#------------------------------------------------------------------------------ #$Date: 2021-05-20 04:32:54 +0300 (Thu, 20 May 2021) $ #$Revision: 265346 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/28/7242876.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_7242876 loop_ _publ_author_name 'Richardson, Jonathan' 'Mizuno, Asato' 'Shuku, Yoshiaki' 'Awaga, Kunio' 'Robertson, Neil' 'Morrison, Carole A.' 'Warren, Mark R.' 'Allan, David Robert' 'Moggach, Stephen A.' _publ_section_title ; Evaluating the high-pressure structural response and crystal lattice interactions of the magnetically-bistable organic radical TTTA ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D1CE00577D _journal_year 2021 _chemical_formula_moiety 'C2 N3 S3' _chemical_formula_sum 'C2 N3 S3' _chemical_formula_weight 162.24 _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _audit_creation_date 2021-04-22 _audit_creation_method CRYSTALS_ver_14.61_build_6999 _audit_update_record ; 2021-04-27 deposited with the CCDC. 2021-05-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.44(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.191(12) _cell_length_b 3.3508(4) _cell_length_c 14.562(3) _cell_measurement_reflns_used 865 _cell_measurement_temperature 293 _cell_measurement_theta_max 20 _cell_measurement_theta_min 4 _cell_volume 434.3(6) _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_collection 'USER DEFINED DATA COLLECTION' _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 'SHELXS 86 (Sheldrick, 1986)' _diffrn_ambient_pressure 2910000 _diffrn_ambient_temperature 293 _diffrn_measured_fraction_theta_full 0.341 _diffrn_measured_fraction_theta_max 0.309 _diffrn_measurement_device Area _diffrn_measurement_device_type Synchrotron _diffrn_measurement_method \w _diffrn_radiation_monochromator 'focussing mirrors' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.48590 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_unetI/netI 0.058 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 2098 _diffrn_reflns_theta_full 15.857 _diffrn_reflns_theta_max 20.329 _diffrn_reflns_theta_min 3.870 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.481 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 324 _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.53 _refine_diff_density_min -0.48 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 0.9887 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 73 _refine_ls_number_reflns 403 _refine_ls_number_restraints 104 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0707 _refine_ls_shift/su_max 0.0003129 _refine_ls_shift/su_mean 0.0000268 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.15P)^2^ + 0.25P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.2935 _refine_ls_wR_factor_gt 0.2252 _refine_ls_wR_factor_ref 0.1772 _reflns_limit_h_max 4 _reflns_limit_h_min -6 _reflns_limit_k_max 4 _reflns_limit_k_min 0 _reflns_limit_l_max 18 _reflns_limit_l_min 0 _reflns_number_gt 305 _reflns_number_total 411 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _oxford_refine_ls_r_factor_ref 0.0754 _oxford_refine_ls_scale 0.802(12) _oxford_reflns_number_all 411 _iucr_refine_instructions_details ; # # Punched on 22/04/21 at 21:27:24 # #LIST 12 BLOCK SCALE X'S U'S END # # Punched on 22/04/21 at 21:27:24 # #LIST 16 DIST 1.659,.01= S(1) TO N(2) DIST 1.734,.01= S(1) TO C(5) DIST 1.656,.01= N(2) TO S(3) DIST 1.735,.01= S(3) TO C(4) DIST 1.430,.01= C(4) TO C(5) DIST 1.313,.01= C(4) TO N(8) DIST 1.318,.01= C(5) TO N(6) DIST 1.645,.01= N(6) TO S(7) DIST 1.646,.01= S(7) TO N(8) ANGL 98,1= C(5) TO S(1) TO N(2) ANGL 117,1= S(3) TO N(2) TO S(1) ANGL 98,1= C(4) TO S(3) TO N(2) ANGL 114,1= C(5) TO C(4) TO S(3) ANGL 132,1= N(8) TO C(4) TO S(3) ANGL 114,1= N(8) TO C(4) TO C(5) ANGL 114,1= C(4) TO C(5) TO S(1) ANGL 132,1= N(6) TO C(5) TO S(1) ANGL 114,1= N(6) TO C(5) TO C(4) ANGL 106,1= S(7) TO N(6) TO C(5) ANGL 99,1= N(8) TO S(7) TO N(6) ANGL 106,1= S(7) TO N(8) TO C(4) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) PLANAR 0.01 N(2) S(1) S(3) C(4) C(5) N(6) S(7) N(8) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = S(1) TO N(2) VIBR .0, 0.00200 = S(1) TO C(5) VIBR .0, 0.00500 = C(5) TO N(2) VIBR .0, 0.00200 = N(2) TO S(3) VIBR .0, 0.00500 = S(3) TO S(1) VIBR .0, 0.00200 = S(3) TO C(4) VIBR .0, 0.00500 = C(4) TO N(2) VIBR .0, 0.00200 = C(4) TO C(5) VIBR .0, 0.00200 = C(4) TO N(8) VIBR .0, 0.00500 = C(5) TO S(3) VIBR .0, 0.00500 = N(8) TO S(3) VIBR .0, 0.00500 = N(8) TO C(5) VIBR .0, 0.00200 = C(5) TO N(6) VIBR .0, 0.00500 = S(1) TO C(4) VIBR .0, 0.00500 = N(6) TO C(4) VIBR .0, 0.00500 = N(6) TO S(1) VIBR .0, 0.00200 = N(6) TO S(7) VIBR .0, 0.00500 = S(7) TO C(5) VIBR .0, 0.00200 = S(7) TO N(8) VIBR .0, 0.00500 = N(8) TO N(6) VIBR .0, 0.00500 = S(7) TO C(4) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = S(1) TO N(2) U(IJ) .0, 0.04000 = S(1) TO C(5) U(IJ) .0, 0.04000 = N(2) TO S(3) U(IJ) .0, 0.04000 = S(3) TO C(4) U(IJ) .0, 0.04000 = C(4) TO C(5) U(IJ) .0, 0.04000 = C(4) TO N(8) U(IJ) .0, 0.04000 = C(5) TO N(6) U(IJ) .0, 0.04000 = N(6) TO S(7) U(IJ) .0, 0.04000 = S(7) TO N(8) REM THERMSIM END (DO NOT REMOVE THIS LINE) END ; _cod_data_source_file d1ce00577d2.cif _cod_data_source_block 291GPa _cod_depositor_comments ; The following automatic conversions were performed: 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_original_sg_symbol_H-M 'P 1 21/c 1 ' _cod_database_code 7242876 _oxford_refine_reflns_threshold_expression_ref I>-10.0\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 -1 0 0.22 0.54 0. 1.0000 0. 0 -1 0 0.80 0.79 0. 1.0000 0. 0 1 0 0.90 0.94 0. 1.0000 0. 0 1 0 0.41 0.46 0. 1.0000 0. 0 1 0 0.29 0.82 0. 1.0000 0. 0 1 0 0.81 0.65 0. 1.0000 0. -1 -1 0 9743.74 401.62 0. 1.0000 0. -1 -1 0 9721.23 434.13 0. 1.0000 0. 1 -1 0 8861.08 474.02 0. 1.0000 0. 1 -1 0 9999.99 446.85 0. 1.0000 0. -1 1 0 9394.55 403.91 0. 1.0000 0. 1 1 0 9844.41 403.50 0. 1.0000 0. -1 1 0 9811.56 397.50 0. 1.0000 0. -1 1 0 9800.91 395.59 0. 1.0000 0. 0 2 0 824.64 34.13 0. 1.0000 0. 0 2 0 773.43 37.33 0. 1.0000 0. 0 2 0 784.87 35.42 0. 1.0000 0. 1 -2 0 877.98 46.50 0. 1.0000 0. 1 -2 0 864.96 43.66 0. 1.0000 0. 1 2 0 953.73 39.07 0. 1.0000 0. 1 2 0 928.00 42.45 0. 1.0000 0. 1 2 0 867.46 43.11 0. 1.0000 0. -1 2 0 913.34 43.10 0. 1.0000 0. 1 2 0 928.15 37.71 0. 1.0000 0. -1 2 0 925.62 39.34 0. 1.0000 0. -1 2 0 926.15 38.70 0. 1.0000 0. -2 -2 0 44.54 3.60 0. 1.0000 0. 2 -2 0 41.92 6.33 0. 1.0000 0. 2 2 0 45.19 3.66 0. 1.0000 0. -2 2 0 38.70 4.67 0. 1.0000 0. 1 -3 0 -1.47 6.70 0. 1.0000 0. -1 -3 0 -2.23 3.15 0. 1.0000 0. 1 -3 0 5.25 2.34 0. 1.0000 0. -1 -3 0 3.73 2.17 0. 1.0000 0. -1 -3 0 -0.48 3.44 0. 1.0000 0. 1 -3 0 4.46 2.25 0. 1.0000 0. 1 3 0 -3.27 3.25 0. 1.0000 0. -1 3 0 -5.14 3.69 0. 1.0000 0. 1 3 0 -1.77 3.08 0. 1.0000 0. 1 3 0 -2.20 2.22 0. 1.0000 0. 1 3 0 -10.94 6.02 0. 1.0000 0. -1 3 0 -2.42 4.56 0. 1.0000 0. -1 3 0 -2.52 3.15 0. 1.0000 0. -1 3 0 6.56 2.60 0. 1.0000 0. 2 -3 0 633.22 32.80 0. 1.0000 0. -2 -3 0 605.01 26.23 0. 1.0000 0. -2 -3 0 585.62 27.88 0. 1.0000 0. 2 -3 0 548.37 28.36 0. 1.0000 0. -2 3 0 589.41 27.44 0. 1.0000 0. -2 3 0 585.38 28.93 0. 1.0000 0. 2 3 0 579.48 25.18 0. 1.0000 0. -2 3 0 574.21 25.57 0. 1.0000 0. 3 3 0 8.11 2.85 0. 1.0000 0. -3 3 0 13.05 5.39 0. 1.0000 0. 3 3 0 5.42 3.56 0. 1.0000 0. 1 -1 -1 76.03 3.97 0. 1.0000 0. -1 -1 1 73.16 3.78 0. 1.0000 0. -1 -1 1 74.42 3.53 0. 1.0000 0. 1 -1 -1 68.73 4.85 0. 1.0000 0. 1 1 -1 73.55 3.88 0. 1.0000 0. -1 1 1 74.62 3.82 0. 1.0000 0. -1 1 1 72.96 3.52 0. 1.0000 0. 1 1 -1 75.38 3.87 0. 1.0000 0. -1 1 1 72.42 3.57 0. 1.0000 0. -1 1 1 73.55 4.21 0. 1.0000 0. 0 -1 -1 450.84 18.54 0. 1.0000 0. 0 -1 1 430.08 20.39 0. 1.0000 0. 0 1 1 417.45 18.94 0. 1.0000 0. 0 1 -1 440.95 19.26 0. 1.0000 0. 0 1 1 431.09 20.75 0. 1.0000 0. 0 1 1 453.13 18.42 0. 1.0000 0. 0 1 -1 453.50 18.28 0. 1.0000 0. 0 1 -1 453.84 18.81 0. 1.0000 0. 0 1 1 429.42 19.95 0. 1.0000 0. 0 1 -1 443.90 21.01 0. 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0. 1.0000 0. 1 2 1 2.36 1.36 0. 1.0000 0. 1 2 1 3.58 1.85 0. 1.0000 0. -1 2 -1 7.33 2.58 0. 1.0000 0. -2 -2 -1 1458.48 59.03 0. 1.0000 0. 2 -2 1 1407.20 69.52 0. 1.0000 0. 2 2 1 1379.17 62.74 0. 1.0000 0. -2 2 -1 1396.57 58.82 0. 1.0000 0. -2 2 -1 1354.06 59.31 0. 1.0000 0. 2 2 1 1388.41 56.94 0. 1.0000 0. -2 2 -1 1344.49 66.56 0. 1.0000 0. 3 -3 -1 18.25 2.99 0. 1.0000 0. -3 3 1 15.46 3.97 0. 1.0000 0. 3 3 -1 18.52 3.00 0. 1.0000 0. 3 3 -1 7.57 3.54 0. 1.0000 0. -3 3 1 7.56 4.76 0. 1.0000 0. 2 -3 -1 96.21 9.38 0. 1.0000 0. -2 -3 1 101.20 6.26 0. 1.0000 0. 2 -3 -1 70.87 5.55 0. 1.0000 0. -2 -3 1 77.40 5.50 0. 1.0000 0. -2 3 1 94.46 5.77 0. 1.0000 0. -2 3 1 95.95 7.61 0. 1.0000 0. 2 3 -1 91.00 4.75 0. 1.0000 0. -2 3 1 93.17 6.50 0. 1.0000 0. 2 3 -1 91.47 5.88 0. 1.0000 0. 1 -3 -1 180.82 13.53 0. 1.0000 0. -1 -3 1 197.49 9.03 0. 1.0000 0. -1 -3 1 176.26 10.85 0. 1.0000 0. 1 -3 -1 189.19 9.80 0. 1.0000 0. -1 -3 1 185.02 9.95 0. 1.0000 0. 1 3 -1 178.99 10.50 0. 1.0000 0. -1 3 1 189.67 10.51 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1.0000 0. 2 1 -14 4.37 4.09 0. 1.0000 0. -2 1 14 6.65 2.85 0. 1.0000 0. -1 -1 14 895.23 49.36 0. 1.0000 0. 1 -1 -14 897.99 45.58 0. 1.0000 0. -1 -1 14 963.39 41.91 0. 1.0000 0. 1 -1 -14 900.47 40.27 0. 1.0000 0. 1 1 -14 926.46 39.56 0. 1.0000 0. 1 1 -14 939.19 45.01 0. 1.0000 0. -1 1 14 873.65 38.80 0. 1.0000 0. -1 1 14 966.99 41.71 0. 1.0000 0. 0 -1 14 94.28 5.68 0. 1.0000 0. 0 -1 -14 88.28 8.03 0. 1.0000 0. 0 -1 14 89.27 10.17 0. 1.0000 0. 0 -1 -14 98.79 5.90 0. 1.0000 0. 0 1 -14 96.13 6.57 0. 1.0000 0. 0 1 -14 92.87 7.60 0. 1.0000 0. 0 1 14 89.52 5.34 0. 1.0000 0. 0 1 14 100.69 10.18 0. 1.0000 0. -1 1 -14 21.38 4.81 0. 1.0000 0. 1 1 14 17.59 2.71 0. 1.0000 0. -2 1 -14 609.83 31.31 0. 1.0000 0. 6 -2 -14 -0.75 1.22 0. 1.0000 0. 4 -2 -14 -0.42 2.99 0. 1.0000 0. 4 2 -14 -3.13 4.01 0. 1.0000 0. 4 2 -14 -1.37 4.33 0. 1.0000 0. -4 2 14 1.07 4.33 0. 1.0000 0. -4 2 14 0.22 5.71 0. 1.0000 0. 3 -2 -14 21.85 4.09 0. 1.0000 0. -3 -2 14 22.03 3.59 0. 1.0000 0. 3 -2 -14 25.86 4.02 0. 1.0000 0. 3 2 -14 24.00 4.34 0. 1.0000 0. 3 2 -14 25.61 4.39 0. 1.0000 0. -3 2 14 27.37 7.44 0. 1.0000 0. -3 2 14 24.28 4.38 0. 1.0000 0. 2 -2 -14 38.47 4.13 0. 1.0000 0. -2 -2 14 40.50 8.98 0. 1.0000 0. -2 -2 14 38.30 3.95 0. 1.0000 0. 2 -2 -14 23.32 4.36 0. 1.0000 0. 2 2 -14 36.86 5.34 0. 1.0000 0. 2 2 -14 45.96 4.72 0. 1.0000 0. -2 2 14 35.81 4.09 0. 1.0000 0. -2 2 14 24.73 8.58 0. 1.0000 0. 1 -2 -14 5.09 4.30 0. 1.0000 0. 1 -2 -14 10.64 3.05 0. 1.0000 0. -1 -2 14 7.79 3.26 0. 1.0000 0. -1 -2 14 9.34 7.51 0. 1.0000 0. 1 2 -14 9.79 3.48 0. 1.0000 0. -1 2 14 11.33 7.76 0. 1.0000 0. -1 2 14 12.50 3.28 0. 1.0000 0. 1 2 -14 14.02 4.71 0. 1.0000 0. 0 -2 14 3.26 8.87 0. 1.0000 0. 0 -2 -14 3.51 3.12 0. 1.0000 0. 0 -2 14 6.38 3.27 0. 1.0000 0. 0 -2 -14 12.40 5.78 0. 1.0000 0. 0 2 -14 5.57 3.64 0. 1.0000 0. 0 2 14 2.07 2.89 0. 1.0000 0. 0 2 14 5.57 6.09 0. 1.0000 0. 0 2 -14 10.78 4.82 0. 1.0000 0. -2 2 -14 -6.48 5.42 0. 1.0000 0. 6 -3 -14 20.05 4.68 0. 1.0000 0. 6 3 -14 12.13 5.10 0. 1.0000 0. -6 3 14 29.48 7.80 0. 1.0000 0. -5 -3 14 44.24 5.89 0. 1.0000 0. -5 3 14 39.03 6.98 0. 1.0000 0. -3 -3 14 -2.86 9.36 0. 1.0000 0. 3 -3 -14 0.84 3.64 0. 1.0000 0. -3 -3 14 2.68 4.00 0. 1.0000 0. 3 -3 -14 4.61 3.81 0. 1.0000 0. -3 3 14 -0.30 7.27 0. 1.0000 0. 3 3 -14 5.33 4.46 0. 1.0000 0. -3 3 14 0.16 4.60 0. 1.0000 0. 3 3 -14 3.92 4.27 0. 1.0000 0. -2 -3 14 22.28 9.38 0. 1.0000 0. -2 -3 14 15.78 3.95 0. 1.0000 0. 2 -3 -14 11.08 4.31 0. 1.0000 0. 2 -3 -14 16.94 3.87 0. 1.0000 0. -2 3 14 9.13 8.60 0. 1.0000 0. 2 3 -14 24.54 4.71 0. 1.0000 0. -2 3 14 11.45 4.00 0. 1.0000 0. 2 3 -14 15.65 4.65 0. 1.0000 0. -1 -3 14 -2.26 8.05 0. 1.0000 0. 1 -3 -14 2.09 3.30 0. 1.0000 0. -1 -3 14 3.80 3.92 0. 1.0000 0. 1 -3 -14 -3.22 4.29 0. 1.0000 0. -1 3 14 -1.62 3.85 0. 1.0000 0. 1 3 -14 -3.77 5.01 0. 1.0000 0. -1 3 14 -4.09 7.83 0. 1.0000 0. 1 3 -14 3.37 3.95 0. 1.0000 0. -1 -3 -14 0.30 6.15 0. 1.0000 0. 1 -3 14 23.24 10.48 0. 1.0000 0. 1 -3 14 9.76 4.15 0. 1.0000 0. -1 -3 -14 18.78 4.19 0. 1.0000 0. 1 3 14 10.33 3.13 0. 1.0000 0. -1 3 -14 7.72 5.47 0. 1.0000 0. -1 3 -14 18.29 5.11 0. 1.0000 0. 2 -3 14 -2.95 11.94 0. 1.0000 0. 2 -3 14 2.67 3.76 0. 1.0000 0. -2 3 -14 1.94 6.54 0. 1.0000 0. 5 -1 -15 354.69 17.42 0. 1.0000 0. -5 1 15 338.18 18.65 0. 1.0000 0. 5 1 -15 331.71 17.34 0. 1.0000 0. 4 -1 -15 185.82 10.36 0. 1.0000 0. -4 1 15 174.14 10.12 0. 1.0000 0. -4 1 15 179.52 11.52 0. 1.0000 0. 4 1 -15 180.00 10.63 0. 1.0000 0. 3 -1 -15 65.40 5.01 0. 1.0000 0. 3 -1 -15 64.94 5.29 0. 1.0000 0. 3 1 -15 67.78 5.12 0. 1.0000 0. -3 1 15 67.66 5.23 0. 1.0000 0. -3 1 15 64.07 7.14 0. 1.0000 0. 2 -1 -15 277.65 14.80 0. 1.0000 0. 2 -1 -15 271.92 13.22 0. 1.0000 0. -2 1 15 274.67 12.78 0. 1.0000 0. 2 1 -15 276.17 13.39 0. 1.0000 0. -2 1 15 281.48 16.66 0. 1.0000 0. 1 -1 -15 113.68 6.67 0. 1.0000 0. 1 -1 -15 121.00 8.50 0. 1.0000 0. -1 1 15 122.38 6.60 0. 1.0000 0. 1 1 -15 122.04 8.34 0. 1.0000 0. 1 1 -15 127.21 7.21 0. 1.0000 0. -1 1 15 124.57 10.63 0. 1.0000 0. 0 -1 -15 15.18 3.32 0. 1.0000 0. 0 -1 -15 12.28 4.94 0. 1.0000 0. 0 1 -15 16.18 5.34 0. 1.0000 0. 0 1 15 12.17 2.69 0. 1.0000 0. -1 1 -15 86.07 7.61 0. 1.0000 0. 1 1 15 79.33 5.05 0. 1.0000 0. -6 2 15 217.40 14.83 0. 1.0000 0. -5 -2 15 31.06 5.11 0. 1.0000 0. 5 -2 -15 37.52 4.58 0. 1.0000 0. -5 2 15 42.96 5.68 0. 1.0000 0. 5 2 -15 36.13 5.79 0. 1.0000 0. -5 2 15 42.68 7.63 0. 1.0000 0. 4 -2 -15 99.97 7.15 0. 1.0000 0. -4 -2 15 100.30 7.35 0. 1.0000 0. 4 2 -15 110.19 7.61 0. 1.0000 0. -4 2 15 109.05 7.46 0. 1.0000 0. -4 2 15 100.46 9.91 0. 1.0000 0. 4 2 -15 99.65 7.60 0. 1.0000 0. -3 -2 15 316.36 15.42 0. 1.0000 0. -3 -2 15 319.93 20.18 0. 1.0000 0. 3 -2 -15 306.19 15.21 0. 1.0000 0. 3 -2 -15 305.87 16.85 0. 1.0000 0. 3 2 -15 301.32 16.15 0. 1.0000 0. 3 2 -15 306.76 15.19 0. 1.0000 0. -3 2 15 305.76 19.69 0. 1.0000 0. -3 2 15 302.55 14.70 0. 1.0000 0. -2 -2 15 38.69 9.62 0. 1.0000 0. -2 -2 15 25.90 3.83 0. 1.0000 0. 2 -2 -15 20.86 3.77 0. 1.0000 0. 2 -2 -15 22.93 4.66 0. 1.0000 0. 2 2 -15 21.41 5.21 0. 1.0000 0. -2 2 15 24.63 8.44 0. 1.0000 0. -2 2 15 20.29 3.88 0. 1.0000 0. -1 -2 15 11.02 3.55 0. 1.0000 0. 1 -2 -15 12.03 3.29 0. 1.0000 0. 1 -2 -15 8.87 4.61 0. 1.0000 0. -1 -2 15 8.48 8.26 0. 1.0000 0. 1 2 -15 3.62 4.75 0. 1.0000 0. -1 2 15 7.39 3.44 0. 1.0000 0. -1 2 15 11.32 6.98 0. 1.0000 0. 1 2 -15 6.62 3.66 0. 1.0000 0. 0 -2 -15 86.66 5.96 0. 1.0000 0. 0 -2 -15 70.74 8.51 0. 1.0000 0. 0 -2 15 118.80 12.91 0. 1.0000 0. 0 2 -15 83.30 6.37 0. 1.0000 0. 0 2 -15 88.00 7.49 0. 1.0000 0. 0 2 15 87.37 5.28 0. 1.0000 0. 0 2 15 60.59 10.23 0. 1.0000 0. -1 -2 -15 -3.13 3.46 0. 1.0000 0. 1 -2 15 2.08 3.13 0. 1.0000 0. 1 -2 15 8.49 11.47 0. 1.0000 0. 1 2 15 1.61 3.24 0. 1.0000 0. -1 2 -15 -0.92 5.71 0. 1.0000 0. -2 2 -15 -2.48 6.21 0. 1.0000 0. 6 -3 -15 45.95 5.56 0. 1.0000 0. -6 3 15 48.42 9.37 0. 1.0000 0. 6 3 -15 38.23 6.84 0. 1.0000 0. 5 -3 -15 0.20 4.34 0. 1.0000 0. -5 -3 15 5.10 4.82 0. 1.0000 0. 5 3 -15 3.06 5.16 0. 1.0000 0. -5 3 15 -0.20 5.67 0. 1.0000 0. -5 3 15 4.14 7.81 0. 1.0000 0. 5 3 -15 4.36 5.27 0. 1.0000 0. -4 -3 15 -4.33 4.49 0. 1.0000 0. 4 -3 -15 1.39 4.15 0. 1.0000 0. 4 -3 -15 -0.51 3.72 0. 1.0000 0. 4 3 -15 -1.18 4.58 0. 1.0000 0. 4 3 -15 -2.27 4.76 0. 1.0000 0. -4 3 15 -6.77 8.30 0. 1.0000 0. -4 3 15 -0.19 5.26 0. 1.0000 0. -3 -3 15 33.91 9.98 0. 1.0000 0. 3 -3 -15 26.06 4.70 0. 1.0000 0. 3 -3 -15 33.72 4.82 0. 1.0000 0. -3 -3 15 35.07 4.80 0. 1.0000 0. 3 3 -15 46.48 5.78 0. 1.0000 0. -3 3 15 19.16 9.90 0. 1.0000 0. 3 3 -15 24.66 4.92 0. 1.0000 0. -3 3 15 38.00 5.41 0. 1.0000 0. 2 -3 -15 4.43 4.31 0. 1.0000 0. 2 -3 -15 -2.47 3.92 0. 1.0000 0. -2 -3 15 3.02 8.96 0. 1.0000 0. -2 -3 15 1.48 3.62 0. 1.0000 0. 2 3 -15 4.26 4.09 0. 1.0000 0. -2 3 15 -2.36 3.81 0. 1.0000 0. -2 3 15 0.38 8.76 0. 1.0000 0. 2 3 -15 -1.44 4.58 0. 1.0000 0. -1 -3 15 47.13 10.33 0. 1.0000 0. -1 -3 15 42.98 5.47 0. 1.0000 0. 1 -3 -15 43.95 5.90 0. 1.0000 0. 1 -3 -15 37.09 4.47 0. 1.0000 0. 1 3 -15 40.82 5.33 0. 1.0000 0. -1 3 15 45.06 4.79 0. 1.0000 0. 1 3 -15 52.56 6.17 0. 1.0000 0. -1 3 15 35.25 10.29 0. 1.0000 0. 0 -3 15 17.88 10.24 0. 1.0000 0. 0 -3 -15 7.71 3.76 0. 1.0000 0. 0 -3 15 0.33 3.79 0. 1.0000 0. 0 -3 -15 7.63 5.50 0. 1.0000 0. 0 3 15 4.48 8.57 0. 1.0000 0. 0 3 15 8.68 3.63 0. 1.0000 0. 0 3 -15 4.33 4.25 0. 1.0000 0. 0 3 -15 3.52 5.76 0. 1.0000 0. 1 -3 15 8.03 11.93 0. 1.0000 0. 1 -3 15 4.61 4.19 0. 1.0000 0. -1 -3 -15 4.45 6.69 0. 1.0000 0. -1 -3 -15 9.65 3.83 0. 1.0000 0. -1 3 -15 5.04 4.37 0. 1.0000 0. -1 3 -15 6.57 5.78 0. 1.0000 0. 1 3 15 6.21 3.34 0. 1.0000 0. 6 -2 -16 53.82 5.46 0. 1.0000 0. 6 2 -16 32.47 5.77 0. 1.0000 0. -6 2 16 45.41 8.11 0. 1.0000 0. -5 -2 16 3.16 4.31 0. 1.0000 0. 5 -2 -16 -3.90 3.30 0. 1.0000 0. -5 2 16 0.25 6.41 0. 1.0000 0. -5 2 16 1.97 4.98 0. 1.0000 0. 5 2 -16 2.75 4.66 0. 1.0000 0. -4 -2 16 4.93 4.34 0. 1.0000 0. 4 -2 -16 3.35 3.36 0. 1.0000 0. 4 -2 -16 5.72 3.83 0. 1.0000 0. -4 2 16 4.61 4.94 0. 1.0000 0. 4 2 -16 -0.61 3.94 0. 1.0000 0. 4 2 -16 6.29 4.78 0. 1.0000 0. -4 2 16 9.54 6.94 0. 1.0000 0. 3 -2 -16 621.16 27.70 0. 1.0000 0. 3 -2 -16 646.70 31.71 0. 1.0000 0. -3 -2 16 587.92 34.66 0. 1.0000 0. -3 -2 16 622.35 28.94 0. 1.0000 0. 3 2 -16 626.98 28.05 0. 1.0000 0. -3 2 16 593.42 33.65 0. 1.0000 0. 3 2 -16 621.61 29.99 0. 1.0000 0. -3 2 16 595.24 26.93 0. 1.0000 0. 2 -2 -16 -1.39 3.45 0. 1.0000 0. -2 -2 16 3.96 3.53 0. 1.0000 0. 2 -2 -16 -4.39 3.97 0. 1.0000 0. -2 -2 16 -2.67 8.13 0. 1.0000 0. -2 2 16 7.28 8.27 0. 1.0000 0. 2 2 -16 3.90 4.83 0. 1.0000 0. 2 2 -16 -0.70 3.63 0. 1.0000 0. -2 2 16 3.40 3.78 0. 1.0000 0. 1 -2 -16 31.32 3.94 0. 1.0000 0. -1 -2 16 27.10 8.69 0. 1.0000 0. 1 -2 -16 27.58 5.13 0. 1.0000 0. -1 -2 16 35.46 4.47 0. 1.0000 0. 1 2 -16 33.89 5.99 0. 1.0000 0. -1 2 16 14.66 7.63 0. 1.0000 0. -1 2 16 28.72 4.29 0. 1.0000 0. 1 2 -16 31.95 4.40 0. 1.0000 0. 0 -2 -16 316.39 15.37 0. 1.0000 0. 0 -2 -16 336.96 19.49 0. 1.0000 0. 0 -2 16 334.94 21.63 0. 1.0000 0. 0 2 16 306.49 14.79 0. 1.0000 0. 0 2 -16 323.15 17.65 0. 1.0000 0. 0 2 -16 304.56 16.26 0. 1.0000 0. -1 -2 -16 0.92 6.07 0. 1.0000 0. 1 -2 16 3.17 3.44 0. 1.0000 0. 1 -2 16 1.12 14.11 0. 1.0000 0. -1 2 -16 5.97 6.21 0. 1.0000 0. 1 2 16 4.25 3.37 0. 1.0000 0. -2 2 -16 3.25 6.32 0. 1.0000 0. 4 -3 -16 74.93 6.54 0. 1.0000 0. -4 -3 16 82.22 12.35 0. 1.0000 0. 4 -3 -16 67.15 6.46 0. 1.0000 0. -4 -3 16 78.67 7.05 0. 1.0000 0. -4 3 16 65.41 11.57 0. 1.0000 0. -4 3 16 65.79 7.26 0. 1.0000 0. 4 3 -16 71.24 7.20 0. 1.0000 0. 4 3 -16 75.88 6.86 0. 1.0000 0. 3 -3 -16 2.99 3.92 0. 1.0000 0. -3 -3 16 8.08 9.59 0. 1.0000 0. -3 -3 16 5.52 4.10 0. 1.0000 0. 3 -3 -16 2.38 4.35 0. 1.0000 0. -3 3 16 8.43 10.15 0. 1.0000 0. 3 3 -16 -2.91 4.95 0. 1.0000 0. -3 3 16 2.68 4.83 0. 1.0000 0. 3 3 -16 8.70 4.66 0. 1.0000 0. 2 -3 -16 144.51 8.95 0. 1.0000 0. 2 -3 -16 143.50 10.33 0. 1.0000 0. -2 -3 16 145.54 9.19 0. 1.0000 0. -2 -3 16 172.05 14.50 0. 1.0000 0. 2 3 -16 153.93 9.21 0. 1.0000 0. -2 3 16 147.96 8.67 0. 1.0000 0. 2 3 -16 163.76 10.20 0. 1.0000 0. -2 3 16 113.92 15.80 0. 1.0000 0. 1 -3 -16 61.78 5.12 0. 1.0000 0. -1 -3 16 65.25 10.78 0. 1.0000 0. -1 -3 16 53.86 5.35 0. 1.0000 0. 1 -3 -16 28.28 5.86 0. 1.0000 0. 1 3 -16 59.52 5.58 0. 1.0000 0. 1 3 -16 49.04 6.84 0. 1.0000 0. -1 3 16 27.90 9.58 0. 1.0000 0. -1 3 16 57.19 5.21 0. 1.0000 0. 6 -2 -17 11.96 4.22 0. 1.0000 0. -6 2 17 2.56 6.93 0. 1.0000 0. 6 2 -17 2.30 5.23 0. 1.0000 0. -4 -2 17 39.36 10.18 0. 1.0000 0. 4 -2 -17 34.59 4.91 0. 1.0000 0. -4 -2 17 45.03 5.40 0. 1.0000 0. 4 -2 -17 46.41 5.12 0. 1.0000 0. 4 2 -17 39.16 5.31 0. 1.0000 0. 4 2 -17 41.08 5.75 0. 1.0000 0. -4 2 17 49.53 6.05 0. 1.0000 0. -4 2 17 27.02 7.71 0. 1.0000 0. -3 -2 17 87.52 11.50 0. 1.0000 0. -3 -2 17 104.10 6.70 0. 1.0000 0. 3 -2 -17 105.13 7.56 0. 1.0000 0. 3 -2 -17 86.18 6.68 0. 1.0000 0. 3 2 -17 91.06 7.52 0. 1.0000 0. -3 2 17 89.16 12.42 0. 1.0000 0. -3 2 17 89.42 6.96 0. 1.0000 0. 3 2 -17 105.53 7.46 0. 1.0000 0. 2 -2 -17 24.27 4.90 0. 1.0000 0. -2 -2 17 38.94 4.76 0. 1.0000 0. -2 -2 17 24.76 9.02 0. 1.0000 0. 2 -2 -17 28.74 4.14 0. 1.0000 0. -2 2 17 26.85 9.72 0. 1.0000 0. 2 2 -17 40.61 6.03 0. 1.0000 0. 2 2 -17 25.61 4.57 0. 1.0000 0. -2 2 17 31.28 4.59 0. 1.0000 0. -1 -2 17 -3.35 10.64 0. 1.0000 0. 1 -2 -17 -0.13 3.48 0. 1.0000 0. -1 2 17 -3.92 6.83 0. 1.0000 0. 1 2 -17 -3.29 5.60 0. 1.0000 0. 1 2 -17 0.16 4.24 0. 1.0000 0. -1 -2 -17 58.10 8.07 0. 1.0000 0. 1 -2 17 57.62 5.37 0. 1.0000 0. -1 2 -17 70.94 7.96 0. 1.0000 0. 1 2 17 56.24 4.69 0. 1.0000 0. 6 -2 -18 79.29 6.65 0. 1.0000 0. -6 2 18 74.26 10.12 0. 1.0000 0. 5 -2 -18 0.17 3.71 0. 1.0000 0. 5 -2 -18 0.15 4.43 0. 1.0000 0. -5 2 18 -5.27 7.29 0. 1.0000 0. 5 2 -18 -1.82 4.28 0. 1.0000 0. -5 2 18 -1.92 5.68 0. 1.0000 0. 4 -2 -18 2.65 3.67 0. 1.0000 0. 4 -2 -18 -1.47 4.02 0. 1.0000 0. 4 2 -18 4.59 4.43 0. 1.0000 0. -4 2 18 0.30 7.27 0. 1.0000 0. -4 2 18 -0.35 5.31 0. 1.0000 0. 3 -2 -18 0.56 4.27 0. 1.0000 0. 3 -2 -18 3.01 3.69 0. 1.0000 0. 3 2 -18 0.15 3.87 0. 1.0000 0. -3 2 18 -3.39 4.83 0. 1.0000 0. -3 2 18 -0.33 7.61 0. 1.0000 0. 2 -2 -18 1.16 4.21 0. 1.0000 0. 2 -2 -18 2.13 3.63 0. 1.0000 0. -2 2 18 4.14 7.38 0. 1.0000 0. -2 2 18 -0.69 4.02 0. 1.0000 0. 2 2 -18 1.88 4.25 0. 1.0000 0. 1 -2 -18 8.29 4.95 0. 1.0000 0. 1 -2 -18 1.37 3.78 0. 1.0000 0. -1 2 18 0.43 8.18 0. 1.0000 0. 1 2 -18 7.79 4.65 0. 1.0000 0. -1 2 18 7.15 4.21 0. 1.0000 0. 0 -2 -18 27.58 4.45 0. 1.0000 0. 0 -2 -18 23.83 6.94 0. 1.0000 0. 0 2 18 34.56 4.50 0. 1.0000 0. -512 # 2168 reflections output ; loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 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 S1 S 0.4418(5) 0.2956(5) 0.33843(12) 0.0378 1.0000 Uani D U . . . . N2 N 0.3149(8) 0.1856(13) 0.2401(3) 0.0366 1.0000 Uani D U . . . . S3 S 0.1446(4) 0.0651(4) 0.24927(9) 0.0328 1.0000 Uani D U . . . . C4 C 0.1778(8) 0.1243(13) 0.3715(3) 0.0264 1.0000 Uani D U . . . . C5 C 0.3279(8) 0.2443(13) 0.4160(3) 0.0282 1.0000 Uani D U . . . . N6 N 0.3532(8) 0.2963(12) 0.5087(3) 0.0293 1.0000 Uani D U . . . . S7 S 0.1945(4) 0.1835(4) 0.53681(11) 0.0289 1.0000 Uani D U . . . . N8 N 0.0908(8) 0.0747(12) 0.4300(3) 0.0278 1.0000 Uani D U . . . . 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 S1 0.041(6) 0.0543(9) 0.0224(10) 0.0103(5) 0.016(2) 0.0085(12) N2 0.052(6) 0.045(2) 0.0184(19) 0.0038(17) 0.019(3) 0.003(4) S3 0.044(6) 0.0429(8) 0.0127(8) 0.0020(4) 0.0101(17) 0.0058(10) C4 0.034(7) 0.034(2) 0.0123(17) 0.0020(15) 0.008(3) 0.003(4) C5 0.033(7) 0.037(2) 0.0165(19) 0.0016(16) 0.009(3) 0.003(4) N6 0.032(7) 0.040(2) 0.017(2) 0.0004(15) 0.008(3) 0.001(3) S7 0.036(6) 0.0388(8) 0.0138(9) -0.0005(4) 0.0097(18) -0.0021(9) N8 0.033(7) 0.0354(19) 0.0168(18) 0.0011(14) 0.009(2) 0.000(3) 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 0.0006 0.0007 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' N 0.0016 0.0014 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' S 0.0630 0.0572 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 '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 N2 . S1 . C5 . 97.6(3) yes S1 . N2 . S3 . 117.6(3) yes N2 . S3 . C4 . 97.3(3) yes S3 . C4 . C5 . 113.5(4) yes S3 . C4 . N8 . 131.9(4) yes C5 . C4 . N8 . 114.5(4) yes C4 . C5 . S1 . 113.9(3) yes C4 . C5 . N6 . 113.9(4) yes S1 . C5 . N6 . 132.2(5) yes C5 . N6 . S7 . 106.3(4) yes N6 . S7 . N8 . 98.9(3) yes C4 . N8 . S7 . 106.3(4) yes 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 S1 . N2 . 1.647(6) yes S1 . C5 . 1.729(5) yes N2 . S3 . 1.654(7) yes S3 . C4 . 1.740(4) yes C4 . C5 . 1.428(7) yes C4 . N8 . 1.317(6) yes C5 . N6 . 1.323(5) yes N6 . S7 . 1.654(7) yes S7 . N8 . 1.649(5) yes loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details -5 2 8 x . -3 1 4 x . -6 2 14 x . 3 3 4 x . 2 2 12 x . 3 4 5 x . -6 3 11 x . 3 3 6 x .