#------------------------------------------------------------------------------ #$Date: 2019-08-17 06:49:59 +0300 (Sat, 17 Aug 2019) $ #$Revision: 217574 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021746.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_2021746 loop_ _publ_author_name 'Wang, Shengpei' 'Yu, Shasha' 'Feng, Jianxiang' 'Liu, Shenggao' _publ_section_title ; A highly efficient antioxidant based on boron and a Schiff base bridged phenolic diphenylamine: synthesis, crystal structure and thermal and antioxidant properties ; _journal_coeditor_code JX3038 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229619011331 _journal_volume 75 _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_iupac 'C39 H41 B N2 O' _chemical_formula_moiety 'C39 H41 B N2 O' _chemical_formula_sum 'C39 H41 B N2 O' _chemical_formula_weight 564.55 _chemical_name_common ; (E)-4-({3,5-Di-tert-butyl-2-[(diphenylboranyl)oxy]\ benzylidene}amino)-N-phenylaniline ; _chemical_name_systematic ; {2-[(4-Anilinophenyl)iminomethyl-\kN]-4,6-di-tert-\ butylphenolato-\kO}diphenylboron ; _space_group_crystal_system monoclinic _space_group_IT_number 7 _space_group_name_Hall 'P -2yac' _space_group_name_H-M_alt 'P 1 n 1' _symmetry_space_group_name_Hall 'P -2yac' _symmetry_space_group_name_H-M 'P 1 n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 90 _cell_angle_beta 96.0950(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.6730(5) _cell_length_b 10.0539(4) _cell_length_c 15.0271(7) _cell_measurement_reflns_used 9977 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 2.2 _cell_volume 1603.37(12) _computing_cell_refinement ; SAINT (Bruker, 2010) ; _computing_data_collection ; APEX2 (Bruker, 2010) ; _computing_data_reduction ; SAINT (Bruker, 2010) ; _computing_molecular_graphics ; SHELXTL (Bruker, 2010) ; _computing_publication_material ; SHELXTL (Bruker, 2010) ; _computing_structure_refinement ; SHELXL2016 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_unetI/netI 0.0476 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 23747 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.998 _diffrn_reflns_theta_min 2.442 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_correction_T_min 0.614 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.169 _exptl_crystal_description prismatic _exptl_crystal_F_000 604 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.130 _refine_diff_density_max 0.150 _refine_diff_density_min -0.153 _refine_ls_abs_structure_details ; Flack (1983), 3116 Friedel pairs The experimental value of the Flack parameter is unreliable, as it has a large s.u. The following item in the CIF and the Table is the refined Flack parameter, 0.1(4). ; _refine_ls_abs_structure_Flack 0.1(4) _refine_ls_extinction_coef 0.080(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2016 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 396 _refine_ls_number_reflns 6249 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0430 _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^)+(0.0513P)^2^+0.1760P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1021 _refine_ls_wR_factor_ref 0.1095 _reflns_number_gt 5477 _reflns_number_total 6249 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jx3038sup1.cif _cod_data_source_block I _cod_database_code 2021746 _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 0.986 _shelx_estimated_absorpt_t_max 0.991 _shelx_hkl_file ; 0 1 0 4.80 1.00 0 -3 0 1037.30 54.49 0 -3 0 1005.20 54.49 0 -3 0 1229.48 57.49 0 -3 0 1159.38 56.79 0 3 0 1134.69 57.19 0 3 0 1024.30 54.39 0 3 0 1108.99 54.59 0 -4 0 2078.19 99.79 0 -4 0 2190.58 100.69 0 -4 0 1883.61 96.59 0 -4 0 1809.32 96.59 0 4 0 2029.10 100.29 0 4 0 1912.81 96.59 0 4 0 1849.71 96.29 0 -5 0 255.77 17.50 0 -5 0 211.48 13.30 0 -5 0 199.48 13.30 0 -5 0 213.38 16.10 0 5 0 198.88 12.60 0 5 0 211.08 13.00 0 5 0 240.38 17.10 0 -6 0 77.69 7.20 0 -6 0 102.99 10.80 0 -6 0 73.79 6.90 0 -6 0 76.69 9.00 0 -7 0 51.89 6.00 0 -7 0 47.70 9.00 0 -7 0 61.79 8.70 0 -7 0 45.90 5.50 0 -8 0 2.20 3.90 0 -8 0 3.50 2.10 0 -8 0 -8.00 3.40 0 -9 0 35.80 5.50 0 -9 0 32.00 9.20 0 -9 0 39.40 9.70 0 -9 0 47.60 5.50 0 -10 0 318.57 26.90 0 -11 0 16.40 7.50 0 -12 0 -4.60 5.90 0 -13 0 -1.60 7.90 1 -13 0 13.30 8.00 1 -12 0 6.00 5.80 1 -11 0 59.49 7.90 1 -11 0 66.79 12.70 1 -11 0 60.69 8.30 1 -10 0 133.29 12.00 1 -10 0 117.09 12.40 1 -10 0 130.89 15.30 1 -9 0 155.98 15.70 1 -9 0 119.49 12.40 1 -9 0 141.89 12.50 1 -9 0 137.29 14.70 1 -8 0 34.90 6.50 1 -8 0 30.40 7.50 1 -8 0 20.40 6.60 1 -8 0 26.70 5.80 -1 7 0 286.17 19.80 -1 7 0 284.67 22.40 1 -7 0 304.47 20.40 1 -7 0 309.67 20.80 1 -7 0 285.27 21.70 1 -7 0 338.47 22.60 -1 6 0 327.37 22.20 -1 6 0 349.67 22.00 -1 6 0 391.56 24.80 1 -6 0 389.96 24.00 1 -6 0 359.36 22.80 1 -6 0 331.67 22.30 1 -6 0 366.16 23.90 -1 5 0 1175.98 59.19 -1 5 0 1027.30 56.89 -1 5 0 1085.29 57.69 1 -5 0 1107.89 58.19 1 -5 0 1165.88 58.39 1 -5 0 1025.70 57.19 1 -5 0 1036.50 57.19 -1 4 0 70.29 6.70 -1 4 0 78.29 7.10 -1 4 0 68.79 7.10 1 -4 0 71.99 6.70 1 -4 0 74.89 6.90 1 -4 0 70.19 6.90 -1 3 0 2583.94 112.69 -1 3 0 2094.89 112.19 -1 3 0 2147.19 112.39 1 -3 0 2502.75 112.19 1 -3 0 2128.29 112.19 1 -3 0 2117.59 112.09 -1 2 0 236.08 14.20 -1 2 0 220.68 14.10 -1 2 0 267.07 13.70 1 -2 0 255.67 13.30 1 -2 0 224.98 14.00 1 -2 0 210.58 13.90 -1 1 0 1052.79 52.99 -1 0 0 -0.30 0.20 -1 0 0 -0.10 0.20 1 0 0 0.00 0.10 -1 -1 0 2858.61 144.59 1 1 0 3056.09 145.99 1 1 0 2859.31 144.29 1 1 0 3156.08 144.69 -1 -2 0 219.58 10.80 -1 -2 0 200.78 10.80 -1 -2 0 192.08 13.00 1 2 0 202.48 13.40 -1 -3 0 1862.51 96.39 -1 -3 0 1941.31 97.59 1 3 0 1912.21 96.89 -1 -4 0 56.29 7.20 -1 -4 0 54.19 6.50 1 4 0 64.89 7.30 -1 -5 0 1028.80 54.59 -1 -5 0 917.21 54.89 -1 -6 0 353.56 25.70 -1 -6 0 412.26 27.90 -1 -7 0 213.18 22.80 -1 -7 0 285.57 30.40 -1 -8 0 26.00 7.30 -1 -8 0 35.10 8.20 -1 -9 0 145.69 16.80 -1 -10 0 119.19 16.60 -1 -11 0 75.19 14.30 -1 -12 0 4.20 7.30 -1 -13 0 15.70 9.80 2 -12 0 -3.30 4.40 2 -12 0 -5.50 4.30 2 -11 0 28.90 7.40 2 -11 0 23.60 6.00 2 -11 0 17.30 5.30 2 -10 0 0.40 3.90 2 -10 0 1.30 3.90 2 -10 0 -2.40 3.30 2 -10 0 11.50 6.00 2 -9 0 445.86 31.20 2 -9 0 496.85 31.20 2 -9 0 474.65 32.80 2 -9 0 458.75 32.50 -2 8 0 108.69 12.40 -2 8 0 157.38 15.00 2 -8 0 116.19 12.40 2 -8 0 119.29 12.60 2 -8 0 135.39 13.90 2 -8 0 139.29 14.00 -2 7 0 268.97 20.20 -2 7 0 253.67 19.80 2 -7 0 250.27 19.50 2 -7 0 243.18 18.10 2 -7 0 254.67 19.40 2 -7 0 260.37 20.10 -2 6 0 424.86 28.50 -2 6 0 497.75 30.10 -2 6 0 495.05 29.40 2 -6 0 449.46 29.10 2 -6 0 430.16 27.10 2 -6 0 446.06 29.30 -2 5 0 500.95 28.00 -2 5 0 440.26 28.30 -2 5 0 418.06 28.50 2 -5 0 455.05 28.60 2 -5 0 441.96 26.20 2 -5 0 486.25 28.80 -2 4 0 2186.78 114.59 -2 4 0 2301.57 114.49 -2 4 0 2252.47 114.39 2 -4 0 2223.78 114.09 2 -4 0 2200.78 114.19 2 -4 0 2305.37 111.39 -2 3 0 5009.00 240.28 -2 3 0 5067.19 237.78 2 -3 0 4903.61 240.08 2 -3 0 4800.02 236.88 2 -3 0 4632.14 239.88 -2 2 0 2202.88 115.99 -2 2 0 2205.88 111.69 2 -2 0 2224.18 114.69 2 -2 0 2296.67 112.39 2 -2 0 2506.65 115.09 -2 -2 0 2357.56 116.09 -2 -2 0 2425.46 115.59 -2 -2 0 2268.47 117.79 2 2 0 2370.96 115.19 2 2 0 2340.17 115.99 2 2 0 2346.67 118.79 -2 -3 0 4352.56 228.08 -2 -3 0 4899.91 224.28 2 3 0 4670.03 223.58 2 3 0 4570.64 229.18 -2 -4 0 2116.59 108.09 -2 -4 0 2085.19 109.89 2 4 0 2080.49 108.89 -2 -5 0 418.16 29.60 -2 -5 0 395.26 27.70 2 5 0 458.25 29.30 -2 -6 0 477.85 33.40 -2 -6 0 504.95 31.70 2 6 0 407.66 30.90 -2 -7 0 269.87 23.40 -2 -7 0 243.48 20.80 -2 -8 0 164.38 18.00 -2 -9 0 576.64 42.40 -2 -10 0 -1.80 5.80 -2 -11 0 18.30 9.70 -2 -12 0 14.30 8.40 3 -12 0 21.90 7.30 3 -12 0 21.20 6.80 3 -11 0 32.50 6.80 3 -11 0 22.50 7.80 3 -11 0 25.40 7.30 3 -10 0 64.59 11.70 3 -10 0 59.19 11.80 3 -10 0 42.80 8.20 3 -10 0 60.49 11.30 -3 9 0 321.07 24.70 3 -9 0 269.77 23.30 3 -9 0 284.07 26.10 3 -9 0 235.68 27.30 3 -9 0 299.27 26.50 -3 8 0 16.50 6.30 -3 8 0 12.00 4.90 3 -8 0 14.70 5.50 3 -8 0 30.50 7.40 3 -8 0 9.50 4.00 3 -8 0 14.00 5.30 -3 7 0 21.40 6.00 -3 7 0 19.40 6.30 3 -7 0 18.90 4.30 3 -7 0 19.00 6.00 3 -7 0 20.30 5.70 -3 6 0 753.72 47.00 -3 6 0 801.82 47.90 -3 6 0 886.41 45.20 3 -6 0 682.23 50.09 3 -6 0 778.12 47.40 3 -6 0 771.82 42.20 -3 5 0 496.15 28.70 -3 5 0 445.66 30.90 -3 5 0 484.15 31.90 3 -5 0 511.15 31.60 3 -5 0 460.95 26.80 -3 4 0 4425.66 216.48 -3 4 0 4443.66 220.58 3 -4 0 4435.46 215.78 3 -4 0 4461.95 220.78 3 -4 0 4308.37 220.08 -3 3 0 456.25 29.00 -3 3 0 467.15 25.60 3 -3 0 492.75 29.60 3 -3 0 445.06 25.70 3 -3 0 458.05 28.90 -3 2 0 5180.18 252.77 -3 2 0 5180.18 253.37 -3 2 0 4831.12 248.68 3 -2 0 5432.76 253.47 3 -2 0 5130.39 249.58 3 -2 0 4974.90 252.37 -3 1 0 3956.10 199.08 -3 1 0 3971.80 196.18 -3 1 0 4018.10 198.48 3 -1 0 4071.69 198.48 3 -1 0 4040.60 198.98 3 -1 0 3985.70 196.08 -3 0 0 2.10 1.60 -3 0 0 1.50 1.10 -3 0 0 5.30 2.10 3 0 0 -1.40 1.00 3 0 0 -1.00 1.10 3 0 0 1.10 1.10 -3 -1 0 4054.49 200.78 -3 -1 0 4055.69 201.58 -3 -1 0 3970.40 200.78 3 1 0 4026.20 200.58 3 1 0 4301.57 202.08 -3 -2 0 5045.29 253.77 -3 -2 0 5045.40 251.97 -3 -2 0 5399.46 253.37 3 2 0 5175.38 253.17 3 2 0 5220.08 255.17 3 2 0 5081.39 251.77 -3 -3 0 483.65 25.70 -3 -3 0 440.86 28.40 -3 -3 0 472.75 26.70 3 3 0 434.16 25.00 3 3 0 448.26 26.20 3 3 0 471.65 29.80 -3 -4 0 4606.94 203.48 -3 -4 0 4030.10 208.48 3 4 0 3784.22 202.68 3 4 0 4215.08 210.58 3 4 0 4201.68 202.38 -3 -5 0 390.36 23.70 -3 -5 0 475.45 23.70 -3 -5 0 467.25 32.80 -3 -5 0 470.85 30.30 3 5 0 447.46 31.20 -3 -6 0 715.43 48.20 -3 -6 0 703.93 45.10 3 6 0 794.12 47.80 -3 -7 0 22.20 8.10 3 7 0 25.10 7.70 -3 -8 0 24.80 8.60 -3 -9 0 292.27 28.50 -3 -10 0 34.20 11.00 -3 -11 0 15.60 8.70 -3 -12 0 10.00 11.00 4 -12 0 22.80 9.60 4 -12 0 9.90 6.00 4 -12 0 2.30 5.90 4 -11 0 68.59 9.80 4 -11 0 63.79 14.20 4 -11 0 61.19 11.90 -4 10 0 14.50 7.30 -4 10 0 -0.10 6.50 4 -10 0 13.30 6.10 4 -10 0 6.10 5.80 4 -10 0 15.70 7.30 4 -10 0 9.90 4.50 -4 9 0 21.50 6.90 -4 9 0 27.40 8.40 4 -9 0 15.30 6.50 4 -9 0 31.90 8.00 4 -9 0 24.50 8.90 4 -9 0 19.20 5.20 -4 8 0 31.90 8.50 -4 8 0 30.40 8.10 4 -8 0 59.29 12.10 4 -8 0 28.70 6.00 4 -8 0 55.09 10.80 -4 7 0 901.11 53.29 -4 7 0 828.92 47.30 4 -7 0 676.33 63.99 4 -7 0 847.62 52.59 4 -7 0 768.02 44.60 -4 6 0 84.29 9.20 -4 6 0 56.09 10.40 4 -6 0 73.69 10.60 4 -6 0 75.99 10.90 4 -6 0 76.49 7.90 -4 5 0 530.35 30.70 -4 5 0 557.84 35.60 4 -5 0 528.25 30.40 4 -5 0 512.35 34.80 4 -5 0 500.35 35.30 -4 4 0 158.88 14.80 -4 4 0 126.09 10.50 -4 4 0 157.08 15.20 4 -4 0 156.38 15.00 4 -4 0 156.18 14.60 4 -4 0 164.18 11.90 -4 3 0 4247.18 215.98 -4 3 0 4400.36 215.18 -4 3 0 3979.10 208.78 4 -3 0 4308.77 210.48 4 -3 0 4454.15 215.08 4 -3 0 4289.27 215.58 -4 2 0 2187.48 113.99 -4 2 0 2299.67 115.39 -4 2 0 2107.49 109.89 4 -2 0 2161.88 113.69 4 -2 0 2198.08 110.29 4 -2 0 2226.08 114.89 -4 1 0 2642.84 133.99 -4 1 0 2641.44 132.89 -4 1 0 2493.75 129.99 4 -1 0 2676.63 130.19 4 -1 0 2674.43 133.89 4 -1 0 2475.15 134.09 -4 0 0 569.64 31.40 4 0 0 545.35 31.60 4 0 0 505.95 32.20 -4 -1 0 2702.53 136.39 -4 -1 0 2663.93 137.49 -4 -1 0 2712.33 135.69 4 1 0 2678.93 135.99 4 1 0 2733.63 136.89 -4 -2 0 2365.86 117.29 -4 -2 0 2295.97 115.59 -4 -2 0 2193.78 116.29 4 2 0 2252.27 115.19 4 2 0 2259.07 116.89 4 2 0 2305.17 118.59 -4 -3 0 4376.86 207.28 -4 -3 0 4316.77 209.08 -4 -3 0 4023.00 209.48 4 3 0 4090.79 211.68 4 3 0 4109.59 206.58 4 3 0 4257.77 208.58 -4 -4 0 147.69 12.30 -4 -4 0 149.69 11.20 -4 -4 0 147.39 13.80 4 4 0 149.69 11.80 4 4 0 150.48 10.80 4 4 0 137.19 14.60 -4 -5 0 564.24 29.30 -4 -5 0 522.55 30.40 -4 -5 0 529.15 34.50 -4 -5 0 541.45 38.10 4 5 0 447.56 27.90 4 5 0 517.75 27.70 4 5 0 550.24 37.10 -4 -6 0 67.69 6.20 -4 -6 0 71.89 6.00 -4 -6 0 69.09 14.10 4 6 0 79.19 13.90 -4 -7 0 942.91 59.69 4 7 0 819.82 56.19 -4 -8 0 23.40 9.40 4 8 0 39.30 10.60 -4 -9 0 30.30 9.30 -4 -10 0 17.80 9.60 -4 -11 0 59.19 15.50 -4 -12 0 1.80 8.60 5 -12 0 1.50 6.10 5 -11 0 0.90 5.80 5 -11 0 20.40 7.10 5 -11 0 11.70 5.00 -5 10 0 -12.30 6.00 -5 10 0 8.20 6.30 5 -10 0 0.80 6.10 5 -10 0 2.10 5.40 5 -10 0 -4.10 4.80 5 -10 0 -1.40 4.00 -5 9 0 115.39 15.80 -5 9 0 95.89 17.40 5 -9 0 127.49 15.90 5 -9 0 99.39 14.00 5 -9 0 120.49 11.80 5 -9 0 122.79 17.70 -5 8 0 132.79 14.10 -5 8 0 128.59 17.80 5 -8 0 137.59 18.00 5 -8 0 119.19 11.90 5 -8 0 104.69 22.50 -5 7 0 48.20 8.80 -5 7 0 47.20 11.60 5 -7 0 40.90 7.40 5 -7 0 61.19 12.10 5 -7 0 48.30 10.60 -5 6 0 236.28 18.50 5 -6 0 261.57 18.70 5 -6 0 284.27 24.80 5 -6 0 284.97 24.00 -5 5 0 133.59 11.30 -5 5 0 129.59 15.60 -5 5 0 131.49 15.50 5 -5 0 126.39 15.20 5 -5 0 154.88 15.90 5 -5 0 152.28 12.20 -5 4 0 394.16 29.40 -5 4 0 382.76 30.30 -5 4 0 365.36 23.20 5 -4 0 407.26 29.40 5 -4 0 416.46 25.20 5 -4 0 447.66 31.30 -5 3 0 3034.30 157.28 -5 3 0 3212.68 165.58 -5 3 0 3096.49 163.68 5 -3 0 3319.87 158.88 5 -3 0 3096.59 163.28 5 -3 0 3300.57 165.48 -5 2 0 1877.01 101.19 -5 2 0 2034.30 106.09 -5 2 0 2052.39 107.69 5 -2 0 1957.10 101.39 5 -2 0 2018.20 105.79 5 -2 0 1998.00 107.09 -5 1 0 740.03 44.10 -5 1 0 670.93 39.20 -5 1 0 616.84 49.70 5 -1 0 694.13 41.90 5 -1 0 704.53 39.40 5 -1 0 671.93 43.00 -5 0 0 -2.30 1.90 -5 0 0 0.10 1.90 -5 0 0 -0.70 2.30 5 0 0 -1.10 1.40 5 0 0 1.10 1.80 5 0 0 3.20 2.70 -5 -1 0 703.53 41.60 -5 -1 0 706.33 43.20 -5 -1 0 708.23 40.90 5 1 0 709.23 42.00 5 1 0 670.33 41.00 -5 -2 0 2119.39 104.19 -5 -2 0 1937.41 103.79 -5 -2 0 2075.59 106.29 5 2 0 1933.51 105.99 5 2 0 1969.10 103.39 5 2 0 1939.21 105.49 -5 -3 0 3198.68 152.58 -5 -3 0 2853.51 158.78 -5 -3 0 2904.21 160.38 5 3 0 3171.28 154.48 5 3 0 3002.30 154.38 5 3 0 2904.81 164.68 -5 -4 0 413.96 28.60 -5 -4 0 410.86 27.70 -5 -4 0 404.36 25.70 5 4 0 402.06 30.60 5 4 0 389.46 24.80 5 4 0 418.86 27.20 -5 -5 0 145.79 11.80 5 5 0 131.39 11.70 5 5 0 133.79 16.00 -5 -6 0 273.37 17.10 -5 -6 0 288.67 27.00 -5 -6 0 248.18 18.00 5 6 0 219.18 14.70 5 6 0 253.37 24.10 -5 -7 0 48.50 13.70 -5 -7 0 38.80 5.20 -5 -7 0 50.19 5.20 5 7 0 63.19 13.50 -5 -8 0 118.29 20.70 5 8 0 116.69 19.60 -5 -9 0 66.39 16.60 5 9 0 104.19 18.10 -5 -10 0 0.30 8.20 -5 -11 0 9.00 10.80 -5 -12 0 -6.60 11.00 6 -11 0 20.30 6.80 6 -11 0 6.00 8.30 -6 10 0 19.30 9.60 -6 10 0 19.50 9.30 6 -10 0 12.20 5.90 6 -10 0 15.00 7.10 6 -10 0 16.80 9.00 6 -9 0 115.09 14.60 6 -9 0 142.79 19.70 6 -9 0 127.29 17.70 -6 8 0 82.49 11.80 -6 8 0 79.89 17.00 6 -8 0 99.19 10.70 6 -8 0 82.49 15.30 6 -8 0 70.99 13.00 -6 7 0 435.46 30.30 6 -7 0 545.45 40.70 6 -7 0 437.46 29.80 6 -7 0 537.25 38.60 -6 6 0 330.37 22.80 -6 6 0 314.77 29.50 6 -6 0 368.16 29.40 6 -6 0 315.37 22.90 6 -6 0 391.86 32.00 -6 5 0 256.07 34.10 -6 5 0 319.77 21.50 6 -5 0 368.26 30.10 6 -5 0 350.86 23.00 6 -5 0 362.26 28.70 -6 4 0 103.89 9.30 -6 4 0 102.79 13.90 6 -4 0 102.99 14.70 6 -4 0 96.79 10.30 -6 3 0 699.53 43.60 -6 3 0 594.34 36.50 -6 3 0 658.43 44.60 6 -3 0 601.24 41.80 6 -3 0 670.23 38.00 6 -3 0 630.54 43.80 -6 2 0 3080.69 162.98 -6 2 0 3301.67 168.58 6 -2 0 3136.99 167.48 6 -2 0 3323.27 170.48 6 -2 0 3373.56 163.48 -6 1 0 977.60 56.99 -6 1 0 943.31 53.59 6 -1 0 943.51 56.29 6 -1 0 933.61 58.19 6 -1 0 952.70 53.69 -6 0 0 10.70 5.00 -6 0 0 15.00 4.80 -6 0 0 7.50 4.20 6 0 0 6.20 3.30 6 0 0 7.60 3.80 6 0 0 3.60 3.30 -6 -1 0 928.71 57.09 -6 -1 0 992.90 55.39 -6 -1 0 935.41 54.39 6 1 0 922.41 54.39 6 1 0 935.81 56.89 6 1 0 915.21 55.09 -6 -2 0 3315.17 170.28 -6 -2 0 3618.84 174.48 -6 -2 0 3173.38 170.18 6 2 0 3446.16 173.58 6 2 0 3326.77 173.08 6 2 0 3211.38 169.78 -6 -3 0 628.74 40.40 -6 -3 0 697.33 42.90 -6 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577.64 44.40 10 -1 0 565.74 47.90 10 -1 0 535.75 40.90 -10 0 0 15.30 6.80 -10 0 0 19.10 9.90 10 0 0 41.20 10.70 10 0 0 23.90 7.80 -10 -1 0 628.24 49.40 -10 -1 0 577.04 43.60 10 1 0 555.44 43.90 10 1 0 533.25 46.00 -10 -2 0 59.49 15.30 -10 -2 0 65.79 13.80 10 2 0 74.49 24.70 10 2 0 52.09 13.70 -10 -3 0 287.87 29.90 -10 -3 0 283.57 26.30 10 3 0 256.17 29.30 10 3 0 250.87 27.80 -10 -4 0 60.59 15.40 -10 -4 0 37.20 10.10 10 4 0 39.20 14.00 10 4 0 44.90 13.40 -10 -5 0 26.00 8.30 -10 -5 0 33.60 11.50 10 5 0 48.90 14.00 10 5 0 51.59 13.50 -10 -6 0 96.19 14.20 10 6 0 106.59 20.60 10 6 0 93.19 16.30 -10 -7 0 241.48 25.70 -10 -7 0 234.38 31.70 -10 -7 0 238.68 22.30 10 7 0 229.68 29.10 -10 -8 0 1.10 4.70 -10 -8 0 12.70 6.80 -10 -8 0 10.10 10.90 10 8 0 10.40 12.30 -10 -9 0 4.80 10.50 10 9 0 21.10 13.40 -11 7 0 -14.00 11.20 11 -7 0 5.20 8.00 11 -7 0 -1.80 6.50 11 -6 0 -0.60 8.20 11 -6 0 2.90 7.00 -11 5 0 28.00 12.50 11 -5 0 35.00 11.10 11 -5 0 28.60 8.90 -11 4 0 53.29 15.20 11 -4 0 64.49 19.40 11 -4 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22.90 13.80 13 2 1 -7.30 8.40 -13 -2 -1 8.30 9.50 13 1 1 14.40 11.50 -13 -1 -1 22.20 10.60 13 0 1 260.17 36.30 13 0 1 223.38 27.80 -13 0 -1 236.38 35.00 13 -1 1 12.00 13.10 13 -1 1 9.20 10.50 -13 1 -1 20.50 13.40 13 -2 1 31.80 14.20 13 -2 1 17.60 10.70 -13 2 -1 -5.00 7.00 13 -3 1 11.40 13.10 13 -3 1 -14.50 7.00 -13 3 -1 3.70 7.80 13 -4 1 -8.80 14.50 13 -4 1 9.30 10.30 -13 4 -1 -15.00 8.80 12 6 1 94.29 22.80 -12 -6 -1 82.79 21.20 -12 -6 -1 81.39 22.80 12 5 1 -14.30 8.80 -12 -5 -1 -4.00 7.90 -12 -5 -1 16.30 9.40 12 4 1 17.20 12.60 12 3 1 25.20 11.50 -12 -3 -1 31.00 12.20 12 2 1 8.90 7.70 12 2 1 9.60 10.60 -12 -2 -1 1.50 6.80 12 1 1 38.90 13.70 12 1 1 73.29 18.60 -12 -1 -1 28.80 13.10 12 0 1 6.40 8.00 12 0 1 -4.50 9.70 -12 0 -1 3.00 7.70 12 -1 1 35.10 10.60 12 -1 1 20.80 11.20 -12 1 -1 45.90 14.20 12 -2 1 -1.50 8.70 12 -2 1 -1.60 8.40 -12 2 -1 20.70 12.70 12 -3 1 24.90 11.20 12 -3 1 21.90 14.30 -12 3 -1 34.20 16.40 12 -4 1 24.50 9.80 12 -4 1 2.40 9.70 -12 4 -1 15.20 10.50 12 -5 1 17.60 13.20 12 -5 1 4.90 7.80 -12 5 -1 1.70 12.90 12 -6 1 106.19 16.10 12 -6 1 80.39 21.70 -12 6 -1 54.19 16.10 11 7 1 105.69 23.30 -11 -7 -1 102.09 21.00 -11 -7 -1 102.09 25.30 -11 -7 -1 133.49 16.10 11 6 1 9.00 11.50 -11 -6 -1 1.10 7.00 -11 -6 -1 5.50 8.20 -11 -6 -1 5.90 10.60 11 5 1 68.39 17.20 -11 -5 -1 50.99 11.60 -11 -5 -1 45.10 12.70 11 4 1 -11.10 4.90 -11 -4 -1 -1.40 7.60 -11 -4 -1 10.10 12.40 11 3 1 8.00 7.60 11 3 1 10.30 8.80 -11 -3 -1 4.10 6.40 -11 -3 -1 8.10 6.70 11 2 1 50.89 13.60 11 2 1 54.89 14.80 -11 -2 -1 79.09 15.40 -11 -2 -1 43.70 13.60 11 1 1 8.60 10.00 11 1 1 14.50 9.30 -11 -1 -1 13.70 7.80 -11 -1 -1 11.90 7.80 11 0 1 948.91 70.29 11 0 1 911.91 64.39 -11 0 -1 878.21 69.39 -11 0 -1 906.01 63.19 11 -1 1 38.00 10.40 11 -1 1 16.80 11.90 -11 1 -1 32.80 11.20 -11 1 -1 37.30 11.80 11 -2 1 32.80 12.70 11 -2 1 60.89 13.80 -11 2 -1 100.19 22.90 -11 2 -1 53.19 11.40 11 -3 1 -3.80 7.50 11 -3 1 12.40 7.70 -11 3 -1 1.60 7.70 11 -4 1 13.90 8.40 11 -4 1 -4.00 6.10 -11 4 -1 2.60 8.40 11 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2 -18 86.39 19.50 -3 -3 18 37.30 11.70 3 3 -18 46.00 12.20 -3 -4 18 13.70 8.90 3 4 -18 6.80 7.30 -4 4 18 7.70 13.00 4 -4 -18 31.40 12.60 4 -4 -18 47.70 12.20 -4 3 18 91.69 19.20 4 -3 -18 62.49 16.80 4 -3 -18 76.99 16.10 -4 2 18 38.10 14.80 4 -2 -18 43.20 11.90 4 -2 -18 37.50 14.00 -4 1 18 2.50 14.30 4 -1 -18 -13.60 5.20 4 -1 -18 -6.30 7.90 -4 0 18 -3.70 6.90 4 0 -18 -0.20 7.80 4 0 -18 19.00 8.40 -4 -1 18 0.10 6.60 4 1 -18 -6.40 6.20 -4 -2 18 25.20 12.10 4 2 -18 24.90 17.50 4 2 -18 30.90 11.70 -4 -3 18 88.69 19.90 4 3 -18 69.19 14.20 -4 -4 18 28.60 14.50 4 4 -18 37.90 10.80 -5 3 18 32.90 13.30 5 -3 -18 28.30 13.70 5 -3 -18 20.80 9.50 -5 2 18 9.80 11.40 5 -2 -18 32.30 10.30 5 -2 -18 30.00 11.50 -5 1 18 9.10 8.10 5 -1 -18 14.90 9.90 5 -1 -18 0.80 7.60 -5 0 18 1.70 7.30 5 0 -18 4.30 7.90 5 0 -18 -6.00 6.10 -5 -1 18 14.80 9.00 5 1 -18 5.60 7.60 5 1 -18 -6.60 9.80 -5 -2 18 47.70 15.10 5 2 -18 25.20 9.60 -5 -3 18 13.00 10.90 5 3 -18 16.70 8.70 -6 2 18 15.40 11.00 6 -2 -18 -2.90 12.00 6 -2 -18 17.00 10.60 -6 1 18 -10.80 9.00 6 -1 -18 10.30 8.30 6 -1 -18 3.80 8.80 -6 0 18 93.09 21.20 6 0 -18 53.09 15.20 6 0 -18 91.89 18.50 -6 -1 18 14.60 10.40 6 1 -18 24.70 11.70 -6 -2 18 19.20 10.00 6 2 -18 -2.90 7.70 1 2 19 10.90 12.30 -1 -2 -19 9.00 6.80 1 1 19 42.10 17.00 -1 -1 -19 18.70 14.60 -1 -1 -19 31.50 9.60 1 0 19 185.98 27.10 -1 0 -19 139.29 26.50 -1 0 -19 155.98 18.00 1 -1 19 9.30 11.60 -1 1 -19 26.40 8.90 -1 1 -19 35.70 15.20 1 -2 19 11.40 10.30 -1 2 -19 2.50 6.70 0 2 19 32.70 15.90 0 -2 -19 13.40 7.20 0 -2 -19 21.50 12.60 0 1 19 62.19 16.40 0 -1 -19 102.39 16.40 0 -1 -19 56.29 18.30 0 0 19 7.60 8.90 0 0 -19 7.90 9.40 0 0 -19 4.40 7.20 0 -1 19 55.69 15.30 0 1 -19 75.79 18.20 0 1 -19 76.29 13.70 0 -2 19 21.30 12.00 0 2 -19 22.60 9.00 -1 3 19 -21.90 8.60 1 -3 -19 3.60 7.10 -1 2 19 1.60 10.80 1 -2 -19 35.70 11.30 1 -2 -19 36.50 13.40 -1 1 19 79.89 22.00 1 -1 -19 65.19 13.80 1 -1 -19 75.89 19.50 -1 0 19 232.88 30.90 1 0 -19 218.78 30.40 1 0 -19 173.88 21.00 -1 -1 19 67.39 19.20 1 1 -19 75.09 20.10 1 1 -19 68.09 13.60 -1 -2 19 17.10 8.00 1 2 -19 42.40 11.10 -1 -3 19 -10.90 5.70 1 3 -19 2.10 8.30 -2 3 19 50.39 15.20 2 -3 -19 32.00 9.90 -2 2 19 8.00 10.70 2 -2 -19 24.70 15.20 2 -2 -19 16.60 18.70 -2 1 19 -3.60 11.60 2 -1 -19 14.70 10.60 2 -1 -19 2.20 7.90 -2 0 19 5.10 9.80 2 0 -19 -5.50 5.90 2 0 -19 8.70 9.30 -2 -1 19 18.90 10.80 2 1 -19 13.60 9.10 2 1 -19 8.20 11.50 -2 -2 19 20.00 7.60 2 2 -19 9.10 7.70 -2 -3 19 33.50 10.70 2 3 -19 29.50 10.70 3 -2 -19 104.59 18.40 3 -2 -19 78.29 20.00 -3 1 19 39.90 12.90 3 -1 -19 20.00 13.30 3 -1 -19 58.19 13.60 -3 0 19 12.10 11.10 3 0 -19 24.50 10.00 3 0 -19 3.40 11.20 -3 -1 19 33.40 11.90 3 1 -19 49.80 12.80 3 1 -19 62.19 19.30 -3 -2 19 104.39 21.80 3 2 -19 129.89 17.70 4 -2 -19 24.80 10.40 -4 1 19 2.50 9.90 4 -1 -19 7.00 11.10 4 -1 -19 10.70 8.80 -4 0 19 -3.80 8.30 4 0 -19 -19.00 8.60 4 0 -19 3.50 6.50 -4 -1 19 11.60 10.00 4 1 -19 6.00 8.30 4 2 -19 59.99 14.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 35201 _shelx_res_file ; TITL d8v18991_a.res in Pn d8v18991.res created by SHELXL-2016/6 at 15:00:07 on 12-Aug-2019 CELL 0.71073 10.673 10.0539 15.0271 90 96.095 90 ZERR 2 0.0005 0.0004 0.0007 0 0.001 0 LATT -1 SYMM 0.5+X,-Y,0.5+Z SFAC C H B N O UNIT 78 82 2 4 2 OMIT -1 1 1 OMIT 0 1 0 OMIT -3.00 52.00 L.S. 9 ACTA BOND $H FMAP 2 PLAN 20 LIST 4 conf htab mpla c34 > c39 mpla c28 > c33 mpla c22 > c27 mpla c16 > c21 mpla c2 > c7 wpdb -1 size 0.20 0.17 0.13 twin -1 0 0 0 -1 0 0 0 -1 TEMP 19.86 WGHT 0.051300 0.176000 EXTI 0.080496 BASF 0.06304 FVAR 1.76782 O1 5 0.582905 0.293851 0.585309 11.00000 0.05292 0.03945 = 0.03324 -0.00345 0.00938 0.00260 N1 4 0.496429 0.467771 0.479091 11.00000 0.05051 0.03926 = 0.03862 0.00198 0.00855 0.00124 N2 4 0.137143 0.876095 0.416322 11.00000 0.04691 0.04789 = 0.06859 -0.00541 -0.00896 0.00421 AFIX 43 H2 2 0.069857 0.852951 0.383366 11.00000 -1.20000 AFIX 0 C1 1 0.514248 0.384999 0.415146 11.00000 0.05733 0.04935 = 0.03360 0.00210 0.00711 0.00196 AFIX 43 H1 2 0.480869 0.406135 0.357181 11.00000 -1.20000 AFIX 0 C2 1 0.582525 0.263162 0.429380 11.00000 0.04817 0.04473 = 0.03986 -0.00106 0.00830 0.00231 C3 1 0.610421 0.217402 0.517567 11.00000 0.03944 0.04214 = 0.03392 -0.00511 0.00703 -0.00146 C4 1 0.658736 0.086781 0.533261 11.00000 0.03504 0.04150 = 0.03869 -0.00426 0.00534 -0.00182 C5 1 0.678270 0.012956 0.457612 11.00000 0.03514 0.04690 = 0.04332 -0.00749 0.00418 0.00213 AFIX 43 H5 2 0.710546 -0.072473 0.466659 11.00000 -1.20000 AFIX 0 C6 1 0.653329 0.056675 0.368873 11.00000 0.03912 0.05406 = 0.03937 -0.01067 0.00317 0.00391 C7 1 0.604129 0.182626 0.356080 11.00000 0.05343 0.05999 = 0.03246 -0.00352 0.00589 0.00531 AFIX 43 H7 2 0.584944 0.214840 0.298223 11.00000 -1.20000 AFIX 0 C8 1 0.685285 0.030206 0.628246 11.00000 0.04254 0.04339 = 0.03863 -0.00278 0.00716 -0.00207 C9 1 0.560997 0.011580 0.668177 11.00000 0.05675 0.07490 = 0.05198 0.00659 0.01693 -0.00256 AFIX 137 H9A 2 0.519887 0.096092 0.671495 11.00000 -1.50000 H9B 2 0.577082 -0.025465 0.727164 11.00000 -1.50000 H9C 2 0.507751 -0.047618 0.631018 11.00000 -1.50000 AFIX 0 C10 1 0.770009 0.123561 0.688055 11.00000 0.06388 0.06192 = 0.04362 0.00090 -0.00772 -0.00529 AFIX 137 H10A 2 0.844744 0.142770 0.660072 11.00000 -1.50000 H10B 2 0.792871 0.081776 0.744907 11.00000 -1.50000 H10C 2 0.725652 0.204802 0.696772 11.00000 -1.50000 AFIX 0 C11 1 0.752512 -0.103858 0.628637 11.00000 0.07197 0.05207 = 0.04905 0.00507 0.00684 0.00929 AFIX 137 H11A 2 0.700400 -0.166604 0.593653 11.00000 -1.50000 H11B 2 0.768454 -0.135614 0.689026 11.00000 -1.50000 H11C 2 0.830955 -0.093656 0.603480 11.00000 -1.50000 AFIX 0 C12 1 0.677197 -0.036740 0.291141 11.00000 0.05068 0.06504 = 0.04049 -0.01795 0.00341 0.00531 C13 1 0.813911 -0.083626 0.302537 11.00000 0.05100 0.10081 = 0.06334 -0.02937 0.01490 0.00966 AFIX 137 H13A 2 0.868894 -0.008303 0.300877 11.00000 -1.50000 H13B 2 0.827893 -0.143725 0.254940 11.00000 -1.50000 H13C 2 0.830972 -0.128355 0.358964 11.00000 -1.50000 AFIX 0 C14 1 0.593692 -0.161882 0.295743 11.00000 0.06279 0.08464 = 0.07750 -0.03290 0.00002 -0.00520 AFIX 137 H14A 2 0.619185 -0.209824 0.349898 11.00000 -1.50000 H14B 2 0.602955 -0.217905 0.245124 11.00000 -1.50000 H14C 2 0.507139 -0.135542 0.295062 11.00000 -1.50000 AFIX 0 C15 1 0.649980 0.030120 0.201754 11.00000 0.13509 0.09350 = 0.04216 -0.02156 0.00795 0.02336 AFIX 137 H15A 2 0.563378 0.057609 0.193724 11.00000 -1.50000 H15B 2 0.665710 -0.031042 0.155155 11.00000 -1.50000 H15C 2 0.703463 0.106510 0.199271 11.00000 -1.50000 AFIX 0 C16 1 0.720887 0.500560 0.570041 11.00000 0.05426 0.03839 = 0.04501 -0.00728 0.01275 -0.00045 C17 1 0.812276 0.481353 0.641865 11.00000 0.05629 0.06639 = 0.05105 -0.00738 0.00676 -0.00781 AFIX 43 H17 2 0.789907 0.436802 0.692064 11.00000 -1.20000 AFIX 0 C18 1 0.935315 0.525617 0.642064 11.00000 0.05208 0.07576 = 0.08148 -0.01831 0.00290 -0.00191 AFIX 43 H18 2 0.993902 0.509222 0.691179 11.00000 -1.20000 AFIX 0 C19 1 0.970622 0.594218 0.568990 11.00000 0.05053 0.07254 = 0.09887 -0.01429 0.02569 -0.00933 AFIX 43 H19 2 1.052254 0.626532 0.568899 11.00000 -1.20000 AFIX 0 C20 1 0.884116 0.613408 0.497646 11.00000 0.06867 0.06848 = 0.08791 0.00384 0.03563 -0.00811 AFIX 43 H20 2 0.907595 0.657729 0.447688 11.00000 -1.20000 AFIX 0 C21 1 0.760807 0.568371 0.497268 11.00000 0.05813 0.05503 = 0.05913 0.00415 0.01931 0.00076 AFIX 43 H21 2 0.703633 0.583907 0.447221 11.00000 -1.20000 AFIX 0 C22 1 0.508862 0.498264 0.657983 11.00000 0.04984 0.03934 = 0.03853 0.00043 0.00713 0.00287 C23 1 0.397904 0.440094 0.679153 11.00000 0.06209 0.06286 = 0.06042 -0.01123 0.02185 -0.00970 AFIX 43 H23 2 0.365239 0.367485 0.646062 11.00000 -1.20000 AFIX 0 C24 1 0.334741 0.487740 0.748438 11.00000 0.07609 0.09525 = 0.07931 -0.01039 0.04158 -0.01198 AFIX 43 H24 2 0.260711 0.446715 0.761383 11.00000 -1.20000 AFIX 0 C25 1 0.380688 0.595393 0.798321 11.00000 0.09780 0.07649 = 0.06660 -0.01118 0.04278 0.01174 AFIX 43 H25 2 0.336914 0.628389 0.843878 11.00000 -1.20000 AFIX 0 C26 1 0.491081 0.653434 0.780425 11.00000 0.09809 0.05197 = 0.05087 -0.01243 0.02012 0.00369 AFIX 43 H26 2 0.523989 0.724856 0.814634 11.00000 -1.20000 AFIX 0 C27 1 0.553453 0.605177 0.711090 11.00000 0.06916 0.04488 = 0.04634 -0.00453 0.01678 -0.00229 AFIX 43 H27 2 0.628277 0.645808 0.699448 11.00000 -1.20000 AFIX 0 C28 1 0.406335 0.573085 0.460985 11.00000 0.04962 0.04007 = 0.03891 0.00372 0.00584 0.00247 C29 1 0.296052 0.554221 0.405642 11.00000 0.05758 0.04020 = 0.04599 -0.00266 0.00341 -0.00434 AFIX 43 H29 2 0.279566 0.471796 0.378836 11.00000 -1.20000 AFIX 0 C30 1 0.209873 0.656132 0.389555 11.00000 0.04891 0.04709 = 0.04839 -0.00140 -0.00513 -0.00235 AFIX 43 H30 2 0.137514 0.642332 0.350431 11.00000 -1.20000 AFIX 0 C31 1 0.229777 0.779202 0.431065 11.00000 0.04710 0.04201 = 0.04515 0.00506 0.00424 0.00120 C32 1 0.339774 0.796219 0.488017 11.00000 0.05356 0.03851 = 0.05623 -0.00479 -0.00689 0.00104 AFIX 43 H32 2 0.354994 0.877312 0.516931 11.00000 -1.20000 AFIX 0 C33 1 0.427100 0.694966 0.502573 11.00000 0.04969 0.04438 = 0.04908 -0.00161 -0.00467 -0.00043 AFIX 43 H33 2 0.500447 0.708916 0.540658 11.00000 -1.20000 AFIX 0 C34 1 0.139912 1.006999 0.448589 11.00000 0.04568 0.04573 = 0.03986 0.00632 0.00199 0.00328 C35 1 0.030130 1.061960 0.475552 11.00000 0.04320 0.06121 = 0.04621 0.00408 0.00564 0.00165 AFIX 43 H35 2 -0.042477 1.010437 0.473608 11.00000 -1.20000 AFIX 0 C36 1 0.027775 1.191286 0.504973 11.00000 0.05822 0.06399 = 0.05129 0.00115 0.01100 0.01491 AFIX 43 H36 2 -0.047157 1.227639 0.520253 11.00000 -1.20000 AFIX 0 C37 1 0.135016 1.266930 0.511928 11.00000 0.07743 0.04684 = 0.07224 -0.00094 0.00780 0.00645 AFIX 43 H37 2 0.134259 1.353132 0.534314 11.00000 -1.20000 AFIX 0 C38 1 0.243287 1.214207 0.485559 11.00000 0.05954 0.04570 = 0.08545 0.00727 0.00993 -0.00505 AFIX 43 H38 2 0.316224 1.265472 0.490443 11.00000 -1.20000 AFIX 0 C39 1 0.246847 1.086726 0.451875 11.00000 0.04885 0.04841 = 0.07071 0.00627 0.01509 0.00205 AFIX 43 H39 2 0.320265 1.054314 0.431500 11.00000 -1.20000 AFIX 0 B1 3 0.579950 0.442511 0.575970 11.00000 0.04858 0.03909 = 0.03608 -0.00323 0.00673 0.00117 HKLF 4 REM d8v18991_a.res in Pn REM R1 = 0.0430 for 5477 Fo > 4sig(Fo) and 0.0517 for all 6249 data REM 396 parameters refined using 2 restraints END WGHT 0.0511 0.1769 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.150, deepest hole -0.153, 1-sigma level 0.034 Q1 1 0.8952 0.6047 0.5641 11.00000 0.05 0.15 Q2 1 0.3254 0.5943 0.7372 11.00000 0.05 0.15 Q3 1 0.2687 0.7795 0.4781 11.00000 0.05 0.14 Q4 1 0.4757 0.6107 0.6605 11.00000 0.05 0.13 Q5 1 0.3412 0.6318 0.7363 11.00000 0.05 0.13 Q6 1 0.5746 -0.0783 0.2592 11.00000 0.05 0.13 Q7 1 0.4518 0.3776 0.3570 11.00000 0.05 0.13 Q8 1 0.3004 0.7887 0.4429 11.00000 0.05 0.13 Q9 1 0.3551 0.6165 0.6833 11.00000 0.05 0.13 Q10 1 0.5375 0.4547 0.5279 11.00000 0.05 0.12 Q11 1 1.0592 0.6267 0.5415 11.00000 0.05 0.12 Q12 1 0.6333 0.2604 0.4679 11.00000 0.05 0.12 Q13 1 0.7112 0.0581 0.4141 11.00000 0.05 0.12 Q14 1 0.6627 0.0092 0.3267 11.00000 0.05 0.12 Q15 1 0.7550 0.5050 0.6081 11.00000 0.05 0.11 Q16 1 0.2675 0.5992 0.6371 11.00000 0.05 0.11 Q17 1 0.7098 0.0684 0.5775 11.00000 0.05 0.11 Q18 1 0.3885 0.5855 0.4153 11.00000 0.05 0.11 Q19 1 0.6850 0.0283 0.2647 11.00000 0.05 0.11 Q20 1 0.9677 0.5990 0.5215 11.00000 0.05 0.10 ; _shelx_res_checksum 5239 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y, 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 O O1 0.58291(17) 0.29385(18) 0.58531(12) 0.0415(4) Uani d 1 N N1 0.4964(2) 0.4678(2) 0.47909(15) 0.0425(5) Uani d 1 N N2 0.1371(2) 0.8761(3) 0.41632(19) 0.0555(7) Uani d 1 H H2 0.069857 0.852951 0.383366 0.067 Uiso calc 1 C C1 0.5142(3) 0.3850(3) 0.41515(19) 0.0466(6) Uani d 1 H H1 0.480869 0.406135 0.357181 0.056 Uiso calc 1 C C2 0.5825(3) 0.2632(3) 0.42938(19) 0.0440(6) Uani d 1 C C3 0.6104(2) 0.2174(3) 0.51757(17) 0.0383(6) Uani d 1 C C4 0.6587(2) 0.0868(3) 0.53326(17) 0.0383(6) Uani d 1 C C5 0.6783(2) 0.0130(3) 0.45761(19) 0.0418(6) Uani d 1 H H5 0.710546 -0.072473 0.466659 0.050 Uiso calc 1 C C6 0.6533(3) 0.0567(3) 0.36887(19) 0.0443(7) Uani d 1 C C7 0.6041(3) 0.1826(3) 0.35608(19) 0.0485(7) Uani d 1 H H7 0.584944 0.214840 0.298223 0.058 Uiso calc 1 C C8 0.6853(3) 0.0302(3) 0.62825(18) 0.0413(6) Uani d 1 C C9 0.5610(3) 0.0116(4) 0.6682(2) 0.0604(8) Uani d 1 H H9A 0.519887 0.096092 0.671495 0.091 Uiso calc 1 H H9B 0.577082 -0.025465 0.727164 0.091 Uiso calc 1 H H9C 0.507751 -0.047618 0.631018 0.091 Uiso calc 1 C C10 0.7700(3) 0.1236(3) 0.6881(2) 0.0574(8) Uani d 1 H H10A 0.844744 0.142770 0.660072 0.086 Uiso calc 1 H H10B 0.792871 0.081776 0.744907 0.086 Uiso calc 1 H H10C 0.725652 0.204802 0.696772 0.086 Uiso calc 1 C C11 0.7525(3) -0.1039(3) 0.6286(2) 0.0577(8) Uani d 1 H H11A 0.700400 -0.166604 0.593653 0.087 Uiso calc 1 H H11B 0.768454 -0.135614 0.689026 0.087 Uiso calc 1 H H11C 0.830955 -0.093656 0.603480 0.087 Uiso calc 1 C C12 0.6772(3) -0.0367(3) 0.2911(2) 0.0522(7) Uani d 1 C C13 0.8139(3) -0.0836(5) 0.3025(2) 0.0711(11) Uani d 1 H H13A 0.868894 -0.008303 0.300877 0.107 Uiso calc 1 H H13B 0.827893 -0.143725 0.254940 0.107 Uiso calc 1 H H13C 0.830972 -0.128355 0.358964 0.107 Uiso calc 1 C C14 0.5937(4) -0.1619(4) 0.2957(3) 0.0755(11) Uani d 1 H H14A 0.619185 -0.209824 0.349898 0.113 Uiso calc 1 H H14B 0.602955 -0.217905 0.245124 0.113 Uiso calc 1 H H14C 0.507139 -0.135542 0.295062 0.113 Uiso calc 1 C C15 0.6500(5) 0.0301(5) 0.2018(3) 0.0904(14) Uani d 1 H H15A 0.563378 0.057609 0.193724 0.136 Uiso calc 1 H H15B 0.665710 -0.031042 0.155155 0.136 Uiso calc 1 H H15C 0.703463 0.106510 0.199271 0.136 Uiso calc 1 C C16 0.7209(3) 0.5006(3) 0.57004(19) 0.0454(6) Uani d 1 C C17 0.8123(3) 0.4814(4) 0.6419(2) 0.0578(8) Uani d 1 H H17 0.789907 0.436802 0.692064 0.069 Uiso calc 1 C C18 0.9353(3) 0.5256(4) 0.6421(3) 0.0701(10) Uani d 1 H H18 0.993902 0.509222 0.691179 0.084 Uiso calc 1 C C19 0.9706(3) 0.5942(4) 0.5690(3) 0.0727(11) Uani d 1 H H19 1.052254 0.626532 0.568899 0.087 Uiso calc 1 C C20 0.8841(4) 0.6134(4) 0.4976(3) 0.0731(11) Uani d 1 H H20 0.907595 0.657729 0.447688 0.088 Uiso calc 1 C C21 0.7608(3) 0.5684(3) 0.4973(2) 0.0565(8) Uani d 1 H H21 0.703633 0.583907 0.447221 0.068 Uiso calc 1 C C22 0.5089(3) 0.4983(3) 0.65798(19) 0.0424(6) Uani d 1 C C23 0.3979(3) 0.4401(4) 0.6792(2) 0.0607(8) Uani d 1 H H23 0.365239 0.367485 0.646062 0.073 Uiso calc 1 C C24 0.3347(4) 0.4877(5) 0.7484(3) 0.0812(12) Uani d 1 H H24 0.260711 0.446715 0.761383 0.097 Uiso calc 1 C C25 0.3807(4) 0.5954(4) 0.7983(3) 0.0779(11) Uani d 1 H H25 0.336914 0.628389 0.843878 0.093 Uiso calc 1 C C26 0.4911(4) 0.6534(4) 0.7804(2) 0.0661(9) Uani d 1 H H26 0.523989 0.724856 0.814634 0.079 Uiso calc 1 C C27 0.5535(3) 0.6052(3) 0.7111(2) 0.0527(7) Uani d 1 H H27 0.628277 0.645808 0.699448 0.063 Uiso calc 1 C C28 0.4063(3) 0.5731(3) 0.46099(18) 0.0428(6) Uani d 1 C C29 0.2961(3) 0.5542(3) 0.4056(2) 0.0481(7) Uani d 1 H H29 0.279566 0.471796 0.378836 0.058 Uiso calc 1 C C30 0.2099(3) 0.6561(3) 0.3896(2) 0.0489(7) Uani d 1 H H30 0.137514 0.642332 0.350431 0.059 Uiso calc 1 C C31 0.2298(3) 0.7792(3) 0.43106(19) 0.0448(6) Uani d 1 C C32 0.3398(3) 0.7962(3) 0.4880(2) 0.0503(7) Uani d 1 H H32 0.354994 0.877312 0.516931 0.060 Uiso calc 1 C C33 0.4271(3) 0.6950(3) 0.5026(2) 0.0484(7) Uani d 1 H H33 0.500447 0.708916 0.540658 0.058 Uiso calc 1 C C34 0.1399(3) 1.0070(3) 0.44859(19) 0.0439(6) Uani d 1 C C35 0.0301(3) 1.0620(3) 0.4756(2) 0.0501(7) Uani d 1 H H35 -0.042477 1.010437 0.473608 0.060 Uiso calc 1 C C36 0.0278(3) 1.1913(3) 0.5050(2) 0.0575(8) Uani d 1 H H36 -0.047157 1.227639 0.520253 0.069 Uiso calc 1 C C37 0.1350(4) 1.2669(4) 0.5119(3) 0.0655(9) Uani d 1 H H37 0.134259 1.353132 0.534314 0.079 Uiso calc 1 C C38 0.2433(3) 1.2142(3) 0.4856(3) 0.0634(9) Uani d 1 H H38 0.316224 1.265472 0.490443 0.076 Uiso calc 1 C C39 0.2468(3) 1.0867(3) 0.4519(2) 0.0554(8) Uani d 1 H H39 0.320265 1.054314 0.431500 0.066 Uiso calc 1 B B1 0.5800(3) 0.4425(3) 0.5760(2) 0.0411(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 O1 0.0529(11) 0.0394(10) 0.0332(9) 0.0026(8) 0.0094(8) -0.0035(7) N1 0.0505(13) 0.0393(12) 0.0386(12) 0.0012(10) 0.0086(10) 0.0020(10) N2 0.0469(14) 0.0479(15) 0.0686(17) 0.0042(11) -0.0090(12) -0.0054(13) C1 0.0573(17) 0.0494(16) 0.0336(13) 0.0020(13) 0.0071(12) 0.0021(12) C2 0.0482(15) 0.0447(15) 0.0399(14) 0.0023(12) 0.0083(12) -0.0011(12) C3 0.0394(14) 0.0421(14) 0.0339(13) -0.0015(11) 0.0070(10) -0.0051(11) C4 0.0350(13) 0.0415(14) 0.0387(13) -0.0018(11) 0.0053(11) -0.0043(11) C5 0.0351(13) 0.0469(15) 0.0433(14) 0.0021(11) 0.0042(11) -0.0075(12) C6 0.0391(14) 0.0541(17) 0.0394(15) 0.0039(12) 0.0032(11) -0.0107(12) C7 0.0534(17) 0.0600(18) 0.0325(13) 0.0053(14) 0.0059(12) -0.0035(12) C8 0.0425(15) 0.0434(14) 0.0386(14) -0.0021(11) 0.0072(11) -0.0028(11) C9 0.0567(19) 0.075(2) 0.0520(19) -0.0026(16) 0.0169(15) 0.0066(16) C10 0.064(2) 0.062(2) 0.0436(16) -0.0053(15) -0.0077(14) 0.0009(14) C11 0.072(2) 0.0521(18) 0.0491(17) 0.0093(15) 0.0068(15) 0.0051(14) C12 0.0507(17) 0.0650(19) 0.0405(15) 0.0053(15) 0.0034(13) -0.0179(14) C13 0.0510(18) 0.101(3) 0.063(2) 0.0097(18) 0.0149(16) -0.029(2) C14 0.063(2) 0.085(3) 0.077(2) -0.0052(19) 0.0000(18) -0.033(2) C15 0.135(4) 0.094(3) 0.0422(19) 0.023(3) 0.008(2) -0.0216(19) C16 0.0543(16) 0.0384(14) 0.0450(15) -0.0005(12) 0.0128(12) -0.0073(11) C17 0.0563(18) 0.066(2) 0.0511(17) -0.0078(15) 0.0068(14) -0.0074(15) C18 0.052(2) 0.076(2) 0.081(3) -0.0019(17) 0.0029(18) -0.018(2) C19 0.051(2) 0.073(2) 0.099(3) -0.0093(17) 0.026(2) -0.014(2) C20 0.069(2) 0.068(2) 0.088(3) -0.0081(18) 0.036(2) 0.004(2) C21 0.0581(18) 0.0550(18) 0.0591(19) 0.0008(15) 0.0193(15) 0.0042(14) C22 0.0498(16) 0.0393(14) 0.0385(14) 0.0029(11) 0.0071(11) 0.0004(11) C23 0.062(2) 0.063(2) 0.060(2) -0.0097(16) 0.0218(16) -0.0112(16) C24 0.076(2) 0.095(3) 0.079(3) -0.012(2) 0.042(2) -0.010(2) C25 0.098(3) 0.076(3) 0.067(2) 0.012(2) 0.043(2) -0.011(2) C26 0.098(3) 0.0520(19) 0.0509(18) 0.0037(18) 0.0201(18) -0.0124(14) C27 0.069(2) 0.0449(16) 0.0463(16) -0.0023(14) 0.0168(14) -0.0045(13) C28 0.0496(15) 0.0401(14) 0.0389(14) 0.0025(12) 0.0058(12) 0.0037(11) C29 0.0576(17) 0.0402(15) 0.0460(15) -0.0043(12) 0.0034(13) -0.0027(12) C30 0.0489(16) 0.0471(16) 0.0484(16) -0.0023(13) -0.0051(13) -0.0014(13) C31 0.0471(15) 0.0420(15) 0.0451(15) 0.0012(12) 0.0042(12) 0.0051(12) C32 0.0536(17) 0.0385(15) 0.0562(17) 0.0010(12) -0.0069(13) -0.0048(13) C33 0.0497(15) 0.0444(15) 0.0491(16) -0.0004(12) -0.0047(13) -0.0016(12) C34 0.0457(16) 0.0457(16) 0.0399(14) 0.0033(12) 0.0020(12) 0.0063(12) C35 0.0432(15) 0.0612(19) 0.0462(16) 0.0017(13) 0.0056(13) 0.0041(14) C36 0.0582(19) 0.064(2) 0.0513(18) 0.0149(16) 0.0110(14) 0.0012(15) C37 0.077(2) 0.0468(18) 0.072(2) 0.0064(17) 0.0078(18) -0.0009(16) C38 0.060(2) 0.0457(17) 0.085(2) -0.0051(14) 0.0099(17) 0.0073(16) C39 0.0489(17) 0.0484(17) 0.071(2) 0.0020(13) 0.0151(15) 0.0063(15) B1 0.0486(17) 0.0391(15) 0.0361(15) 0.0012(13) 0.0067(13) -0.0032(12) 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' B B 0.0013 0.0007 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C3 O1 B1 120.5(2) ? C1 N1 C28 118.6(2) ? C1 N1 B1 116.6(2) ? C28 N1 B1 124.8(2) y C31 N2 C34 127.9(2) ? C31 N2 H2 116.0 ? C34 N2 H2 116.0 ? N1 C1 C2 123.4(3) y N1 C1 H1 118.3 ? C2 C1 H1 118.3 ? C3 C2 C7 121.0(3) ? C3 C2 C1 118.4(2) ? C7 C2 C1 120.0(3) ? O1 C3 C2 119.3(2) ? O1 C3 C4 120.8(2) ? C2 C3 C4 119.7(2) ? C5 C4 C3 116.1(2) ? C5 C4 C8 122.2(2) ? C3 C4 C8 121.6(2) ? C4 C5 C6 125.4(3) ? C4 C5 H5 117.3 ? C6 C5 H5 117.3 ? C7 C6 C5 116.9(2) ? C7 C6 C12 123.1(3) ? C5 C6 C12 120.0(3) ? C6 C7 C2 120.8(3) ? C6 C7 H7 119.6 ? C2 C7 H7 119.6 ? C9 C8 C11 108.6(3) ? C9 C8 C10 109.2(3) ? C11 C8 C10 107.0(3) ? C9 C8 C4 109.2(2) ? C11 C8 C4 111.8(2) ? C10 C8 C4 111.0(2) ? C8 C9 H9A 109.5 ? C8 C9 H9B 109.5 ? H9A C9 H9B 109.5 ? C8 C9 H9C 109.5 ? H9A C9 H9C 109.5 ? H9B C9 H9C 109.5 ? C8 C10 H10A 109.5 ? C8 C10 H10B 109.5 ? H10A C10 H10B 109.5 ? C8 C10 H10C 109.5 ? H10A C10 H10C 109.5 ? H10B C10 H10C 109.5 ? C8 C11 H11A 109.5 ? C8 C11 H11B 109.5 ? H11A C11 H11B 109.5 ? C8 C11 H11C 109.5 ? H11A C11 H11C 109.5 ? H11B C11 H11C 109.5 ? C15 C12 C13 109.3(3) ? C15 C12 C6 111.9(3) ? C13 C12 C6 109.7(2) ? C15 C12 C14 110.2(3) ? C13 C12 C14 107.0(3) ? C6 C12 C14 108.6(3) ? C12 C13 H13A 109.5 ? C12 C13 H13B 109.5 ? H13A C13 H13B 109.5 ? C12 C13 H13C 109.5 ? H13A C13 H13C 109.5 ? H13B C13 H13C 109.5 ? C12 C14 H14A 109.5 ? C12 C14 H14B 109.5 ? H14A C14 H14B 109.5 ? C12 C14 H14C 109.5 ? H14A C14 H14C 109.5 ? H14B C14 H14C 109.5 ? C12 C15 H15A 109.5 ? C12 C15 H15B 109.5 ? H15A C15 H15B 109.5 ? C12 C15 H15C 109.5 ? H15A C15 H15C 109.5 ? H15B C15 H15C 109.5 ? C17 C16 C21 115.5(3) ? C17 C16 B1 119.0(3) ? C21 C16 B1 125.5(3) ? C18 C17 C16 122.9(3) ? C18 C17 H17 118.5 ? C16 C17 H17 118.5 ? C19 C18 C17 119.8(4) ? C19 C18 H18 120.1 ? C17 C18 H18 120.1 ? C20 C19 C18 118.7(3) ? C20 C19 H19 120.7 ? C18 C19 H19 120.7 ? C19 C20 C21 121.5(4) ? C19 C20 H20 119.2 ? C21 C20 H20 119.2 ? C20 C21 C16 121.6(4) ? C20 C21 H21 119.2 ? C16 C21 H21 119.2 ? C23 C22 C27 116.2(3) ? C23 C22 B1 120.7(3) ? C27 C22 B1 123.1(3) ? C24 C23 C22 121.5(3) ? C24 C23 H23 119.3 ? C22 C23 H23 119.3 ? C25 C24 C23 120.5(4) ? C25 C24 H24 119.7 ? C23 C24 H24 119.7 ? C26 C25 C24 119.5(3) ? C26 C25 H25 120.2 ? C24 C25 H25 120.2 ? C25 C26 C27 119.5(3) ? C25 C26 H26 120.2 ? C27 C26 H26 120.2 ? C26 C27 C22 122.7(3) ? C26 C27 H27 118.6 ? C22 C27 H27 118.6 ? C29 C28 C33 118.7(3) ? C29 C28 N1 121.6(2) ? C33 C28 N1 119.7(2) ? C28 C29 C30 120.9(3) ? C28 C29 H29 119.6 ? C30 C29 H29 119.6 ? C29 C30 C31 120.9(3) ? C29 C30 H30 119.5 ? C31 C30 H30 119.5 ? C32 C31 N2 123.6(3) ? C32 C31 C30 117.7(3) ? N2 C31 C30 118.7(3) ? C33 C32 C31 121.3(3) ? C33 C32 H32 119.4 ? C31 C32 H32 119.4 ? C32 C33 C28 120.5(3) ? C32 C33 H33 119.7 ? C28 C33 H33 119.7 ? C39 C34 C35 118.2(3) ? C39 C34 N2 122.7(3) ? C35 C34 N2 119.0(3) ? C36 C35 C34 120.9(3) ? C36 C35 H35 119.6 ? C34 C35 H35 119.6 ? C37 C36 C35 120.4(3) ? C37 C36 H36 119.8 ? C35 C36 H36 119.8 ? C38 C37 C36 119.2(3) ? C38 C37 H37 120.4 ? C36 C37 H37 120.4 ? C37 C38 C39 121.5(3) ? C37 C38 H38 119.2 ? C39 C38 H38 119.2 ? C38 C39 C34 119.6(3) ? C38 C39 H39 120.2 ? C34 C39 H39 120.2 ? O1 B1 C22 106.3(2) ? O1 B1 C16 110.6(2) y C22 B1 C16 115.5(2) y O1 B1 N1 103.9(2) y C22 B1 N1 111.6(2) y C16 B1 N1 108.3(2) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 C3 1.333(3) y O1 B1 1.501(4) y N1 C1 1.300(4) y N1 C28 1.437(4) y N1 B1 1.644(4) y N2 C31 1.389(4) y N2 C34 1.402(4) y N2 H2 0.8600 ? C1 C2 1.430(4) y C1 H1 0.9300 ? C2 C3 1.405(4) y C2 C7 1.406(4) y C3 C4 1.421(4) y C4 C5 1.392(4) y C4 C8 1.535(4) y C5 C6 1.402(4) y C5 H5 0.9300 ? C6 C7 1.377(4) y C6 C12 1.541(4) y C7 H7 0.9300 ? C8 C9 1.524(4) ? C8 C11 1.527(4) ? C8 C10 1.528(4) ? C9 H9A 0.9600 ? C9 H9B 0.9600 ? C9 H9C 0.9600 ? C10 H10A 0.9600 ? C10 H10B 0.9600 ? C10 H10C 0.9600 ? C11 H11A 0.9600 ? C11 H11B 0.9600 ? C11 H11C 0.9600 ? C12 C15 1.503(5) ? C12 C13 1.526(5) ? C12 C14 1.548(5) ? C13 H13A 0.9600 ? C13 H13B 0.9600 ? C13 H13C 0.9600 ? C14 H14A 0.9600 ? C14 H14B 0.9600 ? C14 H14C 0.9600 ? C15 H15A 0.9600 ? C15 H15B 0.9600 ? C15 H15C 0.9600 ? C16 C17 1.389(5) ? C16 C21 1.393(4) ? C16 B1 1.625(4) y C17 C18 1.386(5) ? C17 H17 0.9300 ? C18 C19 1.383(6) ? C18 H18 0.9300 ? C19 C20 1.352(6) ? C19 H19 0.9300 ? C20 C21 1.391(5) ? C20 H20 0.9300 ? C21 H21 0.9300 ? C22 C23 1.388(4) ? C22 C27 1.392(4) ? C22 B1 1.615(4) y C23 C24 1.385(5) ? C23 H23 0.9300 ? C24 C25 1.377(6) ? C24 H24 0.9300 ? C25 C26 1.367(6) ? C25 H25 0.9300 ? C26 C27 1.383(4) ? C26 H26 0.9300 ? C27 H27 0.9300 ? C28 C29 1.380(4) ? C28 C33 1.383(4) ? C29 C30 1.381(4) ? C29 H29 0.9300 ? C30 C31 1.392(4) ? C30 H30 0.9300 ? C31 C32 1.388(4) ? C32 C33 1.382(4) ? C32 H32 0.9300 ? C33 H33 0.9300 ? C34 C39 1.391(4) ? C34 C35 1.394(4) ? C35 C36 1.374(5) ? C35 H35 0.9300 ? C36 C37 1.369(5) ? C36 H36 0.9300 ? C37 C38 1.368(5) ? C37 H37 0.9300 ? C38 C39 1.380(5) ? C38 H38 0.9300 ? C39 H39 0.9300 ? 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 _geom_torsion_publ_flag C28 N1 C1 C2 -167.8(3) ? B1 N1 C1 C2 12.0(4) y N1 C1 C2 C3 12.9(4) y N1 C1 C2 C7 -176.3(3) y B1 O1 C3 C2 -28.1(3) y B1 O1 C3 C4 156.6(2) y C7 C2 C3 O1 -176.7(2) y C1 C2 C3 O1 -6.0(4) y C7 C2 C3 C4 -1.3(4) y C1 C2 C3 C4 169.4(3) y O1 C3 C4 C5 176.9(2) y C2 C3 C4 C5 1.6(4) y O1 C3 C4 C8 -2.1(4) ? C2 C3 C4 C8 -177.3(2) ? C3 C4 C5 C6 -0.5(4) ? C8 C4 C5 C6 178.4(3) ? C4 C5 C6 C7 -0.8(4) ? C4 C5 C6 C12 -178.9(3) ? C5 C6 C7 C2 1.1(4) ? C12 C6 C7 C2 179.1(3) ? C3 C2 C7 C6 0.0(4) ? C1 C2 C7 C6 -170.6(3) ? C5 C4 C8 C9 -111.5(3) ? C3 C4 C8 C9 67.4(3) y C5 C4 C8 C11 8.7(4) y C3 C4 C8 C11 -172.5(2) ? C5 C4 C8 C10 128.0(3) y C3 C4 C8 C10 -53.1(3) ? C7 C6 C12 C15 4.4(5) y C5 C6 C12 C15 -177.6(3) ? C7 C6 C12 C13 125.9(3) y C5 C6 C12 C13 -56.1(4) ? C7 C6 C12 C14 -117.5(3) y C5 C6 C12 C14 60.5(4) ? C21 C16 C17 C18 -0.2(5) ? B1 C16 C17 C18 179.0(3) y C16 C17 C18 C19 1.2(5) y C17 C18 C19 C20 -1.7(6) ? C18 C19 C20 C21 1.4(6) ? C19 C20 C21 C16 -0.5(6) ? C17 C16 C21 C20 -0.1(4) ? B1 C16 C21 C20 -179.3(3) y C27 C22 C23 C24 1.0(5) ? B1 C22 C23 C24 -179.1(3) y C22 C23 C24 C25 0.2(7) ? C23 C24 C25 C26 -1.5(7) ? C24 C25 C26 C27 1.5(6) ? C25 C26 C27 C22 -0.3(5) ? C23 C22 C27 C26 -1.0(5) ? B1 C22 C27 C26 179.1(3) y C1 N1 C28 C29 36.4(4) ? B1 N1 C28 C29 -143.3(3) ? C1 N1 C28 C33 -146.4(3) ? B1 N1 C28 C33 33.9(4) ? C33 C28 C29 C30 2.2(4) ? N1 C28 C29 C30 179.4(3) ? C28 C29 C30 C31 -2.2(5) y C34 N2 C31 C32 5.2(5) y C34 N2 C31 C30 -177.5(3) ? C29 C30 C31 C32 0.9(5) ? C29 C30 C31 N2 -176.6(3) ? N2 C31 C32 C33 177.9(3) ? C30 C31 C32 C33 0.5(5) ? C31 C32 C33 C28 -0.5(5) ? C29 C28 C33 C32 -0.8(4) ? N1 C28 C33 C32 -178.1(3) ? C31 N2 C34 C39 41.0(5) y C31 N2 C34 C35 -141.5(3) ? C39 C34 C35 C36 -0.3(4) ? N2 C34 C35 C36 -178.0(3) y C34 C35 C36 C37 -2.8(5) ? C35 C36 C37 C38 2.8(5) ? C36 C37 C38 C39 0.2(6) ? C37 C38 C39 C34 -3.3(5) ? C35 C34 C39 C38 3.2(5) ? N2 C34 C39 C38 -179.2(3) ? C3 O1 B1 C22 165.3(2) ? C3 O1 B1 C16 -68.7(3) ? C3 O1 B1 N1 47.4(3) y C23 C22 B1 O1 -45.9(4) ? C27 C22 B1 O1 134.1(3) ? C23 C22 B1 C16 -169.0(3) ? C27 C22 B1 C16 10.9(4) ? C23 C22 B1 N1 66.8(3) ? C27 C22 B1 N1 -113.3(3) ? C17 C16 B1 O1 -61.7(3) ? C21 C16 B1 O1 117.4(3) ? C17 C16 B1 C22 59.1(4) ? C21 C16 B1 C22 -121.8(3) ? C17 C16 B1 N1 -175.0(2) ? C21 C16 B1 N1 4.1(4) ? C1 N1 B1 O1 -38.5(3) ? C28 N1 B1 O1 141.2(2) ? C1 N1 B1 C22 -152.7(2) ? C28 N1 B1 C22 27.0(4) ? C1 N1 B1 C16 79.1(3) ? C28 N1 B1 C16 -101.1(3) ? _cod_database_fobs_code 2021746