# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2BENACID_publ _database_code_depnum_ccdc_archive 'CCDC 894243' #TrackingRef '1.cif' _pd_block_id 2012-07-17T15:44|2BENACID|| _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2012-07-17T15:44 _audit_update_record ; 2012-07-17T15:44 Initial CIF as created by GSAS2CIF ; #============================================================================= # this information describes the project, paper etc. for the CIF # # Acta Cryst. Section C papers and editorial correspondence is generated # # from the information in this section # # # # (from) CIF submission form for Rietveld refinements (Acta Cryst. C) # # Version 14 December 1998 # #============================================================================= # #============================================================================= # 5. OVERALL REFINEMENT & COMPUTING DETAILS _refine_special_details ; ? ; _pd_proc_ls_special_details ; ? ; # The following items are used to identify the programs used. _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method Nil _refine_ls_extinction_coef ? _refine_ls_number_constraints ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? #============================================================================== # 6. SAMPLE PREPARATION DATA # (In the unusual case where multiple samples are used in a single # Rietveld study, this information should be moved into the phase # blocks) # The following three fields describe the preparation of the material. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _pd_char_colour white # use ICDD colour descriptions _refine_ls_shift/su_max 0.03 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 84 _refine_ls_goodness_of_fit_all 1.64 _refine_ls_number_restraints 62 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ;from E:/Basab/powder/benzyloxybenzoicacid/2- benzyloxybenzoicacid/g ; _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from E:/Basab/powder/benzyloxybenzoicacid/2-benzyloxybenzoicacid/g' _cell_length_a 22.1797(13) _cell_length_b 7.7545(4) _cell_length_c 6.7479(4) _cell_angle_alpha 90.0 _cell_angle_beta 93.2506(32) _cell_angle_gamma 90.0 _cell_volume 1158.7(2) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x+1/2,+y+1/2,-z+1/2 -1 -x,-y,-z -2 +x+1/2,-y+1/2,+z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity C C2 0.33182(4) 0.09223(30) 0.5878(4) 1.0 Uiso 0.04 4 C C3 0.31109(11) 0.19951(32) 0.73447(20) 1.0 Uiso 0.04 4 C C4 0.25509(12) 0.27888(25) 0.71093(31) 1.0 Uiso 0.04 4 C C5 0.21946(4) 0.25006(28) 0.5390(4) 1.0 Uiso 0.04 4 C C6 0.24107(11) 0.14250(26) 0.39432(29) 1.0 Uiso 0.04 4 C C1 0.29689(12) 0.06196(23) 0.41431(30) 1.0 Uiso 0.04 4 C C7 0.20212(11) 0.11209(6) 0.21002(15) 1.0 Uiso 0.04 4 C C8 0.10094(9) 0.17497(25) 0.08438(31) 1.0 Uiso 0.04 4 C C9 0.04491(11) 0.25462(23) 0.09738(33) 1.0 Uiso 0.04 4 C C13 0.11500(5) 0.08685(24) -0.0858(4) 1.0 Uiso 0.04 4 C C10 0.00223(5) 0.24506(25) -0.0615(4) 1.0 Uiso 0.04 4 C C11 0.01612(9) 0.15674(31) -0.23198(28) 1.0 Uiso 0.04 4 C C12 0.07220(12) 0.07826(25) -0.24353(20) 1.0 Uiso 0.04 4 C C14 0.02939(14) 0.3499(4) 0.2784(4) 1.0 Uiso 0.04 4 O O1 0.14341(10) 0.18218(31) 0.2388(4) 1.0 Uiso 0.04 4 O O2 -0.02372(14) 0.3666(6) 0.3136(7) 1.0 Uiso 0.04 4 O O3 0.07236(13) 0.4351(5) 0.3904(4) 1.0 Uiso 0.04 4 H H2 0.37024 0.04521 0.60824 1.0 Uiso 0.06 4 H H3 0.33404 0.22213 0.85122 1.0 Uiso 0.06 4 H H4 0.23927 0.34933 0.80669 1.0 Uiso 0.06 4 H H5 0.18103 0.29632 0.51541 1.0 Uiso 0.06 4 H H1 0.31214 -0.0073 0.31636 1.0 Uiso 0.06 4 H H7B 0.19879 -0.00913 0.17574 1.0 Uiso 0.06 4 H H7A 0.21863 0.1627 0.09335 1.0 Uiso 0.06 4 H H13 0.15183 0.0326 -0.10122 1.0 Uiso 0.06 4 H H10 -0.03464 0.29896 -0.04561 1.0 Uiso 0.06 4 H H11 -0.01371 0.1541 -0.33448 1.0 Uiso 0.06 4 H H12 0.07892 0.021 -0.36134 1.0 Uiso 0.06 4 H H3A 0.05752 0.48333 0.48417 1.0 Uiso 0.06 4 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C14 H12 O3' _chemical_formula_weight 228.25 _cell_formula_units_Z 4 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2 C3 1.3909(15) . 1_555 N C2 C1 1.3868(15) . 1_555 N C2 H2 0.92994 . 1_555 N C3 C2 1.3909(15) . 1_555 N C3 C4 1.3873(15) . 1_555 N C3 H3 0.92999 . 1_555 N C4 C3 1.3873(15) . 1_555 N C4 C5 1.3843(15) . 1_555 N C4 H4 0.92995 . 1_555 N C5 C4 1.3843(15) . 1_555 N C5 C6 1.3898(15) . 1_555 N C5 H5 0.93005 . 1_555 N C6 C5 1.3898(15) . 1_555 N C6 C1 1.3864(14) . 1_555 N C6 C7 1.4922(15) . 1_555 N C1 C2 1.3868(15) . 1_555 N C1 C6 1.3864(14) . 1_555 N C1 H1 0.93007 . 1_555 N C7 C6 1.4922(15) . 1_555 N C7 O1 1.4344(15) . 1_555 N C7 H7B 0.96986 . 1_555 N C7 H7A 0.96985 . 1_555 N C8 C9 1.3949(15) . 1_555 N C8 C13 1.3870(15) . 1_555 N C8 O1 1.3655(15) . 1_555 N C9 C8 1.3949(15) . 1_555 N C9 C10 1.3916(15) . 1_555 N C9 C14 1.4843(15) . 1_555 N C13 C8 1.3870(15) . 1_555 N C13 C12 1.3868(15) . 1_555 N C13 H13 0.93000 . 1_555 N C10 C9 1.3916(15) . 1_555 N C10 C11 1.3882(15) . 1_555 N C10 H10 0.92999 . 1_555 N C11 C10 1.3882(15) . 1_555 N C11 C12 1.3908(15) . 1_555 N C11 H11 0.92997 . 1_555 N C12 C13 1.3868(15) . 1_555 N C12 C11 1.3908(15) . 1_555 N C12 H12 0.92998 . 1_555 N C14 C9 1.4843(15) . 1_555 N C14 O2 1.2217(16) . 1_555 N C14 O3 1.3545(16) . 1_555 N O1 C7 1.4344(15) . 1_555 N O1 C8 1.3655(15) . 1_555 N O2 C14 1.2217(16) . 1_555 N O3 C14 1.3545(16) . 1_555 N O3 H3A 0.82003 . 1_555 N loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C2 C1 120.70(5) 1_555 . 1_555 N C3 C2 H2 117.78 1_555 . 1_555 N C1 C2 H2 121.49 1_555 . 1_555 N C2 C3 C4 120.92(5) 1_555 . 1_555 N C2 C3 H3 121.90 1_555 . 1_555 N C4 C3 H3 117.18 1_555 . 1_555 N C3 C4 C5 119.29(5) 1_555 . 1_555 N C3 C4 H4 123.48 1_555 . 1_555 N C5 C4 H4 117.21 1_555 . 1_555 N C4 C5 C6 118.84(9) 1_555 . 1_555 N C4 C5 H5 123.72 1_555 . 1_555 N C6 C5 H5 117.41 1_555 . 1_555 N C5 C6 C1 122.93(12) 1_555 . 1_555 N C5 C6 C7 118.29(20) 1_555 . 1_555 N C1 C6 C7 118.78(21) 1_555 . 1_555 N C2 C1 C6 117.32(9) 1_555 . 1_555 N C2 C1 H1 119.30 1_555 . 1_555 N C6 C1 H1 123.35 1_555 . 1_555 N C6 C7 O1 108.33(13) 1_555 . 1_555 N C6 C7 H7B 112.63 1_555 . 1_555 N C6 C7 H7A 112.66 1_555 . 1_555 N O1 C7 H7B 110.00 1_555 . 1_555 N O1 C7 H7A 110.12 1_555 . 1_555 N C9 C8 C13 120.87(14) 1_555 . 1_555 N C9 C8 O1 120.82(18) 1_555 . 1_555 N C13 C8 O1 118.31(18) 1_555 . 1_555 N C8 C9 C10 119.84(14) 1_555 . 1_555 N C8 C9 C14 121.41(17) 1_555 . 1_555 N C10 C9 C14 118.76(17) 1_555 . 1_555 N C8 C13 C12 118.87(9) 1_555 . 1_555 N C8 C13 H13 123.75 1_555 . 1_555 N C12 C13 H13 117.38 1_555 . 1_555 N C9 C10 C11 119.44(10) 1_555 . 1_555 N C9 C10 H10 116.83 1_555 . 1_555 N C11 C10 H10 123.74 1_555 . 1_555 N C10 C11 C12 120.23(5) 1_555 . 1_555 N C10 C11 H11 116.43 1_555 . 1_555 N C12 C11 H11 123.34 1_555 . 1_555 N C13 C12 C11 120.75(5) 1_555 . 1_555 N C13 C12 H12 122.88 1_555 . 1_555 N C11 C12 H12 116.37 1_555 . 1_555 N C9 C14 O2 118.95(20) 1_555 . 1_555 N C9 C14 O3 120.87(15) 1_555 . 1_555 N O2 C14 O3 119.69(19) 1_555 . 1_555 N C7 O1 C8 118.27(18) 1_555 . 1_555 N C14 O3 H3A 110.66 1_555 . 1_555 N # Powder diffraction data for histogram 1 #============================================================================== # 9. INSTRUMENT CHARACTERIZATION _exptl_special_details ; ? ; # if regions of the data are excluded, the reason(s) are supplied here: _pd_proc_info_excluded_regions ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 293 _diffrn_source X-ray _diffrn_source_target CuK/a _diffrn_source_type 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker D8 Advance powder diffractometer' _diffrn_detector 'linear position-sensitive Lynxeye detector' _diffrn_detector_type 'Bruker AXS' # make or model of detector _pd_meas_scan_method Step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection EVA _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction ? # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator ? # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 10. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode reflection # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 56.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C O 12.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C H 48.0 0.000 0.000 0.49300 10.5109 0.32291 26.1257 0.14019 3.14236 0.04081 57.7997 0.00304 International_Tables_Vol_C _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 0.5 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type ? _pd_proc_ls_prof_R_factor 0.0381 _pd_proc_ls_prof_wR_factor 0.0520 _pd_proc_ls_prof_wR_expected 0.0346 _refine_ls_R_Fsqd_factor 0.07368 _pd_proc_ls_background_function ; GSAS Background function number 1 with 20 terms. Shifted Chebyshev function of 1st kind 1: 623.406 2: -743.315 3: 427.836 4: -248.145 5: 175.039 6: -145.966 7: 122.721 8: -98.3531 9: 85.1069 10: -64.3923 11: 47.3046 12: -35.0670 13: 25.8357 14: -13.4661 15: 2.18439 16: 11.7962 17: -14.8226 18: 6.47263 19: -0.909734 20: -3.64108 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 No correction is applied. ; _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_correction_T_max 1.00000 # Extinction correction _gsas_exptl_extinct_corr_T_min 1.00000 _gsas_exptl_extinct_corr_T_max 1.00000 _pd_proc_ls_profile_function ; CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 241.202 #2(GV) = -2.000 #3(GW) = 48.668 #4(LX) = 1.000 #5(LY) = 23.414 #6(trns) = 0.000 #7(asym) = -1.3506 #8(shft) = 7.3973 #9(GP) = 0.000 #10(stec)= 9.98 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = -0.001 #17(L13) = -0.002 #18(L23) = 0.008 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.01000 _pd_proc_info_datetime 2012-07-17T15:44:57 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 5.0 _pd_meas_2theta_range_max 100.0018 _pd_meas_2theta_range_inc 0.0199 _pd_proc_2theta_range_min 5.0 _pd_proc_2theta_range_max 100.0018 _pd_proc_2theta_range_inc 0.0199 loop_ _pd_meas_counts_total _pd_proc_ls_weight _pd_proc_intensity_bkg_calc _pd_calc_intensity_total 2999.0 0.0003334 2827.77808 2827.77808 2995.0 0.0003339 2811.42139 2811.42163 2976.0 0.0003360 2795.15576 2795.15527 2939.0 0.0003403 2778.98120 2778.98071 2903.0 0.0003445 2762.89844 2762.89868 2870.0 0.0003484 2746.90796 2746.90820 2832.0 0.000353 2731.00952 2731.01001 2799.0 0.000357 2715.20313 2715.20313 2767.0 0.000361 2699.49023 2699.49097 2735.0 0.000366 2683.86987 2683.86963 2707.0 0.000369 2668.34229 2668.34302 2676.0 0.000374 2652.90820 2652.90820 2649.0 0.000378 2637.56738 2637.56738 2627.0 0.000381 2622.32031 2622.32056 2602.0 0.000384 2607.16650 2607.16724 2577.0 0.000388 2592.10718 2592.10718 2560.0 0.000391 2577.14160 2577.14209 2539.0 0.000394 2562.27002 2562.27002 2518.0 0.000397 2547.49243 2547.49243 2499.0 0.000400 2532.81030 2532.81030 2479.0 0.000403 2518.22144 2518.22168 2464.0 0.000406 2503.72705 2503.72778 2444.0 0.000409 2489.32788 2489.32886 2427.0 0.000412 2475.02319 2475.02295 2412.0 0.000415 2460.81299 2460.81323 2396.0 0.000417 2446.69775 2446.69775 2377.0 0.000421 2432.67603 2432.67700 2365.0 0.000423 2418.75024 2418.75098 2349.0 0.000426 2404.91919 2404.91968 2334.0 0.000428 2391.18237 2391.18286 2323.0 0.000430 2377.54102 2377.54126 2307.0 0.000433 2363.99438 2363.99463 2294.0 0.000436 2350.54150 2350.54199 2283.0 0.000438 2337.18384 2337.18408 2264.0 0.000442 2323.92090 2323.92114 2252.0 0.000444 2310.75195 2310.75269 2237.0 0.000447 2297.67749 2297.67773 2224.0 0.000450 2284.69849 2284.69897 2211.0 0.000452 2271.81274 2271.81323 2197.0 0.000455 2259.02197 2259.02222 2184.0 0.000458 2246.32446 2246.32544 2173.0 0.000460 2233.72192 2233.72241 2159.0 0.000463 2221.21289 2221.21362 2147.0 0.000466 2208.79712 2208.79736 2136.0 0.000468 2196.47607 2196.47607 2123.0 0.000471 2184.24780 2184.24805 2113.0 0.000473 2172.11279 2172.11353 2101.0 0.000476 2160.07178 2160.07202 2091.0 0.000478 2148.12378 2148.12402 2081.0 0.000481 2136.26782 2136.26855 2069.0 0.000483 2124.50562 2124.50586 2060.0 0.000485 2112.83496 2112.83521 2048.0 0.000488 2101.25757 2101.25781 2039.0 0.000490 2089.77222 2089.77197 2028.0 0.000493 2078.37842 2078.37817 2020.0 0.000495 2067.07593 2067.07617 2011.0 0.000497 2055.86670 2055.86670 2000.0 0.000500 2044.74707 2044.74768 1992.0 0.000502 2033.71924 2033.71973 1985.0 0.000504 2022.78247 2022.78284 1975.0 0.000506 2011.93604 2011.93591 1968.0 0.000508 2001.18066 2001.18103 1959.0 0.000510 1990.51501 1990.51501 1952.0 0.000512 1979.93835 1979.93811 1943.0 0.000515 1969.45227 1969.45227 1936.0 0.000517 1959.05554 1959.05566 1928.0 0.000519 1948.74756 1948.74756 1918.0 0.000521 1938.52893 1938.52881 1912.0 0.000523 1928.39819 1928.39844 1905.0 0.000525 1918.35632 1918.35657 1895.0 0.000528 1908.40222 1908.40234 1888.0 0.000530 1898.53577 1898.53564 1882.0 0.000531 1888.75635 1888.75647 1875.0 0.000533 1879.06458 1879.06458 1867.0 0.000536 1869.45898 1869.45886 1860.0 0.000538 1859.94006 1859.94019 1853.0 0.000540 1850.50696 1850.50696 1847.0 0.000541 1841.16028 1841.15991 1840.0 0.000543 1831.89832 1831.89807 1830.0 0.000546 1822.72229 1822.72205 1824.0 0.000548 1813.63025 1813.63025 1818.0 0.000550 1804.62317 1804.62305 1809.0 0.000553 1795.69934 1795.69922 1803.0 0.000555 1786.85974 1786.85986 1798.0 0.000556 1778.10400 1778.10388 1792.0 0.000558 1769.43079 1769.43054 1786.0 0.000560 1760.84021 1760.84009 1781.0 0.000561 1752.33240 1752.33203 1773.0 0.000564 1743.90588 1743.90552 1766.0 0.000566 1735.56079 1735.56030 1758.0 0.000569 1727.29749 1727.29736 1750.0 0.000571 1719.11450 1719.11426 1744.0 0.000573 1711.01245 1711.01208 1738.0 0.000575 1702.99023 1702.98999 1729.0 0.000578 1695.04773 1695.04688 1725.0 0.000580 1687.18420 1687.18359 1718.0 0.000582 1679.39929 1679.39893 1713.0 0.000584 1671.69324 1671.69275 1708.0 0.000585 1664.06543 1664.06482 1702.0 0.000588 1656.51477 1656.51428 1696.0 0.000590 1649.04150 1649.04089 1692.0 0.000591 1641.64539 1641.64478 1685.0 0.000593 1634.32495 1634.32446 1677.0 0.000596 1627.08130 1627.08057 1673.0 0.000598 1619.91370 1619.91296 1666.0 0.000600 1612.81982 1612.81897 1659.0 0.000603 1605.80188 1605.80127 1654.0 0.000605 1598.85767 1598.85706 1650.0 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189.0 0.00529 166.90413 198.46051 189.0 0.00529 166.90306 197.52092 189.0 0.00529 166.90115 196.59853 188.0 0.00532 166.89841 195.72940 189.0 0.00529 166.89485 194.87260 189.0 0.00529 166.89044 194.06163 188.0 0.00532 166.88510 193.30164 188.0 0.00532 166.87891 192.59648 189.0 0.00529 166.87181 191.95924 188.0 0.00532 166.86374 191.36899 188.0 0.00532 166.85478 190.84227 188.0 0.00532 166.84488 190.36301 188.0 0.00532 166.83411 189.93576 187.0 0.00535 166.82231 189.55412 189.0 0.00529 166.80959 189.21436 189.0 0.00529 166.79584 188.91080 188.0 0.00532 166.78116 188.63766 188.0 0.00532 166.76544 188.38907 188.0 0.00532 166.74873 188.15916 187.0 0.00535 166.73100 187.95715 187.0 0.00535 166.71225 187.75040 187.0 0.00535 166.69244 187.54662 187.0 0.00535 166.67155 187.35118 187.0 0.00535 166.64967 187.16115 186.0 0.00538 166.62669 186.89848 187.0 0.00535 166.60260 186.72917 186.0 0.00538 166.57747 186.57608 186.0 0.00538 166.55121 186.44481 185.0 0.00541 166.52388 186.34209 185.0 0.00541 166.49544 186.27069 185.0 0.00541 166.46587 186.23755 185.0 0.00541 166.43517 186.27690 185.0 0.00541 166.40332 186.32506 185.0 0.00541 166.37036 186.41383 185.0 0.00541 166.33623 186.54353 185.0 0.00541 166.30090 186.71111 185.0 0.00541 166.26445 186.91237 186.0 0.00538 166.22685 187.12576 186.0 0.00538 166.18806 187.37624 187.0 0.00535 166.14809 187.64363 187.0 0.00535 166.10689 187.90869 187.0 0.00535 166.06451 188.16515 187.0 0.00535 166.02095 188.40158 187.0 0.00535 165.97614 188.52107 187.0 0.00535 165.93021 188.68524 186.0 0.00538 165.88300 188.79733 186.0 0.00538 165.83459 188.85547 187.0 0.00535 165.78497 188.84277 186.0 0.00538 165.73413 188.79510 186.0 0.00538 165.68202 188.64745 186.0 0.00538 165.62871 188.43515 186.0 0.00538 165.57416 188.16350 186.0 0.00538 165.51834 187.83978 186.0 0.00538 165.46132 187.47243 186.0 0.00538 165.40305 187.07881 186.0 0.00538 165.34352 186.65427 186.0 0.00538 165.28282 186.21666 186.0 0.00538 165.22081 185.77666 186.0 0.00538 165.15750 185.34517 186.0 0.00538 165.09303 184.93709 186.0 0.00538 165.02736 184.55173 186.0 0.00538 164.96037 184.20859 186.0 0.00538 164.89212 183.90372 186.0 0.00538 164.82263 183.66777 186.0 0.00538 164.75195 183.47330 186.0 0.00538 164.67999 183.34175 187.0 0.00535 164.60686 183.29477 187.0 0.00535 164.53242 183.31702 188.0 0.00532 164.45677 183.44962 189.0 0.00529 164.37996 183.61430 190.0 0.00526 164.30186 183.81374 191.0 0.00524 164.22255 184.09929 193.0 0.00518 164.14204 184.44785 193.0 0.00518 164.06036 184.85481 195.0 0.00513 163.97737 185.32780 195.0 0.00513 163.89323 185.83401 196.0 0.00510 163.80791 186.40251 196.0 0.00510 163.72144 186.98062 196.0 0.00510 163.63376 187.59018 197.0 0.00508 163.54491 188.21307 196.0 0.00510 163.45491 188.84885 195.0 0.00513 163.36372 189.49190 195.0 0.00513 163.27142 190.11363 195.0 0.00513 163.17801 190.75356 194.0 0.00515 163.08342 191.39125 194.0 0.00515 162.98778 192.00204 195.0 0.00513 162.89096 192.58974 196.0 0.00510 162.79306 193.16531 197.0 0.00508 162.69406 193.68968 197.0 0.00508 162.59409 194.13658 198.0 0.00505 162.49300 194.51965 198.0 0.00505 162.39082 194.86723 197.0 0.00508 162.28769 195.08743 196.0 0.00510 162.18349 195.21863 195.0 0.00513 162.07822 195.30919 194.0 0.00515 161.97211 195.26071 193.0 0.00518 161.86493 195.14452 191.0 0.00524 161.75681 194.92998 191.0 0.00524 161.64781 194.64165 190.0 0.00526 161.53777 194.28601 190.0 0.00526 161.42683 193.87451 189.0 0.00529 161.31508 193.40927 189.0 0.00529 161.20245 192.86848 189.0 0.00529 161.08888 192.29642 188.0 0.00532 160.97464 191.67838 188.0 0.00532 160.85939 191.02753 188.0 0.00532 160.74339 190.32555 187.0 0.00535 160.62668 189.58685 186.0 0.00538 160.50920 188.81578 185.0 0.00541 160.39098 188.01819 184.0 0.00543 160.27196 187.19672 184.0 0.00543 160.15233 186.35957 183.0 0.00546 160.03204 185.51155 182.0 0.00549 159.91115 184.66049 182.0 0.00549 159.78960 183.80682 182.0 0.00549 159.66743 182.94925 182.0 0.00549 159.54471 182.10954 181.0 0.00552 159.42133 181.25934 182.0 0.00549 159.29759 180.44841 181.0 0.00552 159.17329 179.65575 181.0 0.00552 159.04857 178.88654 181.0 0.00552 158.92340 178.14436 180.0 0.00556 158.79773 177.48050 180.0 0.00556 158.67172 176.80296 179.0 0.00559 158.54543 176.17319 179.0 0.00559 158.41872 175.57736 178.0 0.00562 158.29178 175.01443 179.0 0.00559 158.16458 174.49112 178.0 0.00562 158.03712 174.01360 178.0 0.00562 157.90941 173.56918 178.0 0.00562 157.78159 173.14249 177.0 0.00565 157.65363 172.77190 177.0 0.00565 157.52556 172.44891 177.0 0.00565 157.39740 172.14262 176.0 0.00568 157.26921 171.86436 177.0 0.00565 157.14102 171.61124 177.0 0.00565 157.01280 171.38156 178.0 0.00562 156.88475 171.20953 177.0 0.00565 156.75677 170.84924 178.0 0.00562 156.62885 170.67029 177.0 0.00565 156.50124 170.50240 177.0 0.00565 156.37369 170.34251 177.0 0.00565 156.24640 170.19624 177.0 0.00565 156.11949 170.05766 177.0 0.00565 155.99281 169.91135 176.0 0.00568 155.86656 169.76678 176.0 0.00568 155.74062 169.62480 176.0 0.00568 155.61522 169.48558 175.0 0.00571 155.49023 169.35153 175.0 0.00571 155.36581 169.22539 175.0 0.00571 155.24191 169.11064 175.0 0.00571 155.11861 169.01128 175.0 0.00571 154.99599 168.93890 175.0 0.00571 154.87396 168.88452 175.0 0.00571 154.75272 168.85855 175.0 0.00571 154.63222 168.86722 175.0 0.00571 154.51257 168.90880 174.0 0.00575 154.39372 168.98920 175.0 0.00571 154.27571 169.07909 176.0 0.00568 154.15877 169.25113 175.0 0.00571 154.04272 169.46036 175.0 0.00571 153.92772 169.72232 175.0 0.00571 153.81380 170.04401 175.0 0.00571 153.70094 170.38370 175.0 0.00571 153.58931 170.76848 175.0 0.00571 153.47879 171.18570 175.0 0.00571 153.36963 171.63634 176.0 0.00568 153.26167 172.11623 176.0 0.00568 153.15508 172.62061 176.0 0.00568 153.04990 173.14436 176.0 0.00568 152.94611 173.68286 176.0 0.00568 152.84383 174.19765 176.0 0.00568 152.74303 174.74057 176.0 0.00568 152.64381 175.27580 175.0 0.00571 152.54617 175.79745 175.0 0.00571 152.45030 176.29356 175.0 0.00571 152.35599 176.75813 176.0 0.00568 152.26353 177.18224 175.0 0.00571 152.17291 177.56151 176.0 0.00568 152.08403 177.88225 176.0 0.00568 151.99704 178.15024 176.0 0.00568 151.91200 178.35060 176.0 0.00568 151.82899 178.49727 176.0 0.00568 151.74799 178.58549 176.0 0.00568 151.66908 178.61844 175.0 0.00571 151.59230 178.60303 175.0 0.00571 151.51765 178.54958 176.0 0.00568 151.44524 178.46294 176.0 0.00568 151.37509 178.35490 175.0 0.00571 151.30721 178.23517 176.0 0.00568 151.24171 178.11276 176.0 0.00568 151.17857 177.99591 176.0 0.00568 151.11794 177.89166 176.0 0.00568 151.05974 177.81082 176.0 0.00568 151.00406 177.74870 176.0 0.00568 150.95096 177.65703 176.0 0.00568 150.90053 177.65269 175.0 0.00571 150.85271 177.68001 175.0 0.00571 150.80759 177.74710 176.0 0.00568 150.76517 177.84076 175.0 0.00571 150.72559 177.96986 176.0 0.00568 150.68878 178.12192 176.0 0.00568 150.65486 178.31374 176.0 0.00568 150.62383 178.54173 177.0 0.00565 150.59572 178.79237 177.0 0.00565 150.57059 179.07193 177.0 0.00565 150.54849 179.36261 177.0 0.00565 150.52942 179.68266 177.0 0.00565 150.51347 180.01958 178.0 0.00562 150.50064 180.37314 178.0 0.00562 150.49095 180.76070 178.0 0.00562 150.48444 181.12807 178.0 0.00562 150.48117 181.49866 178.0 0.00562 150.48114 181.86780 178.0 0.00562 150.48438 182.23135 178.0 0.00562 150.49091 182.58490 178.0 0.00562 150.50081 182.92325 179.0 0.00559 150.51405 183.20520 178.0 0.00562 150.53070 183.49567 179.0 0.00559 150.55078 183.75342 179.0 0.00559 150.57422 183.97057 180.0 0.00556 150.60118 184.14265 180.0 0.00556 150.63159 184.26472 179.0 0.00559 150.66551 184.33380 179.0 0.00559 150.70294 184.35355 179.0 0.00559 150.74391 184.31715 178.0 0.00562 150.78838 184.21980 178.0 0.00562 150.83638 184.06985 178.0 0.00562 150.88809 183.87082 178.0 0.00562 150.94325 183.63768 178.0 0.00562 151.00200 183.35425 179.0 0.00559 151.06436 183.03604 179.0 0.00559 151.13033 182.68774 180.0 0.00556 151.19981 182.31679 178.0 0.00562 151.27293 181.92230 179.0 0.00559 151.34969 181.50958 178.0 0.00562 151.42995 181.08383 177.0 0.00565 151.51379 180.64917 177.0 0.00565 151.60121 180.15913 176.0 0.00568 151.69218 179.59880 177.0 0.00565 151.78668 179.16544 176.0 0.00568 151.88466 178.74806 176.0 0.00568 151.98621 178.33623 176.0 0.00568 152.09116 177.94061 175.0 0.00571 152.19958 177.56329 175.0 0.00571 152.31142 177.20613 175.0 0.00571 152.42667 176.86916 175.0 0.00571 152.54527 176.57066 175.0 0.00571 152.66721 176.27701 175.0 0.00571 152.79236 175.99129 175.0 0.00571 152.92079 175.72502 175.0 0.00571 153.05241 175.45763 175.0 0.00571 153.18716 175.19365 175.0 0.00571 153.32503 174.89755 174.0 0.00575 153.46588 174.63333 175.0 0.00571 153.60963 174.36610 174.0 0.00575 153.75641 174.09558 174.0 0.00575 153.90599 173.82294 174.0 0.00575 154.05826 173.54765 174.0 0.00575 154.21333 173.27235 174.0 0.00575 154.37102 173.00157 174.0 0.00575 154.53110 172.73737 173.0 0.00578 154.69365 172.47711 173.0 0.00578 154.85855 172.22876 174.0 0.00575 155.02580 171.99113 173.0 0.00578 155.19499 171.77554 174.0 0.00575 155.36630 171.57005 173.0 0.00578 155.53960 171.38332 173.0 0.00578 155.71461 171.21783 173.0 0.00578 155.89130 171.09659 173.0 0.00578 156.06961 170.97185 173.0 0.00578 156.24939 170.86810 173.0 0.00578 156.43037 170.78522 174.0 0.00575 156.61250 170.71523 174.0 0.00575 156.79562 170.67441 174.0 0.00575 156.97963 170.64008 173.0 0.00578 157.16437 170.63466 174.0 0.00575 157.34958 170.64688 173.0 0.00578 157.53508 170.67505 173.0 0.00578 157.72078 170.71875 174.0 0.00575 157.90649 170.77591 174.0 0.00575 158.09189 170.84534 174.0 0.00575 158.27704 170.92766 174.0 0.00575 158.46149 171.01805 174.0 0.00575 158.64514 171.11508 174.0 0.00575 158.82771 171.21677 174.0 0.00575 159.00911 171.32085 174.0 0.00575 159.18904 171.42590 174.0 0.00575 159.36708 171.52737 174.0 0.00575 159.54329 171.62384 174.0 0.00575 159.71712 171.72557 174.0 0.00575 159.88850 171.80490 174.0 0.00575 160.05721 171.87265 173.0 0.00578 160.22275 171.92741 173.0 0.00578 160.38510 171.96846 173.0 0.00578 160.54373 171.97293 173.0 0.00578 160.69846 171.98650 173.0 0.00578 160.84883 171.98616 172.0 0.00581 160.99474 171.98697 173.0 0.00578 161.13571 171.98181 172.0 0.00581 161.27145 171.95682 172.0 0.00581 161.40164 171.92639 172.0 0.00581 161.52582 171.88272 172.0 0.00581 161.64362 171.85567 172.0 0.00581 161.75479 171.82623 172.0 0.00581 161.85890 171.81403 171.0 0.00585 161.95551 171.79442 172.0 0.00581 162.04419 171.77184 171.0 0.00585 162.12453 171.76405 171.0 0.00585 162.19614 171.76245 171.0 0.00585 162.25854 171.76714 171.0 0.00585 162.31131 171.77141 171.0 0.00585 162.35397 171.79863 171.0 0.00585 162.38589 171.81911 171.0 0.00585 162.40681 171.84268 171.0 0.00585 162.41621 171.86705 170.0 0.00588 162.41338 171.89072 171.0 0.00585 162.39801 171.91142 171.0 0.00585 162.36940 171.92667 171.0 0.00585 162.32709 171.93367 171.0 0.00585 162.27043 171.92923 171.0 0.00585 162.19888 171.91061 171.0 0.00585 162.11194 171.87358 170.0 0.00588 162.00885 171.81125 171.0 0.00585 161.88902 171.72887 170.0 0.00588 161.75191 171.61929 171.0 0.00585 161.59683 171.47543 170.0 0.00588 161.42305 171.30757 171.0 0.00585 161.23001 171.08209 171.0 0.00585 161.01680 170.85173 171.0 0.00585 160.78282 170.58960 171.0 0.00585 160.52737 170.25021 171.0 0.00585 160.24982 169.92737 171.0 0.00585 159.94914 169.57417 170.0 0.00588 159.62462 169.17136 172.0 . . . _pd_meas_number_of_points 4774 _pd_proc_number_of_points 4774 data_4BENACID_publ _database_code_depnum_ccdc_archive 'CCDC 894244' #TrackingRef '2.cif' _pd_block_id 2012-04-20T15:47|4BENACID|| _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2012-04-20T15:47 _audit_update_record ; 2012-04-20T15:47 Initial CIF as created by GSAS2CIF ; #============================================================================= # this information describes the project, paper etc. for the CIF # # Acta Cryst. Section C papers and editorial correspondence is generated # # from the information in this section # # # # (from) CIF submission form for Rietveld refinements (Acta Cryst. C) # # Version 14 December 1998 # #============================================================================= #============================================================================= # 5. OVERALL REFINEMENT & COMPUTING DETAILS _refine_special_details ; ? ; _pd_proc_ls_special_details ; ? ; # The following items are used to identify the programs used. _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method Nil _refine_ls_extinction_coef ? _refine_ls_number_constraints ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? #============================================================================== # 6. SAMPLE PREPARATION DATA # (In the unusual case where multiple samples are used in a single # Rietveld study, this information should be moved into the phase # blocks) # The following three fields describe the preparation of the material. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _pd_char_colour white # use ICDD colour descriptions _refine_ls_shift/su_max 0.04 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 80 _refine_ls_goodness_of_fit_all 0.90 _refine_ls_number_restraints 61 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common 'from D:/basab/4benzoic_re/gsas/global_1.cif' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from D:/basab/4benzoic_re/gsas/global_1.cif' _cell_length_a 28.2251(20) _cell_length_b 4.00072(25) _cell_length_c 10.0848(9) _cell_angle_alpha 90.0 _cell_angle_beta 97.8086(35) _cell_angle_gamma 90.0 _cell_volume 1128.2(2) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x+1/2,+y+1/2,-z+1/2 -1 -x,-y,-z -2 +x+1/2,-y+1/2,+z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity C C2 0.19328(7) 0.44242(30) 0.59305(11) 1.0 Uiso 0.04 4 C C3 0.24133(5) 0.37468(33) 0.58696(12) 1.0 Uiso 0.04 4 C C4 0.254324(19 0.1945(4) 0.47938(19) 1.0 Uiso 0.04 4 C C5 0.21946(7) 0.08230(27) 0.37811(10) 1.0 Uiso 0.04 4 C C6 0.17142(5) 0.14975(28) 0.38427(12) 1.0 Uiso 0.04 4 C C1 0.158449(18 0.32975(34) 0.49185(18) 1.0 Uiso 0.04 4 C C7 0.13346(7) 0.028179(34 0.27426(17) 1.0 Uiso 0.04 4 C C8 0.11690(5) 0.06077(28) 0.02815(13) 1.0 Uiso 0.04 4 C C13 0.07400(5) -0.10796(34) 0.03302(8) 1.0 Uiso 0.04 4 C C9 0.133321(22 0.11292(28) -0.09448(17) 1.0 Uiso 0.04 4 C C12 0.047654(22 -0.22402(27) -0.08484(18) 1.0 Uiso 0.04 4 C C11 0.06416(5) -0.17229(27) -0.20719(14) 1.0 Uiso 0.04 4 C C10 0.10701(5) -0.00363(34) -0.21211(8) 1.0 Uiso 0.04 4 C C14 0.03603(7) -0.2970(4) -0.33339(18) 1.0 Uiso 0.04 4 O O1 0.14120(6) 0.17025(34) 0.14752(16) 1.0 Uiso 0.04 4 O O2 0.04972(10) -0.2856(11) -0.44306(23) 1.0 Uiso 0.04 4 O O3 -0.00561(11) -0.4500(12) -0.31905(14) 1.0 Uiso 0.04 4 H H2 0.18447 0.55689 0.66617 1.0 Uiso 0.06 4 H H3 0.26482 0.45394 0.65312 1.0 Uiso 0.06 4 H H4 0.28645 0.16239 0.47141 1.0 Uiso 0.06 4 H H5 0.22817 -0.02629 0.30354 1.0 Uiso 0.06 4 H H1 0.12632 0.36676 0.49845 1.0 Uiso 0.06 4 H H7A 0.1343 -0.20399 0.27064 1.0 Uiso 0.06 4 H H7B 0.10333 0.09558 0.29325 1.0 Uiso 0.06 4 H H13 0.06338 -0.14726 0.11497 1.0 Uiso 0.06 4 H H9 0.16211 0.22314 -0.09834 1.0 Uiso 0.06 4 H H12 0.01914 -0.33816 -0.08138 1.0 Uiso 0.06 4 H H10 0.11785 0.02903 -0.2942 1.0 Uiso 0.06 4 H H3a -0.01891 -0.51819 -0.39134 1.0 Uiso 0.06 4 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C14 H12 O3' _chemical_formula_weight 228.25 _cell_formula_units_Z 4 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2 C3 1.3927(8) . 1_555 N C2 C1 1.3923(8) . 1_555 N C2 H2 0.93002 . 1_555 N C3 C2 1.3927(8) . 1_555 N C3 C4 1.3926(8) . 1_555 N C3 H3 0.93003 . 1_555 N C4 C3 1.3926(8) . 1_555 N C4 C5 1.3928(8) . 1_555 N C4 H4 0.93001 . 1_555 N C5 C4 1.3928(8) . 1_555 N C5 C6 1.3921(8) . 1_555 N C5 H5 0.93002 . 1_555 N C6 C5 1.3921(8) . 1_555 N C6 C1 1.3920(8) . 1_555 N C6 C7 1.5142(9) . 1_555 N C1 C2 1.3923(8) . 1_555 N C1 C6 1.3920(8) . 1_555 N C1 H1 0.93001 . 1_555 N C7 C6 1.5142(9) . 1_555 N C7 O1 1.4423(9) . 1_555 N C7 H7A 0.93000 . 1_555 N C7 H7B 0.9363 . 1_555 N C8 C13 1.3930(8) . 1_555 N C8 C9 1.3941(8) . 1_555 N C8 O1 1.3737(9) . 1_555 N C13 C8 1.3930(8) . 1_555 N C13 C12 1.3933(9) . 1_555 N C13 H13 0.93004 . 1_555 N C9 C8 1.3941(8) . 1_555 N C9 C10 1.3917(8) . 1_555 N C9 H9 0.93004 . 1_555 N C12 C13 1.3933(9) . 1_555 N C12 C11 1.3924(8) . 1_555 N C12 H12 0.93002 . 1_555 N C11 C12 1.3924(8) . 1_555 N C11 C10 1.3915(8) . 1_555 N C11 C14 1.4914(9) . 1_555 N C10 C9 1.3917(8) . 1_555 N C10 C11 1.3915(8) . 1_555 N C10 H10 0.93002 . 1_555 N C14 C11 1.4914(9) . 1_555 N C14 O2 1.2209(9) . 1_555 N C14 O3 1.3504(9) . 1_555 N O1 C7 1.4423(9) . 1_555 N O1 C8 1.3737(9) . 1_555 N O2 C14 1.2209(9) . 1_555 N O3 C14 1.3504(9) . 1_555 N O3 H3a 0.82001 . 1_555 N loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C2 C1 119.965(27) 1_555 . 1_555 N C3 C2 H2 119.83 1_555 . 1_555 N C1 C2 H2 120.17 1_555 . 1_555 N C2 C3 C4 119.750(27) 1_555 . 1_555 N C2 C3 H3 120.36 1_555 . 1_555 N C4 C3 H3 119.87 1_555 . 1_555 N C3 C4 C5 120.234(27) 1_555 . 1_555 N C3 C4 H4 120.12 1_555 . 1_555 N C5 C4 H4 119.48 1_555 . 1_555 N C4 C5 C6 120.01(5) 1_555 . 1_555 N C4 C5 H5 120.35 1_555 . 1_555 N C6 C5 H5 119.53 1_555 . 1_555 N C5 C6 C1 119.74(7) 1_555 . 1_555 N C5 C6 C7 120.11(12) 1_555 . 1_555 N C1 C6 C7 120.15(12) 1_555 . 1_555 N C2 C1 C6 120.30(5) 1_555 . 1_555 N C2 C1 H1 119.61 1_555 . 1_555 N C6 C1 H1 120.03 1_555 . 1_555 N C6 C7 O1 110.20(10) 1_555 . 1_555 N C6 C7 H7A 109.28 1_555 . 1_555 N C6 C7 H7B 109.24 1_555 . 1_555 N O1 C7 H7A 110.56 1_555 . 1_555 N O1 C7 H7B 108.60 1_555 . 1_555 N C13 C8 C9 119.94(7) 1_555 . 1_555 N C13 C8 O1 117.16(10) 1_555 . 1_555 N C9 C8 O1 122.90(11) 1_555 . 1_555 N C8 C13 C12 119.81(6) 1_555 . 1_555 N C8 C13 H13 120.00 1_555 . 1_555 N C12 C13 H13 120.17 1_555 . 1_555 N C8 C9 C10 120.18(6) 1_555 . 1_555 N C8 C9 H9 120.38 1_555 . 1_555 N C10 C9 H9 119.43 1_555 . 1_555 N C13 C12 C11 120.16(5) 1_555 . 1_555 N C13 C12 H12 119.73 1_555 . 1_555 N C11 C12 H12 120.11 1_555 . 1_555 N C12 C11 C10 120.05(7) 1_555 . 1_555 N C12 C11 C14 120.20(10) 1_555 . 1_555 N C10 C11 C14 119.75(10) 1_555 . 1_555 N C9 C10 C11 119.86(6) 1_555 . 1_555 N C9 C10 H10 120.64 1_555 . 1_555 N C11 C10 H10 119.51 1_555 . 1_555 N C11 C14 O2 124.29(12) 1_555 . 1_555 N C11 C14 O3 115.50(10) 1_555 . 1_555 N O2 C14 O3 120.06(11) 1_555 . 1_555 N C7 O1 C8 122.22(11) 1_555 . 1_555 N C14 O3 H3a 110.82 1_555 . 1_555 N # Powder diffraction data for histogram 1 #============================================================================== # 9. INSTRUMENT CHARACTERIZATION _exptl_special_details ; ? ; # if regions of the data are excluded, the reason(s) are supplied here: _pd_proc_info_excluded_regions ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 293 _diffrn_source X-ray _diffrn_source_target CuK/a _diffrn_source_type 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker D8 Advance powder diffractometer' _diffrn_detector 'linear position-sensitive Lynxeye detector' _diffrn_detector_type 'Bruker AXS' # make or model of detector _pd_meas_scan_method Step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection EVA _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction ? # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator ? # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 10. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode reflection # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 56.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C O 12.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C H 48.0 0.000 0.000 0.49300 10.5109 0.32291 26.1257 0.14019 3.14236 0.04081 57.7997 0.00304 International_Tables_Vol_C _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 0.5 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type ? _pd_proc_ls_prof_R_factor 0.0363 _pd_proc_ls_prof_wR_factor 0.0545 _pd_proc_ls_prof_wR_expected 0.0638 _refine_ls_R_Fsqd_factor 0.15718 _pd_proc_ls_background_function ; GSAS Background function number 1 with 15 terms. Shifted Chebyshev function of 1st kind 1: 141.660 2: -16.3502 3: -16.9303 4: 21.8190 5: -14.7682 6: 2.98256 7: 0.669531 8: -3.80897 9: 5.61200 10: -5.24067 11: 3.47944 12: -1.03937 13: -2.31830 14: 2.18986 15: -0.630292 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 No correction is applied. ; _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_correction_T_max 1.00000 # Extinction correction _gsas_exptl_extinct_corr_T_min 1.00000 _gsas_exptl_extinct_corr_T_max 1.00000 _pd_proc_ls_profile_function ; CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 343.425 #2(GV) = 33.843 #3(GW) = 35.411 #4(LX) = 1.000 #5(LY) = 27.285 #6(trns) = 0.000 #7(asym) = -0.5950 #8(shft) = 1.7393 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.012 #17(L13) = 0.000 #18(L23) = 0.028 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.01000 _pd_proc_info_datetime 2012-04-20T15:47:54 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 5.0 _pd_meas_2theta_range_max 100.0018 _pd_meas_2theta_range_inc 0.0199 _pd_proc_2theta_range_min 5.0 _pd_proc_2theta_range_max 100.0018 _pd_proc_2theta_range_inc 0.0199 loop_ _pd_meas_counts_total _pd_proc_ls_weight _pd_proc_intensity_bkg_calc _pd_calc_intensity_total 111.0 0.00901 116.22167 116.22202 112.0 0.00893 116.18655 116.18687 112.0 0.00893 116.15002 116.15030 112.0 0.00893 116.11213 116.11241 112.0 0.00893 116.07294 116.07320 112.0 0.00893 116.03251 116.03276 112.0 0.00893 115.99089 115.99111 112.0 0.00893 115.94815 115.94835 112.0 0.00893 115.90434 115.90452 112.0 0.00893 115.85949 115.85967 112.0 0.00893 115.81369 115.81386 112.0 0.00893 115.76696 115.76711 112.0 0.00893 115.71939 115.71953 112.0 0.00893 115.67098 115.67110 112.0 0.00893 115.62184 115.62194 111.0 0.00901 115.57197 115.57204 111.0 0.00901 115.52141 115.52151 111.0 0.00901 115.47031 115.47035 111.0 0.00901 115.41858 115.41864 111.0 0.00901 115.36636 115.36640 111.0 0.00901 115.31367 115.31371 111.0 0.00901 115.26056 115.26057 111.0 0.00901 115.20704 115.20706 110.0 0.00909 115.15322 115.15321 110.0 0.00909 115.09910 115.09908 110.0 0.00909 115.04470 115.04469 110.0 0.00909 114.99011 114.99008 110.0 0.00909 114.93537 114.93534 110.0 0.00909 114.88051 114.88046 111.0 0.00901 114.82555 114.82550 111.0 0.00901 114.77056 114.77050 111.0 0.00901 114.71556 114.71550 112.0 0.00893 114.66061 114.66055 112.0 0.00893 114.60573 114.60563 113.0 0.00885 114.55096 114.55087 113.0 0.00885 114.49635 114.49624 113.0 0.00885 114.44191 114.44180 114.0 0.00877 114.38770 114.38759 113.0 0.00885 114.33374 114.33363 113.0 0.00885 114.28010 114.27995 113.0 0.00885 114.22677 114.22664 113.0 0.00885 114.17379 114.17366 113.0 0.00885 114.12125 114.12109 114.0 0.00877 114.06908 114.06892 115.0 0.00870 114.01738 114.01723 116.0 0.00862 113.96621 113.96605 118.0 0.00847 113.91551 113.91536 120.0 0.00833 113.86540 119.97131 123.0 0.00813 113.81585 120.57581 126.0 0.00794 113.76691 121.29152 131.0 0.00763 113.71866 122.14821 136.0 0.00735 113.67104 123.19507 143.0 0.00699 113.62411 124.52690 152.0 0.00658 113.57793 126.34836 164.0 0.00610 113.53249 129.11568 178.0 0.00562 113.48782 133.80682 198.0 0.00505 113.44398 142.35886 221.0 0.00452 113.40096 158.22346 253.0 0.00395 113.35877 186.80266 292.0 0.003425 113.31747 235.29204 346.0 0.002890 113.27709 311.35779 422.0 0.002370 113.23766 420.29260 528.0 0.001894 113.19914 561.19611 667.0 0.001499 113.16161 723.48206 832.0 0.001202 113.12508 885.48273 989.0 0.001011 113.08956 1016.81104 1102.0 0.000907 113.05508 1086.20630 1144.0 0.000874 113.02165 1075.29675 1107.0 0.000903 112.98933 988.60889 975.0 0.001026 112.95808 849.26953 768.0 0.001302 112.92795 687.53796 576.0 0.001736 112.89899 530.94379 403.0 0.002481 112.87118 398.09247 263.0 0.00380 112.84455 296.97903 181.0 0.00552 112.81911 226.95023 147.0 0.00680 112.79488 182.32574 135.0 0.00741 112.77190 155.82214 129.0 0.00775 112.75013 140.87941 127.0 0.00787 112.72967 132.64816 124.0 0.00806 112.71046 128.02338 123.0 0.00813 112.69255 125.23830 122.0 0.00820 112.67596 123.38013 121.0 0.00826 112.66065 122.00980 121.0 0.00826 112.64674 120.92425 120.0 0.00833 112.63417 120.02747 120.0 0.00833 112.62296 119.26962 120.0 0.00833 112.61316 112.61295 119.0 0.00840 112.60472 112.60452 120.0 0.00833 112.59771 112.59752 119.0 0.00840 112.59211 112.59189 119.0 0.00840 112.58795 112.58775 120.0 0.00833 112.58525 112.58501 120.0 0.00833 112.58397 112.58376 120.0 0.00833 112.58416 112.58398 120.0 0.00833 112.58585 112.58565 120.0 0.00833 112.58904 112.58884 120.0 0.00833 112.59369 112.59349 120.0 0.00833 112.59987 112.59968 119.0 0.00840 112.60758 112.60738 119.0 0.00840 112.61681 112.61660 119.0 0.00840 112.62754 112.62737 118.0 0.00847 112.63986 112.63968 118.0 0.00847 112.65372 112.65353 117.0 0.00855 112.66913 112.66894 117.0 0.00855 112.68610 112.68592 117.0 0.00855 112.70466 112.70447 117.0 0.00855 112.72478 112.72462 116.0 0.00862 112.74654 112.74635 116.0 0.00862 112.76984 112.76969 117.0 0.00855 112.79478 112.79460 116.0 0.00862 112.82132 112.82116 117.0 0.00855 112.84946 112.84927 116.0 0.00862 112.87923 112.87906 116.0 0.00862 112.91061 112.91045 116.0 0.00862 112.94363 112.94347 116.0 0.00862 112.97827 112.97813 116.0 0.00862 113.01454 113.01439 116.0 0.00862 113.05251 113.05235 116.0 0.00862 113.09205 113.09190 116.0 0.00862 113.13327 113.13314 116.0 0.00862 113.17616 113.17601 116.0 0.00862 113.22069 113.22054 116.0 0.00862 113.26687 113.26670 116.0 0.00862 113.31471 113.31457 116.0 0.00862 113.36423 113.36410 115.0 0.00870 113.41541 113.41526 115.0 0.00870 113.46823 113.46810 115.0 0.00870 113.52271 113.52260 115.0 0.00870 113.57890 113.57877 115.0 0.00870 113.63675 113.63663 115.0 0.00870 113.69627 113.69614 115.0 0.00870 113.75746 113.75735 115.0 0.00870 113.82030 113.82018 115.0 0.00870 113.88486 113.88473 115.0 0.00870 113.95105 113.95093 115.0 0.00870 114.01892 114.01884 115.0 0.00870 114.08848 114.08836 115.0 0.00870 114.15972 114.15960 115.0 0.00870 114.23260 114.23248 115.0 0.00870 114.30717 114.30705 115.0 0.00870 114.38339 114.38332 115.0 0.00870 114.46130 114.46122 115.0 0.00870 114.54087 114.54076 115.0 0.00870 114.62207 114.62200 115.0 0.00870 114.70499 114.70490 115.0 0.00870 114.78956 114.78945 116.0 0.00862 114.87575 114.87566 115.0 0.00870 114.96362 114.96355 115.0 0.00870 115.05315 115.05309 115.0 0.00870 115.14434 115.14424 115.0 0.00870 115.23714 115.23705 115.0 0.00870 115.33163 115.33154 115.0 0.00870 115.42773 115.42764 116.0 0.00862 115.52547 115.52538 116.0 0.00862 115.62486 115.62479 116.0 0.00862 115.72583 115.72578 116.0 0.00862 115.82850 115.82843 116.0 0.00862 115.93273 115.93267 117.0 0.00855 116.03863 116.03856 116.0 0.00862 116.14615 116.14608 116.0 0.00862 116.25520 116.25517 116.0 0.00862 116.36592 116.36588 116.0 0.00862 116.47824 116.47816 116.0 0.00862 116.59212 116.59206 116.0 0.00862 116.70762 116.70758 116.0 0.00862 116.82471 116.82464 116.0 0.00862 116.94335 116.94332 116.0 0.00862 117.06360 117.06354 116.0 0.00862 117.18537 117.18534 116.0 0.00862 117.30875 117.30869 116.0 0.00862 117.43365 117.43361 116.0 0.00862 117.56011 117.56007 116.0 0.00862 117.68812 117.68810 116.0 0.00862 117.81768 117.81765 116.0 0.00862 117.94878 117.94871 116.0 0.00862 118.08134 118.08132 116.0 0.00862 118.21550 118.21547 117.0 0.00855 118.35112 118.35108 116.0 0.00862 118.48826 118.48825 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127.0 0.00787 124.54005 126.08819 127.0 0.00787 124.52855 126.08609 127.0 0.00787 124.51706 126.10339 127.0 0.00787 124.50558 126.16139 128.0 0.00781 124.49414 126.24955 128.0 0.00781 124.48273 126.36865 128.0 0.00781 124.47132 126.51479 129.0 0.00775 124.45995 126.68737 128.0 0.00781 124.44859 126.88374 129.0 0.00775 124.43726 127.09909 129.0 0.00775 124.42594 127.33224 129.0 0.00775 124.41463 127.57880 129.0 0.00775 124.40334 127.85522 129.0 0.00775 124.39211 128.11452 129.0 0.00775 124.38087 128.37689 129.0 0.00775 124.36964 128.63972 129.0 0.00775 124.35845 128.89404 128.0 0.00781 124.34729 129.15364 128.0 0.00781 124.33614 129.40334 128.0 0.00781 124.32501 129.63846 127.0 0.00787 124.31389 129.86099 127.0 0.00787 124.30279 130.07660 127.0 0.00787 124.29175 130.28142 127.0 0.00787 124.28071 130.47746 127.0 0.00787 124.26968 130.65955 127.0 0.00787 124.25870 130.82654 127.0 0.00787 124.24772 131.00279 127.0 0.00787 124.23676 131.14964 127.0 0.00787 124.22580 131.28612 128.0 0.00781 124.21490 131.41145 128.0 0.00781 124.20401 131.52521 128.0 0.00781 124.19315 131.62761 128.0 0.00781 124.18230 131.71912 129.0 0.00775 124.17145 131.79805 128.0 0.00781 124.16064 131.86482 129.0 0.00775 124.14986 131.90501 128.0 0.00781 124.13909 131.94449 129.0 0.00775 124.12836 131.97267 128.0 0.00781 124.11763 131.98227 128.0 0.00781 124.10693 131.97595 129.0 0.00775 124.09624 131.96700 129.0 0.00775 124.08559 131.94327 128.0 0.00781 124.07494 131.90930 128.0 0.00781 124.06435 131.86935 129.0 0.00775 124.05374 131.81982 128.0 0.00781 124.04317 131.76202 128.0 0.00781 124.03262 131.70451 128.0 0.00781 124.02209 131.65755 128.0 0.00781 124.01160 131.59947 128.0 0.00781 124.00110 131.54555 128.0 0.00781 123.99063 131.49541 128.0 0.00781 123.98019 131.45027 128.0 0.00781 123.96976 131.41208 128.0 0.00781 123.95935 131.38132 128.0 0.00781 123.94897 131.35573 128.0 0.00781 123.93860 131.34506 128.0 0.00781 123.92826 131.33795 128.0 0.00781 123.91793 131.33978 128.0 0.00781 123.90764 131.34872 128.0 0.00781 123.89734 131.37306 128.0 0.00781 123.88708 131.40796 128.0 0.00781 123.87685 131.44139 128.0 0.00781 123.86662 131.46378 128.0 0.00781 123.85643 131.51443 129.0 0.00775 123.84624 131.58093 129.0 0.00775 123.83606 131.64848 130.0 0.00769 123.82593 131.72346 130.0 0.00769 123.81580 131.80667 131.0 0.00763 123.80567 131.89659 131.0 0.00763 123.79558 131.98471 132.0 0.00758 123.78551 132.08392 132.0 0.00758 123.77546 132.18578 132.0 0.00758 123.76543 132.28758 132.0 0.00758 123.75542 132.39821 132.0 0.00758 123.74541 132.49045 132.0 0.00758 123.73544 132.60620 132.0 0.00758 123.72546 132.68875 132.0 0.00758 123.71553 132.75946 132.0 0.00758 123.70562 132.81795 132.0 0.00758 123.69571 132.86273 131.0 0.00763 123.68581 132.89252 132.0 0.00758 123.67592 132.90619 132.0 0.00758 123.66605 132.90282 132.0 0.00758 123.65621 132.88155 133.0 0.00752 123.64639 132.84164 132.0 0.00758 123.63660 132.72267 133.0 0.00752 123.62680 132.64568 134.0 0.00746 123.61701 132.54924 134.0 0.00746 123.60724 132.43340 135.0 0.00741 123.59750 132.28621 135.0 0.00741 123.58777 132.13365 136.0 0.00735 123.57806 131.96153 135.0 0.00741 123.56834 131.77541 135.0 0.00741 123.55864 131.58133 136.0 0.00735 123.54895 131.38817 135.0 0.00741 123.53929 131.18494 136.0 0.00735 123.52966 130.97392 136.0 0.00735 123.52000 130.76442 137.0 0.00730 123.51038 130.55807 137.0 0.00730 123.50076 130.36037 138.0 0.00725 123.49115 130.17220 138.0 0.00725 123.48158 129.99513 139.0 0.00719 123.47199 129.83208 140.0 0.00714 123.46242 129.68605 141.0 0.00709 123.45287 129.55786 141.0 0.00709 123.44331 129.44930 141.0 0.00709 123.43378 129.36046 141.0 0.00709 123.42426 129.29362 139.0 0.00719 123.41475 129.25082 139.0 0.00719 123.40524 129.22488 138.0 0.00725 123.39574 129.21959 137.0 0.00730 123.38625 129.23450 136.0 0.00735 123.37678 129.26653 135.0 0.00741 123.36729 129.31961 135.0 0.00741 123.35783 129.38989 135.0 0.00741 123.34835 129.47586 135.0 0.00741 123.33890 129.57272 134.0 0.00746 123.32946 129.68402 134.0 0.00746 123.32002 129.80446 134.0 0.00746 123.31058 129.93102 133.0 0.00752 123.30114 130.06122 133.0 0.00752 123.29170 130.22838 133.0 0.00752 123.28229 130.35498 133.0 0.00752 123.27288 130.47491 132.0 0.00758 123.26347 130.58463 132.0 0.00758 123.25406 130.68092 132.0 0.00758 123.24464 130.76076 131.0 0.00763 123.23522 130.79047 131.0 0.00763 123.22582 130.83130 130.0 0.00769 123.21642 130.84933 129.0 0.00775 123.20701 130.84311 129.0 0.00775 123.19761 130.81340 128.0 0.00781 123.18819 130.76315 128.0 0.00781 123.17879 130.68985 128.0 0.00781 123.16939 130.59366 128.0 0.00781 123.15997 130.48505 128.0 0.00781 123.15055 130.36464 128.0 0.00781 123.14115 130.23888 129.0 0.00775 123.13173 130.08336 129.0 0.00775 123.12230 129.94473 129.0 0.00775 123.11288 129.79596 129.0 0.00775 123.10344 129.65225 128.0 0.00781 123.09401 129.50879 128.0 0.00781 123.08454 129.37453 128.0 0.00781 123.07511 129.24728 127.0 0.00787 123.06565 129.12817 127.0 0.00787 123.05617 129.01819 127.0 0.00787 123.04669 128.91797 127.0 0.00787 123.03721 128.82838 126.0 0.00794 123.02770 128.74861 127.0 0.00787 123.01820 128.67894 126.0 0.00794 123.00869 128.59747 127.0 0.00787 122.99917 128.54781 126.0 0.00794 122.98964 128.50746 127.0 0.00787 122.98008 128.47572 127.0 0.00787 122.97051 128.45213 126.0 0.00794 122.96093 128.43570 127.0 0.00787 122.95132 128.42610 127.0 0.00787 122.94171 128.42249 126.0 0.00794 122.93208 128.42453 126.0 0.00794 122.92245 128.43124 127.0 0.00787 122.91278 128.44218 126.0 0.00794 122.90311 128.46149 126.0 0.00794 122.89340 128.47916 126.0 0.00794 122.88368 128.49934 126.0 0.00794 122.87395 128.52213 126.0 0.00794 122.86418 128.54506 126.0 0.00794 122.85439 128.56799 126.0 0.00794 122.84458 128.59230 126.0 0.00794 122.83475 128.62086 127.0 0.00787 122.82491 128.63731 127.0 0.00787 122.81503 128.65091 127.0 0.00787 122.80514 128.65596 127.0 0.00787 122.79520 128.67941 127.0 0.00787 122.78522 128.66907 127.0 0.00787 122.77522 128.64850 127.0 0.00787 122.76523 128.61687 127.0 0.00787 122.75517 128.57300 128.0 0.00781 122.74510 128.51631 128.0 0.00781 122.73499 128.44611 128.0 0.00781 122.72485 128.36209 128.0 0.00781 122.71467 128.26447 128.0 0.00781 122.70448 128.15326 127.0 0.00787 122.69421 128.03108 127.0 0.00787 122.68392 127.90770 127.0 0.00787 122.67361 127.75959 127.0 0.00787 122.66326 127.60065 127.0 0.00787 122.65285 127.41965 127.0 0.00787 122.64243 127.24260 126.0 0.00794 122.63195 127.05817 127.0 0.00787 122.62144 126.86773 126.0 0.00794 122.61087 126.67271 126.0 0.00794 122.60027 126.47514 126.0 0.00794 122.58961 126.27561 126.0 0.00794 122.57892 126.07740 126.0 0.00794 122.56818 125.88025 126.0 0.00794 122.55739 125.68771 126.0 0.00794 122.54656 125.50021 126.0 0.00794 122.53568 125.32005 127.0 0.00787 122.52472 125.14878 126.0 0.00794 122.51373 124.98801 126.0 0.00794 122.50270 124.84196 127.0 0.00787 122.49160 124.70557 127.0 0.00787 122.48045 124.58247 127.0 0.00787 122.46922 124.47323 126.0 0.00794 122.45795 124.35607 126.0 0.00794 122.44664 124.27518 125.0 0.00800 122.43526 124.20799 124.0 0.00806 122.42382 124.15408 124.0 0.00806 122.41231 124.11266 124.0 0.00806 122.40073 124.08284 124.0 0.00806 122.38908 124.06401 125.0 0.00800 122.37740 124.05500 125.0 0.00800 122.36563 124.05477 124.0 0.00806 122.35379 124.06362 125.0 0.00800 122.34190 124.07780 124.0 0.00806 122.32991 124.09748 124.0 0.00806 122.31787 124.12158 124.0 0.00806 122.30574 124.14900 124.0 0.00806 122.29355 124.17873 124.0 0.00806 122.28129 124.20966 124.0 0.00806 122.26895 124.24541 125.0 0.00800 122.25652 124.27607 125.0 0.00800 122.24400 124.30531 125.0 0.00800 122.23143 124.30595 125.0 0.00800 122.21875 124.33042 125.0 0.00800 122.20602 124.35147 124.0 0.00806 122.19319 124.36913 124.0 0.00806 122.18024 124.38214 125.0 0.00800 122.16723 124.38983 125.0 0.00800 122.15414 124.39416 124.0 0.00806 122.14096 124.39355 124.0 0.00806 122.12768 124.36740 125.0 0.00800 122.11430 124.35946 124.0 0.00806 122.10083 124.35134 124.0 0.00806 122.08726 124.33653 124.0 0.00806 122.07360 124.31888 124.0 0.00806 122.05984 124.29877 124.0 0.00806 122.04598 124.28416 124.0 0.00806 122.03199 124.26065 124.0 0.00806 122.01795 124.23593 125.0 0.00800 122.00375 124.21088 125.0 0.00800 121.98948 124.19304 125.0 0.00800 121.97508 124.16760 125.0 0.00800 121.96058 124.14380 125.0 0.00800 121.94597 124.12121 125.0 0.00800 121.93124 124.10111 125.0 0.00800 121.91638 124.08555 125.0 0.00800 121.90144 124.06783 125.0 0.00800 121.88636 124.05351 124.0 0.00806 121.87116 124.04188 124.0 0.00806 121.85583 124.03307 124.0 0.00806 121.84038 124.02713 124.0 0.00806 121.82481 124.02410 124.0 0.00806 121.80912 124.02775 124.0 0.00806 121.79328 124.03228 124.0 0.00806 121.77733 124.03861 124.0 0.00806 121.76122 124.04402 124.0 0.00806 121.74500 124.05396 124.0 0.00806 121.72865 124.06582 124.0 0.00806 121.71214 124.08111 124.0 0.00806 121.69550 124.10756 124.0 0.00806 121.67873 124.12374 124.0 0.00806 121.66179 124.12202 124.0 0.00806 121.64473 124.13994 124.0 0.00806 121.62750 124.15871 124.0 0.00806 121.61014 124.17707 124.0 0.00806 121.59261 124.19696 125.0 0.00800 121.57494 124.21923 124.0 0.00806 121.55711 124.24136 124.0 0.00806 121.53911 124.26758 125.0 0.00800 121.52097 124.29406 124.0 0.00806 121.50266 124.32378 125.0 0.00800 121.48417 124.35890 125.0 0.00800 121.46553 124.39747 125.0 0.00800 121.44674 124.44179 125.0 0.00800 121.42775 124.47998 125.0 0.00800 121.40860 124.53891 125.0 0.00800 121.38927 124.60545 126.0 0.00794 121.36977 124.68056 126.0 0.00794 121.35008 124.75776 126.0 0.00794 121.33022 124.85139 126.0 0.00794 121.31018 124.95455 125.0 0.00800 121.28993 125.06712 125.0 0.00800 121.26953 125.18887 125.0 0.00800 121.24892 125.31844 125.0 0.00800 121.22810 125.45760 125.0 0.00800 121.20710 125.60812 125.0 0.00800 121.18591 125.78104 126.0 0.00794 121.16452 125.94227 126.0 0.00794 121.14292 126.10700 126.0 0.00794 121.12114 126.26659 126.0 0.00794 121.09912 126.43681 126.0 0.00794 121.07690 126.60824 126.0 0.00794 121.05448 126.77661 126.0 0.00794 121.03182 126.94147 126.0 0.00794 121.00897 127.10058 126.0 0.00794 120.98588 127.25204 126.0 0.00794 120.96259 127.39246 125.0 0.00800 120.93906 127.52215 126.0 0.00794 120.91529 127.63783 126.0 0.00794 120.89130 127.73760 126.0 0.00794 120.86710 127.81825 126.0 0.00794 120.84264 127.88167 127.0 0.00787 120.81796 127.91838 127.0 0.00787 120.79300 127.94118 127.0 0.00787 120.76784 127.94458 126.0 0.00794 120.74243 127.92545 127.0 0.00787 120.71675 127.88424 127.0 0.00787 120.69085 127.82436 126.0 0.00794 120.66466 127.74670 126.0 0.00794 120.63822 127.65051 126.0 0.00794 120.61153 127.52547 125.0 0.00800 120.58457 127.40199 125.0 0.00800 120.55735 127.25865 124.0 0.00806 120.52984 127.10322 124.0 0.00806 120.50209 126.93715 124.0 0.00806 120.47405 126.76011 125.0 0.00800 120.44570 126.57574 125.0 0.00800 120.41711 126.38419 125.0 0.00800 120.38825 126.18573 125.0 0.00800 120.35906 125.98776 125.0 0.00800 120.32958 125.78478 125.0 0.00800 120.29984 125.58104 125.0 0.00800 120.26978 125.36822 125.0 0.00800 120.23941 125.16722 125.0 0.00800 120.20878 124.96411 125.0 0.00800 120.17783 124.79129 124.0 0.00806 120.14655 124.60201 125.0 0.00800 120.11494 124.41819 124.0 0.00806 120.08304 124.24088 124.0 0.00806 120.05080 124.07048 124.0 0.00806 120.01829 123.91142 123.0 0.00813 119.98539 123.75650 123.0 0.00813 119.95219 123.61707 123.0 0.00813 119.91864 123.47871 123.0 0.00813 119.88477 123.34885 123.0 0.00813 119.85056 123.22774 123.0 0.00813 119.81600 123.11890 123.0 0.00813 119.78108 123.01619 123.0 0.00813 119.74582 122.92242 123.0 0.00813 119.71017 122.83776 123.0 0.00813 119.67422 122.76211 123.0 0.00813 119.63787 122.69510 123.0 0.00813 119.60116 122.63625 123.0 0.00813 119.56406 122.58564 123.0 0.00813 119.52663 122.54276 123.0 0.00813 119.48880 122.50740 123.0 0.00813 119.45059 122.48013 123.0 0.00813 119.41199 122.45700 122.0 0.00820 119.37301 122.44218 122.0 0.00820 119.33364 122.43370 122.0 0.00820 119.29384 122.43068 122.0 0.00820 119.25365 122.45145 122.0 0.00820 119.21306 122.45934 122.0 0.00820 119.17210 122.47205 123.0 0.00813 119.13067 122.48732 123.0 0.00813 119.08882 122.50900 124.0 0.00806 119.04658 122.53496 124.0 0.00806 119.00390 122.56429 124.0 0.00806 118.96078 122.59157 124.0 0.00806 118.91727 122.62719 125.0 0.00800 118.87327 122.66529 124.0 0.00806 118.82883 122.70522 124.0 0.00806 118.78394 122.74545 124.0 0.00806 118.73861 122.78641 124.0 0.00806 118.69284 122.82878 124.0 0.00806 118.64658 122.87013 124.0 0.00806 118.59988 122.90950 124.0 0.00806 118.55267 122.94621 124.0 0.00806 118.50500 122.97965 124.0 0.00806 118.45686 123.01008 124.0 0.00806 118.40823 123.03602 124.0 0.00806 118.35910 123.07790 124.0 0.00806 118.30952 123.09558 124.0 0.00806 118.25939 123.10880 124.0 0.00806 118.20874 123.12520 124.0 0.00806 118.15764 123.12878 124.0 0.00806 118.10599 123.12769 123.0 0.00813 118.05384 123.12193 123.0 0.00813 118.00115 123.11163 123.0 0.00813 117.94791 123.09612 123.0 0.00813 117.89417 123.07715 122.0 0.00820 117.83988 123.05347 123.0 0.00813 117.78506 123.02535 123.0 0.00813 117.72968 122.99268 123.0 0.00813 117.67374 122.95537 122.0 0.00820 117.61726 122.91325 123.0 0.00813 117.56017 122.86622 123.0 0.00813 117.50250 122.81424 123.0 0.00813 117.44433 122.75735 123.0 0.00813 117.38551 122.69518 123.0 0.00813 117.32610 122.62806 122.0 . . . _pd_meas_number_of_points 4774 _pd_proc_number_of_points 4774 data_2BENANILINE_publ _database_code_depnum_ccdc_archive 'CCDC 894245' #TrackingRef '3.cif' _pd_block_id 2008-02-27T13:00|2BENANILINE|| _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2008-02-27T13:00 _audit_update_record ; 2008-02-27T13:00 Initial CIF as created by GSAS2CIF ; #============================================================================= # this information describes the project, paper etc. for the CIF # # Acta Cryst. Section C papers and editorial correspondence is generated # # from the information in this section # # # # (from) CIF submission form for Rietveld refinements (Acta Cryst. C) # # Version 14 December 1998 # #============================================================================= # 1. SUBMISSION DETAILS #============================================================================= # 5. OVERALL REFINEMENT & COMPUTING DETAILS _refine_special_details ; ? ; _pd_proc_ls_special_details ; ? ; # The following items are used to identify the programs used. _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method Nil _refine_ls_extinction_coef ? _refine_ls_number_constraints ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? #============================================================================== # 6. SAMPLE PREPARATION DATA # (In the unusual case where multiple samples are used in a single # Rietveld study, this information should be moved into the phase # blocks) # The following three fields describe the preparation of the material. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _pd_char_colour white # use ICDD colour descriptions _refine_ls_shift/su_max 0.03 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 69 _refine_ls_goodness_of_fit_all 1.64 _refine_ls_number_restraints 57 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ;from D:/basab/POWDER/data_benzyloxyaniline/2aniline_re/gsas/tr4_fo ; _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from D:/basab/POWDER/data_benzyloxyaniline/2aniline_re/gsas/tr4_fo' _cell_length_a 7.7590(5) _cell_length_b 23.4338(21) _cell_length_c 6.1425(6) _cell_angle_alpha 90.0 _cell_angle_beta 96.1833(35) _cell_angle_gamma 90.0 _cell_volume 1110.4(2) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x+1/2,+y+1/2,-z -1 -x,-y,-z -2 +x+1/2,-y+1/2,+z # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity C C9 0.14095(21) 0.36535(7) 0.45033(25) 1.0 Uiso 0.04 4 C C8 0.22902(24) 0.39402(7) 0.29715(29) 1.0 Uiso 0.04 4 C C13 0.31532(24) 0.36280(9) 0.14929(25) 1.0 Uiso 0.04 4 C C12 0.31395(26) 0.30338(9) 0.15459(28) 1.0 Uiso 0.04 4 C C11 0.22616(31) 0.274856(9) 0.3081(4) 1.0 Uiso 0.04 4 C C10 0.13961(24) 0.30591(9) 0.45605(25) 1.0 Uiso 0.04 4 C C7 0.31233(8) 0.48195(9) 0.14442(15) 1.0 Uiso 0.04 4 C C6 0.30177(24) 0.54665(8) 0.15290(33) 1.0 Uiso 0.04 4 C C5 0.39044(24) 0.57745(9) 0.32419(28) 1.0 Uiso 0.04 4 C C4 0.38173(28) 0.63683(10) 0.32809(28) 1.0 Uiso 0.04 4 C C3 0.28582(30) 0.666153(11 0.1588(5) 1.0 Uiso 0.04 4 C C2 0.19876(27) 0.63573(10) -0.01403(30) 1.0 Uiso 0.04 4 C C1 0.20770(25) 0.57635(10) -0.01744(25) 1.0 Uiso 0.04 4 N N1 0.05354(28) 0.396138(8) 0.59965(29) 1.0 Uiso 0.04 4 O O1 0.22267(34) 0.45289(9) 0.3045(4) 1.0 Uiso 0.04 4 H H13 0.37507 0.38069 0.045 1.0 Uiso 0.06 4 H H12 0.37173 0.28184 0.05801 1.0 Uiso 0.06 4 H H11 0.22455 0.23522 0.31527 1.0 Uiso 0.06 4 H H10 0.08031 0.28768 0.55998 1.0 Uiso 0.06 4 H H7a 0.27098 0.46956 -0.00262 1.0 Uiso 0.06 4 H H7b 0.4335 0.47092 0.15894 1.0 Uiso 0.06 4 H H5 0.45761 0.55744 0.43325 1.0 Uiso 0.06 4 H H4 0.43972 0.65608 0.44656 1.0 Uiso 0.06 4 H H3 0.27834 0.7057 0.16641 1.0 Uiso 0.06 4 H H2 0.13414 0.65566 -0.12557 1.0 Uiso 0.06 4 H H1 0.15282 0.55706 -0.13785 1.0 Uiso 0.06 4 H H1a -0.00188 0.37813 0.69229 1.0 Uiso 0.06 4 H H1b 0.05203 0.43282 0.59629 1.0 Uiso 0.06 4 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C13 H13 N O' _chemical_formula_weight 199.25 _cell_formula_units_Z 4 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C9 C8 1.3936(14) . 1_555 N C9 C10 1.3934(15) . 1_555 N C9 N1 1.3985(13) . 1_555 N C8 C9 1.3936(14) . 1_555 N C8 C13 1.3927(15) . 1_555 N C8 O1 1.3814(15) . 1_555 N C13 C8 1.3927(15) . 1_555 N C13 C12 1.3929(15) . 1_555 N C13 H13 0.93001 . 1_555 N C12 C13 1.3929(15) . 1_555 N C12 C11 1.3923(15) . 1_555 N C12 H12 0.93004 . 1_555 N C11 C12 1.3923(15) . 1_555 N C11 C10 1.3920(15) . 1_555 N C11 H11 0.93005 . 1_555 N C10 C9 1.3934(15) . 1_555 N C10 C11 1.3920(15) . 1_555 N C10 H10 0.93004 . 1_555 N C7 C6 1.5196(15) . 1_555 N C7 O1 1.4360(15) . 1_555 N C7 H7a 0.96990 . 1_555 N C7 H7b 0.96986 . 1_555 N C6 C7 1.5196(15) . 1_555 N C6 C5 1.3947(15) . 1_555 N C6 C1 1.3954(15) . 1_555 N C5 C6 1.3947(15) . 1_555 N C5 C4 1.3936(15) . 1_555 N C5 H5 0.93001 . 1_555 N C4 C5 1.3936(15) . 1_555 N C4 C3 1.3929(15) . 1_555 N C4 H4 0.93003 . 1_555 N C3 C4 1.3929(15) . 1_555 N C3 C2 1.3919(15) . 1_555 N C3 H3 0.93006 . 1_555 N C2 C3 1.3919(15) . 1_555 N C2 C1 1.3935(15) . 1_555 N C2 H2 0.93002 . 1_555 N C1 C6 1.3954(15) . 1_555 N C1 C2 1.3935(15) . 1_555 N C1 H1 0.93003 . 1_555 N N1 C9 1.3985(13) . 1_555 N N1 H1a 0.86000 . 1_555 N N1 H1b 0.85999 . 1_555 N O1 C8 1.3814(15) . 1_555 N O1 C7 1.4360(15) . 1_555 N loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 C9 C10 120.30(10) 1_555 . 1_555 N C8 C9 N1 120.12(14) 1_555 . 1_555 N C10 C9 N1 119.59(15) 1_555 . 1_555 N C9 C8 C13 119.49(11) 1_555 . 1_555 N C9 C8 O1 115.95(13) 1_555 . 1_555 N C13 C8 O1 124.57(14) 1_555 . 1_555 N C8 C13 C12 120.30(8) 1_555 . 1_555 N C8 C13 H13 121.52 1_555 . 1_555 N C12 C13 H13 118.18 1_555 . 1_555 N C13 C12 C11 120.08(5) 1_555 . 1_555 N C13 C12 H12 121.48 1_555 . 1_555 N C11 C12 H12 118.43 1_555 . 1_555 N C12 C11 C10 119.79(5) 1_555 . 1_555 N C12 C11 H11 121.43 1_555 . 1_555 N C10 C11 H11 118.78 1_555 . 1_555 N C9 C10 C11 120.04(7) 1_555 . 1_555 N C9 C10 H10 118.82 1_555 . 1_555 N C11 C10 H10 121.14 1_555 . 1_555 N C6 C7 O1 114.69(10) 1_555 . 1_555 N C6 C7 H7a 108.49 1_555 . 1_555 N C6 C7 H7b 108.55 1_555 . 1_555 N O1 C7 H7a 111.08 1_555 . 1_555 N O1 C7 H7b 110.29 1_555 . 1_555 N C7 C6 C5 121.20(17) 1_555 . 1_555 N C7 C6 C1 119.85(17) 1_555 . 1_555 N C5 C6 C1 118.90(12) 1_555 . 1_555 N C6 C5 C4 120.58(9) 1_555 . 1_555 N C6 C5 H5 118.37 1_555 . 1_555 N C4 C5 H5 121.03 1_555 . 1_555 N C5 C4 C3 120.18(5) 1_555 . 1_555 N C5 C4 H4 118.52 1_555 . 1_555 N C3 C4 H4 121.29 1_555 . 1_555 N C4 C3 C2 119.54(5) 1_555 . 1_555 N C4 C3 H3 119.04 1_555 . 1_555 N C2 C3 H3 121.38 1_555 . 1_555 N C3 C2 C1 120.14(5) 1_555 . 1_555 N C3 C2 H2 118.92 1_555 . 1_555 N C1 C2 H2 120.94 1_555 . 1_555 N C6 C1 C2 120.64(9) 1_555 . 1_555 N C6 C1 H1 120.77 1_555 . 1_555 N C2 C1 H1 118.56 1_555 . 1_555 N C9 N1 H1a 119.54 1_555 . 1_555 N C9 N1 H1b 120.42 1_555 . 1_555 N C8 O1 C7 115.44(16) 1_555 . 1_555 N # Powder diffraction data for histogram 1 #============================================================================== # 9. INSTRUMENT CHARACTERIZATION _exptl_special_details ; ? ; # if regions of the data are excluded, the reason(s) are supplied here: _pd_proc_info_excluded_regions ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 293 _diffrn_source X-ray _diffrn_source_target CuK/a _diffrn_source_type 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker D8 Advance powder diffractometer' _diffrn_detector 'linear position-sensitive Lynxeye detector' _diffrn_detector_type 'Bruker AXS' # make or model of detector _pd_meas_scan_method Step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection EVA _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction ? # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator ? # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 10. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode reflection # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 52.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C N 4.0 0.000 0.000 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630 0.58260 -11.529 International_Tables_Vol_C O 4.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C H 52.0 0.000 0.000 0.49300 10.5109 0.32291 26.1257 0.14019 3.14236 0.04081 57.7997 0.00304 International_Tables_Vol_C _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 0.5 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type ? _pd_proc_ls_prof_R_factor 0.0354 _pd_proc_ls_prof_wR_factor 0.0565 _pd_proc_ls_prof_wR_expected 0.0442 _refine_ls_R_Fsqd_factor 0.11382 _pd_proc_ls_background_function ; GSAS Background function number 1 with 10 terms. Shifted Chebyshev function of 1st kind 1: 366.823 2: -24.7013 3: -15.2709 4: 25.1304 5: -27.7187 6: 12.0626 7: -2.30843 8: -7.57692 9: 9.38217 10: -6.78810 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 No correction is applied. ; _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_correction_T_max 1.00000 # Extinction correction _gsas_exptl_extinct_corr_T_min 1.00000 _gsas_exptl_extinct_corr_T_max 1.00000 _pd_proc_ls_profile_function ; CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 3467.880 #2(GV) = -528.445 #3(GW) = 38.285 #4(LX) = 1.000 #5(LY) = 6.341 #6(trns) = 0.000 #7(asym) = 2.1648 #8(shft) = -11.5288 #9(GP) = 0.000 #10(stec)= 39.63 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.010 #17(L13) = -0.019 #18(L23) = 0.008 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.01000 _pd_proc_info_datetime 2008-02-27T13:00:31 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 5.0 _pd_meas_2theta_range_max 100.0018 _pd_meas_2theta_range_inc 0.0199 _pd_proc_2theta_range_min 5.0 _pd_proc_2theta_range_max 100.0018 _pd_proc_2theta_range_inc 0.0199 loop_ _pd_meas_counts_total _pd_proc_ls_weight _pd_proc_intensity_bkg_calc _pd_calc_intensity_total 327.0 0.003058 332.78046 332.78104 326.0 0.003067 332.60226 332.60278 327.0 0.003058 332.42874 332.42926 327.0 0.003058 332.25989 332.26044 327.0 0.003058 332.09573 332.09625 328.0 0.003049 331.93610 331.93668 327.0 0.003058 331.78113 331.78165 327.0 0.003058 331.63077 331.63123 327.0 0.003058 331.48480 331.48526 328.0 0.003049 331.34344 331.34393 328.0 0.003049 331.20648 331.20691 328.0 0.003049 331.07401 331.07443 328.0 0.003049 330.94583 330.94632 329.0 0.003040 330.82214 330.82257 329.0 0.003040 330.70279 330.70319 328.0 0.003049 330.58780 330.58817 329.0 0.003040 330.47699 330.47739 328.0 0.003049 330.37054 330.37094 328.0 0.003049 330.26831 330.26871 328.0 0.003049 330.17035 330.17065 327.0 0.003058 330.07648 330.07687 327.0 0.003058 329.98672 329.98712 326.0 0.003067 329.90128 329.90152 326.0 0.003067 329.81976 329.82010 326.0 0.003067 329.74234 329.74268 326.0 0.003067 329.66901 329.66937 326.0 0.003067 329.59967 329.60007 327.0 0.003058 329.53436 329.53464 328.0 0.003049 329.47305 329.47330 327.0 0.003058 329.41559 329.41583 328.0 0.003049 329.36209 329.36234 329.0 0.003040 329.31244 329.31268 329.0 0.003040 329.26663 329.26685 329.0 0.003040 329.22464 329.22491 328.0 0.003049 329.18652 329.18677 327.0 0.003058 329.15213 329.15234 327.0 0.003058 329.12155 329.12180 326.0 0.003067 329.09464 329.09482 327.0 0.003058 329.07138 329.07166 327.0 0.003058 329.05188 329.05212 328.0 0.003049 329.03601 329.03622 328.0 0.003049 329.02377 329.02390 328.0 0.003049 329.01511 329.01532 328.0 0.003049 329.00995 329.01019 328.0 0.003049 329.00848 329.00861 327.0 0.003058 329.01047 329.01059 327.0 0.003058 329.01590 329.01605 327.0 0.003058 329.02481 329.02496 326.0 0.003067 329.03720 329.03732 327.0 0.003058 329.05298 329.05310 327.0 0.003058 329.07217 329.07224 326.0 0.003067 329.09473 329.09488 328.0 0.003049 329.12064 329.12070 327.0 0.003058 329.14984 329.14996 328.0 0.003049 329.18231 329.18250 328.0 0.003049 329.21814 329.21829 327.0 0.003058 329.25720 329.25726 328.0 0.003049 329.29947 329.29956 327.0 0.003058 329.34497 329.34503 328.0 0.003049 329.39359 329.39362 328.0 0.003049 329.44534 329.44540 329.0 0.003040 329.50027 329.50034 328.0 0.003049 329.55829 329.55832 328.0 0.003049 329.61938 329.61948 328.0 0.003049 329.68353 329.68359 329.0 0.003040 329.75070 329.75076 329.0 0.003040 329.82095 329.82095 328.0 0.003049 329.89420 329.89417 329.0 0.003040 329.97031 329.97031 329.0 0.003040 330.04935 330.04941 329.0 0.003040 330.13144 330.13147 329.0 0.003040 330.21637 330.21637 328.0 0.003049 330.30411 330.30414 328.0 0.003049 330.39478 330.39481 327.0 0.003058 330.48822 330.48825 327.0 0.003058 330.58453 330.58450 327.0 0.003058 330.68356 330.68362 327.0 0.003058 330.78537 330.78543 328.0 0.003049 330.89001 330.88998 329.0 0.003040 330.99725 330.99728 329.0 0.003040 331.10721 331.10730 329.0 0.003040 331.21994 331.21988 329.0 0.003040 331.33521 331.33521 329.0 0.003040 331.45313 331.45313 328.0 0.003049 331.57370 331.57367 328.0 0.003049 331.69684 331.69678 328.0 0.003049 331.82254 331.82254 329.0 0.003040 331.95084 331.95074 331.0 0.003021 332.08160 332.08157 331.0 0.003021 332.21490 332.21484 334.0 0.002994 332.35065 332.35065 336.0 0.002976 332.48883 332.48886 336.0 0.002976 332.62955 332.62952 338.0 0.002959 332.77264 332.77261 340.0 0.002941 332.91812 332.91809 339.0 0.002950 333.06601 333.06595 339.0 0.002950 333.21625 333.21619 338.0 0.002959 333.36874 333.36877 337.0 0.002967 333.52368 333.52365 336.0 0.002976 333.68085 333.68085 335.0 0.002985 333.84033 333.84030 334.0 0.002994 334.00211 334.00201 334.0 0.002994 334.16605 334.16595 334.0 0.002994 334.33224 334.33215 334.0 0.002994 334.50058 334.50052 335.0 0.002985 334.67114 334.67114 335.0 0.002985 334.84384 334.84381 338.0 0.002959 335.01874 335.01871 341.0 0.002933 335.19574 335.19568 345.0 0.002899 335.37482 335.37479 350.0 0.002857 335.55594 335.55597 356.0 0.002809 335.73923 335.73920 363.0 0.002755 335.92450 353.01328 355.0 0.002817 336.11182 355.24460 363.0 0.002755 336.30112 357.87558 366.0 0.002732 336.49240 361.02634 367.0 0.002725 336.68573 364.90219 374.0 0.002674 336.88095 369.96063 383.0 0.002611 337.07809 377.43304 406.0 0.002463 337.27713 390.62305 430.0 0.002326 337.47809 417.32281 468.0 0.002137 337.68094 472.87189 570.0 0.001754 337.88565 581.84863 750.0 0.001333 338.09216 775.31012 1012.0 0.000988 338.30057 1081.00305 1433.0 0.000698 338.51068 1506.42139 1946.0 0.000514 338.72269 2026.67065 2497.0 0.000400 338.93646 2594.38892 3003.0 0.0003330 339.15192 3153.66577 3522.0 0.0002839 339.36911 3676.44092 3968.0 0.0002520 339.58807 4168.16602 4380.0 0.0002283 339.80872 4569.43018 4549.0 0.0002198 340.03101 4722.19824 4357.0 0.0002295 340.25507 4463.53662 3632.0 0.0002753 340.48065 3769.13574 2789.0 0.000359 340.70792 2823.86646 2021.0 0.000495 340.93674 1907.39746 1305.0 0.000766 341.16721 1210.77100 781.0 0.001280 341.39932 778.74023 528.0 0.001894 341.63290 554.86426 443.0 0.002257 341.86804 454.67920 417.0 0.002398 342.10474 413.16290 409.0 0.002445 342.34302 394.96725 403.0 0.002481 342.58267 385.21274 396.0 0.002525 342.82391 378.72995 391.0 0.002558 343.06653 343.06656 386.0 0.002591 343.31058 343.31061 381.0 0.002625 343.55615 343.55618 377.0 0.002653 343.80304 343.80310 375.0 0.002667 344.05139 344.05139 372.0 0.002688 344.30115 344.30121 369.0 0.002710 344.55225 344.55231 367.0 0.002725 344.80472 344.80469 365.0 0.002740 345.05847 345.05850 364.0 0.002747 345.31360 345.31360 364.0 0.002747 345.56995 345.57007 364.0 0.002747 345.82770 345.82773 365.0 0.002740 346.08661 346.08670 364.0 0.002747 346.34689 346.34695 364.0 0.002747 346.60837 346.60843 363.0 0.002755 346.87112 346.87112 362.0 0.002762 347.13495 347.13498 363.0 0.002755 347.40012 347.40012 363.0 0.002755 347.66635 347.66644 362.0 0.002762 347.93384 347.93387 363.0 0.002755 348.20251 348.20251 362.0 0.002762 348.47220 348.47229 362.0 0.002762 348.74313 348.74323 360.0 0.002778 349.01511 349.01520 360.0 0.002778 349.28821 349.28821 359.0 0.002786 349.56235 349.56244 359.0 0.002786 349.83755 349.83765 358.0 0.002793 350.11386 350.11392 360.0 0.002778 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353.05167 351.0 0.002849 342.16635 353.18109 353.0 0.002833 342.12177 353.31967 353.0 0.002833 342.07666 353.44553 353.0 0.002833 342.03101 353.57690 354.0 0.002825 341.98492 353.70840 355.0 0.002817 341.93826 353.84003 355.0 0.002817 341.89102 353.97159 355.0 0.002817 341.84332 354.10217 355.0 0.002817 341.79507 354.23163 355.0 0.002817 341.74622 354.36029 354.0 0.002825 341.69684 354.48715 354.0 0.002825 341.64685 354.61270 354.0 0.002825 341.59634 354.73590 354.0 0.002825 341.54529 354.85715 354.0 0.002825 341.49362 354.97641 353.0 0.002833 341.44141 355.09406 353.0 0.002833 341.38858 355.20724 352.0 0.002841 341.33521 355.31696 351.0 0.002849 341.28122 355.42349 351.0 0.002849 341.22665 355.52618 350.0 0.002857 341.17145 355.62952 350.0 0.002857 341.11563 355.72354 351.0 0.002849 341.05923 355.81427 350.0 0.002857 341.00223 355.89771 351.0 0.002849 340.94452 355.97751 351.0 0.002849 340.88620 356.05234 351.0 0.002849 340.82727 356.12134 351.0 0.002849 340.76773 356.18463 351.0 0.002849 340.70749 356.24405 351.0 0.002849 340.64667 356.29596 352.0 0.002841 340.58508 356.34250 351.0 0.002849 340.52295 356.38251 352.0 0.002841 340.46008 356.41055 350.0 0.002857 340.39655 356.43759 349.0 0.002865 340.33234 356.45837 350.0 0.002857 340.26749 356.47293 348.0 0.002874 340.20187 356.48123 349.0 0.002865 340.13556 356.48257 350.0 0.002857 340.06863 356.47778 349.0 0.002865 340.00095 356.46725 350.0 0.002857 339.93253 356.44998 348.0 0.002874 339.86340 356.42981 349.0 0.002865 339.79355 356.40042 348.0 0.002874 339.72296 356.36447 347.0 0.002882 339.65161 356.32242 348.0 0.002874 339.57962 356.27499 349.0 0.002865 339.50677 356.22125 348.0 0.002874 339.43323 356.16235 349.0 0.002865 339.35892 356.09793 350.0 0.002857 339.28375 356.02817 350.0 0.002857 339.20792 355.95331 351.0 0.002849 339.13123 355.87314 350.0 0.002857 339.05386 355.78870 351.0 0.002849 338.97562 355.69925 351.0 0.002849 338.89661 355.59930 350.0 0.002857 338.81677 355.50046 350.0 0.002857 338.73611 355.39670 350.0 0.002857 338.65472 355.28610 350.0 0.002857 338.57239 355.17435 351.0 0.002849 338.48923 355.05829 351.0 0.002849 338.40533 354.93811 351.0 0.002849 338.32053 354.81415 352.0 0.002841 338.23486 354.68634 352.0 0.002841 338.14838 354.55988 351.0 0.002849 338.06107 354.42484 350.0 0.002857 337.97290 354.28659 351.0 0.002849 337.88370 354.14471 350.0 0.002857 337.79373 353.99951 352.0 0.002841 337.70288 353.85165 352.0 0.002841 337.61115 353.70001 352.0 0.002841 337.51849 353.54596 353.0 0.002833 337.42490 353.38846 352.0 0.002841 337.33038 353.22900 352.0 0.002841 337.23492 353.06616 351.0 0.002849 337.13861 352.90030 350.0 0.002857 337.04129 352.73309 349.0 0.002865 336.94308 352.56259 349.0 0.002865 336.84390 352.38269 350.0 0.002857 336.74380 352.20718 349.0 0.002865 336.64261 352.02951 350.0 0.002857 336.54056 351.84903 349.0 0.002865 336.43753 351.66724 349.0 0.002865 336.33347 351.48657 348.0 0.002874 336.22849 351.30142 347.0 0.002882 336.12234 351.11292 346.0 0.002890 336.01535 350.92294 346.0 0.002890 335.90732 350.73099 346.0 0.002890 335.79819 350.53860 347.0 0.002882 335.68802 350.34283 348.0 0.002874 335.57687 350.14590 350.0 0.002857 335.46469 349.94693 350.0 0.002857 335.35141 349.74673 351.0 0.002849 335.23712 349.54480 352.0 0.002841 335.12177 349.34125 351.0 0.002849 335.00525 349.13666 352.0 0.002841 334.88773 348.93036 352.0 0.002841 334.76904 348.72232 352.0 0.002841 334.64932 348.51270 352.0 0.002841 334.52847 348.30206 351.0 0.002849 334.40656 348.09052 352.0 0.002841 334.28342 347.87698 350.0 0.002857 334.15915 347.65628 350.0 0.002857 334.03381 347.44110 351.0 0.002849 333.90735 347.22861 349.0 0.002865 333.77966 347.01096 350.0 0.002857 333.65088 346.79233 350.0 0.002857 333.52084 346.57248 349.0 0.002865 333.38968 346.35168 348.0 0.002874 333.25726 346.12936 349.0 0.002865 333.12372 345.90637 348.0 0.002874 332.98889 345.68225 347.0 0.002882 332.85297 345.45770 347.0 0.002882 332.71579 345.23154 347.0 0.002882 332.57730 345.00540 347.0 0.002882 332.43762 344.77786 347.0 0.002882 332.29678 344.54974 348.0 0.002874 332.15457 344.32098 348.0 0.002874 332.01111 344.09137 349.0 0.002865 331.86646 343.86133 348.0 0.002874 331.72043 343.63077 350.0 0.002857 331.57312 343.39948 350.0 0.002857 331.42462 343.16599 349.0 0.002865 331.27469 342.93396 351.0 0.002849 331.12350 342.70148 349.0 0.002865 330.97104 342.46878 349.0 0.002865 330.81708 342.23526 349.0 0.002865 330.66187 342.00189 349.0 0.002865 330.50528 341.76788 348.0 0.002874 330.34741 341.53412 349.0 0.002865 330.18811 341.29980 349.0 0.002865 330.02753 341.06531 349.0 0.002865 329.86542 340.83102 350.0 0.002857 329.70190 340.59561 350.0 0.002857 329.53705 340.36053 350.0 0.002857 329.37082 340.12543 351.0 0.002849 329.20309 339.88983 349.0 0.002865 329.03387 339.65402 351.0 . . . _pd_meas_number_of_points 4774 _pd_proc_number_of_points 4774 data_3BENANILINE_publ _database_code_depnum_ccdc_archive 'CCDC 894246' #TrackingRef '4.cif' _pd_block_id 2008-03-04T12:50|3BENANILINE|basab_chattopadhyay| _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2008-03-04T12:50 _audit_author_name 'basab chattopadhyay' _audit_update_record ; 2008-03-04T12:50 Initial CIF as created by GSAS2CIF ; #============================================================================= # this information describes the project, paper etc. for the CIF # # Acta Cryst. Section C papers and editorial correspondence is generated # # from the information in this section # # # # (from) CIF submission form for Rietveld refinements (Acta Cryst. C) # # Version 14 December 1998 # #============================================================================= # 1. SUBMISSION DETAILS #============================================================================= # 5. OVERALL REFINEMENT & COMPUTING DETAILS _refine_special_details ; ? ; _pd_proc_ls_special_details ; ? ; # The following items are used to identify the programs used. _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method Nil _refine_ls_extinction_coef ? _refine_ls_number_constraints ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? #============================================================================== # 6. SAMPLE PREPARATION DATA # (In the unusual case where multiple samples are used in a single # Rietveld study, this information should be moved into the phase # blocks) # The following three fields describe the preparation of the material. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _pd_char_colour white # use ICDD colour descriptions _refine_ls_shift/su_max 0.04 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 77 _refine_ls_goodness_of_fit_all 1.48 _refine_ls_number_restraints 57 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common 'from D:/basab/3-anilin/gsas/1.cif' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from D:/basab/3-anilin/gsas/1.cif' _cell_length_a 18.3731(6) _cell_length_b 10.2938(6) _cell_length_c 5.66026(23) _cell_angle_alpha 90.0 _cell_angle_beta 92.8742(19) _cell_angle_gamma 90.0 _cell_volume 1069.2(1) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x+1/2,+y+1/2,-z -1 -x,-y,-z -2 +x+1/2,-y+1/2,+z # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity C C2 0.98159(9) 0.83027(27) 1.20393(27) 1.0 Uiso 0.04 4 C C3 0.93431(14) 0.93458(16) 1.17514(33) 1.0 Uiso 0.04 4 C C4 0.88194(10) 0.93469(15) 0.9898(5) 1.0 Uiso 0.04 4 C C5 0.87683(8) 0.83068(25) 0.83342(25) 1.0 Uiso 0.04 4 C C6 0.92437(11) 0.72645(18) 0.86342(34) 1.0 Uiso 0.04 4 C C1 0.97685(9) 0.72598(14) 1.0486(5) 1.0 Uiso 0.04 4 C C7 0.91890(6) 0.61313(18) 0.69488(9) 1.0 Uiso 0.04 4 C C8 0.84768(9) 0.41897(21) 0.6554(4) 1.0 Uiso 0.04 4 C C9 0.79907(10) 0.33676(20) 0.76205(18) 1.0 Uiso 0.04 4 C C10 0.78155(7) 0.21763(17) 0.65803(31) 1.0 Uiso 0.04 4 C C11 0.81285(11) 0.18201(22) 0.4491(4) 1.0 Uiso 0.04 4 C C12 0.86154(10) 0.26466(24) 0.34335(15) 1.0 Uiso 0.04 4 C C13 0.87903(7) 0.38379(19) 0.4467(4) 1.0 Uiso 0.04 4 N N1 0.73253(11) 0.13364(8) 0.76280(20) 1.0 Uiso 0.04 4 O O1 0.86091(11) 0.53369(23) 0.7720(4) 1.0 Uiso 0.04 4 H H2 1.01667 0.82987 1.32823 1.0 Uiso 0.06 4 H H3 0.93726 1.00374 1.2809 1.0 Uiso 0.06 4 H H4 0.84948 1.00372 0.97185 1.0 Uiso 0.06 4 H H5 0.84128 0.8302 0.71053 1.0 Uiso 0.06 4 H H1 1.00873 0.65619 1.06789 1.0 Uiso 0.06 4 H H7a 0.91098 0.64323 0.53324 1.0 Uiso 0.06 4 H H7b 0.9634 0.56229 0.70472 1.0 Uiso 0.06 4 H H9 0.77799 0.36141 0.90115 1.0 Uiso 0.06 4 H H11 0.80158 0.10185 0.38043 1.0 Uiso 0.06 4 H H12 0.88292 0.23947 0.20507 1.0 Uiso 0.06 4 H H13 0.91184 0.43908 0.37734 1.0 Uiso 0.06 4 H H1a 0.72466 0.05744 0.70467 1.0 Uiso 0.06 4 H H1b 0.71558 0.15418 0.89669 1.0 Uiso 0.06 4 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C13 H13 N O' _chemical_formula_weight 199.25 _cell_formula_units_Z 4 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2 C3 1.3857(13) . 1_555 N C2 C1 1.3875(13) . 1_555 N C2 H2 0.92995 . 1_555 N C3 C2 1.3857(13) . 1_555 N C3 C4 1.3874(13) . 1_555 N C3 H3 0.92997 . 1_555 N C4 C3 1.3874(13) . 1_555 N C4 C5 1.3894(14) . 1_555 N C4 H4 0.92999 . 1_555 N C5 C4 1.3894(14) . 1_555 N C5 C6 1.3885(13) . 1_555 N C5 H5 0.93001 . 1_555 N C6 C5 1.3885(13) . 1_555 N C6 C1 1.3883(13) . 1_555 N C6 C7 1.5070(13) . 1_555 N C1 C2 1.3875(13) . 1_555 N C1 C6 1.3883(13) . 1_555 N C1 H1 0.92999 . 1_555 N C7 C6 1.5070(13) . 1_555 N C7 O1 1.4288(14) . 1_555 N C7 H7a 0.96998 . 1_555 N C7 H7b 0.96999 . 1_555 N C8 C9 1.3900(14) . 1_555 N C8 C13 1.3882(14) . 1_555 N C8 O1 1.3687(14) . 1_555 N C9 C8 1.3900(14) . 1_555 N C9 C10 1.3911(14) . 1_555 N C9 H9 0.93001 . 1_555 N C10 C9 1.3911(14) . 1_555 N C10 C11 1.3902(14) . 1_555 N C10 N1 1.4014(13) . 1_555 N C11 C10 1.3902(14) . 1_555 N C11 C12 1.3913(14) . 1_555 N C11 H11 0.9309 . 1_555 N C12 C11 1.3913(14) . 1_555 N C12 C13 1.3894(14) . 1_555 N C12 H12 0.93001 . 1_555 N C13 C8 1.3882(14) . 1_555 N C13 C12 1.3894(14) . 1_555 N C13 H13 0.93001 . 1_555 N N1 C10 1.4014(13) . 1_555 N N1 H1a 0.86000 . 1_555 N N1 H1b 0.86001 . 1_555 N O1 C7 1.4288(14) . 1_555 N O1 C8 1.3687(14) . 1_555 N loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C2 C1 120.39(4) 1_555 . 1_555 N C3 C2 H2 119.93 1_555 . 1_555 N C1 C2 H2 119.68 1_555 . 1_555 N C2 C3 C4 119.77(4) 1_555 . 1_555 N C2 C3 H3 120.11 1_555 . 1_555 N C4 C3 H3 120.12 1_555 . 1_555 N C3 C4 C5 120.21(4) 1_555 . 1_555 N C3 C4 H4 120.00 1_555 . 1_555 N C5 C4 H4 119.78 1_555 . 1_555 N C4 C5 C6 119.71(8) 1_555 . 1_555 N C4 C5 H5 120.21 1_555 . 1_555 N C6 C5 H5 120.08 1_555 . 1_555 N C5 C6 C1 120.25(10) 1_555 . 1_555 N C5 C6 C7 119.95(19) 1_555 . 1_555 N C1 C6 C7 119.80(19) 1_555 . 1_555 N C2 C1 C6 119.67(8) 1_555 . 1_555 N C2 C1 H1 120.28 1_555 . 1_555 N C6 C1 H1 120.06 1_555 . 1_555 N C6 C7 O1 106.06(11) 1_555 . 1_555 N C6 C7 H7a 110.61 1_555 . 1_555 N C6 C7 H7b 110.62 1_555 . 1_555 N O1 C7 H7a 113.09 1_555 . 1_555 N O1 C7 H7b 108.23 1_555 . 1_555 N C9 C8 C13 120.93(13) 1_555 . 1_555 N C9 C8 O1 114.72(16) 1_555 . 1_555 N C13 C8 O1 124.35(16) 1_555 . 1_555 N C8 C9 C10 119.53(10) 1_555 . 1_555 N C8 C9 H9 120.37(21) 1_555 . 1_555 N C10 C9 H9 120.09(21) 1_555 . 1_555 N C9 C10 C11 119.72(12) 1_555 . 1_555 N C9 C10 N1 120.32(17) 1_555 . 1_555 N C11 C10 N1 119.96(16) 1_555 . 1_555 N C10 C11 C12 120.46(14) 1_555 . 1_555 N C10 C11 H11 119.73 1_555 . 1_555 N C12 C11 H11 119.80 1_555 . 1_555 N C11 C12 C13 119.93(11) 1_555 . 1_555 N C11 C12 H12 119.95 1_555 . 1_555 N C13 C12 H12 120.12 1_555 . 1_555 N C8 C13 C12 119.43(11) 1_555 . 1_555 N C8 C13 H13 120.32 1_555 . 1_555 N C12 C13 H13 120.25 1_555 . 1_555 N C10 N1 H1a 120.00 1_555 . 1_555 N C10 N1 H1b 119.34 1_555 . 1_555 N C7 O1 C8 117.62(17) 1_555 . 1_555 N # Powder diffraction data for histogram 1 #============================================================================== # 9. INSTRUMENT CHARACTERIZATION _exptl_special_details ; ? ; # if regions of the data are excluded, the reason(s) are supplied here: _pd_proc_info_excluded_regions ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 293 _diffrn_source X-ray _diffrn_source_target CuK/a _diffrn_source_type 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker D8 Advance powder diffractometer' _diffrn_detector 'linear position-sensitive Lynxeye detector' _diffrn_detector_type 'Bruker AXS' # make or model of detector _pd_meas_scan_method Step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection EVA _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction ? # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator ? # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 10. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode reflection # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 52.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C N 4.0 0.000 0.000 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630 0.58260 -11.529 International_Tables_Vol_C O 4.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C H 52.0 0.000 0.000 0.49300 10.5109 0.32291 26.1257 0.14019 3.14236 0.04081 57.7997 0.00304 International_Tables_Vol_C _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 0.5 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type ? _pd_proc_ls_prof_R_factor 0.0366 _pd_proc_ls_prof_wR_factor 0.0520 _pd_proc_ls_prof_wR_expected 0.0354 _refine_ls_R_Fsqd_factor 0.04865 _pd_proc_ls_background_function ; GSAS Background function number 1 with 20 terms. Shifted Chebyshev function of 1st kind 1: 524.662 2: -519.568 3: 255.095 4: -130.121 5: 102.710 6: -109.854 7: 107.639 8: -97.7508 9: 84.6793 10: -49.0536 11: 12.4722 12: 0.566710 13: 10.3764 14: -17.0502 15: 13.9535 16: -3.91007 17: -2.91607 18: 4.47242 19: -3.22374 20: 3.81031 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 No correction is applied. ; _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_correction_T_max 1.00000 # Extinction correction _gsas_exptl_extinct_corr_T_min 1.00000 _gsas_exptl_extinct_corr_T_max 1.00000 _pd_proc_ls_profile_function ; CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 659.919 #2(GV) = -2.000 #3(GW) = 94.982 #4(LX) = 1.000 #5(LY) = 24.510 #6(trns) = 0.000 #7(asym) = -0.0804 #8(shft) = -11.0178 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = -0.003 #17(L13) = 0.002 #18(L23) = 0.005 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.01000 _pd_proc_info_datetime 2008-03-04T12:50:56 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 5.0 _pd_meas_2theta_range_max 100.12122 _pd_meas_2theta_range_inc 0.0199 _pd_proc_2theta_range_min 5.0 _pd_proc_2theta_range_max 100.12122 _pd_proc_2theta_range_inc 0.0199 loop_ _pd_meas_counts_total _pd_proc_ls_weight _pd_proc_intensity_bkg_calc _pd_calc_intensity_total 2113.0 0.000473 2023.90576 2023.89331 2112.0 0.000473 2011.44080 2011.42944 2100.0 0.000476 1999.05090 1999.04028 2084.0 0.000480 1986.73621 1986.72644 2064.0 0.000484 1974.49756 1974.48804 2041.0 0.000490 1962.33618 1962.32788 2018.0 0.000496 1950.25085 1950.24341 1993.0 0.000502 1938.24316 1938.23621 1972.0 0.000507 1926.31299 1926.30652 1951.0 0.000513 1914.46155 1914.45618 1930.0 0.000518 1902.68774 1902.68274 1912.0 0.000523 1890.99268 1890.98865 1893.0 0.000528 1879.37756 1879.37378 1874.0 0.000534 1867.84070 1867.83740 1857.0 0.000539 1856.38416 1856.38135 1839.0 0.000544 1845.00708 1845.00500 1822.0 0.000549 1833.70984 1833.70825 1807.0 0.000553 1822.49316 1822.49207 1791.0 0.000558 1811.35608 1811.35522 1776.0 0.000563 1800.30066 1800.30005 1763.0 0.000567 1789.32544 1789.32556 1748.0 0.000572 1778.43066 1778.43091 1736.0 0.000576 1767.61780 1767.61829 1724.0 0.000580 1756.88501 1756.88623 1711.0 0.000584 1746.23340 1746.23450 1700.0 0.000588 1735.66321 1735.66479 1688.0 0.000592 1725.17383 1725.17566 1677.0 0.000596 1714.76575 1714.76782 1666.0 0.000600 1704.43909 1704.44177 1655.0 0.000604 1694.19373 1694.19629 1644.0 0.000608 1684.02844 1684.03186 1635.0 0.000612 1673.94604 1673.94934 1624.0 0.000616 1663.94360 1663.94690 1613.0 0.000620 1654.02222 1654.02637 1604.0 0.000623 1644.18201 1644.18591 1594.0 0.000627 1634.42261 1634.42676 1584.0 0.000631 1624.74402 1624.74817 1575.0 0.000635 1615.14612 1615.15027 1565.0 0.000639 1605.62817 1605.63269 1557.0 0.000642 1596.19153 1596.19604 1548.0 0.000646 1586.83423 1586.83887 1538.0 0.000650 1577.55725 1577.56213 1529.0 0.000654 1568.36084 1568.36536 1520.0 0.000658 1559.24268 1559.24792 1511.0 0.000662 1550.20508 1550.20996 1502.0 0.000666 1541.24695 1541.25183 1493.0 0.000670 1532.36707 1532.37195 1485.0 0.000673 1523.56689 1523.57129 1477.0 0.000677 1514.84485 1514.85010 1469.0 0.000681 1506.20093 1506.20593 1461.0 0.000684 1497.63538 1497.64038 1453.0 0.000688 1489.14807 1489.15308 1445.0 0.000692 1480.73804 1480.74268 1438.0 0.000695 1472.40491 1472.40991 1430.0 0.000699 1464.14917 1464.15430 1423.0 0.000703 1455.97034 1455.97534 1417.0 0.000706 1447.86768 1447.87256 1410.0 0.000709 1439.84094 1439.84619 1404.0 0.000712 1431.89038 1431.89551 1398.0 0.000715 1424.01538 1424.02051 1392.0 0.000718 1416.21497 1416.21985 1386.0 0.000722 1408.49011 1408.49487 1381.0 0.000724 1400.83899 1400.84375 1374.0 0.000728 1393.26270 1393.26672 1369.0 0.000730 1385.75952 1385.76379 1362.0 0.000734 1378.32996 1378.33447 1356.0 0.000737 1370.97302 1370.97754 1352.0 0.000740 1363.68933 1363.69348 1345.0 0.000743 1356.47742 1356.48169 1340.0 0.000746 1349.33765 1349.34204 1336.0 0.000749 1342.26965 1342.27368 1330.0 0.000752 1335.27246 1335.27649 1325.0 0.000755 1328.34583 1328.35010 1320.0 0.000758 1321.48987 1321.49341 1316.0 0.000760 1314.70313 1314.70667 1310.0 0.000763 1307.98682 1307.99011 1305.0 0.000766 1301.33887 1301.34241 1300.0 0.000769 1294.75989 1294.76306 1295.0 0.000772 1288.24902 1288.25232 1289.0 0.000776 1281.80615 1281.80933 1284.0 0.000779 1275.43018 1275.43298 1278.0 0.000782 1269.12195 1269.12451 1273.0 0.000786 1262.87976 1262.88220 1266.0 0.000790 1256.70337 1256.70581 1260.0 0.000794 1250.59351 1250.59558 1253.0 0.000798 1244.54785 1244.54980 1248.0 0.000801 1238.56750 1238.56934 1242.0 0.000805 1232.65112 1232.65320 1237.0 0.000808 1226.79871 1226.80042 1233.0 0.000811 1221.01001 1221.01147 1228.0 0.000814 1215.28394 1215.28577 1224.0 0.000817 1209.62000 1209.62158 1219.0 0.000820 1204.01880 1204.02014 1215.0 0.000823 1198.47913 1198.48035 1211.0 0.000826 1193.00024 1193.00098 1206.0 0.000829 1187.58203 1187.58276 1202.0 0.000832 1182.22400 1182.22473 1198.0 0.000835 1176.92554 1176.92651 1194.0 0.000838 1171.68726 1171.68762 1190.0 0.000840 1166.50696 1166.50708 1186.0 0.000843 1161.38489 1161.38513 1182.0 0.000846 1156.32129 1156.32117 1178.0 0.000849 1151.31470 1151.31433 1173.0 0.000853 1146.36523 1146.36487 1168.0 0.000856 1141.47229 1141.47156 1164.0 0.000859 1136.63513 1136.63416 1158.0 0.000864 1131.85376 1131.85278 1154.0 0.000867 1127.12695 1127.12634 1150.0 0.000870 1122.45508 1122.45422 1144.0 0.000874 1117.83716 1117.83594 1141.0 0.000876 1113.27356 1113.27209 1137.0 0.000880 1108.76233 1108.76086 1133.0 0.000883 1104.30408 1104.30249 1129.0 0.000886 1099.89819 1099.89673 1125.0 0.000889 1095.54419 1095.54236 1122.0 0.000891 1091.24133 1091.23938 1118.0 0.000894 1086.98914 1086.98706 1114.0 0.000898 1082.78796 1082.78552 1109.0 0.000902 1078.63623 1078.63391 1106.0 0.000904 1074.53418 1074.53125 1102.0 0.000907 1070.48096 1070.47827 1097.0 0.000912 1066.47644 1066.47388 1094.0 0.000914 1062.51953 1062.51672 1090.0 0.000917 1058.61096 1058.60779 1086.0 0.000921 1054.74939 1054.74597 1083.0 0.000923 1050.93445 1050.93103 1079.0 0.000927 1047.16541 1047.16223 1075.0 0.000930 1043.44250 1043.43909 1071.0 0.000934 1039.76477 1039.76123 1067.0 0.000937 1036.13220 1036.12854 1063.0 0.000941 1032.54419 1032.54028 1058.0 0.000945 1028.99976 1028.99597 1055.0 0.000948 1025.49915 1025.49512 1051.0 0.000951 1022.04114 1022.03729 1048.0 0.000954 1018.62665 1018.62231 1044.0 0.000958 1015.25372 1015.24969 1040.0 0.000962 1011.92267 1011.91846 1036.0 0.000965 1008.63324 1008.62915 1031.0 0.000970 1005.38477 1005.38019 1028.0 0.000973 1002.17645 1002.17200 1024.0 0.000977 999.00848 999.00397 1020.0 0.000980 995.88000 995.87518 1017.0 0.000983 992.79053 992.78601 1014.0 0.000986 989.74005 989.73535 1011.0 0.000989 986.72815 986.72302 1008.0 0.000992 983.75385 983.74866 1005.0 0.000995 980.81702 980.81183 1002.0 0.000998 977.91730 977.91193 998.0 0.001002 975.05402 975.04907 996.0 0.001004 972.22760 972.22235 992.0 0.001008 969.43658 969.43109 989.0 0.001011 966.68109 966.67566 986.0 0.001014 963.96094 963.95538 983.0 0.001017 961.27484 961.26923 980.0 0.001020 958.62372 958.61768 977.0 0.001024 956.00580 956.00012 974.0 0.001027 953.42145 953.41565 971.0 0.001030 950.87042 950.86456 967.0 0.001034 948.35168 948.34583 965.0 0.001036 945.86554 945.85968 961.0 0.001041 943.41125 943.40527 957.0 0.001045 940.98828 940.98230 953.0 0.001049 938.59656 938.59045 949.0 0.001054 936.23578 936.22955 946.0 0.001057 933.90509 933.89880 942.0 0.001062 931.60443 931.59796 939.0 0.001065 929.33374 929.32733 936.0 0.001068 927.09198 927.08545 932.0 0.001073 924.87915 924.87280 930.0 0.001075 922.69495 922.68842 927.0 0.001079 920.53876 920.53235 924.0 0.001082 918.41064 918.40417 921.0 0.001086 916.30969 916.30322 917.0 0.001091 914.23621 914.22980 915.0 0.001093 912.18945 912.18280 911.0 0.001098 910.16895 910.16223 909.0 0.001100 908.17462 908.16821 906.0 0.001104 906.20618 906.19965 904.0 0.001106 904.26288 904.25629 902.0 0.001109 902.34515 902.33838 900.0 0.001111 900.45184 900.44501 898.0 0.001114 898.58282 898.57611 896.0 0.001116 896.73846 896.73175 894.0 0.001119 894.91754 894.91058 893.0 0.001120 893.11981 893.11298 890.0 0.001124 891.34583 891.33905 888.0 0.001126 889.59406 889.58722 886.0 0.001129 887.86517 887.85852 884.0 0.001131 886.15869 886.15167 881.0 0.001135 884.47363 884.46680 878.0 0.001139 882.81042 882.80365 876.0 0.001142 881.16888 881.16199 872.0 0.001147 879.54803 879.54114 870.0 0.001149 877.94763 877.94080 867.0 0.001153 876.36798 876.36108 864.0 0.001157 874.80859 874.80176 862.0 0.001160 873.26910 873.26215 860.0 0.001163 871.74878 871.74194 858.0 0.001166 870.24829 870.24133 856.0 0.001168 868.76666 868.75989 854.0 0.001171 867.30353 867.29675 852.0 0.001174 865.85913 865.85242 850.0 0.001176 864.43286 864.42615 847.0 0.001181 863.02441 863.01770 846.0 0.001182 861.63403 861.62732 843.0 0.001186 860.26111 860.25421 841.0 0.001189 858.90485 858.89813 839.0 0.001192 857.56586 857.55902 838.0 0.001193 856.24359 856.23688 836.0 0.001196 854.93768 854.93103 836.0 0.001196 853.64795 853.64130 835.0 0.001198 852.37433 852.36749 834.0 0.001199 851.11609 852.58905 832.0 0.001202 849.87360 851.45837 831.0 0.001203 848.64600 850.35760 830.0 0.001205 847.43365 849.29010 828.0 0.001208 846.23627 848.26282 828.0 0.001208 845.05304 847.28674 827.0 0.001209 843.88434 846.38141 827.0 0.001209 842.72980 845.58032 826.0 0.001211 841.58923 844.93890 827.0 0.001209 840.46216 844.54584 827.0 0.001209 839.34851 844.53979 828.0 0.001208 838.24786 845.12323 829.0 0.001206 837.16083 846.58051 830.0 0.001205 836.08636 849.28674 832.0 0.001202 835.02454 853.70416 833.0 0.001200 833.97540 860.35944 838.0 0.001193 832.93817 869.79187 843.0 0.001186 831.91315 882.47009 850.0 0.001176 830.89966 898.96899 859.0 0.001164 829.89819 919.03693 872.0 0.001147 828.90826 942.53162 887.0 0.001127 827.92938 968.80341 906.0 0.001104 826.96155 996.85162 928.0 0.001078 826.00525 1025.42456 953.0 0.001049 825.05908 1053.20935 981.0 0.001019 824.12378 1079.07056 1009.0 0.000991 823.19879 1102.34705 1035.0 0.000966 822.28400 1123.17700 1059.0 0.000944 821.37939 1142.63660 1080.0 0.000926 820.48474 1162.51001 1095.0 0.000913 819.59985 1184.65881 1109.0 0.000902 818.72424 1210.25049 1124.0 0.000890 817.85834 1239.15637 1144.0 0.000874 817.00183 1269.68909 1171.0 0.000854 816.15411 1298.71704 1208.0 0.000828 815.31567 1322.16638 1250.0 0.000800 814.48602 1335.78870 1291.0 0.000775 813.66504 1336.04041 1324.0 0.000755 812.85260 1320.86523 1339.0 0.000747 812.04816 1290.16077 1329.0 0.000752 811.25250 1245.84119 1291.0 0.000775 810.46472 1191.45667 1230.0 0.000813 809.68500 1131.53076 1152.0 0.000868 808.91327 1070.75342 1069.0 0.000935 808.14893 1013.24701 990.0 0.001010 807.39215 962.07153 924.0 0.001082 806.64337 918.99768 874.0 0.001144 805.90167 884.55957 840.0 0.001190 805.16693 858.31812 819.0 0.001221 804.43958 839.18884 808.0 0.001238 803.71924 825.79309 802.0 0.001247 803.00543 816.72925 799.0 0.001252 802.29877 810.75012 798.0 0.001253 801.59839 806.85089 796.0 0.001256 800.90515 802.86774 795.0 0.001258 800.21753 801.20868 793.0 0.001261 799.53687 800.01617 792.0 0.001263 798.86230 798.85724 790.0 0.001266 798.19366 798.18872 789.0 0.001267 797.53119 797.52612 787.0 0.001271 796.87457 796.86945 787.0 0.001271 796.22345 796.21893 785.0 0.001274 795.57837 795.57361 785.0 0.001274 794.93903 794.93439 784.0 0.001276 794.30493 794.30035 784.0 0.001276 793.67645 793.67163 783.0 0.001277 793.05341 793.04865 783.0 0.001277 792.43549 792.43091 782.0 0.001279 791.82281 791.81805 781.0 0.001280 791.21509 791.21063 781.0 0.001280 790.61249 790.60797 780.0 0.001282 790.01495 790.01038 779.0 0.001284 789.42224 789.41779 779.0 0.001284 788.83423 788.82990 777.0 0.001287 788.25098 788.24646 777.0 0.001287 787.67242 787.66803 776.0 0.001289 787.09821 787.09381 776.0 0.001289 786.52875 786.52460 776.0 0.001289 785.96387 785.95953 776.0 0.001289 785.40314 785.39868 776.0 0.001289 784.84656 784.84216 777.0 0.001287 784.29462 784.29016 777.0 0.001287 783.74628 783.74207 778.0 0.001285 783.20245 783.19818 778.0 0.001285 782.66266 782.65839 778.0 0.001285 782.12683 782.12250 778.0 0.001285 781.59485 781.59076 777.0 0.001287 781.06683 781.06268 776.0 0.001289 780.54272 780.53864 776.0 0.001289 780.02209 780.01813 775.0 0.001290 779.50568 779.50153 775.0 0.001290 778.99274 778.98871 774.0 0.001292 778.48340 778.47925 774.0 0.001292 777.97748 777.97345 774.0 0.001292 777.47534 777.47150 775.0 0.001290 776.97668 776.97272 775.0 0.001290 776.48132 776.47736 775.0 0.001290 775.98932 775.98553 775.0 0.001290 775.50079 775.49701 775.0 0.001290 775.01569 775.01178 774.0 0.001292 774.53400 774.53009 774.0 0.001292 774.05518 774.05157 774.0 0.001292 773.57977 773.57593 774.0 0.001292 773.10767 773.10376 774.0 0.001292 772.63837 772.63470 774.0 0.001292 772.17242 772.16864 775.0 0.001290 771.70947 771.70575 774.0 0.001292 771.24963 771.24603 775.0 0.001290 770.79285 770.78900 775.0 0.001290 770.33893 770.33521 775.0 0.001290 769.88818 769.88452 775.0 0.001290 769.44006 769.43646 775.0 0.001290 768.99518 768.99146 775.0 0.001290 768.55310 768.54926 776.0 0.001289 768.11346 768.11011 776.0 0.001289 767.67712 767.67365 776.0 0.001289 767.24377 767.23981 776.0 0.001289 766.81274 766.80914 777.0 0.001287 766.38483 766.38098 777.0 0.001287 765.95947 765.95587 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775.66486 3866.66870 2947.0 0.0003393 775.99005 3227.41577 2331.0 0.000429 776.31439 2704.09521 1899.0 0.000527 776.63806 2291.86523 1619.0 0.000618 776.96094 1979.00146 1451.0 0.000689 777.28308 1749.75854 1357.0 0.000737 777.60431 1587.14087 1314.0 0.000761 777.92456 1475.31311 1300.0 0.000769 778.24402 1401.09399 1309.0 0.000764 778.56250 1354.93433 1338.0 0.000747 778.88007 1331.26477 1384.0 0.000723 779.19684 1328.32971 1454.0 0.000688 779.51233 1347.73779 1545.0 0.000647 779.82697 1393.91956 1664.0 0.000601 780.14026 1473.50232 1814.0 0.000551 780.45282 1594.61292 1996.0 0.000501 780.76398 1766.00195 2215.0 0.000451 781.07404 1995.90796 2475.0 0.000404 781.38306 2290.81812 2776.0 0.000360 781.69080 2654.00659 3123.0 0.0003202 781.99713 3083.98779 3514.0 0.0002846 782.30261 3509.27319 3947.0 0.0002534 782.60645 4047.69141 4416.0 0.0002264 782.90906 4620.08154 4906.0 0.0002038 783.21014 5176.79736 5403.0 0.0001851 783.51025 5693.43408 5874.0 0.0001702 783.80872 6130.99756 6287.0 0.0001591 784.10565 6450.23535 6596.0 0.0001516 784.40143 6618.08691 6763.0 0.0001479 784.69537 6615.30127 6750.0 0.0001481 784.98798 6442.34863 6539.0 0.0001529 785.27930 6119.10791 6132.0 0.0001631 785.56873 5679.06299 5561.0 0.0001798 785.85675 5161.45703 4878.0 0.0002050 786.14288 4604.78271 4147.0 0.0002411 786.42767 4042.37061 3433.0 0.0002913 786.71082 3504.57788 2796.0 0.000358 786.99194 3011.30176 2268.0 0.000441 787.27148 2576.41943 1863.0 0.000537 787.54956 2207.22559 1577.0 0.000634 787.82574 1905.30933 1392.0 0.000718 788.09985 1668.05591 1285.0 0.000778 788.37238 1490.21252 1234.0 0.000810 788.64307 1365.24902 1221.0 0.000819 788.91180 1286.59717 1234.0 0.000810 789.17865 1248.44580 1265.0 0.000791 789.44348 1246.09314 1311.0 0.000763 789.70654 1275.95764 1371.0 0.000729 789.96759 1335.23474 1445.0 0.000692 790.22662 1421.36646 1533.0 0.000652 790.48370 1531.40979 1635.0 0.000612 790.73865 1661.41516 1751.0 0.000571 790.99158 1805.95313 1881.0 0.000532 791.24261 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