \w 129.00 155.00 0.50 2.12 -- 104.29 15.00 0.00 52 55 \w 118.00 144.00 0.50 2.12 -- 104.29 45.00 0.00 52 56 \w 78.00 117.00 0.50 2.12 -- 104.29 133.00-180.00 78 57 \w 80.00 157.00 0.50 2.12 -- 104.29 111.00-150.00 154 58 \w 108.00 152.00 0.50 2.12 -- 104.29 133.00 150.00 88 59 \w 57.00 83.00 0.50 0.53 -- 38.95 54.00 150.00 52 60 \w -39.00 -14.00 0.50 0.53 -- 4.00 112.00 -98.86 50 61 \w -16.00 10.00 0.50 0.53 -- 20.00 106.00 -27.58 52 62 \w -8.00 17.00 0.50 0.53 -- 28.00 100.00-157.66 50 63 \w -1.00 24.00 0.50 0.53 -- 32.00 92.00 60.01 50 64 \w -1.00 24.00 0.50 0.53 -- 32.00 94.00 166.70 50 65 \w 6.00 31.00 0.50 0.53 -- 36.00 86.00-100.43 50 66 \w 6.00 31.00 0.50 0.53 -- 36.00 87.00 100.27 50 67 \w 5.00 30.00 0.50 0.53 -- 36.00 88.00 -24.17 50 68 \w 11.00 36.00 0.50 0.53 -- 40.00 84.00 34.47 50 69 \w 16.00 41.00 0.50 0.53 -- 44.00 82.00 56.70 50 70 \w 16.00 41.00 0.50 0.53 -- 44.00 80.00 89.97 50 71 \w 16.00 41.00 0.50 0.53 -- 44.00 81.00-171.93 50 72 \w 16.00 41.00 0.50 0.53 -- 44.00 82.00 133.16 50 73 \w 17.00 42.00 0.50 0.53 -- 44.00 79.00 -19.76 50 74 \w 16.00 41.00 0.50 0.53 -- 44.00 82.00 -83.99 50 75 \w 16.00 41.00 0.50 0.53 -- 44.00 82.00-129.09 50 76 \w 28.00 67.00 0.50 0.53 -- 48.00 71.00 44.87 78 77 \w 26.00 52.00 0.50 0.53 -- 52.00 77.00-161.73 52 78 \w 26.00 51.00 0.50 0.53 -- 52.00 76.00 161.90 50 79 \w 85.00 111.00 0.50 0.53 -- 56.00 77.00 44.15 52 80 \w 32.00 79.00 0.50 0.53 -- 56.00 77.00 44.15 94 81 \w 32.00 63.00 0.50 0.53 -- 56.00 69.00 -39.42 62 82 \w 35.00 110.00 0.50 0.53 -- 60.00 70.00 139.57 150 83 \w 100.00 126.00 0.50 0.53 -- 60.00 77.00 94.94 52 84 \w 33.00 83.00 0.50 0.53 -- 60.00 77.00 -6.97 100 85 \w 70.00 96.00 0.50 0.53 -- 60.00 64.00-166.07 52 86 \w 39.00 65.00 0.50 0.53 -- 60.00 64.00-166.07 52 87 \w 35.00 75.00 0.50 0.53 -- 60.00 76.00 -90.87 80 88 \w 37.00 63.00 0.50 0.53 -- 60.00 69.00-140.27 52 89 \w 35.00 75.00 0.50 0.53 -- 60.00 77.00 94.94 80 90 \w 42.00 67.00 0.50 0.53 -- 64.00 59.00-103.48 50 91 \w 80.00 123.00 0.50 0.53 -- 64.00 60.00-142.80 86 92 \w 43.00 69.00 0.50 0.53 -- 64.00 60.00-142.80 52 93 \w 41.00 80.00 0.50 0.53 -- 64.00 77.00 -44.19 78 94 \w 55.00 111.00 0.50 2.12 -- 80.00 73.00 88.75 112 95 \w 58.00 84.00 0.50 2.12 -- 84.00 76.00-126.20 52 96 \w 68.00 106.00 0.50 2.12 -- 92.00 68.00-171.76 76 97 \w 80.00 96.00 0.50 2.12 -- 104.29 77.00 -60.00 32 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, HyPix3000' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0286982000 _diffrn_orient_matrix_UB_12 -0.0832870000 _diffrn_orient_matrix_UB_13 -0.1106522000 _diffrn_orient_matrix_UB_21 -0.2095822000 _diffrn_orient_matrix_UB_22 -0.0419815000 _diffrn_orient_matrix_UB_23 -0.0422830000 _diffrn_orient_matrix_UB_31 -0.0207517000 _diffrn_orient_matrix_UB_32 0.1396163000 _diffrn_orient_matrix_UB_33 -0.0722394000 _diffrn_oxdiff_ac3_digest_frames ; 018a3a8329d960e9738ef92793e58bd39c000270d6d ; _diffrn_oxdiff_ac3_digest_hkl ; 01d9f97a38fe4ca6efd7efcae1c5d4f7fffafa ; _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2488 _reflns_number_total 2990 _reflns_odcompleteness_completeness 99.66 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 70.93 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.235 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.040 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 202 _refine_ls_number_reflns 2990 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0411 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+0.2111P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.1156 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C4(H4) 2.b Aromatic/amide H refined with riding coordinates: C7(H7), C6(H6), C12(H12), C10(H10), C9(H9), C15(H15), C14(H14) 2.c Idealised Me refined as rotating group: C18(H18A,H18B,H18C), C3(H3A,H3B,H3C), C17(H17A,H17B,H17C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group F1 F 0.84471(13) -0.10066(10) 0.68862(9) 0.0434(3) Uani 1 1 d . . . . . O1 O 0.00854(14) 0.35477(11) 0.42342(9) 0.0317(3) Uani 1 1 d . . . . . N2 N 0.29035(17) 0.35308(13) 0.53764(11) 0.0282(3) Uani 1 1 d . . . . . N1 N -0.00558(17) 0.26342(14) 0.52030(11) 0.0305(3) Uani 1 1 d . . . . . C5 C 0.3857(2) 0.10784(15) 0.69811(12) 0.0257(3) Uani 1 1 d . . . . . C4 C 0.21392(19) 0.18464(15) 0.69668(12) 0.0256(3) Uani 1 1 d . . . . . H4 H 0.1105 0.1067 0.6926 0.031 Uiso 1 1 calc R . . . . C1 C 0.1643(2) 0.26816(15) 0.58342(13) 0.0260(3) Uani 1 1 d . . . . . C11 C 0.22738(19) 0.28005(15) 0.80976(13) 0.0259(3) Uani 1 1 d . . . . . C7 C 0.7166(2) 0.10312(16) 0.74982(14) 0.0306(3) Uani 1 1 d . . . . . H7 H 0.8366 0.1474 0.7872 0.037 Uiso 1 1 calc R . . . . C6 C 0.5610(2) 0.17222(15) 0.75253(13) 0.0280(3) Uani 1 1 d . . . . . H6 H 0.5748 0.2652 0.7923 0.034 Uiso 1 1 calc R . . . . C8 C 0.6922(2) -0.03145(17) 0.69142(14) 0.0316(3) Uani 1 1 d . . . . . C12 C 0.2359(2) 0.43123(16) 0.80524(13) 0.0284(3) Uani 1 1 d . . . . . H12 H 0.2389 0.4754 0.7312 0.034 Uiso 1 1 calc R . . . . C16 C 0.2264(2) 0.21328(16) 0.91884(13) 0.0300(3) Uani 1 1 d . . . . . C2 C 0.1881(2) 0.40156(16) 0.44157(13) 0.0288(3) Uani 1 1 d . . . . . C13 C 0.2404(2) 0.52025(17) 0.90612(14) 0.0322(3) Uani 1 1 d . . . . . C10 C 0.3675(2) -0.02810(16) 0.63981(14) 0.0324(3) Uani 1 1 d . . . . . H10 H 0.2480 -0.0730 0.6020 0.039 Uiso 1 1 calc R . . . . C9 C 0.5213(2) -0.09914(17) 0.63603(15) 0.0359(4) Uani 1 1 d . . . . . H9 H 0.5087 -0.1920 0.5962 0.043 Uiso 1 1 calc R . . . . C15 C 0.2306(2) 0.30316(18) 1.01919(14) 0.0375(4) Uani 1 1 d . . . . . H15 H 0.2295 0.2601 1.0939 0.045 Uiso 1 1 calc R . . . . C14 C 0.2363(2) 0.45313(18) 1.01258(15) 0.0383(4) Uani 1 1 d . . . . . H14 H 0.2375 0.5108 1.0823 0.046 Uiso 1 1 calc R . . . . C18 C 0.2233(2) 0.05082(17) 0.93090(15) 0.0359(4) Uani 1 1 d . . . . . H18A H 0.1186 0.0023 0.8705 0.054 Uiso 1 1 calc GR . . . . H18B H 0.2109 0.0258 1.0116 0.054 Uiso 1 1 calc GR . . . . H18C H 0.3384 0.0186 0.9184 0.054 Uiso 1 1 calc GR . . . . C3 C 0.2437(2) 0.49633(18) 0.35087(15) 0.0373(4) Uani 1 1 d . . . . . H3A H 0.2178 0.4421 0.2734 0.056 Uiso 1 1 calc GR . . . . H3B H 0.3760 0.5277 0.3771 0.056 Uiso 1 1 calc GR . . . . H3C H 0.1741 0.5820 0.3420 0.056 Uiso 1 1 calc GR . . . . C17 C 0.2488(3) 0.68344(18) 0.89801(16) 0.0419(4) Uani 1 1 d . . . . . H17A H 0.3729 0.7269 0.9386 0.063 Uiso 1 1 calc GR . . . . H17B H 0.1584 0.7207 0.9369 0.063 Uiso 1 1 calc GR . . . . H17C H 0.2207 0.7090 0.8132 0.063 Uiso 1 1 calc GR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.0366(5) 0.0407(5) 0.0537(6) -0.0069(4) 0.0098(4) 0.0136(4) O1 0.0317(6) 0.0350(6) 0.0261(5) 0.0030(4) 0.0023(4) 0.0035(4) N2 0.0290(6) 0.0298(6) 0.0260(6) 0.0016(5) 0.0068(5) 0.0033(5) N1 0.0312(7) 0.0317(7) 0.0266(6) 0.0016(5) 0.0037(5) 0.0013(5) C5 0.0303(7) 0.0247(7) 0.0224(7) 0.0022(5) 0.0073(6) 0.0018(6) C4 0.0275(7) 0.0241(7) 0.0244(7) 0.0003(5) 0.0061(6) -0.0006(5) C1 0.0284(7) 0.0246(7) 0.0246(7) -0.0036(5) 0.0058(6) 0.0025(5) C11 0.0244(7) 0.0287(7) 0.0245(7) -0.0008(6) 0.0058(5) 0.0034(5) C7 0.0276(7) 0.0308(8) 0.0325(8) 0.0003(6) 0.0060(6) 0.0019(6) C6 0.0317(8) 0.0243(7) 0.0276(7) -0.0007(6) 0.0072(6) 0.0016(6) C8 0.0335(8) 0.0313(8) 0.0323(8) 0.0007(6) 0.0098(6) 0.0106(6) C12 0.0301(7) 0.0288(7) 0.0250(7) 0.0003(6) 0.0045(6) 0.0033(6) C16 0.0305(8) 0.0317(8) 0.0281(8) 0.0021(6) 0.0073(6) 0.0034(6) C2 0.0309(8) 0.0291(7) 0.0269(7) -0.0015(6) 0.0075(6) 0.0054(6) C13 0.0348(8) 0.0308(8) 0.0300(8) -0.0039(6) 0.0056(6) 0.0054(6) C10 0.0332(8) 0.0279(7) 0.0335(8) -0.0049(6) 0.0042(6) 0.0006(6) C9 0.0412(9) 0.0276(8) 0.0377(9) -0.0068(6) 0.0072(7) 0.0048(6) C15 0.0469(9) 0.0414(9) 0.0258(8) 0.0029(6) 0.0106(7) 0.0075(7) C14 0.0486(10) 0.0389(9) 0.0278(8) -0.0064(7) 0.0095(7) 0.0069(7) C18 0.0438(9) 0.0337(8) 0.0315(8) 0.0073(6) 0.0107(7) 0.0057(7) C3 0.0406(9) 0.0413(9) 0.0307(8) 0.0077(7) 0.0088(7) 0.0068(7) C17 0.0541(11) 0.0319(8) 0.0385(9) -0.0064(7) 0.0086(8) 0.0063(7) _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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F1 C8 1.3670(17) . ? O1 N1 1.4214(16) . ? O1 C2 1.3419(18) . ? N2 C1 1.3778(19) . ? N2 C2 1.2921(19) . ? N1 C1 1.3017(19) . ? C5 C4 1.523(2) . ? C5 C6 1.386(2) . ? C5 C10 1.391(2) . ? C4 H4 1.0000 . ? C4 C1 1.505(2) . ? C4 C11 1.5317(19) . ? C11 C12 1.392(2) . ? C11 C16 1.402(2) . ? C7 H7 0.9500 . ? C7 C6 1.388(2) . ? C7 C8 1.376(2) . ? C6 H6 0.9500 . ? C8 C9 1.373(2) . ? C12 H12 0.9500 . ? C12 C13 1.399(2) . ? C16 C15 1.399(2) . ? C16 C18 1.505(2) . ? C2 C3 1.479(2) . ? C13 C14 1.381(2) . ? C13 C17 1.506(2) . ? C10 H10 0.9500 . ? C10 C9 1.388(2) . ? C9 H9 0.9500 . ? C15 H15 0.9500 . ? C15 C14 1.383(2) . ? C14 H14 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 O1 N1 106.04(11) . . ? C2 N2 C1 102.59(12) . . ? C1 N1 O1 102.95(11) . . ? C6 C5 C4 121.67(13) . . ? C6 C5 C10 118.85(14) . . ? C10 C5 C4 119.44(13) . . ? C5 C4 H4 106.8 . . ? C5 C4 C11 114.24(12) . . ? C1 C4 C5 109.66(11) . . ? C1 C4 H4 106.8 . . ? C1 C4 C11 112.07(11) . . ? C11 C4 H4 106.8 . . ? N2 C1 C4 124.08(12) . . ? N1 C1 N2 114.86(13) . . ? N1 C1 C4 121.07(13) . . ? C12 C11 C4 121.12(13) . . ? C12 C11 C16 119.65(13) . . ? C16 C11 C4 119.21(13) . . ? C6 C7 H7 120.9 . . ? C8 C7 H7 120.9 . . ? C8 C7 C6 118.11(14) . . ? C5 C6 C7 121.09(13) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? F1 C8 C7 118.56(14) . . ? F1 C8 C9 118.65(14) . . ? C9 C8 C7 122.79(14) . . ? C11 C12 H12 118.9 . . ? C11 C12 C13 122.15(14) . . ? C13 C12 H12 118.9 . . ? C11 C16 C18 122.37(13) . . ? C15 C16 C11 117.79(14) . . ? C15 C16 C18 119.84(14) . . ? O1 C2 C3 117.60(13) . . ? N2 C2 O1 113.55(13) . . ? N2 C2 C3 128.83(14) . . ? C12 C13 C17 120.79(15) . . ? C14 C13 C12 117.68(14) . . ? C14 C13 C17 121.52(14) . . ? C5 C10 H10 119.5 . . ? C9 C10 C5 121.00(14) . . ? C9 C10 H10 119.5 . . ? C8 C9 C10 118.15(14) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? C16 C15 H15 119.1 . . ? C14 C15 C16 121.76(15) . . ? C14 C15 H15 119.1 . . ? C13 C14 C15 120.96(15) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _shelx_res_file ; 9827-10660_ca263.res created by SHELXL-2014/7 TITL 9827-10660_ca263_a.res in P-1 REM Old TITL 9827-10660_CA263 in P-1 REM SHELXT solution in P-1 REM R1 0.116, Rweak 0.004, Alpha 0.028, Orientation as input REM Formula found by SHELXT: C18 N2 O F1 CELL 1.54184 7.504745 9.22106 11.449888 90.8837 103.9559 95.2641 ZERR 2 0.000329 0.000415 0.00055 0.0038 0.0039 0.0036 LATT 1 SFAC C H F N O UNIT 36 34 2 4 2 L.S. 4 PLAN 5 TEMP -159(2) BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.053100 0.211100 FVAR 5.25037 F1 3 0.844715 -0.100665 0.688619 11.00000 0.03663 0.04072 = 0.05373 -0.00691 0.00977 0.01358 O1 5 0.008541 0.354773 0.423416 11.00000 0.03172 0.03501 = 0.02611 0.00304 0.00227 0.00353 N2 4 0.290351 0.353077 0.537636 11.00000 0.02897 0.02981 = 0.02601 0.00158 0.00681 0.00334 N1 4 -0.005576 0.263419 0.520298 11.00000 0.03124 0.03171 = 0.02660 0.00159 0.00366 0.00128 C5 1 0.385660 0.107843 0.698110 11.00000 0.03032 0.02465 = 0.02239 0.00223 0.00731 0.00179 C4 1 0.213924 0.184636 0.696679 11.00000 0.02754 0.02412 = 0.02444 0.00032 0.00607 -0.00063 AFIX 13 H4 2 0.110522 0.106709 0.692636 11.00000 -1.20000 AFIX 0 C1 1 0.164336 0.268161 0.583421 11.00000 0.02844 0.02455 = 0.02460 -0.00364 0.00582 0.00248 C11 1 0.227380 0.280053 0.809756 11.00000 0.02436 0.02869 = 0.02452 -0.00083 0.00578 0.00337 C7 1 0.716636 0.103120 0.749819 11.00000 0.02759 0.03081 = 0.03253 0.00035 0.00596 0.00186 AFIX 43 H7 2 0.836641 0.147439 0.787214 11.00000 -1.20000 AFIX 0 C6 1 0.560966 0.172224 0.752533 11.00000 0.03170 0.02434 = 0.02765 -0.00073 0.00721 0.00161 AFIX 43 H6 2 0.574760 0.265201 0.792350 11.00000 -1.20000 AFIX 0 C8 1 0.692248 -0.031449 0.691416 11.00000 0.03353 0.03126 = 0.03231 0.00070 0.00979 0.01061 C12 1 0.235949 0.431228 0.805242 11.00000 0.03010 0.02883 = 0.02502 0.00033 0.00447 0.00330 AFIX 43 H12 2 0.238890 0.475386 0.731227 11.00000 -1.20000 AFIX 0 C16 1 0.226405 0.213279 0.918844 11.00000 0.03045 0.03174 = 0.02806 0.00213 0.00727 0.00338 C2 1 0.188106 0.401563 0.441575 11.00000 0.03094 0.02913 = 0.02691 -0.00151 0.00751 0.00539 C13 1 0.240373 0.520248 0.906121 11.00000 0.03478 0.03082 = 0.02995 -0.00388 0.00559 0.00545 C10 1 0.367491 -0.028097 0.639812 11.00000 0.03320 0.02787 = 0.03348 -0.00494 0.00423 0.00059 AFIX 43 H10 2 0.247961 -0.072996 0.602005 11.00000 -1.20000 AFIX 0 C9 1 0.521320 -0.099143 0.636035 11.00000 0.04115 0.02764 = 0.03773 -0.00676 0.00724 0.00484 AFIX 43 H9 2 0.508728 -0.192030 0.596241 11.00000 -1.20000 AFIX 0 C15 1 0.230604 0.303155 1.019189 11.00000 0.04689 0.04144 = 0.02579 0.00289 0.01059 0.00747 AFIX 43 H15 2 0.229499 0.260065 1.093875 11.00000 -1.20000 AFIX 0 C14 1 0.236324 0.453131 1.012585 11.00000 0.04863 0.03894 = 0.02777 -0.00645 0.00950 0.00686 AFIX 43 H14 2 0.237483 0.510790 1.082292 11.00000 -1.20000 AFIX 0 C18 1 0.223306 0.050816 0.930898 11.00000 0.04375 0.03374 = 0.03146 0.00732 0.01069 0.00575 AFIX 137 H18A 2 0.118570 0.002270 0.870478 11.00000 -1.50000 H18B 2 0.210920 0.025837 1.011637 11.00000 -1.50000 H18C 2 0.338411 0.018559 0.918428 11.00000 -1.50000 AFIX 0 C3 1 0.243687 0.496326 0.350868 11.00000 0.04060 0.04131 = 0.03070 0.00768 0.00878 0.00678 AFIX 137 H3A 2 0.217829 0.442106 0.273373 11.00000 -1.50000 H3B 2 0.375994 0.527651 0.377103 11.00000 -1.50000 H3C 2 0.174078 0.582030 0.342010 11.00000 -1.50000 AFIX 0 C17 1 0.248836 0.683439 0.898007 11.00000 0.05409 0.03191 = 0.03852 -0.00639 0.00865 0.00632 AFIX 137 H17A 2 0.372860 0.726914 0.938640 11.00000 -1.50000 H17B 2 0.158425 0.720661 0.936910 11.00000 -1.50000 H17C 2 0.220731 0.708966 0.813189 11.00000 -1.50000 AFIX 0 HKLF 4 REM 9827-10660_ca263_a.res in P-1 REM R1 = 0.0411 for 2488 Fo > 4sig(Fo) and 0.0497 for all 2990 data REM 202 parameters refined using 0 restraints END WGHT 0.0531 0.2111 REM Highest difference peak 0.235, deepest hole -0.264, 1-sigma level 0.040 Q1 1 0.1420 0.5159 0.2856 11.00000 0.05 0.24 Q2 1 0.1305 0.7116 0.8467 11.00000 0.05 0.22 Q3 1 0.3376 0.7123 0.8400 11.00000 0.05 0.21 Q4 1 0.2913 0.5759 0.3841 11.00000 0.05 0.19 Q5 1 0.3490 0.4532 0.3221 11.00000 0.05 0.19 ; _shelx_res_checksum 82750 _shelx_hkl_file ; 0 0 1 16288.4 645.025 68 0 0 -1 15943.3 634.892 60 0 0 -1 16223.4 646.450 21 0 0 1 16369.1 645.410 12 0 0 2 293.563 34.8117 12 0 0 2 254.479 33.4614 16 0 0 -2 282.840 22.6030 17 0 0 2 388.446 38.9137 68 0 0 -2 294.672 23.5437 60 0 0 -2 258.939 36.4093 21 0 0 -3 36660.9 1539.91 21 0 0 3 37833.4 1537.04 68 0 0 3 37866.0 1537.49 84 0 0 3 39849.3 1540.01 12 0 0 3 38306.9 1533.87 16 0 0 -3 38365.0 1537.77 7 0 0 4 277.748 50.9755 16 0 0 4 312.455 50.6810 68 0 0 4 389.173 51.7164 63 0 0 4 414.663 57.9148 12 0 0 -4 414.305 60.9339 21 0 0 4 299.818 52.7235 84 0 0 -4 350.213 58.7313 7 0 0 5 6637.24 331.166 84 0 0 -5 6346.27 336.454 21 0 0 5 6314.39 329.270 76 0 0 -5 6225.45 327.500 7 0 0 5 6385.65 328.646 68 0 0 5 6251.36 322.825 16 0 0 5 6170.57 325.710 12 0 0 5 6380.11 314.450 63 0 0 -6 394.880 73.4459 7 0 0 6 414.821 72.5206 84 0 0 6 440.976 77.1058 68 0 0 6 569.970 86.6571 12 0 0 6 351.572 69.5194 69 0 0 -6 416.427 77.1125 21 0 0 6 503.880 79.5391 76 0 0 6 355.349 75.2684 80 0 0 7 84.0791 50.2910 76 0 0 7 28.5329 51.1997 80 0 0 -7-14.1622 49.2120 7 0 0 7 67.9127 50.2457 84 0 0 8 6388.61 403.575 76 0 0 -8 6769.61 412.602 7 0 0 -8 6800.52 325.868 45 0 0 8 7040.26 407.053 84 0 0 8 6794.93 411.982 80 0 0 9 3253.46 276.882 80 0 0 -9 3310.46 279.869 7 0 0 -9 3423.29 199.214 45 0 0 -9 3370.21 295.736 27 0 0 9 3918.58 293.025 76 0 0 -10 2331.61 159.963 45 0 0 -10 2612.94 144.752 58 0 0 10 2390.40 237.053 76 0 0 -11 1829.50 111.064 58 0 0 -11 1543.88 124.660 45 0 0 -12 458.115 61.4665 45 0 0 -12 465.453 52.9569 58 0 0 13 146.747 30.6058 39 0 0 -13 165.352 31.3734 58 0 1 -13 855.862 61.2749 58 0 1 -12 1055.96 77.0176 58 0 1 -11 2490.80 141.673 58 0 -1 10 2679.84 264.568 76 0 -1 10 2857.53 265.919 80 0 1 -10 3045.64 162.936 58 0 1 -9 1887.05 114.583 58 0 1 -9 1684.56 117.313 47 0 1 -9 2002.94 218.189 27 0 -1 9 1619.12 189.873 76 0 1 -9 1716.28 195.478 7 0 -1 9 2125.72 216.552 80 0 -1 8 1374.43 160.875 76 0 1 -8 1250.63 163.132 27 0 1 -8 1449.04 164.837 7 0 -1 8 1129.48 145.491 69 0 -1 8 1462.68 170.724 80 0 -1 7 2786.84 212.703 84 0 -1 7 2933.19 222.413 68 0 -1 7 2875.47 220.104 69 0 -1 7 3061.63 225.756 76 0 1 -7 2709.66 216.587 7 0 -1 6 1787.71 161.537 68 0 1 -6 2381.38 176.882 7 0 -1 6 2269.63 176.048 76 0 -1 6 2077.88 164.549 84 0 -1 6 2157.33 163.031 63 0 1 -6 2088.39 169.290 21 0 -1 5 56734.4 2312.91 68 0 -1 5 59192.6 2308.92 84 0 1 -5 55212.2 2315.54 21 0 1 -5 57295.9 2312.12 7 0 -1 5 55814.9 2303.11 63 0 -1 4 5871.78 285.332 84 0 1 -4 5558.57 285.814 7 0 1 -4 5807.09 288.286 21 0 -1 4 5942.62 290.293 68 0 -1 4 5740.77 280.201 12 0 -1 4 5303.77 272.720 73 0 -1 3 128573. 5112.13 12 0 1 -3 133857. 5120.70 21 0 -1 3 129398. 5113.49 67 0 1 -3 127964. 5121.26 7 0 -1 3 130161. 5112.38 73 0 -1 2 107031. 4134.81 67 0 1 -2 106812. 4140.88 14 0 1 -2 106996. 4141.04 7 0 1 -2 103911. 4129.24 23 0 1 -2 105578. 4111.80 26 0 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101.041 25.4890 35 -8 1 -3 84.6885 30.3082 41 -8 1 -4 706.418 50.7066 41 -8 0 9 1496.30 94.0533 38 -8 0 9 1318.80 83.3581 34 -8 0 9 1582.22 81.7473 29 8 0 -9 1379.62 89.8335 45 -8 0 8 4.62493 31.8779 38 -8 0 8 29.5055 24.9825 29 -8 0 7 386.080 57.6987 38 -8 0 7 563.058 51.8754 29 -8 0 6 187.747 51.7813 38 -8 0 6 245.382 39.7103 29 -8 0 5 3.75522 26.3110 29 8 0 -4 14.2196 32.3874 35 8 0 -3 167.528 40.5801 35 8 0 -2 1388.31 96.8626 35 8 0 -1 2721.83 149.980 35 8 0 0 1771.89 110.537 35 8 0 0 1846.75 107.617 94 8 0 1 715.271 62.7115 35 8 0 2 6.88035 25.0731 35 8 0 3 586.704 46.9511 35 -8 0 -3 388.497 43.1020 41 -8 -1 9 13.6885 27.1149 38 -8 -1 9 6.38543 18.2177 29 -8 -1 8 30.6598 34.9310 38 -8 -1 8 13.7948 22.4240 29 -8 -1 7 911.065 83.9537 38 -8 -1 7 1116.45 72.2961 29 -8 -1 6 21.0605 28.1759 29 -8 -1 5 508.390 52.4316 29 8 1 -4 778.797 70.5792 35 8 1 -3 68.7223 35.2176 35 8 1 -2 489.711 58.6718 35 8 1 -1 1108.44 82.0670 35 8 1 0 49.3712 30.9396 35 8 1 1 96.7913 32.4264 35 8 1 2 121.624 31.6786 35 8 1 3 17.8012 20.0303 35 -8 -2 8 180.314 38.7435 38 -8 -2 8 229.517 30.2995 29 -8 -2 7 592.283 64.1744 38 -8 -2 7 715.085 54.5401 29 -8 -2 6 246.952 36.9801 29 -8 -2 5 197.885 35.6742 29 -8 -2 4 1095.01 73.4395 2 -8 -2 4 840.163 67.8247 29 8 2 -3 4.07787 28.3404 35 -8 -2 3 21.4729 28.3586 2 8 2 -2 36.2484 29.2119 35 -8 -2 2 50.6255 33.5798 53 -8 -2 2 79.8380 28.7928 2 8 2 -1 30.9340 29.4544 35 -8 -2 1 26.0787 28.7711 53 8 2 0 530.910 51.6298 35 8 2 1 105.011 27.5378 35 8 2 2-15.8435 21.1963 35 -8 -3 8 232.547 37.0325 38 -8 -3 8 346.616 31.2230 29 -8 -3 7 132.778 27.0997 29 -8 -3 7 150.784 25.5781 97 -8 -3 6 35.7040 22.2178 29 -8 -3 5 383.872 40.1250 2 -8 -3 5 354.593 40.0129 29 -8 -3 4 49.2983 25.6411 29 8 3 -4 26.7388 22.9043 28 -8 -3 4 6.08587 22.8611 2 -8 -3 3 6.62153 24.6760 53 8 3 -3-28.1989 24.4004 28 -8 -3 3-9.31101 22.2796 2 -8 -3 2 33.4384 24.9226 53 8 3 -2-11.2727 24.1222 28 -8 -3 2 26.8627 23.8041 2 -8 -3 1 216.770 35.2266 53 -8 -3 1 216.742 31.8818 2 -8 -3 0 8.51046 21.1417 53 8 3 1 92.7120 21.1046 28 -8 -4 6 40.1041 19.9207 29 -8 -4 5 36.6067 21.2476 29 -8 -4 5 10.8746 18.3224 2 -8 -4 4 80.3020 23.4790 29 8 4 -4 82.5191 21.7257 28 -8 -4 4 67.5267 23.0922 2 -8 -4 3 50.9818 23.7517 53 8 4 -3 127.144 26.4492 28 -8 -4 3 135.445 27.0649 2 -8 -4 2 577.862 46.1439 2 -8 -4 2 577.789 48.2043 53 8 4 -2 691.210 48.0313 28 -8 -4 1 140.250 25.9550 53 -8 -4 1 127.798 22.6219 2 8 4 -1 89.1501 22.2830 28 -8 -4 0 21.1646 18.3122 53 8 4 0-1.67175 15.2968 28 -9 3 5 306.126 28.9976 3 -9 3 4 194.898 25.5757 3 -9 3 3 366.356 33.0646 50 -9 3 3 389.655 34.3462 3 -9 3 2 1.81725 16.4666 3 -9 3 2 13.6970 17.9887 50 -9 3 1 244.332 26.5295 50 -9 2 5 13.5562 17.7248 3 -9 2 4 58.0321 20.9783 3 -9 2 3 311.607 33.4983 3 -9 2 2 52.6569 21.1313 3 -9 1 6 121.587 26.2734 34 -9 1 5-6.05926 17.0948 3 -9 1 4 26.6632 20.6445 3 -9 1 3 143.578 25.9094 3 -9 1 2 1012.07 60.8937 3 9 -1 -1 311.746 33.3458 35 -9 0 5-1.95816 17.1216 3 -9 0 4 109.815 23.5719 3 -9 0 3 86.6467 22.4965 3 -9 0 2 59.8308 20.6872 3 9 0 -1 217.440 28.9377 35 -9 -1 5 145.011 22.8215 3 -9 -1 4 228.576 26.6570 3 -9 -1 3-3.88135 16.9692 3 -9 -1 2 380.693 33.2102 3 9 1 -2 436.356 33.6582 28 0 0 0 0.00 0.00 0 TITL 9827-10660_CA263 in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 7.504745 9.221060 11.449888 90.8837 103.9559 95.2641 ZERR 2.00 0.000329 0.000415 0.000550 0.0038 0.0039 0.0036 LATT 1 SFAC C N O F UNIT 34.00 4.00 2.00 2.00 TREF HKLF 4 END ; _shelx_hkl_checksum 26936 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.048 _oxdiff_exptl_absorpt_empirical_full_min 0.766