#------------------------------------------------------------------------------ #$Date: 2021-11-04 03:31:31 +0200 (Thu, 04 Nov 2021) $ #$Revision: 270287 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061038.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7061038 loop_ _publ_author_name 'Duffy, Conor' 'Roe, William E.' 'Harkin, Aislinn M.' 'McNamee, Ryan' 'Knipe, Peter Clarke' _publ_section_title ; Enantioselective organocatalytic formal [3+2]-cycloaddition of isatin-derived ketimines with benzylidenemalononitriles and benzylidineindanones ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D1NJ04002B _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_moiety 'C31 H21 F3 N4 O' _chemical_formula_sum 'C31 H21 F3 N4 O' _chemical_formula_weight 522.52 _chemical_melting_point ? _chemical_name_common (3R,4'S,5'S)-1-benzyl-4'-(naphthalen-2-yl)-2-oxo-5'-(trifluoromethyl)spiro[indoline-3,2'-pyrrolidine]-3',3'-dicarbonitrile _chemical_name_systematic 3d _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary other _audit_creation_date 2021-08-17 _audit_creation_method CRYSTALS_ver_14.61_build_6999 _audit_update_record ; 2021-08-17 deposited with the CCDC. 2021-10-25 downloaded from the CCDC. ; _cell_angle_alpha 90.0 _cell_angle_beta 91.462(5) _cell_angle_gamma 90.0 _cell_formula_units_Z 2 _cell_length_a 11.6334(6) _cell_length_b 6.6182(4) _cell_length_c 16.7064(9) _cell_measurement_reflns_used 19017 _cell_measurement_temperature 150 _cell_measurement_theta_max 71 _cell_measurement_theta_min 4 _cell_volume 1285.84(12) _computing_cell_refinement ; CrysAlisPro (Rigaku Oxford Diffraction, 2017) ; _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_data_reduction ; CrysAlisPro (Rigaku Oxford Diffraction, 2017) ; _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_pressure 100 _diffrn_ambient_temperature 150 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.960 _diffrn_measurement_device Area _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_method \w _diffrn_radiation_monochromator 'focussing mirrors' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_reflns_av_R_equivalents 0.108 _diffrn_reflns_av_unetI/netI 0.052 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 39351 _diffrn_reflns_theta_full 69.307 _diffrn_reflns_theta_max 74.523 _diffrn_reflns_theta_min 3.801 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_T_max 0.88 _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro (Rigaku Oxford Diffraction, 2017) ; _exptl_crystal_colour clear_pale_colourless _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 540 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: ethanol, hexane' _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.160 _refine_diff_density_max 1.52 _refine_diff_density_min -0.66 _refine_ls_abs_structure_details ; Parsons, Flack & Wagner (2013), 1925 Friedel Pairs ; _refine_ls_abs_structure_Flack 0.11(7) _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.6196 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 408 _refine_ls_number_reflns 4910 _refine_ls_number_restraints 127 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.1081 _refine_ls_shift/su_max 0.0116005 _refine_ls_shift/su_mean 0.0007826 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.20P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.3538 _refine_ls_wR_factor_gt 0.3428 _refine_ls_wR_factor_ref 0.3538 _reflns_limit_h_max 14 _reflns_limit_h_min -14 _reflns_limit_k_max 7 _reflns_limit_k_min -8 _reflns_limit_l_max 20 _reflns_limit_l_min 0 _reflns_number_gt 4258 _reflns_number_total 4910 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 4.40 _oxford_diffrn_Wilson_scale 0.01 _oxford_refine_ls_r_factor_ref 0.1160 _oxford_refine_ls_scale 9.4(12) _oxford_reflns_number_all 4910 _oxford_structure_analysis_title 'P:\X-Ray\WR-2.190-02\WR-2.190-02.cif_od At 1' _iucr_refine_instructions_details ; # # Punched on 17/08/21 at 13:24:17 # #LIST 12 BLOCK SCALE X'S, U'S CONT ENANTIO EQUIVALENCE PART(1001, OCC) CONTINUE PART(1002, OCC) WEIGHT -1 PART(1002, OCC) END # # Punched on 17/08/21 at 13:24:17 # #LIST 16 NO PLANAR 0.010000 C(170) C(250) C(101) C(110) C(120) C(130) SIMU 0.010000 C(170) C(250) C(101) C(110) C(120) C(130) DELU 0.010000 C(170) C(250) C(101) C(110) C(120) C(130) PLANAR 0.01 C(171) C(111) C(121) C(131) C(100) C(251) SIMU 0.01 C(171) C(111) C(121) C(131) C(100) C(251) DELU 0.01 C(171) C(111) C(121) C(131) C(100) C(251) SAME C(26) C(171) C(111) C(121) C(131) C(100) C(251) AND CONT C(26) C(170) C(110) C(120) C(130) C(101) C(250) END ; _cod_data_source_file d1nj04002b2.cif _cod_data_source_block 'global_CCDC1' _cod_depositor_comments ; The following automatic conversions were performed: data item '_chemical_melting_point' value 'not measured' was changed to '?' -- the value is undefined or not given. data item '_exptl_crystal_density_meas' value 'not measured' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 7061038 _oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I) _iucr_refine_reflections_details ; # Data was input as F-squared # punching LIST 6 as LIST 6 with all keys set # NBGNXT= 36 #LIST 6 READ NCOEF= 8 TYPE=FIX, F'S = FSQ UNIT=DATA, CHECK=NO L30=NO ARCH=NO STORE NCOEF= 6 OUTPUT INDICES /FO/ SIGMA(/FO/) RATIO/JCODE CORRECTIONS SERIAL CONT INPUT H K L /FO/ SIGMA(/FO/) JCODE CONT CORRECTIONS SERIAL FOR (I4,I4,I4,F10.2,F8.2,F4.0,F7.4,F7.0) END 0 0 -2 243529.98 2814.10 0. 1.0000 0. 0 0 -2 241552.00 1394.06 0. 1.0000 0. 0 0 2 257339.00 1912.35 0. 1.0000 0. 0 0 -2 246023.00 1940.17 0. 1.0000 0. 0 0 2 235002.00 1611.34 0. 1.0000 0. 0 0 2 324561.03 2308.76 0. 1.0000 0. 0 0 2 317968.03 2277.42 0. 1.0000 0. 0 0 -3 20334.70 506.03 0. 1.0000 0. 0 0 3 21843.60 695.66 0. 1.0000 0. 0 0 -3 21025.90 1056.77 0. 1.0000 0. 0 0 -3 21392.70 706.74 0. 1.0000 0. 0 0 3 20131.60 593.51 0. 1.0000 0. 0 0 -3 15658.30 642.14 0. 1.0000 0. 0 0 -3 16803.80 676.24 0. 1.0000 0. 0 0 -3 16607.90 653.92 0. 1.0000 0. 0 0 3 16114.50 652.25 0. 1.0000 0. 0 0 3 16650.50 658.46 0. 1.0000 0. 0 0 -3 16529.10 654.47 0. 1.0000 0. 0 0 4 502137.03 3877.08 0. 1.0000 0. 0 0 -4 482090.03 2840.59 0. 1.0000 0. 0 0 4 470978.03 3297.70 0. 1.0000 0. 0 0 -4 499276.03 3771.64 0. 1.0000 0. 0 0 4 454421.97 4480.36 0. 1.0000 0. 0 0 -4 507281.03 5904.74 0. 1.0000 0. 0 0 -4 486791.00 4034.75 0. 1.0000 0. 0 0 -4 553150.00 4337.24 0. 1.0000 0. 0 0 -4 561775.06 4323.16 0. 1.0000 0. 0 0 4 556404.00 4279.94 0. 1.0000 0. 0 0 -4 561830.06 4327.60 0. 1.0000 0. 0 0 4 556016.00 4310.94 0. 1.0000 0. 0 0 -4 552760.00 4425.20 0. 1.0000 0. 0 0 -5 359440.00 3909.65 0. 1.0000 0. 0 0 5 361024.00 3243.95 0. 1.0000 0. 0 0 -5 390721.97 5851.62 0. 1.0000 0. 0 0 5 365127.00 3741.87 0. 1.0000 0. 0 0 -5 353279.97 2745.58 0. 1.0000 0. 0 0 5 335371.00 4379.68 0. 1.0000 0. 0 0 -5 438332.00 4366.47 0. 1.0000 0. 0 0 -5 428067.03 4479.82 0. 1.0000 0. 0 0 -5 433782.00 4350.49 0. 1.0000 0. 0 0 5 428316.00 4256.06 0. 1.0000 0. 0 0 -5 435054.97 4345.65 0. 1.0000 0. 0 0 5 421459.00 4329.87 0. 1.0000 0. 0 0 -5 437528.00 4431.45 0. 1.0000 0. 0 0 6 3752.84 445.76 0. 1.0000 0. 0 0 -6 3624.76 754.22 0. 1.0000 0. 0 0 -6 3875.24 496.48 0. 1.0000 0. 0 0 6 2933.32 441.83 0. 1.0000 0. 0 0 6 3498.10 403.73 0. 1.0000 0. 0 0 -6 3556.67 488.44 0. 1.0000 0. 0 0 6 3200.35 371.66 0. 1.0000 0. 0 0 6 3306.57 531.95 0. 1.0000 0. 0 0 6 3317.28 370.30 0. 1.0000 0. 0 0 -6 3274.81 309.94 0. 1.0000 0. 0 0 6 3634.54 485.60 0. 1.0000 0. 0 0 -6 3003.79 449.93 0. 1.0000 0. 0 0 -6 3122.58 469.79 0. 1.0000 0. 0 0 -6 3250.61 457.46 0. 1.0000 0. 0 0 6 3079.14 441.22 0. 1.0000 0. 0 0 6 3243.38 448.28 0. 1.0000 0. 0 0 -6 2933.60 442.08 0. 1.0000 0. 0 0 -6 2880.65 462.28 0. 1.0000 0. 0 0 7 12117.60 789.93 0. 1.0000 0. 0 0 -7 13937.80 1454.53 0. 1.0000 0. 0 0 7 11833.90 1034.43 0. 1.0000 0. 0 0 -7 12198.50 961.63 0. 1.0000 0. 0 0 -7 13258.40 962.31 0. 1.0000 0. 0 0 7 12055.20 925.05 0. 1.0000 0. 0 0 -7 13202.70 944.84 0. 1.0000 0. 0 0 7 12479.80 951.71 0. 1.0000 0. 0 0 7 12210.00 735.60 0. 1.0000 0. 0 0 7 11867.80 836.85 0. 1.0000 0. 0 0 7 12284.50 726.85 0. 1.0000 0. 0 0 -7 11924.30 622.77 0. 1.0000 0. 0 0 -7 17536.60 1105.64 0. 1.0000 0. 0 0 -7 17030.30 1074.71 0. 1.0000 0. 0 0 -7 17254.00 1080.86 0. 1.0000 0. 0 0 7 17653.60 1067.72 0. 1.0000 0. 0 0 -7 16892.10 1111.27 0. 1.0000 0. 0 0 -7 18073.60 1095.97 0. 1.0000 0. 0 0 7 17295.10 1058.58 0. 1.0000 0. 0 0 8 13703.10 834.88 0. 1.0000 0. 0 0 8 13452.20 979.06 0. 1.0000 0. 0 0 -8 15439.00 1655.38 0. 1.0000 0. 0 0 -8 13401.20 708.86 0. 1.0000 0. 0 0 8 13617.00 908.11 0. 1.0000 0. 0 0 8 13675.60 1082.89 0. 1.0000 0. 0 0 -8 13843.50 1095.45 0. 1.0000 0. 0 0 8 13700.00 1183.49 0. 1.0000 0. 0 0 -8 14838.20 1140.72 0. 1.0000 0. 0 0 8 13910.70 1076.31 0. 1.0000 0. 0 0 -8 15228.40 1095.70 0. 1.0000 0. 0 0 -8 15182.70 1096.34 0. 1.0000 0. 0 0 8 14194.60 1045.33 0. 1.0000 0. 0 0 -8 15354.30 1119.39 0. 1.0000 0. 0 0 8 14810.30 1065.66 0. 1.0000 0. 0 0 -8 15559.10 1155.95 0. 1.0000 0. 0 0 -8 15413.40 1107.46 0. 1.0000 0. 0 0 9 129086.00 3796.90 0. 1.0000 0. 0 0 9 134613.02 2790.71 0. 1.0000 0. 0 0 -9 136109.00 3658.05 0. 1.0000 0. 0 0 -9 142182.00 5153.96 0. 1.0000 0. 0 0 9 135100.00 2978.07 0. 1.0000 0. 0 0 9 134446.00 3534.87 0. 1.0000 0. 0 0 9 128759.00 3511.83 0. 1.0000 0. 0 0 9 126815.99 3160.14 0. 1.0000 0. 0 0 -9 114543.99 3174.12 0. 1.0000 0. 0 0 -9 111491.00 3158.79 0. 1.0000 0. 0 0 9 105281.00 3023.12 0. 1.0000 0. 0 0 -9 113952.01 3252.69 0. 1.0000 0. 0 0 -9 117347.00 3236.90 0. 1.0000 0. 0 0 -9 111997.99 3131.02 0. 1.0000 0. 0 0 9 106186.00 3017.33 0. 1.0000 0. 0 0 10 822.21 439.78 0. 1.0000 0. 0 0 -10 650.93 384.83 0. 1.0000 0. 0 0 -10 673.83 678.29 0. 1.0000 0. 0 0 10 603.40 383.57 0. 1.0000 0. 0 0 10 659.04 272.93 0. 1.0000 0. 0 0 10 759.72 308.50 0. 1.0000 0. 0 0 10 518.34 375.87 0. 1.0000 0. 0 0 10 361.30 279.23 0. 1.0000 0. 0 0 -10 691.39 351.93 0. 1.0000 0. 0 0 10 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473.02 0. 1.0000 0. -12 -2 8 891.11 247.89 0. 1.0000 0. -12 -2 8 1344.18 287.60 0. 1.0000 0. 12 2 -8 969.19 285.33 0. 1.0000 0. 12 -2 -8 1492.61 270.66 0. 1.0000 0. -12 -2 8 1201.92 271.52 0. 1.0000 0. 12 2 -7 727.64 374.64 0. 1.0000 0. -12 -2 7 886.67 172.81 0. 1.0000 0. 12 2 -7 396.62 309.37 0. 1.0000 0. 12 -2 -7 334.39 335.13 0. 1.0000 0. -12 -2 7 854.09 155.76 0. 1.0000 0. -12 -2 7 1548.97 309.98 0. 1.0000 0. 12 2 -7 1297.37 447.54 0. 1.0000 0. 12 -2 -7 783.95 243.69 0. 1.0000 0. -12 -2 7 2255.07 366.36 0. 1.0000 0. 12 2 -7 884.52 300.78 0. 1.0000 0. -12 -2 7 1724.87 335.14 0. 1.0000 0. 12 2 -6 1444.17 469.88 0. 1.0000 0. -12 -2 6 1577.19 224.46 0. 1.0000 0. 12 2 -6 1170.09 415.58 0. 1.0000 0. 12 -2 -6 664.71 373.15 0. 1.0000 0. -12 -2 6 1744.39 208.78 0. 1.0000 0. -12 -2 6 1555.55 199.46 0. 1.0000 0. 12 2 -6 964.06 450.54 0. 1.0000 0. -12 -2 6 956.38 267.13 0. 1.0000 0. 12 -2 -6 1228.44 285.38 0. 1.0000 0. -12 -2 6 1214.31 311.79 0. 1.0000 0. 12 2 -6 1676.66 404.26 0. 1.0000 0. 12 2 -6 1175.37 350.44 0. 1.0000 0. -12 -2 6 1190.09 324.54 0. 1.0000 0. -12 -2 5 474.13 137.81 0. 1.0000 0. 12 2 -5 644.65 410.47 0. 1.0000 0. -12 -2 5 469.24 165.95 0. 1.0000 0. 12 2 -5 168.71 306.99 0. 1.0000 0. 12 -2 -5 529.67 357.33 0. 1.0000 0. -12 -2 5 427.83 140.23 0. 1.0000 0. 12 2 -5 553.74 417.51 0. 1.0000 0. -12 -2 5 260.64 223.75 0. 1.0000 0. 12 -2 -5 445.77 221.51 0. 1.0000 0. 12 -2 -5 212.65 298.19 0. 1.0000 0. -12 -2 5 356.10 246.26 0. 1.0000 0. 12 2 -5 898.60 350.14 0. 1.0000 0. 12 2 -5 385.88 285.57 0. 1.0000 0. -12 -2 5 525.73 283.97 0. 1.0000 0. -12 -2 4 88.13 107.54 0. 1.0000 0. 12 2 -4 344.18 397.04 0. 1.0000 0. -12 -2 4 166.75 149.66 0. 1.0000 0. 12 2 -4 -94.40 350.70 0. 1.0000 0. 12 -2 -4 182.68 311.72 0. 1.0000 0. -12 -2 4 81.94 123.49 0. 1.0000 0. 12 2 -4 1111.14 492.12 0. 1.0000 0. -12 -2 4 79.44 203.02 0. 1.0000 0. 12 -2 -4 -108.97 207.74 0. 1.0000 0. 12 -2 -4 337.27 326.95 0. 1.0000 0. -12 -2 4 153.73 214.27 0. 1.0000 0. 12 2 -4 523.10 368.42 0. 1.0000 0. 12 2 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1035.44 433.00 0. 1.0000 0. -12 -2 1 1688.92 241.31 0. 1.0000 0. 12 2 -1 885.37 385.32 0. 1.0000 0. -12 -2 1 1743.18 250.01 0. 1.0000 0. -12 2 1 1363.45 218.92 0. 1.0000 0. 12 2 -1 1407.18 553.69 0. 1.0000 0. -12 -2 1 915.63 287.23 0. 1.0000 0. 12 2 -1 1417.61 527.60 0. 1.0000 0. 12 -2 -1 1523.50 494.59 0. 1.0000 0. -12 -2 1 774.87 274.09 0. 1.0000 0. 12 -2 -1 226.71 366.02 0. 1.0000 0. 12 2 -1 1845.50 515.11 0. 1.0000 0. 12 -2 -1 1920.17 358.54 0. 1.0000 0. -12 -2 1 899.93 318.14 0. 1.0000 0. 12 2 0 981.73 395.54 0. 1.0000 0. -12 -2 0 985.30 196.91 0. 1.0000 0. 12 2 0 981.30 378.59 0. 1.0000 0. -12 -2 0 996.76 247.86 0. 1.0000 0. -12 -2 0 1105.54 222.97 0. 1.0000 0. -12 2 0 829.07 178.55 0. 1.0000 0. 12 2 0 1196.94 533.66 0. 1.0000 0. -12 -2 0 1048.30 298.09 0. 1.0000 0. 12 2 0 1885.45 563.39 0. 1.0000 0. 12 -2 0 820.58 428.05 0. 1.0000 0. -12 -2 0 942.54 312.26 0. 1.0000 0. 12 -2 0 -36.07 371.91 0. 1.0000 0. 12 2 0 1469.72 486.03 0. 1.0000 0. -12 -2 0 1261.44 346.41 0. 1.0000 0. 12 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315.29 0. 1.0000 0. -12 -2 -4 361.34 202.89 0. 1.0000 0. 12 2 4 591.76 359.41 0. 1.0000 0. 12 -2 4 -59.02 345.98 0. 1.0000 0. 12 2 4 386.60 417.60 0. 1.0000 0. -12 -2 -4 224.19 241.88 0. 1.0000 0. 12 -2 4 214.70 204.20 0. 1.0000 0. 12 -2 5 375.02 246.60 0. 1.0000 0. 12 2 5 210.76 299.90 0. 1.0000 0. -12 -2 -5 149.36 113.24 0. 1.0000 0. -12 -2 -5 78.23 148.52 0. 1.0000 0. -12 2 -5 291.44 165.10 0. 1.0000 0. -12 -2 -5 116.27 129.92 0. 1.0000 0. 12 2 5 119.51 315.92 0. 1.0000 0. -12 2 -5 348.05 286.04 0. 1.0000 0. -12 -2 -5 285.59 209.36 0. 1.0000 0. 12 2 5 3.19 570.30 0. 1.0000 0. 12 2 5 -47.64 384.02 0. 1.0000 0. 12 2 5 341.41 407.19 0. 1.0000 0. 12 -2 5 194.39 261.77 0. 1.0000 0. -12 -2 -5 184.41 183.11 0. 1.0000 0. 12 2 5 148.91 287.22 0. 1.0000 0. 12 2 5 345.96 374.69 0. 1.0000 0. -12 -2 -5 194.50 245.86 0. 1.0000 0. 12 -2 6 82.36 208.43 0. 1.0000 0. 12 2 6 283.91 289.68 0. 1.0000 0. -12 -2 -6 93.23 107.37 0. 1.0000 0. -12 -2 -6 194.73 146.19 0. 1.0000 0. -12 2 -6 109.90 146.18 0. 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1.0000 0. 13 2 -4 138.46 303.49 0. 1.0000 0. -13 -2 4 485.77 197.74 0. 1.0000 0. 13 -2 -4 493.97 269.36 0. 1.0000 0. -13 -2 4 332.92 185.76 0. 1.0000 0. 13 2 -4 745.22 293.18 0. 1.0000 0. 13 2 -4 159.62 325.36 0. 1.0000 0. -13 -2 4 377.21 208.77 0. 1.0000 0. 13 -2 -4 780.12 222.96 0. 1.0000 0. 13 2 -3 398.60 282.61 0. 1.0000 0. -13 -2 3 573.17 142.38 0. 1.0000 0. 13 2 -3 136.56 241.15 0. 1.0000 0. -13 -2 3 363.79 150.47 0. 1.0000 0. -13 -2 3 509.95 135.35 0. 1.0000 0. -13 2 3 280.10 119.03 0. 1.0000 0. 13 2 -3 2524.05 489.42 0. 1.0000 0. -13 -2 3 303.99 190.82 0. 1.0000 0. 13 -2 -3 2375.56 426.30 0. 1.0000 0. -13 -2 3 397.17 202.97 0. 1.0000 0. 13 2 -3 419.33 284.34 0. 1.0000 0. 13 2 -3 735.38 386.23 0. 1.0000 0. -13 -2 3 266.61 200.47 0. 1.0000 0. 13 -2 -3 487.62 214.44 0. 1.0000 0. 13 2 -2 1928.19 413.74 0. 1.0000 0. -13 -2 2 2712.88 243.64 0. 1.0000 0. -13 -2 2 2561.23 271.16 0. 1.0000 0. -13 -2 2 2746.45 238.21 0. 1.0000 0. -13 2 2 2234.37 212.29 0. 1.0000 0. 13 2 -2 141.45 340.76 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162.32 0. 1.0000 0. 13 -3 -3 5.26 187.41 0. 1.0000 0. -13 -3 3 348.71 173.36 0. 1.0000 0. 13 3 -3 482.75 245.61 0. 1.0000 0. 13 3 -3 98.85 269.10 0. 1.0000 0. -13 -3 3 297.77 157.96 0. 1.0000 0. 13 -3 -3 632.73 200.50 0. 1.0000 0. -13 -3 2 198.19 95.21 0. 1.0000 0. -13 -3 2 176.14 110.57 0. 1.0000 0. 13 3 -2 377.42 309.79 0. 1.0000 0. -13 -3 2 138.33 149.57 0. 1.0000 0. 13 3 -2 -79.09 282.45 0. 1.0000 0. 13 -3 -2 353.34 239.35 0. 1.0000 0. -13 -3 2 147.98 157.15 0. 1.0000 0. 13 3 -2 506.95 264.62 0. 1.0000 0. 13 3 -2 150.33 315.36 0. 1.0000 0. -13 -3 2 61.26 151.35 0. 1.0000 0. 13 -3 -2 327.10 185.14 0. 1.0000 0. -13 -3 1 701.95 130.73 0. 1.0000 0. -13 -3 1 496.85 135.25 0. 1.0000 0. 13 3 -1 -16.28 290.70 0. 1.0000 0. -13 -3 1 660.29 201.46 0. 1.0000 0. 13 3 -1 -97.53 292.46 0. 1.0000 0. 13 -3 -1 -4.74 201.12 0. 1.0000 0. -13 -3 1 723.33 213.01 0. 1.0000 0. 13 3 -1 454.26 263.53 0. 1.0000 0. 13 3 -1 7.43 293.64 0. 1.0000 0. -13 -3 1 923.36 216.54 0. 1.0000 0. 13 -3 -1 543.46 194.13 0. 1.0000 0. -13 -3 0 454.21 115.02 0. 1.0000 0. -13 -3 0 239.09 117.95 0. 1.0000 0. 13 3 0 639.97 330.05 0. 1.0000 0. -13 -3 0 -33.20 148.90 0. 1.0000 0. 13 3 0 -291.87 299.00 0. 1.0000 0. 13 -3 0 928.36 291.08 0. 1.0000 0. -13 -3 0 -96.36 151.45 0. 1.0000 0. 13 3 0 505.82 263.15 0. 1.0000 0. 13 3 0 353.37 326.98 0. 1.0000 0. -13 -3 0 -27.92 153.71 0. 1.0000 0. 13 -3 0 365.87 179.38 0. 1.0000 0. -13 -3 -1 1487.14 162.24 0. 1.0000 0. -13 -3 -1 1300.80 174.15 0. 1.0000 0. 13 3 1 299.96 284.49 0. 1.0000 0. -13 -3 -1 1030.06 221.03 0. 1.0000 0. -13 3 -1 441.66 220.90 0. 1.0000 0. 13 3 1 398.29 306.12 0. 1.0000 0. 13 -3 1 74.20 213.12 0. 1.0000 0. -13 -3 -1 1028.97 217.77 0. 1.0000 0. 13 3 1 1423.22 313.63 0. 1.0000 0. 13 3 1 363.74 314.54 0. 1.0000 0. -13 -3 -1 1000.05 219.72 0. 1.0000 0. 13 -3 1 832.57 199.58 0. 1.0000 0. -13 -3 -2 666.13 121.59 0. 1.0000 0. 13 3 2 165.35 246.30 0. 1.0000 0. -13 -3 -2 117.08 146.16 0. 1.0000 0. 13 3 2 294.17 289.31 0. 1.0000 0. -13 3 -2 454.38 208.97 0. 1.0000 0. 13 -3 2 263.08 204.26 0. 1.0000 0. -13 -3 -2 110.03 137.97 0. 1.0000 0. 13 3 2 782.43 260.35 0. 1.0000 0. 13 3 2 268.10 295.34 0. 1.0000 0. -13 -3 -2 194.11 152.02 0. 1.0000 0. -13 -3 -3 227.83 149.10 0. 1.0000 0. 13 3 3 604.10 306.93 0. 1.0000 0. -13 -3 -3 263.10 152.75 0. 1.0000 0. -14 0 5 1500.28 226.10 0. 1.0000 0. -14 0 4 35.99 80.99 0. 1.0000 0. -14 0 4 101.55 143.29 0. 1.0000 0. -14 0 3 129.70 100.29 0. 1.0000 0. 14 0 -3 184.67 229.45 0. 1.0000 0. -14 0 3 446.96 179.06 0. 1.0000 0. -14 0 2 416.27 123.09 0. 1.0000 0. -14 0 2 47.13 154.59 0. 1.0000 0. -14 0 1 3322.58 243.28 0. 1.0000 0. -14 0 1 2405.54 299.44 0. 1.0000 0. -14 0 0 139.31 106.30 0. 1.0000 0. -14 0 0 175.85 117.14 0. 1.0000 0. 14 0 0 -11.66 181.72 0. 1.0000 0. 14 0 0 861.05 323.91 0. 1.0000 0. -14 0 0 875.00 219.74 0. 1.0000 0. -14 0 -1 3595.86 257.15 0. 1.0000 0. -14 0 -1 4031.22 261.92 0. 1.0000 0. 14 0 1 3264.80 399.21 0. 1.0000 0. 14 0 1 2087.09 401.17 0. 1.0000 0. -14 0 -1 1541.39 249.82 0. 1.0000 0. -14 0 -2 5364.03 290.79 0. 1.0000 0. -14 0 -2 4407.86 352.67 0. 1.0000 0. -14 0 -3 2209.86 211.29 0. 1.0000 0. -14 0 -3 2186.95 188.55 0. 1.0000 0. -14 -1 5 920.54 194.24 0. 1.0000 0. -14 -1 4 1334.71 230.82 0. 1.0000 0. -14 -1 3 100.89 161.63 0. 1.0000 0. -14 -1 2 617.95 135.85 0. 1.0000 0. -14 -1 2 756.64 134.30 0. 1.0000 0. -14 1 2 561.53 116.56 0. 1.0000 0. 14 1 -2 434.96 251.50 0. 1.0000 0. 14 -1 -2 1485.05 314.67 0. 1.0000 0. -14 -1 2 1265.53 238.84 0. 1.0000 0. -14 -1 1 3621.35 264.21 0. 1.0000 0. -14 -1 1 4115.13 256.20 0. 1.0000 0. -14 1 1 3677.47 237.99 0. 1.0000 0. 14 1 -1 697.16 303.47 0. 1.0000 0. 14 -1 -1 2089.92 358.68 0. 1.0000 0. 14 1 -1 3706.40 406.44 0. 1.0000 0. 14 1 -1 1454.24 354.89 0. 1.0000 0. -14 -1 1 925.62 218.87 0. 1.0000 0. -14 -1 0 1578.93 190.55 0. 1.0000 0. -14 -1 0 1987.40 189.60 0. 1.0000 0. -14 1 0 1703.60 174.19 0. 1.0000 0. 14 -1 0 1824.42 353.74 0. 1.0000 0. 14 1 0 1327.39 294.70 0. 1.0000 0. 14 1 0 1297.66 361.81 0. 1.0000 0. -14 -1 0 1822.17 276.97 0. 1.0000 0. -14 -1 -1 1016.91 161.98 0. 1.0000 0. -14 1 -1 881.50 158.14 0. 1.0000 0. -14 -1 -1 1072.24 148.94 0. 1.0000 0. -14 1 -1 767.60 229.83 0. 1.0000 0. 14 1 1 823.03 255.19 0. 1.0000 0. 14 1 1 1748.48 377.95 0. 1.0000 0. -14 -1 -1 1450.25 251.48 0. 1.0000 0. -14 -1 -2 2350.65 213.65 0. 1.0000 0. -14 -1 -2 2747.75 208.62 0. 1.0000 0. 14 -1 2 439.24 224.31 0. 1.0000 0. 14 1 2 1831.77 319.80 0. 1.0000 0. 14 1 2 296.80 273.27 0. 1.0000 0. -14 -1 -2 2084.52 274.04 0. 1.0000 0. -14 -1 -3 364.65 163.09 0. 1.0000 0. -512 # 39384 reflections output ; loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens F1 F 0.3600(4) 0.1825(10) 0.0336(2) 0.1009 1.0000 Uani . . . . . . F2 F 0.5255(4) 0.3024(14) 0.0544(2) 0.1203 1.0000 Uani . . . . . . N3 N 0.5193(4) 0.2451(9) 0.2214(2) 0.0551 1.0000 Uani . . . . . . O4 O 0.5899(4) 0.6647(10) 0.1747(3) 0.0859 1.0000 Uani . . . . . . C1 C 0.2315(4) 0.4572(9) 0.1489(3) 0.0453 1.0000 Uani . . . . . . N6 N 0.2573(4) 0.3108(9) 0.3638(3) 0.0579 1.0000 Uani . . . . . . C2 C 0.5158(4) 0.4208(9) 0.2727(3) 0.0471 1.0000 Uani . . . . . . C31 C 0.3142(4) 0.3857(8) 0.3201(3) 0.0403 1.0000 Uani . . . . . . C30 C 0.3723(6) 0.7113(8) 0.2791(3) 0.0542 1.0000 Uani . . . . . . C29 C 0.3862(4) 0.4931(7) 0.2635(3) 0.0391 1.0000 Uani . . . . . . C32 C 0.4488(6) 0.1805(14) 0.0847(3) 0.0742 1.0000 Uani . . . . . . C3 C 0.4150(4) 0.2325(9) 0.1676(3) 0.0492 1.0000 Uani . . . . . . C4 C 0.3582(4) 0.4391(8) 0.1728(3) 0.0421 1.0000 Uani . . . . . . C5 C 0.1519(4) 0.3171(9) 0.1646(3) 0.0473 1.0000 Uani . . . . . . N1 N 0.6541(5) 0.6742(10) 0.3075(4) 0.0733 1.0000 Uani . . . . . . C7 C 0.5623(4) 0.3847(10) 0.3569(3) 0.0519 1.0000 Uani . . . . . . C8 C 0.0055(5) 0.5254(13) 0.1009(3) 0.0642 1.0000 Uani . . . . . . C9 C 0.0341(5) 0.3442(11) 0.1402(3) 0.0584 1.0000 Uani . . . . . . N10 N 0.3611(7) 0.8790(10) 0.2914(3) 0.0830 1.0000 Uani . . . . . . F29 F 0.4995(8) -0.0033(12) 0.0850(3) 0.1616 1.0000 Uani . . . . . . C28 C 0.5345(5) 0.2401(10) 0.4115(3) 0.0544 1.0000 Uani . . . . . . C27 C 0.2002(5) 0.6370(10) 0.1088(3) 0.0589 1.0000 Uani . . . . . . C14 C 0.6380(5) 0.5468(11) 0.3758(4) 0.0638 1.0000 Uani . . . . . . C15 C 0.0886(6) 0.6674(12) 0.0837(4) 0.0708 1.0000 Uani . . . . . . C16 C 0.5891(5) 0.6091(15) 0.2447(5) 0.0764 1.0000 Uani . . . . . . C18 C -0.0492(6) 0.1965(17) 0.1556(4) 0.0830 1.0000 Uani . . . . . . C19 C -0.1933(6) 0.423(2) 0.0946(4) 0.1098 1.0000 Uani . . . . . . C20 C -0.1146(6) 0.559(2) 0.0779(4) 0.0963 1.0000 Uani . . . . . . C21 C 0.5934(6) 0.2510(16) 0.4863(3) 0.0792 1.0000 Uani . . . . . . C22 C 0.6914(6) 0.5615(16) 0.4508(5) 0.0799 1.0000 Uani . . . . . . C23 C -0.1637(6) 0.239(2) 0.1317(5) 0.1062 1.0000 Uani . . . . . . C24 C 0.6683(6) 0.4156(17) 0.5033(4) 0.0851 1.0000 Uani . . . . . . C26 C 0.7200(5) 0.8576(12) 0.3075(6) 0.0962 1.0000 Uani D . . . . . C170 C 0.8494(5) 0.7970(11) 0.3331(4) 0.0941 0.561(17) Uani D . P 1 2 . C171 C 0.8477(8) 0.8511(11) 0.3275(4) 0.1388 0.439(17) Uani D . P 1 1 . C250 C 0.8992(6) 0.6394(12) 0.3069(5) 0.0898 0.561(17) Uani D . P 1 2 . C251 C 0.9125(9) 0.7126(15) 0.3033(6) 0.1419 0.439(17) Uani D . P 1 1 . C100 C 1.0270(9) 0.738(2) 0.3133(6) 0.1402 0.439(17) Uani D . P 1 1 . C101 C 1.0124(6) 0.6080(13) 0.3299(5) 0.0961 0.561(17) Uani D . P 1 2 . C110 C 0.9056(7) 0.9477(12) 0.3872(5) 0.1122 0.561(17) Uani D . P 1 2 . C111 C 0.8892(12) 1.0356(15) 0.3679(5) 0.1433 0.439(17) Uani D . P 1 1 . C120 C 1.0206(7) 0.9037(15) 0.4077(5) 0.1117 0.561(17) Uani D . P 1 2 . C121 C 1.0071(13) 1.048(2) 0.3766(6) 0.1388 0.439(17) Uani D . P 1 1 . C130 C 1.0728(6) 0.7344(16) 0.3789(5) 0.1093 0.561(17) Uani D . P 1 2 . C131 C 1.0752(10) 0.899(3) 0.3496(7) 0.1391 0.439(17) Uani D . P 1 1 . H99 H 0.3648 0.1336 0.1883 0.0607 1.0000 Uiso . . . . . . H41 H 0.4001 0.5307 0.1402 0.0512 1.0000 Uiso . . . . . . H51 H 0.1738 0.1978 0.1920 0.0560 1.0000 Uiso . . . . . . H281 H 0.4805 0.1385 0.4001 0.0673 1.0000 Uiso . . . . . . H271 H 0.2564 0.7364 0.0972 0.0724 1.0000 Uiso . . . . . . H151 H 0.0668 0.7893 0.0567 0.0875 1.0000 Uiso . . . . . . H181 H -0.0286 0.0688 0.1799 0.0965 1.0000 Uiso . . . . . . H191 H -0.2722 0.4524 0.0811 0.1296 1.0000 Uiso . . . . . . H201 H -0.1388 0.6746 0.0504 0.1137 1.0000 Uiso . . . . . . H211 H 0.5814 0.1502 0.5249 0.0902 1.0000 Uiso . . . . . . H221 H 0.7471 0.6703 0.4625 0.0951 1.0000 Uiso . . . . . . H231 H -0.2220 0.1363 0.1390 0.1221 1.0000 Uiso . . . . . . H241 H 0.6964 0.4291 0.5580 0.0995 1.0000 Uiso . . . . . . H261 H 0.6887 0.9397 0.3532 0.1203 0.439(17) Uiso . . P 1 1 . H264 H 0.7085 0.9252 0.2619 0.1203 0.439(17) Uiso . . P 1 1 . H263 H 0.6919 0.9451 0.3527 0.1203 0.561(17) Uiso . . P 1 2 . H262 H 0.7148 0.9270 0.2619 0.1203 0.561(17) Uiso . . P 1 2 . H2501 H 0.8568 0.5523 0.2687 0.1023 0.561(17) Uiso . . P 1 2 . H2511 H 0.8781 0.5977 0.2741 0.1477 0.439(17) Uiso . . P 1 1 . H1001 H 1.0723 0.6265 0.2919 0.1456 0.439(17) Uiso . . P 1 1 . H1011 H 1.0453 0.4861 0.3065 0.1049 0.561(17) Uiso . . P 1 2 . H1101 H 0.8693 1.0634 0.4098 0.1192 0.561(17) Uiso . . P 1 2 . H1111 H 0.8414 1.1398 0.3896 0.1554 0.439(17) Uiso . . P 1 1 . H1201 H 1.0632 0.9845 0.4448 0.1161 0.561(17) Uiso . . P 1 2 . H1211 H 1.0423 1.1567 0.4055 0.1503 0.439(17) Uiso . . P 1 1 . H1301 H 1.1481 0.6877 0.3944 0.1165 0.561(17) Uiso . . P 1 2 . H1311 H 1.1572 0.8963 0.3554 0.1503 0.439(17) Uiso . . P 1 1 . H31 H 0.5478 0.1440 0.2318 0.0500 1.0000 Uiso . . . . . . 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 0.096(3) 0.156(5) 0.0499(18) -0.040(2) -0.0237(17) 0.038(3) F2 0.079(3) 0.235(8) 0.0468(18) -0.002(3) 0.0080(17) -0.003(4) N3 0.055(2) 0.073(3) 0.0374(18) -0.0032(19) -0.0070(16) 0.030(2) O4 0.065(3) 0.109(4) 0.083(3) 0.045(3) -0.006(2) -0.025(3) C1 0.044(2) 0.049(3) 0.042(2) -0.0120(19) -0.0046(17) 0.011(2) N6 0.056(2) 0.061(3) 0.057(2) 0.003(2) 0.0030(19) -0.001(2) C2 0.044(2) 0.059(3) 0.038(2) 0.009(2) -0.0046(17) -0.001(2) C31 0.046(2) 0.028(2) 0.047(2) -0.0035(17) -0.0014(18) -0.0021(17) C30 0.090(4) 0.026(3) 0.047(2) -0.0041(18) -0.006(2) -0.005(2) C29 0.042(2) 0.026(2) 0.049(2) -0.0019(16) -0.0049(16) 0.0023(16) C32 0.072(4) 0.100(6) 0.049(3) -0.023(3) -0.016(3) 0.046(4) C3 0.053(2) 0.050(3) 0.044(2) 0.004(2) -0.0065(19) 0.016(2) C4 0.048(2) 0.039(2) 0.0386(19) -0.0017(17) -0.0060(16) 0.0094(18) C5 0.049(2) 0.043(3) 0.048(2) -0.0022(19) -0.0112(18) 0.007(2) N1 0.051(3) 0.069(4) 0.100(4) -0.005(3) -0.002(3) -0.003(2) C7 0.049(2) 0.062(3) 0.044(2) 0.000(2) -0.0087(18) 0.002(2) C8 0.054(3) 0.093(5) 0.046(2) -0.002(3) -0.004(2) 0.029(3) C9 0.049(3) 0.085(4) 0.042(2) -0.007(2) -0.0019(19) 0.001(3) N10 0.140(6) 0.041(3) 0.068(3) -0.002(2) -0.009(3) 0.010(3) F29 0.256(9) 0.154(7) 0.073(3) -0.037(3) -0.017(4) 0.141(7) C28 0.053(3) 0.065(4) 0.045(2) 0.012(2) -0.0080(19) 0.003(2) C27 0.063(3) 0.060(4) 0.053(3) 0.002(2) -0.002(2) 0.017(3) C14 0.040(2) 0.068(4) 0.083(4) -0.023(3) -0.008(2) 0.018(2) C15 0.068(4) 0.083(5) 0.060(3) 0.012(3) -0.010(3) 0.031(4) C16 0.039(2) 0.103(6) 0.086(4) 0.027(4) -0.012(3) -0.002(3) C18 0.060(3) 0.127(7) 0.063(3) 0.001(4) -0.001(3) -0.027(4) C19 0.045(3) 0.223(14) 0.061(3) 0.011(6) -0.001(3) 0.020(5) C20 0.053(4) 0.168(10) 0.068(4) 0.005(5) -0.003(3) 0.040(5) C21 0.066(3) 0.129(7) 0.042(2) 0.014(3) -0.015(2) 0.007(4) C22 0.058(3) 0.106(6) 0.075(4) -0.032(4) -0.008(3) 0.005(3) C23 0.059(4) 0.195(13) 0.065(4) -0.004(6) 0.006(3) -0.030(6) C24 0.071(4) 0.118(7) 0.065(3) -0.005(4) -0.026(3) -0.004(4) C26 0.058(4) 0.082(6) 0.149(8) 0.003(6) -0.001(4) -0.017(4) C170 0.027(4) 0.131(9) 0.124(8) -0.041(7) 0.011(5) -0.008(5) C171 0.150(14) 0.174(16) 0.091(9) -0.008(9) -0.023(9) -0.120(13) C250 0.019(4) 0.143(9) 0.107(7) -0.060(7) -0.003(4) -0.003(4) C251 0.156(14) 0.175(16) 0.093(9) -0.012(9) -0.028(8) -0.113(13) C100 0.155(13) 0.171(16) 0.093(9) -0.011(9) -0.025(8) -0.116(13) C101 0.023(4) 0.153(10) 0.112(7) -0.064(7) -0.002(4) 0.002(5) C110 0.050(5) 0.140(10) 0.147(9) -0.042(8) 0.010(5) -0.012(6) C111 0.156(13) 0.173(16) 0.099(9) -0.005(10) -0.016(9) -0.119(13) C120 0.045(5) 0.151(10) 0.139(8) -0.057(8) -0.004(5) -0.014(6) C121 0.155(13) 0.165(16) 0.096(9) -0.008(9) -0.021(8) -0.122(12) C130 0.045(5) 0.157(10) 0.126(8) -0.064(7) 0.002(5) -0.013(5) C131 0.155(13) 0.170(16) 0.091(9) -0.009(9) -0.019(8) -0.119(13) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . N3 . C3 . 111.5(4) yes C2 . N3 . H31 . 126.1 no C3 . N3 . H31 . 115.3 no C4 . C1 . C5 . 124.3(4) yes C4 . C1 . C27 . 115.3(5) yes C5 . C1 . C27 . 120.3(4) yes N3 . C2 . C29 . 103.1(4) yes N3 . C2 . C7 . 114.1(4) yes C29 . C2 . C7 . 117.0(4) yes N3 . C2 . C16 . 115.8(5) yes C29 . C2 . C16 . 104.6(4) yes C7 . C2 . C16 . 102.5(4) yes N6 . C31 . C29 . 177.3(5) yes C29 . C30 . N10 . 179.6(8) yes C2 . C29 . C30 . 112.7(4) yes C2 . C29 . C31 . 110.4(4) yes C30 . C29 . C31 . 107.1(4) yes C2 . C29 . C4 . 101.3(3) yes C30 . C29 . C4 . 111.7(4) yes C31 . C29 . C4 . 113.7(4) yes F1 . C32 . F2 . 105.8(6) yes F1 . C32 . C3 . 112.2(5) yes F2 . C32 . C3 . 114.5(6) yes F1 . C32 . F29 . 110.1(7) yes F2 . C32 . F29 . 104.7(7) yes C3 . C32 . F29 . 109.2(6) yes N3 . C3 . C32 . 110.1(4) yes N3 . C3 . C4 . 105.2(4) yes C32 . C3 . C4 . 112.7(5) yes N3 . C3 . H99 . 108.5 no C32 . C3 . H99 . 111.1 no C4 . C3 . H99 . 109.1 no C3 . C4 . C1 . 118.4(4) yes C3 . C4 . C29 . 100.3(3) yes C1 . C4 . C29 . 114.0(4) yes C3 . C4 . H41 . 108.0 no C1 . C4 . H41 . 107.8 no C29 . C4 . H41 . 107.8 no C1 . C5 . C9 . 121.3(5) yes C1 . C5 . H51 . 119.5 no C9 . C5 . H51 . 119.2 no C14 . N1 . C16 . 110.4(6) yes C14 . N1 . C26 . 125.2(7) yes C16 . N1 . C26 . 124.0(7) yes C2 . C7 . C28 . 130.3(5) yes C2 . C7 . C14 . 107.0(5) yes C28 . C7 . C14 . 122.5(5) yes C9 . C8 . C15 . 121.2(5) yes C9 . C8 . C20 . 118.0(8) yes C15 . C8 . C20 . 120.8(7) yes C5 . C9 . C8 . 117.0(6) yes C5 . C9 . C18 . 121.4(6) yes C8 . C9 . C18 . 121.6(6) yes C7 . C28 . C21 . 116.0(6) yes C7 . C28 . H281 . 122.4 no C21 . C28 . H281 . 121.6 no C1 . C27 . C15 . 120.1(6) yes C1 . C27 . H271 . 120.7 no C15 . C27 . H271 . 119.2 no N1 . C14 . C7 . 111.1(5) yes N1 . C14 . C22 . 127.8(7) yes C7 . C14 . C22 . 121.0(7) yes C8 . C15 . C27 . 120.0(6) yes C8 . C15 . H151 . 119.5 no C27 . C15 . H151 . 120.4 no C2 . C16 . N1 . 108.5(6) yes C2 . C16 . O4 . 122.2(7) yes N1 . C16 . O4 . 128.9(7) yes C9 . C18 . C23 . 117.3(9) yes C9 . C18 . H181 . 121.4 no C23 . C18 . H181 . 121.2 no C20 . C19 . C23 . 121.4(7) yes C20 . C19 . H191 . 118.5 no C23 . C19 . H191 . 120.1 no C8 . C20 . C19 . 120.3(10) yes C8 . C20 . H201 . 122.2 no C19 . C20 . H201 . 117.4 no C28 . C21 . C24 . 119.8(7) yes C28 . C21 . H211 . 119.6 no C24 . C21 . H211 . 120.6 no C14 . C22 . C24 . 116.7(8) yes C14 . C22 . H221 . 120.6 no C24 . C22 . H221 . 122.6 no C18 . C23 . C19 . 121.2(9) yes C18 . C23 . H231 . 118.7 no C19 . C23 . H231 . 120.0 no C21 . C24 . C22 . 123.8(6) yes C21 . C24 . H241 . 116.8 no C22 . C24 . H241 . 119.0 no N1 . C26 . C171 . 119.8(6) yes N1 . C26 . H261 . 104.6 no C171 . C26 . H261 . 102.6 no N1 . C26 . H264 . 110.8 no C171 . C26 . H264 . 109.2 no H261 . C26 . H264 . 109.1 no N1 . C26 . C170 . 106.6(6) yes N1 . C26 . H263 . 107.5 no C170 . C26 . H263 . 105.2 no N1 . C26 . H262 . 114.3 no C170 . C26 . H262 . 113.5 no H263 . C26 . H262 . 109.1 no C26 . C170 . C250 . 122.92(8) yes C26 . C170 . C110 . 112.92(8) yes C250 . C170 . C110 . 124.10(8) yes C26 . C171 . C251 . 122.74(9) yes C26 . C171 . C111 . 112.72(9) yes C251 . C171 . C111 . 124.02(8) yes C170 . C250 . C101 . 117.80(9) yes C170 . C250 . H2501 . 118.5 no C101 . C250 . H2501 . 123.6 no C171 . C251 . C100 . 117.84(9) yes C171 . C251 . H2511 . 118.8 no C100 . C251 . H2511 . 123.1 no C251 . C100 . C131 . 123.59(9) yes C251 . C100 . H1001 . 113.6 no C131 . C100 . H1001 . 122.8 no C250 . C101 . C130 . 123.57(9) yes C250 . C101 . H1011 . 113.1 no C130 . C101 . H1011 . 123.3 no C170 . C110 . C120 . 114.31(9) yes C170 . C110 . H1101 . 125.8 no C120 . C110 . H1101 . 119.8 no C171 . C111 . C121 . 114.32(9) yes C171 . C111 . H1111 . 125.6 no C121 . C111 . H1111 . 120.1 no C110 . C120 . C130 . 120.86(9) yes C110 . C120 . H1201 . 121.5 no C130 . C120 . H1201 . 117.5 no C111 . C121 . C131 . 120.85(9) yes C111 . C121 . H1211 . 120.8 no C131 . C121 . H1211 . 118.2 no C120 . C130 . C101 . 119.36(9) yes C120 . C130 . H1301 . 125.5 no C101 . C130 . H1301 . 114.9 no C121 . C131 . C100 . 119.36(9) yes C121 . C131 . H1311 . 125.0 no C100 . C131 . H1311 . 115.6 no loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag F1 . C32 . 1.324(7) yes F2 . C32 . 1.314(12) yes N3 . C2 . 1.445(7) yes N3 . C3 . 1.494(6) yes N3 . H31 . 0.764 no O4 . C16 . 1.227(9) yes C1 . C4 . 1.522(6) yes C1 . C5 . 1.341(8) yes C1 . C27 . 1.409(8) yes N6 . C31 . 1.114(7) yes C2 . C29 . 1.586(6) yes C2 . C7 . 1.514(6) yes C2 . C16 . 1.586(9) yes C31 . C29 . 1.464(6) yes C30 . C29 . 1.477(6) yes C30 . N10 . 1.137(8) yes C29 . C4 . 1.583(6) yes C32 . C3 . 1.490(7) yes C32 . F29 . 1.352(9) yes C3 . C4 . 1.522(7) yes C3 . H99 . 0.948 no C4 . H41 . 0.956 no C5 . C9 . 1.431(7) yes C5 . H51 . 0.944 no N1 . C14 . 1.435(10) yes N1 . C16 . 1.347(10) yes N1 . C26 . 1.436(10) yes C7 . C28 . 1.366(8) yes C7 . C14 . 1.419(9) yes C8 . C9 . 1.404(10) yes C8 . C15 . 1.384(11) yes C8 . C20 . 1.456(8) yes C9 . C18 . 1.404(10) yes C28 . C21 . 1.412(7) yes C28 . H281 . 0.937 no C27 . C15 . 1.369(8) yes C27 . H271 . 0.951 no C14 . C22 . 1.387(9) yes C15 . H151 . 0.955 no C18 . C23 . 1.411(11) yes C18 . H181 . 0.965 no C19 . C20 . 1.320(17) yes C19 . C23 . 1.403(19) yes C19 . H191 . 0.959 no C20 . H201 . 0.930 no C21 . C24 . 1.419(13) yes C21 . H211 . 0.940 no C22 . C24 . 1.337(13) yes C22 . H221 . 0.986 no C23 . H231 . 0.971 no C24 . H241 . 0.967 no C26 . C171 . 1.516(8) yes C26 . H261 . 1.012 no C26 . H264 . 0.891 no C26 . C170 . 1.606(7) yes C26 . H263 . 1.011 no C26 . H262 . 0.891 no C170 . C250 . 1.276(7) yes C170 . C110 . 1.485(7) yes C171 . C251 . 1.260(8) yes C171 . C111 . 1.470(8) yes C250 . C101 . 1.378(7) yes C250 . H2501 . 0.984 no C251 . C100 . 1.349(8) yes C251 . H2511 . 0.983 no C100 . C131 . 1.344(8) yes C100 . H1001 . 0.978 no C101 . C130 . 1.354(7) yes C101 . H1011 . 0.979 no C110 . C120 . 1.403(7) yes C110 . H1101 . 0.957 no C111 . C121 . 1.378(8) yes C111 . H1111 . 0.962 no C120 . C130 . 1.368(7) yes C120 . H1201 . 0.948 no C121 . C131 . 1.348(8) yes C121 . H1211 . 0.954 no C130 . H1301 . 0.958 no C131 . H1311 . 0.957 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C3 . H99 . N10 1_545 140 0.95 2.41 3.195(11) yes C4 . H41 . O4 . 125 0.96 2.43 3.081(11) yes