#------------------------------------------------------------------------------ #$Date: 2019-01-16 05:21:00 +0200 (Wed, 16 Jan 2019) $ #$Revision: 213103 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/28/2242803.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_2242803 loop_ _publ_author_name 'Mahesha, Ninganayaka' 'Sagar, Belakavadi K.' 'Yathirajan, Hemmige S.' 'Furuya, Tetsundo' 'Haraguchi, Tomoyuki' 'Akitsu, Takashiro' 'Glidewell, Christopher' _publ_section_title ; Three closely related 1-[(1,3-benzodioxol-5-yl)methyl]-4-(halobenzoyl)piperazines: similar molecular structures but different intermolecular interactions ; _journal_coeditor_code ZL2747 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 202 _journal_page_last 207 _journal_paper_doi 10.1107/S2056989019000458 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac 'C19 H19 F N2 O3' _chemical_formula_moiety 'C19 H19 F N2 O3' _chemical_formula_sum 'C19 H19 F N2 O3' _chemical_formula_weight 342.36 _chemical_name_systematic ; 1-[(1,3-Benzodioxol-5-yl)methyl]-4-(3-fluorobenzoyl)piperazine ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014 _cell_angle_alpha 90 _cell_angle_beta 111.199(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.2358(16) _cell_length_b 10.3185(14) _cell_length_c 14.2310(19) _cell_measurement_reflns_used 3689 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.574 _cell_measurement_theta_min 1.887 _cell_volume 1675.2(4) _computing_cell_refinement ; SAINT (Bruker, 2013) ; _computing_data_collection ; APEX2 (Bruker, 2004) ; _computing_data_reduction ; SAINT (Bruker, 2013) ; _computing_molecular_graphics ; PLATON (Spek, 2009) ; _computing_publication_material ; SHELXL2014 and PLATON (Spek, 2009) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick,2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick 2015) ; _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 0.3333 _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.946 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_unetI/netI 0.0279 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 8635 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.573 _diffrn_reflns_theta_min 1.887 _diffrn_source 'fine focus sealed tube' _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_T_max 0.972 _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.357 _exptl_crystal_description block _exptl_crystal_F_000 720 _exptl_crystal_size_max 0.479 _exptl_crystal_size_mid 0.293 _exptl_crystal_size_min 0.282 _refine_diff_density_max 0.238 _refine_diff_density_min -0.179 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 226 _refine_ls_number_reflns 3674 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.096 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0397 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+0.4713P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1084 _refine_ls_wR_factor_ref 0.1141 _reflns_number_gt 2975 _reflns_number_total 3674 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file zl2747sup1.cif _cod_data_source_block I _cod_database_code 2242803 _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 0.954 _shelx_estimated_absorpt_t_max 0.972 _shelx_hkl_file ; 1 0 0 0.00 0.10 1 0 0 0.00 0.10 -2 0 0 29.80 0.90 2 0 0 30.70 1.00 2 0 0 29.80 1.20 -3 0 0 -0.10 0.10 3 0 0 0.20 0.20 3 0 0 0.00 0.30 4 0 0 1675.83 44.80 4 0 0 1688.13 43.80 -4 0 0 1677.83 43.50 5 0 0 0.00 0.40 5 0 0 0.20 0.20 -5 0 0 0.10 0.20 6 0 0 22.20 1.40 -6 0 0 21.50 0.90 6 0 0 22.60 1.00 -7 0 0 0.00 0.30 7 0 0 -0.20 0.30 7 0 0 -0.20 0.50 8 0 0 60.29 2.70 8 0 0 60.39 2.10 9 0 0 0.00 0.40 9 0 0 -0.50 0.70 10 0 0 12.90 1.00 10 0 0 11.90 1.50 11 0 0 0.00 0.90 11 0 0 0.70 0.50 12 0 0 3.70 1.20 13 0 0 0.90 1.10 14 0 0 5.10 1.40 0 -1 0 -2.60 0.10 1 -1 0 54.79 1.80 -1 -1 0 51.89 1.70 -1 1 0 54.69 1.80 -2 -1 0 738.03 19.70 2 -1 0 760.12 20.00 2 -1 0 760.22 19.80 2 1 0 761.52 19.60 -2 1 0 760.52 19.80 3 -1 0 1990.40 65.79 3 -1 0 1942.31 50.69 -3 -1 0 1940.11 54.59 -3 1 0 1983.50 50.59 3 1 0 1919.01 51.79 3 1 0 1944.91 50.39 4 -1 0 98.49 3.00 4 -1 0 98.09 2.80 -4 -1 0 100.19 2.80 4 1 0 100.19 2.80 -4 1 0 100.19 2.80 4 1 0 91.89 3.20 5 -1 0 0.70 0.30 5 -1 0 0.00 0.30 -5 -1 0 0.10 0.20 -5 1 0 0.20 0.20 5 1 0 0.20 0.40 5 1 0 -0.10 0.20 6 -1 0 170.98 4.80 6 -1 0 169.08 5.20 -6 -1 0 167.98 4.70 -6 1 0 172.88 4.70 6 1 0 171.88 4.70 6 1 0 167.08 5.40 7 -1 0 28.60 1.60 -7 -1 0 28.50 1.20 7 -1 0 30.70 1.30 -7 1 0 28.10 1.20 7 1 0 27.40 1.80 7 1 0 28.30 1.20 8 -1 0 56.79 2.50 8 -1 0 53.89 2.00 -8 1 0 52.79 1.90 8 1 0 57.29 2.70 8 1 0 55.89 2.00 9 -1 0 2.60 0.60 9 -1 0 3.20 0.90 9 1 0 2.30 0.90 9 1 0 2.50 0.50 10 -1 0 -0.30 0.40 10 -1 0 0.50 0.80 10 1 0 -0.20 0.80 10 1 0 0.10 0.40 11 -1 0 313.17 9.70 11 -1 0 319.47 9.10 11 1 0 326.67 10.10 12 -1 0 55.69 3.00 12 1 0 54.09 3.20 13 -1 0 1.10 1.60 13 1 0 1.10 1.10 14 1 0 7.40 1.70 0 -2 0 1731.73 45.10 -1 -2 0 4312.57 121.99 1 -2 0 4110.69 122.69 2 -2 0 6236.88 180.28 -2 -2 0 6302.67 176.58 -2 2 0 6383.16 177.68 2 2 0 6546.85 177.38 -3 -2 0 404.16 10.40 3 -2 0 399.76 10.50 3 -2 0 394.26 10.50 3 2 0 394.86 10.40 -3 2 0 400.06 10.40 4 -2 0 25.70 1.10 4 -2 0 27.50 1.10 -4 -2 0 26.70 1.00 4 2 0 26.60 1.00 4 2 0 24.20 1.40 -4 2 0 26.40 1.00 5 -2 0 0.00 0.30 -5 -2 0 0.10 0.20 5 -2 0 0.10 0.40 5 2 0 -0.20 0.30 -5 2 0 0.10 0.20 5 2 0 -0.20 0.50 6 -2 0 152.88 4.60 6 -2 0 151.18 4.40 -6 -2 0 151.88 4.30 -6 2 0 150.08 4.30 6 2 0 149.59 5.00 6 2 0 155.68 4.30 7 -2 0 87.39 2.90 -7 -2 0 88.49 2.70 7 -2 0 88.69 3.10 7 2 0 89.99 2.70 7 2 0 85.89 3.50 -7 2 0 89.79 2.70 8 -2 0 52.39 2.00 8 -2 0 47.80 2.20 -8 2 0 49.20 1.80 8 2 0 50.39 1.80 8 2 0 48.60 2.60 9 -2 0 2.40 0.60 9 -2 0 2.20 0.80 9 2 0 2.00 0.50 9 2 0 2.90 1.10 10 -2 0 10.80 1.30 10 -2 0 11.30 1.10 10 2 0 12.30 1.70 11 -2 0 0.20 0.70 11 -2 0 0.50 0.60 11 2 0 0.80 1.00 12 -2 0 11.00 1.20 12 2 0 6.80 1.60 13 2 0 1.60 1.30 14 2 0 47.30 3.50 0 -3 0 -0.20 0.20 1 -3 0 1948.31 50.89 -1 -3 0 1925.61 50.69 -2 -3 0 112.79 3.30 -3 -3 0 369.16 9.60 3 -3 0 351.56 9.70 3 3 0 384.06 9.60 -3 3 0 349.87 9.70 4 -3 0 538.45 14.20 -4 -3 0 537.65 14.00 4 3 0 534.65 14.00 -4 3 0 534.35 14.10 -5 -3 0 2.90 0.40 5 -3 0 3.10 0.50 -5 3 0 2.90 0.40 5 3 0 3.50 0.40 5 3 0 3.10 0.80 -6 -3 0 14.60 0.80 6 -3 0 16.90 1.00 6 -3 0 16.80 1.10 6 3 0 17.10 1.50 6 3 0 15.80 0.90 -6 3 0 15.70 0.90 7 -3 0 24.40 1.40 7 -3 0 22.20 1.20 -7 3 0 22.70 1.10 7 3 0 22.80 1.80 7 3 0 25.30 1.20 8 -3 0 2.00 0.70 8 -3 0 4.20 0.70 8 3 0 3.30 1.00 -8 3 0 3.20 0.50 8 3 0 3.50 0.60 9 -3 0 0.60 0.60 9 -3 0 1.90 0.60 9 3 0 1.30 0.90 -9 3 0 0.50 0.40 10 -3 0 0.20 0.50 10 3 0 0.20 1.00 11 -3 0 11.00 1.20 11 3 0 11.30 1.80 12 -3 0 95.39 3.60 12 3 0 96.59 4.60 13 -3 0 80.49 3.40 13 3 0 92.79 4.60 14 3 0 3.10 1.60 0 -4 0 188.08 5.40 1 -4 0 66.19 2.20 -1 -4 0 65.19 2.20 -2 -4 0 1.20 0.40 2 -4 0 1.70 0.40 -3 -4 0 347.57 9.30 3 -4 0 343.27 9.40 -3 4 0 348.57 9.40 4 -4 0 70.79 2.50 -4 -4 0 77.69 2.40 -4 4 0 69.09 2.40 4 4 0 79.99 2.40 5 -4 0 85.49 2.80 -5 -4 0 80.69 2.60 5 4 0 85.49 3.30 5 4 0 81.59 2.60 -5 4 0 85.49 2.70 -6 -4 0 2.90 0.50 6 -4 0 1.60 0.50 -6 4 0 1.30 0.40 6 4 0 1.50 0.80 6 4 0 2.00 0.50 7 -4 0 27.50 1.40 -7 4 0 26.60 1.30 7 4 0 27.20 2.00 7 4 0 28.30 1.30 8 -4 0 0.00 0.50 8 4 0 0.10 0.90 -8 4 0 0.30 0.40 8 4 0 0.50 0.70 9 -4 0 8.30 1.00 9 4 0 7.30 1.40 -9 4 0 7.40 0.80 10 4 0 1.60 1.10 11 -4 0 0.00 0.60 11 4 0 -0.80 1.00 12 -4 0 0.00 0.60 12 4 0 -0.40 1.20 13 -4 0 9.00 1.30 13 4 0 12.80 2.10 0 -5 0 0.50 0.40 1 -5 0 128.39 4.00 -1 -5 0 131.39 4.00 -2 -5 0 77.59 2.70 2 -5 0 82.49 2.80 -3 -5 0 31.20 1.40 -3 5 0 28.70 1.40 4 -5 0 98.09 3.30 -4 -5 0 102.29 3.20 4 5 0 97.79 3.10 -4 5 0 95.99 3.20 -5 -5 0 2.30 0.50 5 -5 0 1.40 0.50 5 5 0 1.30 0.40 -5 5 0 1.70 0.40 5 5 0 1.50 0.80 6 -5 0 54.59 2.20 -6 -5 0 48.40 1.90 -6 5 0 49.70 2.00 6 5 0 54.69 1.90 6 5 0 51.79 2.70 7 -5 0 14.80 1.20 7 5 0 17.00 1.80 -7 5 0 15.40 1.00 7 5 0 14.40 1.00 8 -5 0 40.20 2.00 -8 5 0 39.50 1.70 8 5 0 37.90 2.60 9 -5 0 76.29 3.00 9 5 0 77.29 3.80 -9 5 0 76.89 2.80 10 -5 0 1.40 0.70 10 5 0 1.00 1.10 11 -5 0 0.50 0.70 11 5 0 0.50 1.10 12 -5 0 0.90 0.80 12 5 0 -0.20 1.20 13 -5 0 0.20 0.80 13 5 0 1.00 1.40 0 -6 0 22.60 1.30 1 -6 0 1.00 0.50 -1 -6 0 0.50 0.40 -2 -6 0 123.79 4.00 -3 -6 0 21.90 1.30 -3 6 0 20.10 1.20 -4 -6 0 29.00 1.50 -4 6 0 29.50 1.50 -5 -6 0 17.70 1.20 5 -6 0 20.00 1.30 5 6 0 19.80 1.10 -5 6 0 19.50 1.20 5 6 0 19.00 1.70 6 -6 0 245.38 7.10 -6 -6 0 225.78 7.20 -6 6 0 235.58 6.80 6 6 0 229.58 6.70 6 6 0 238.98 7.60 7 -6 0 154.98 5.00 -7 6 0 149.88 4.80 7 6 0 155.98 5.60 8 -6 0 3.70 0.80 -8 6 0 2.90 0.60 8 6 0 2.80 1.10 9 -6 0 12.40 1.30 9 6 0 10.90 1.70 -9 6 0 12.50 1.10 10 -6 0 -0.90 0.60 -10 6 0 -0.10 0.50 10 6 0 -1.10 1.00 11 -6 0 3.70 1.00 11 6 0 3.50 1.40 12 -6 0 -0.50 0.70 12 6 0 -0.20 1.20 13 -6 0 0.10 0.80 0 -7 0 1.10 0.50 -1 -7 0 59.19 2.40 1 -7 0 58.49 2.40 -2 -7 0 49.50 2.20 -3 -7 0 26.20 1.50 -3 7 0 22.80 1.40 -4 -7 0 150.28 4.70 -4 7 0 144.19 4.60 -5 -7 0 206.38 6.10 -5 7 0 196.08 6.00 5 7 0 198.78 5.90 5 7 0 200.08 6.70 6 7 0 11.20 1.50 -6 7 0 13.30 1.10 7 7 0 43.70 2.70 -7 7 0 41.50 2.00 8 -7 0 4.30 1.00 8 7 0 5.00 1.30 -8 7 0 4.20 0.80 9 -7 0 4.60 1.00 -9 7 0 6.50 0.90 9 7 0 6.20 1.50 10 -7 0 1.10 0.80 -10 7 0 0.80 0.60 10 7 0 0.30 1.10 11 -7 0 16.00 1.70 11 7 0 15.20 2.10 12 -7 0 1.50 1.00 12 7 0 2.40 1.50 0 -8 0 1321.77 34.70 -1 -8 0 78.09 3.10 1 -8 0 83.99 3.20 -2 -8 0 12.00 1.20 -3 -8 0 25.70 1.70 -3 8 0 28.80 1.60 -4 -8 0 331.87 9.70 -4 8 0 343.87 9.70 -5 -8 0 73.49 2.90 5 8 0 69.29 3.30 -5 8 0 69.69 2.80 6 8 0 15.60 1.90 -6 8 0 17.50 1.30 -7 8 0 9.00 1.00 7 8 0 8.50 1.50 8 8 0 69.99 3.70 -8 8 0 73.59 2.90 -9 8 0 0.60 0.60 9 8 0 0.20 1.00 10 8 0 8.60 1.80 -10 8 0 7.60 1.10 11 8 0 -0.30 1.10 0 -9 0 0.20 0.70 -1 -9 0 24.90 1.80 -2 -9 0 27.70 1.80 -2 9 0 31.20 1.80 -3 -9 0 180.78 5.90 -3 9 0 178.68 5.70 -4 -9 0 18.50 1.50 4 9 0 17.20 1.90 -4 9 0 19.30 1.50 -5 -9 0 15.60 1.80 -5 9 0 21.90 1.50 5 9 0 25.40 2.10 6 9 0 36.30 2.60 -6 9 0 35.40 2.00 7 9 0 29.80 2.50 -7 9 0 27.50 1.80 8 9 0 3.20 1.30 -8 9 0 2.80 0.80 -9 9 0 8.50 1.10 9 9 0 8.60 1.70 10 9 0 36.00 3.10 -10 9 0 37.60 2.20 -1 -10 0 3.40 0.90 -1 10 0 2.40 0.80 -2 -10 0 256.87 8.40 -2 10 0 292.97 8.40 -3 -10 0 5.20 1.00 -3 10 0 2.70 0.80 -4 -10 0 17.80 1.60 -4 10 0 14.90 1.50 5 10 0 3.30 1.30 -5 10 0 3.90 0.90 6 10 0 12.70 1.80 -6 10 0 13.80 1.50 7 10 0 -0.30 1.00 -7 10 0 -0.50 0.60 -8 10 0 2.40 0.80 8 10 0 1.60 1.30 -9 10 0 24.00 1.80 9 10 0 22.70 2.60 0 11 0 -0.10 0.60 -1 11 0 0.50 0.70 -2 -11 0 2.20 0.90 -2 11 0 2.60 0.80 -3 -11 0 34.30 2.30 -3 11 0 43.30 2.40 -4 -11 0 23.30 1.90 -4 11 0 27.00 1.90 -5 11 0 1.10 0.80 -6 11 0 19.60 1.70 -7 11 0 0.90 0.80 -8 11 0 1.50 0.80 8 11 0 0.90 1.30 0 12 0 27.40 2.00 1 12 0 0.50 0.70 -1 12 0 0.30 0.70 -2 12 0 -0.30 0.70 -3 12 0 0.50 0.80 -4 12 0 29.30 2.20 -5 12 0 -0.40 0.70 0 13 0 0.60 0.80 -1 13 0 -0.20 0.80 1 13 0 -0.30 0.70 -2 13 0 8.70 1.70 2 13 0 7.50 1.30 3 13 0 4.10 1.00 14 0 -1 1.40 1.10 13 0 -1 119.49 5.00 12 0 -1 -1.10 0.90 12 0 -1 0.00 0.50 11 0 -1 129.29 5.00 11 0 -1 128.59 4.20 10 0 -1 0.10 0.40 10 0 -1 -0.50 0.80 9 0 -1 12.90 1.50 9 0 -1 11.20 0.90 8 0 -1 0.20 0.60 8 0 -1 -0.10 0.30 7 0 -1 192.68 5.90 7 0 -1 189.88 5.40 -7 0 1 186.78 5.10 6 0 -1 -0.10 0.50 -6 0 1 -0.10 0.20 6 0 -1 -0.10 0.30 5 0 -1 289.07 7.70 -5 0 1 288.67 7.50 5 0 -1 283.07 8.10 -4 0 1 0.00 0.10 4 0 -1 0.10 0.30 4 0 -1 -0.10 0.20 -3 0 1 649.14 16.70 3 0 -1 647.84 17.10 2 0 -1 -2.50 0.10 1 0 -1 260.67 7.00 0 0 -1 -2.40 0.10 -1 0 -1 346.57 9.30 1 0 1 354.76 9.20 1 0 1 352.36 9.20 2 0 1 0.10 0.10 2 0 1 0.10 0.30 -2 0 -1 0.10 0.20 -3 0 -1 7481.85 205.38 3 0 1 7355.46 210.08 3 0 1 7691.63 204.68 4 0 1 -0.30 0.30 4 0 1 -0.10 0.20 -4 0 -1 -0.10 0.20 5 0 1 68.49 2.10 -5 0 -1 65.19 2.10 5 0 1 66.99 2.50 6 0 1 0.00 0.20 6 0 1 0.40 0.50 -6 0 -1 -0.10 0.30 -7 0 -1 49.90 1.80 7 0 1 51.79 1.80 7 0 1 49.60 2.30 8 0 1 -0.40 0.30 -8 0 -1 -0.20 0.30 8 0 1 -0.10 0.60 9 0 1 2.70 0.50 9 0 1 2.20 0.90 10 0 1 -0.20 0.80 10 0 1 0.00 0.40 11 0 1 6.10 1.30 12 0 1 0.80 1.10 13 0 1 3.90 1.30 14 0 1 -0.10 1.10 15 1 -1 12.10 2.00 14 1 -1 0.20 1.10 13 -1 -1 13.30 2.10 13 1 -1 12.60 1.90 12 -1 -1 4.90 0.90 12 -1 -1 4.70 1.20 12 1 -1 4.40 1.30 11 -1 -1 0.70 0.90 11 -1 -1 0.40 0.50 11 1 -1 0.60 1.00 11 1 -1 1.60 0.60 10 -1 -1 92.89 3.20 10 -1 -1 96.09 3.80 10 1 -1 91.39 4.00 10 1 -1 97.39 3.20 9 -1 -1 4.20 0.70 9 -1 -1 2.40 0.90 9 1 -1 4.00 0.60 9 1 -1 2.80 0.90 8 -1 -1 231.68 7.00 8 -1 -1 232.98 6.60 8 1 -1 238.58 6.50 8 1 -1 235.28 7.30 -8 1 1 228.08 6.40 7 -1 -1 51.49 2.20 7 -1 -1 48.80 1.80 -7 -1 1 50.39 1.60 7 1 -1 47.50 2.30 -7 1 1 51.29 1.60 7 1 -1 51.99 1.80 6 -1 -1 -0.10 0.40 6 -1 -1 -0.10 0.30 -6 -1 1 0.00 0.20 6 1 -1 0.20 0.30 6 1 -1 -0.10 0.50 -6 1 1 0.00 0.20 5 -1 -1 65.39 2.30 -5 -1 1 62.19 1.80 5 -1 -1 64.49 2.00 5 1 -1 62.49 2.00 -5 1 1 63.39 1.90 -4 -1 1 114.79 3.20 4 -1 -1 124.69 3.50 4 -1 -1 115.59 3.40 -4 1 1 121.29 3.30 4 1 -1 119.69 3.40 3 -1 -1 165.68 4.50 3 -1 -1 168.48 4.60 3 1 -1 169.48 4.60 -3 1 1 168.88 4.50 2 -1 -1 6.00 0.40 2 -1 -1 7.50 0.40 2 1 -1 6.70 0.40 0 -1 -1 11.80 0.50 0 1 1 12.50 0.50 0 1 -1 11.70 0.40 -1 -1 -1 1078.39 35.90 -1 1 -1 1102.49 29.10 1 1 1 1161.98 29.70 2 -1 1 39.80 1.60 -2 -1 -1 47.40 1.50 2 -1 1 49.00 1.50 -2 1 -1 49.99 1.50 2 1 1 48.20 1.30 2 1 1 46.70 1.70 -3 -1 -1 196.78 5.30 3 -1 1 192.48 5.20 3 -1 1 198.98 5.40 -3 1 -1 191.38 5.20 3 1 1 193.18 5.60 3 1 1 198.18 5.10 -4 -1 -1 477.75 12.70 4 -1 1 485.85 13.00 4 -1 1 485.45 12.70 4 1 1 469.65 13.10 4 1 1 511.85 12.60 -4 1 -1 491.75 12.70 5 -1 1 65.59 2.00 5 -1 1 60.69 2.30 -5 -1 -1 63.39 2.00 -5 1 -1 63.09 2.00 5 1 1 60.79 2.50 5 1 1 66.29 1.90 6 -1 1 17.60 1.20 6 -1 1 19.10 0.90 -6 -1 -1 19.30 1.00 6 1 1 18.70 0.90 6 1 1 18.00 1.40 -6 1 -1 19.80 0.90 7 -1 1 34.70 1.80 -7 -1 -1 32.00 1.40 7 -1 1 33.70 1.40 -7 1 -1 30.90 1.30 7 1 1 32.00 1.30 7 1 1 32.30 1.90 8 -1 1 24.10 1.70 8 -1 1 24.70 1.20 -8 1 -1 25.90 1.30 8 1 1 27.20 1.90 8 1 1 25.70 1.20 9 -1 1 13.80 1.50 9 -1 1 13.40 1.00 9 1 1 17.10 1.70 9 1 1 14.80 1.00 10 -1 1 15.20 1.60 10 -1 1 18.20 1.20 10 1 1 18.20 1.90 11 -1 1 32.00 2.30 11 1 1 35.90 2.60 12 -1 1 20.40 2.00 12 1 1 20.40 2.20 13 -1 1 27.50 2.40 13 1 1 29.60 2.80 14 1 1 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-15 17.80 2.10 3 7 -15 11.70 1.70 3 7 -15 13.70 1.70 2 7 -15 1.20 1.10 2 7 -15 0.00 0.90 1 7 -15 52.09 3.20 12 0 -16 4.90 1.10 11 0 -16 -0.50 0.80 10 0 -16 0.50 0.90 9 0 -16 0.60 0.80 8 0 -16 2.20 0.90 5 0 -16 -0.10 0.80 4 0 -16 1.20 0.90 3 0 -16 0.90 1.00 2 0 -16 31.30 2.50 1 0 -16 0.20 1.00 0 0 -16 26.60 2.60 -1 0 -16 -1.00 1.10 12 -1 -16 23.20 1.90 12 1 -16 15.50 1.90 11 -1 -16 3.00 1.00 11 1 -16 3.10 1.00 10 -1 -16 1.50 0.80 10 1 -16 0.60 0.90 9 -1 -16 -0.70 0.70 9 1 -16 0.20 0.80 8 1 -16 -0.20 0.80 7 1 -16 8.40 1.30 6 -1 -16 0.60 0.80 5 -1 -16 40.10 2.50 5 1 -16 36.90 2.50 4 -1 -16 0.00 0.80 4 1 -16 0.50 1.00 3 -1 -16 17.90 2.00 3 1 -16 17.20 1.90 2 -1 -16 11.80 1.70 2 1 -16 12.80 1.70 1 -1 -16 29.10 2.60 1 1 -16 31.30 2.60 0 -1 -16 0.00 1.10 0 1 -16 2.40 1.20 -1 -1 -16 19.60 2.20 -1 1 -16 20.10 2.30 12 -2 -16 3.50 1.00 11 -2 -16 1.50 0.80 11 2 -16 1.20 1.10 10 -2 -16 0.00 0.70 10 2 -16 -0.10 0.90 9 2 -16 5.50 1.20 8 2 -16 3.20 1.00 7 2 -16 1.80 0.90 6 -2 -16 2.40 0.90 5 -2 -16 0.30 0.80 5 2 -16 -0.10 0.80 4 -2 -16 0.50 0.80 4 2 -16 -0.60 0.80 3 -2 -16 2.30 1.00 3 2 -16 3.20 1.20 2 -2 -16 33.10 2.60 2 2 -16 32.20 2.60 1 -2 -16 5.90 1.40 1 2 -16 5.70 1.50 0 -2 -16 0.70 1.10 0 2 -16 0.90 1.20 -1 -2 -16 7.00 1.60 -1 2 -16 9.20 1.80 11 -3 -16 5.80 1.10 11 3 -16 3.80 1.30 10 3 -16 0.80 1.00 9 3 -16 2.20 1.10 8 3 -16 -0.30 0.90 7 3 -16 -0.70 0.90 6 -3 -16 9.70 1.40 6 3 -16 9.50 1.40 5 -3 -16 16.70 1.90 4 -3 -16 3.20 1.10 4 3 -16 0.70 1.00 3 -3 -16 1.30 0.90 3 3 -16 -0.80 0.90 2 -3 -16 3.60 1.20 2 3 -16 1.70 1.10 1 -3 -16 0.80 1.00 1 3 -16 1.50 1.10 0 -3 -16 21.70 2.30 0 3 -16 24.00 2.60 -1 3 -16 6.00 1.90 10 4 -16 5.30 1.40 9 4 -16 -1.10 0.90 8 4 -16 4.00 1.20 7 -4 -16 57.69 3.10 7 4 -16 60.79 3.20 6 -4 -16 4.70 1.10 6 4 -16 4.20 1.20 5 -4 -16 1.10 0.80 5 4 -16 -0.10 0.90 4 -4 -16 4.40 1.20 4 4 -16 4.60 1.30 3 -4 -16 1.60 1.00 3 4 -16 1.40 1.10 2 -4 -16 6.90 1.40 2 4 -16 8.60 1.50 1 -4 -16 2.40 1.20 1 4 -16 0.90 1.20 0 -4 -16 0.50 1.60 0 4 -16 -0.40 1.10 9 5 -16 2.10 1.20 8 5 -16 -0.40 1.10 7 -5 -16 5.10 1.20 7 5 -16 4.60 1.40 6 -5 -16 3.40 1.10 6 5 -16 1.30 1.10 5 -5 -16 0.10 0.80 5 5 -16 -1.00 0.90 4 -5 -16 0.90 0.90 4 5 -16 -0.40 0.90 4 5 -16 -0.20 1.40 3 -5 -16 6.30 1.30 3 5 -16 4.90 1.30 2 -5 -16 1.90 1.10 2 5 -16 1.40 1.20 1 5 -16 7.80 1.60 7 -6 -16 3.00 1.10 7 6 -16 2.00 1.20 6 -6 -16 0.50 0.90 6 6 -16 -0.60 1.00 5 -6 -16 3.40 1.20 5 6 -16 1.50 1.20 4 -6 -16 1.00 1.00 4 6 -16 1.60 1.10 3 -6 -16 10.90 2.50 3 6 -16 8.20 1.50 2 6 -16 -1.40 1.10 11 0 -17 7.80 1.30 10 0 -17 0.30 0.90 5 0 -17 14.20 1.80 4 0 -17 -0.30 0.90 3 0 -17 2.00 1.10 2 0 -17 0.70 1.10 1 0 -17 0.10 1.10 11 -1 -17 11.80 1.50 11 1 -17 12.00 1.50 10 1 -17 20.90 1.90 9 1 -17 14.30 1.60 5 -1 -17 0.70 0.90 5 1 -17 0.70 0.90 4 -1 -17 10.80 1.60 4 1 -17 10.60 1.60 3 -1 -17 4.30 1.30 3 1 -17 2.30 1.20 2 -1 -17 12.00 1.80 2 1 -17 10.30 1.70 1 -1 -17 1.10 1.10 1 1 -17 0.60 1.10 10 2 -17 7.20 1.40 9 2 -17 0.80 1.00 8 2 -17 2.70 1.10 6 -2 -17 37.70 2.50 5 -2 -17 1.20 0.90 4 -2 -17 0.90 0.90 4 2 -17 0.30 0.90 3 -2 -17 0.00 0.90 3 2 -17 1.00 1.10 2 -2 -17 10.80 1.70 2 2 -17 11.30 1.80 1 -2 -17 2.20 1.30 1 2 -17 -0.10 1.10 10 3 -17 11.90 1.80 9 3 -17 1.70 1.10 8 3 -17 3.20 1.20 7 3 -17 2.40 1.10 6 -3 -17 3.10 1.10 5 -3 -17 10.50 1.60 4 -3 -17 0.10 0.90 4 3 -17 0.40 1.10 3 -3 -17 10.90 1.70 3 3 -17 11.30 1.80 2 -3 -17 3.80 1.20 2 3 -17 1.90 1.30 1 3 -17 6.80 1.90 9 4 -17 0.10 1.10 8 4 -17 -0.70 1.10 7 4 -17 3.00 1.20 6 -4 -17 17.70 2.00 6 4 -17 10.90 1.80 5 -4 -17 8.50 1.50 4 -4 -17 25.90 2.40 4 4 -17 26.10 2.50 3 -4 -17 8.90 1.60 3 4 -17 10.50 1.70 2 4 -17 11.60 1.90 7 5 -17 20.70 2.20 6 -5 -17 25.00 2.20 6 5 -17 17.00 2.00 5 -5 -17 13.20 1.70 5 0 -18 0.50 1.00 4 0 -18 6.80 1.40 3 0 -18 -0.10 1.00 5 -1 -18 -0.10 0.90 5 1 -18 0.40 1.40 4 -1 -18 0.40 1.00 4 1 -18 1.20 1.10 3 -1 -18 2.10 1.20 3 1 -18 0.90 1.10 6 -2 -18 0.40 1.30 5 -2 -18 0.40 0.90 4 -2 -18 2.50 1.10 4 2 -18 1.30 1.20 3 2 -18 4.40 1.40 6 -3 -18 5.90 1.30 5 -3 -18 14.90 1.90 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 90666 _shelx_res_file ; TITL m1cg CELL 0.71073 12.2358 10.3185 14.2310 90.000 111.199 90.000 ZERR 4.000 0.0016 0.0014 0.0019 0.000 0.002 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O F UNIT 76 76 8 12 4 OMIT -2 180.0 L.S. 20 ACTA BOND $H CONF HTAB OMIT 12 1 6 OMIT 12 0 6 OMIT 11 1 6 OMIT 10 1 7 OMIT 10 1 8 OMIT 10 0 8 OMIT 10 1 6 OMIT 10 2 8 OMIT 9 1 7 OMIT 9 0 7 OMIT 10 2 7 OMIT 11 1 7 OMIT 11 1 5 OMIT 11 0 5 OMIT 10 0 6 FMAP 2 PLAN 20 SIZE 0.479 0.293 0.282 TEMP -100 WGHT 0.047600 0.471300 FVAR 0.56895 N1 3 0.572121 0.474757 0.269542 11.00000 0.03280 0.02768 = 0.03228 0.00332 0.01405 0.00185 C2 1 0.512231 0.447816 0.339845 11.00000 0.03066 0.03414 = 0.03382 0.01059 0.01127 0.00214 AFIX 23 H2A 2 0.562161 0.391831 0.395240 11.00000 -1.20000 H2B 2 0.437890 0.401360 0.304338 11.00000 -1.20000 AFIX 0 C3 1 0.486939 0.574002 0.382722 11.00000 0.03485 0.04444 = 0.02745 0.00798 0.01137 0.00755 AFIX 23 H3A 2 0.443830 0.555984 0.428265 11.00000 -1.20000 H3B 2 0.561595 0.617346 0.422374 11.00000 -1.20000 AFIX 0 N4 3 0.416967 0.659032 0.300927 11.00000 0.03733 0.03455 = 0.02833 0.00676 0.01448 0.00675 C5 1 0.470877 0.682728 0.225515 11.00000 0.03885 0.02997 = 0.03165 0.00606 0.01572 0.00147 AFIX 23 H5A 2 0.544371 0.732534 0.256395 11.00000 -1.20000 H5B 2 0.416951 0.734362 0.169136 11.00000 -1.20000 AFIX 0 C6 1 0.497044 0.554524 0.186093 11.00000 0.03499 0.03105 = 0.02846 0.00254 0.01213 -0.00049 AFIX 23 H6A 2 0.422788 0.508095 0.150241 11.00000 -1.20000 H6B 2 0.536760 0.570402 0.137668 11.00000 -1.20000 AFIX 0 C11 1 0.607112 0.354977 0.232875 11.00000 0.04083 0.02762 = 0.04269 0.00085 0.01603 0.00067 AFIX 23 H11A 2 0.536708 0.312427 0.184481 11.00000 -1.20000 H11B 2 0.642415 0.295113 0.290268 11.00000 -1.20000 AFIX 0 O11 4 0.951611 0.444489 0.065434 11.00000 0.05124 0.05036 = 0.04469 -0.00925 0.02748 -0.00155 C12 1 1.013873 0.544638 0.133221 11.00000 0.03998 0.05241 = 0.04694 -0.00539 0.02087 0.00131 AFIX 23 H12A 2 1.098377 0.523170 0.162415 11.00000 -1.20000 H12B 2 1.004920 0.627934 0.096668 11.00000 -1.20000 AFIX 0 O13 4 0.967225 0.555518 0.211406 11.00000 0.04256 0.05110 = 0.04778 -0.01464 0.02314 -0.00857 C3A 1 0.867869 0.480564 0.181106 11.00000 0.03251 0.02793 = 0.03175 -0.00060 0.00824 0.00593 C14 1 0.787692 0.465906 0.227177 11.00000 0.03670 0.03060 = 0.02901 -0.00220 0.01134 0.00476 AFIX 43 H14 2 0.795046 0.511809 0.287029 11.00000 -1.20000 AFIX 0 C15 1 0.694102 0.379991 0.182013 11.00000 0.03506 0.02725 = 0.03445 0.00130 0.01082 0.00637 C16 1 0.684860 0.315738 0.093690 11.00000 0.03582 0.03435 = 0.03911 -0.00677 0.00657 0.00298 AFIX 43 H16 2 0.620332 0.259210 0.063589 11.00000 -1.20000 AFIX 0 C17 1 0.767618 0.331557 0.047502 11.00000 0.04648 0.03877 = 0.03243 -0.00727 0.01175 0.00766 AFIX 43 H17 2 0.761030 0.286915 -0.012690 11.00000 -1.20000 AFIX 0 C7A 1 0.858012 0.414323 0.093465 11.00000 0.04014 0.03305 = 0.03305 0.00227 0.01596 0.01093 C47 1 0.321035 0.724612 0.297971 11.00000 0.03686 0.02604 = 0.03698 0.00594 0.01502 0.00179 O47 4 0.274752 0.806262 0.232905 11.00000 0.06241 0.05764 = 0.06863 0.03854 0.04011 0.03030 C41 1 0.267845 0.698234 0.376498 11.00000 0.02633 0.02796 = 0.03034 0.00364 0.00707 0.00192 C42 1 0.221514 0.577225 0.385443 11.00000 0.04003 0.02684 = 0.03289 0.00017 0.01284 -0.00012 AFIX 43 H42 2 0.230621 0.504904 0.347614 11.00000 -1.20000 AFIX 0 C43 1 0.162093 0.566070 0.450976 11.00000 0.03827 0.03107 = 0.03977 0.00683 0.01295 -0.00474 F43 5 0.113738 0.449716 0.457752 11.00000 0.07592 0.03784 = 0.07565 0.00611 0.04244 -0.01424 C44 1 0.148668 0.666158 0.509515 11.00000 0.03424 0.04661 = 0.03365 0.00582 0.01413 0.00275 AFIX 43 H44 2 0.107919 0.654158 0.554410 11.00000 -1.20000 AFIX 0 C45 1 0.196600 0.785313 0.500876 11.00000 0.03677 0.03820 = 0.03870 -0.00642 0.01275 0.00205 AFIX 43 H45 2 0.189600 0.856258 0.540875 11.00000 -1.20000 AFIX 0 C46 1 0.254587 0.801409 0.434279 11.00000 0.03319 0.02704 = 0.04310 -0.00062 0.01350 -0.00198 AFIX 43 H46 2 0.285689 0.883927 0.427981 11.00000 -1.20000 AFIX 0 HKLF 4 REM m1cg REM R1 = 0.0397 for 2975 Fo > 4sig(Fo) and 0.0502 for all 3674 data REM 226 parameters refined using 0 restraints END WGHT 0.0476 0.4712 REM Instructions for potential hydrogen bonds EQIV $1 -x+1/2, y-1/2, -z+1/2 HTAB C2 O47_$1 HTAB C42 O47_$1 REM Highest difference peak 0.238, deepest hole -0.179, 1-sigma level 0.038 Q1 1 0.8627 0.4553 0.1329 11.00000 0.05 0.20 Q2 1 0.3000 0.7087 0.3453 11.00000 0.05 0.20 Q3 1 0.2392 0.5622 0.4534 11.00000 0.05 0.20 Q4 1 0.1977 0.5960 0.5110 11.00000 0.05 0.19 Q5 1 0.6611 0.3645 0.2116 11.00000 0.05 0.18 Q6 1 0.4682 0.6161 0.1970 11.00000 0.05 0.18 Q7 1 0.4418 0.6729 0.2613 11.00000 0.05 0.18 Q8 1 0.7082 0.3217 0.1578 11.00000 0.05 0.18 Q9 1 0.8130 0.5010 0.1874 11.00000 0.05 0.18 Q10 1 0.5329 0.4635 0.2961 11.00000 0.05 0.17 Q11 1 0.1559 0.5828 0.3940 11.00000 0.05 0.17 Q12 1 0.6677 0.3816 0.1248 11.00000 0.05 0.17 Q13 1 0.7222 0.4602 0.1844 11.00000 0.05 0.17 Q14 1 0.8978 0.5954 0.1598 11.00000 0.05 0.16 Q15 1 0.1534 0.7353 0.4873 11.00000 0.05 0.16 Q16 1 0.2625 0.7765 0.5001 11.00000 0.05 0.16 Q17 1 0.3796 0.6971 0.3059 11.00000 0.05 0.16 Q18 1 0.6216 0.5137 0.3035 11.00000 0.05 0.15 Q19 1 0.2994 0.7386 0.4290 11.00000 0.05 0.15 Q20 1 0.5451 0.5210 0.2375 11.00000 0.05 0.15 ; _shelx_res_checksum 24443 _shelxl_version_number 2.014 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 N N1 0.57212(10) 0.47476(11) 0.26954(9) 0.0303(3) Uani d 1 C C2 0.51223(13) 0.44782(14) 0.33984(11) 0.0330(3) Uani d 1 H H2A 0.5622 0.3918 0.3952 0.040 Uiso calc 1 H H2B 0.4379 0.4014 0.3043 0.040 Uiso calc 1 C C3 0.48694(13) 0.57400(15) 0.38272(11) 0.0356(3) Uani d 1 H H3A 0.4438 0.5560 0.4283 0.043 Uiso calc 1 H H3B 0.5616 0.6173 0.4224 0.043 Uiso calc 1 N N4 0.41697(11) 0.65903(12) 0.30093(9) 0.0327(3) Uani d 1 C C5 0.47088(13) 0.68273(14) 0.22552(11) 0.0327(3) Uani d 1 H H5A 0.5444 0.7325 0.2564 0.039 Uiso calc 1 H H5B 0.4170 0.7344 0.1691 0.039 Uiso calc 1 C C6 0.49704(13) 0.55452(14) 0.18609(11) 0.0313(3) Uani d 1 H H6A 0.4228 0.5081 0.1502 0.038 Uiso calc 1 H H6B 0.5368 0.5704 0.1377 0.038 Uiso calc 1 C C11 0.60711(14) 0.35498(14) 0.23287(12) 0.0368(3) Uani d 1 H H11A 0.5367 0.3124 0.1845 0.044 Uiso calc 1 H H11B 0.6424 0.2951 0.2903 0.044 Uiso calc 1 O O11 0.95161(10) 0.44449(12) 0.06543(9) 0.0460(3) Uani d 1 C C12 1.01387(15) 0.54464(18) 0.13322(13) 0.0450(4) Uani d 1 H H12A 1.0984 0.5232 0.1624 0.054 Uiso calc 1 H H12B 1.0049 0.6279 0.0967 0.054 Uiso calc 1 O O13 0.96722(10) 0.55552(12) 0.21141(9) 0.0453(3) Uani d 1 C C3A 0.86787(13) 0.48056(14) 0.18111(11) 0.0317(3) Uani d 1 C C14 0.78769(13) 0.46591(14) 0.22718(11) 0.0323(3) Uani d 1 H H14 0.7950 0.5118 0.2870 0.039 Uiso calc 1 C C15 0.69410(13) 0.37999(14) 0.18201(11) 0.0327(3) Uani d 1 C C16 0.68486(14) 0.31574(15) 0.09369(12) 0.0384(4) Uani d 1 H H16 0.6203 0.2592 0.0636 0.046 Uiso calc 1 C C17 0.76762(14) 0.33156(16) 0.04750(12) 0.0399(4) Uani d 1 H H17 0.7610 0.2869 -0.0127 0.048 Uiso calc 1 C C7A 0.85801(14) 0.41432(14) 0.09347(11) 0.0347(3) Uani d 1 C C47 0.32103(13) 0.72461(14) 0.29797(11) 0.0328(3) Uani d 1 O O47 0.27475(12) 0.80626(13) 0.23290(10) 0.0583(4) Uani d 1 C C41 0.26784(12) 0.69823(13) 0.37650(11) 0.0291(3) Uani d 1 C C42 0.22151(13) 0.57722(14) 0.38544(11) 0.0333(3) Uani d 1 H H42 0.2306 0.5049 0.3476 0.040 Uiso calc 1 C C43 0.16209(14) 0.56607(15) 0.45098(12) 0.0367(3) Uani d 1 F F43 0.11374(10) 0.44972(10) 0.45775(9) 0.0590(3) Uani d 1 C C44 0.14867(13) 0.66616(16) 0.50952(12) 0.0377(4) Uani d 1 H H44 0.1079 0.6542 0.5544 0.045 Uiso calc 1 C C45 0.19660(13) 0.78531(16) 0.50088(12) 0.0381(4) Uani d 1 H H45 0.1896 0.8563 0.5409 0.046 Uiso calc 1 C C46 0.25459(13) 0.80141(14) 0.43428(12) 0.0345(3) Uani d 1 H H46 0.2857 0.8839 0.4280 0.041 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 N1 0.0328(6) 0.0277(6) 0.0323(6) 0.0018(5) 0.0140(5) 0.0033(5) C2 0.0307(7) 0.0341(8) 0.0338(8) 0.0021(6) 0.0113(6) 0.0106(6) C3 0.0349(8) 0.0444(9) 0.0275(7) 0.0076(6) 0.0114(6) 0.0080(6) N4 0.0373(7) 0.0345(7) 0.0283(6) 0.0068(5) 0.0145(5) 0.0068(5) C5 0.0388(8) 0.0300(7) 0.0317(7) 0.0015(6) 0.0157(6) 0.0061(6) C6 0.0350(8) 0.0311(7) 0.0285(7) -0.0005(6) 0.0121(6) 0.0025(6) C11 0.0408(8) 0.0276(7) 0.0427(9) 0.0007(6) 0.0160(7) 0.0009(6) O11 0.0512(7) 0.0504(7) 0.0447(7) -0.0015(5) 0.0275(6) -0.0093(5) C12 0.0400(9) 0.0524(10) 0.0469(10) 0.0013(7) 0.0209(8) -0.0054(8) O13 0.0426(6) 0.0511(7) 0.0478(7) -0.0086(5) 0.0231(6) -0.0146(5) C3A 0.0325(7) 0.0279(7) 0.0318(7) 0.0059(6) 0.0082(6) -0.0006(6) C14 0.0367(8) 0.0306(7) 0.0290(7) 0.0048(6) 0.0113(6) -0.0022(6) C15 0.0351(8) 0.0273(7) 0.0344(8) 0.0064(6) 0.0108(6) 0.0013(6) C16 0.0358(8) 0.0344(8) 0.0391(8) 0.0030(6) 0.0066(7) -0.0068(6) C17 0.0465(9) 0.0388(8) 0.0324(8) 0.0077(7) 0.0117(7) -0.0073(6) C7A 0.0401(8) 0.0330(8) 0.0330(8) 0.0109(6) 0.0160(7) 0.0023(6) C47 0.0369(8) 0.0260(7) 0.0370(8) 0.0018(6) 0.0150(6) 0.0059(6) O47 0.0624(8) 0.0576(8) 0.0686(9) 0.0303(6) 0.0401(7) 0.0385(7) C41 0.0263(7) 0.0280(7) 0.0303(7) 0.0019(5) 0.0071(6) 0.0036(5) C42 0.0400(8) 0.0268(7) 0.0329(7) -0.0001(6) 0.0128(7) 0.0002(6) C43 0.0383(8) 0.0311(8) 0.0398(8) -0.0047(6) 0.0130(7) 0.0068(6) F43 0.0759(8) 0.0378(6) 0.0757(7) -0.0142(5) 0.0424(6) 0.0061(5) C44 0.0342(8) 0.0466(9) 0.0337(8) 0.0027(7) 0.0141(7) 0.0058(7) C45 0.0368(8) 0.0382(8) 0.0387(8) 0.0020(6) 0.0127(7) -0.0064(7) C46 0.0332(8) 0.0270(7) 0.0431(8) -0.0020(6) 0.0135(7) -0.0006(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 C6 N1 C11 111.35(11) C6 N1 C2 109.80(11) C11 N1 C2 111.48(11) N1 C2 C3 109.70(12) N1 C2 H2A 109.7 C3 C2 H2A 109.7 N1 C2 H2B 109.7 C3 C2 H2B 109.7 H2A C2 H2B 108.2 N4 C3 C2 109.93(12) N4 C3 H3A 109.7 C2 C3 H3A 109.7 N4 C3 H3B 109.7 C2 C3 H3B 109.7 H3A C3 H3B 108.2 C47 N4 C3 125.54(12) C47 N4 C5 120.78(12) C3 N4 C5 113.15(11) N4 C5 C6 109.62(11) N4 C5 H5A 109.7 C6 C5 H5A 109.7 N4 C5 H5B 109.7 C6 C5 H5B 109.7 H5A C5 H5B 108.2 N1 C6 C5 110.19(12) N1 C6 H6A 109.6 C5 C6 H6A 109.6 N1 C6 H6B 109.6 C5 C6 H6B 109.6 H6A C6 H6B 108.1 N1 C11 C15 111.97(12) N1 C11 H11A 109.2 C15 C11 H11A 109.2 N1 C11 H11B 109.2 C15 C11 H11B 109.2 H11A C11 H11B 107.9 C7A O11 C12 105.29(11) O13 C12 O11 108.48(13) O13 C12 H12A 110.0 O11 C12 H12A 110.0 O13 C12 H12B 110.0 O11 C12 H12B 110.0 H12A C12 H12B 108.4 C3A O13 C12 105.63(12) C14 C3A O13 128.14(13) C14 C3A C7A 122.03(14) O13 C3A C7A 109.82(13) C3A C14 C15 117.14(13) C3A C14 H14 121.4 C15 C14 H14 121.4 C16 C15 C14 120.05(14) C16 C15 C11 120.75(14) C14 C15 C11 119.16(13) C15 C16 C17 122.17(15) C15 C16 H16 118.9 C17 C16 H16 118.9 C7A C17 C16 116.51(14) C7A C17 H17 121.7 C16 C17 H17 121.7 C17 C7A O11 128.17(14) C17 C7A C3A 122.10(14) O11 C7A C3A 109.73(14) O47 C47 N4 121.94(13) O47 C47 C41 118.54(13) N4 C47 C41 119.52(12) C46 C41 C42 119.54(13) C46 C41 C47 118.31(12) C42 C41 C47 121.84(13) C43 C42 C41 117.84(13) C43 C42 H42 121.1 C41 C42 H42 121.1 F43 C43 C44 118.11(14) F43 C43 C42 118.15(14) C44 C43 C42 123.73(14) C43 C44 C45 117.76(14) C43 C44 H44 121.1 C45 C44 H44 121.1 C46 C45 C44 120.34(14) C46 C45 H45 119.8 C44 C45 H45 119.8 C45 C46 C41 120.77(14) C45 C46 H46 119.6 C41 C46 H46 119.6 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C6 1.4638(18) N1 C11 1.4645(18) N1 C2 1.4647(18) C2 C3 1.517(2) C2 H2A 0.9900 C2 H2B 0.9900 C3 N4 1.4619(18) C3 H3A 0.9900 C3 H3B 0.9900 N4 C47 1.3423(19) N4 C5 1.4692(17) C5 C6 1.5156(19) C5 H5A 0.9900 C5 H5B 0.9900 C6 H6A 0.9900 C6 H6B 0.9900 C11 C15 1.510(2) C11 H11A 0.9900 C11 H11B 0.9900 O11 C7A 1.3777(19) O11 C12 1.431(2) C12 O13 1.4268(19) C12 H12A 0.9900 C12 H12B 0.9900 O13 C3A 1.3722(18) C3A C14 1.371(2) C3A C7A 1.389(2) C14 C15 1.406(2) C14 H14 0.9500 C15 C16 1.389(2) C16 C17 1.402(2) C16 H16 0.9500 C17 C7A 1.363(2) C17 H17 0.9500 C47 O47 1.2283(18) C47 C41 1.507(2) C41 C46 1.390(2) C41 C42 1.3960(19) C42 C43 1.379(2) C42 H42 0.9500 C43 F43 1.3572(17) C43 C44 1.374(2) C44 C45 1.387(2) C44 H44 0.9500 C45 C46 1.384(2) C45 H45 0.9500 C46 H46 0.9500 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 C42 H42 O47 2_545 0.95 2.34 3.273(2) 168 y C5 H5A Cg1 2_655 0.99 2.76 3.7310(18) 168 y C45 H45 Cg1 4_576 0.95 2.90 3.7470(18) 149 y loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C6 N1 C2 C3 -60.96(15) C11 N1 C2 C3 175.17(12) N1 C2 C3 N4 57.23(15) C2 C3 N4 C47 133.38(15) C2 C3 N4 C5 -55.00(16) C47 N4 C5 C6 -133.39(14) C3 N4 C5 C6 54.54(16) C11 N1 C6 C5 -175.10(11) C2 N1 C6 C5 60.95(15) N4 C5 C6 N1 -56.63(15) C6 N1 C11 C15 71.31(15) C2 N1 C11 C15 -165.70(12) C7A O11 C12 O13 10.19(17) O11 C12 O13 C3A -9.99(17) C12 O13 C3A C14 -175.37(15) C12 O13 C3A C7A 5.95(17) O13 C3A C14 C15 -178.36(14) C7A C3A C14 C15 0.2(2) C3A C14 C15 C16 -0.9(2) C3A C14 C15 C11 176.73(13) N1 C11 C15 C16 -138.33(14) N1 C11 C15 C14 44.02(18) C14 C15 C16 C17 1.1(2) C11 C15 C16 C17 -176.55(14) C15 C16 C17 C7A -0.4(2) C16 C17 C7A O11 178.28(14) C16 C17 C7A C3A -0.4(2) C12 O11 C7A C17 174.64(16) C12 O11 C7A C3A -6.53(16) C14 C3A C7A C17 0.5(2) O13 C3A C7A C17 179.30(14) C14 C3A C7A O11 -178.38(13) O13 C3A C7A O11 0.39(17) C3 N4 C47 O47 171.03(16) C5 N4 C47 O47 0.0(2) C3 N4 C47 C41 -8.9(2) C5 N4 C47 C41 -179.92(13) O47 C47 C41 C46 -56.5(2) N4 C47 C41 C46 123.39(16) O47 C47 C41 C42 116.97(17) N4 C47 C41 C42 -63.11(19) C46 C41 C42 C43 1.1(2) C47 C41 C42 C43 -172.33(13) C41 C42 C43 F43 178.02(14) C41 C42 C43 C44 -1.7(2) F43 C43 C44 C45 -178.92(14) C42 C43 C44 C45 0.8(2) C43 C44 C45 C46 0.7(2) C44 C45 C46 C41 -1.3(2) C42 C41 C46 C45 0.4(2) C47 C41 C46 C45 174.01(13) _cod_database_fobs_code 2242803