data_TRANDOLAPRIL_C03327 _pd_block_id 2016-01-14T13:02|TRANDOLAPRIL|Joel_Reid|CMCF2 _audit_creation_method "from EXP file using GSAS2CIF" _audit_creation_date 2016-01-14T13:02 _audit_author_name "Joel Reid" _audit_update_record ; 2016-01-14T13:02 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 _publ_contact_author_name 'Reid, Joel' _publ_contact_author_address '44 Innovation Boulevard, Saskatoon, SK, S7H 3G5' _publ_contact_author_email 'joel.reid@lightsource.ca' _publ_contact_author_phone '(306) 374-0387' #============================================================================== # 2. TITLE AND AUTHOR LIST # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Reid, Joel W.' 'Canadian Light Source' 'Kaduk, James A.' 'Illinois Institute of Technology' 'Vickers, Martin' 'Department of Chemistry, University College London' #============================================================================== # 3. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _chemical_name_systematic ; (2S,3aR,7aS)-1-[(2S)-2-[[(2S)-1-ethoxy-1-oxo-4-phenylbutan-2-yl]amino]propanoyl] -2,3,3a,4,5,6,7,7a-octahydroindole-2-carboxylic acid ; _chemical_name_common Trandolapril _chemical_formula_moiety 'C24 H34 N2 O5' _exptl_crystal_density_diffrn 1.251 _cell_measurement_temperature 293 _pd_char_colour white # The following item identifies the program(s) used (if appropriate). _computing_structure_solution FOX # Phase information from GSAS _pd_phase_name TRANDOLAPRIL-22.66-AvogH.cif _cell_length_a 19.77201(22) _cell_length_b 15.07392(20) _cell_length_c 7.67425(11) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 2287.25(6) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M "P 21 21 21" _symmetry_space_group_name_Hall "P 2ac 2ab" loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 +x+1/2,-y+1/2,-z 3 -x,+y+1/2,-z+1/2 4 -x+1/2,-y,+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 C1 0.2164(7) 0.6672(8) 0.5965(20) 1.0 Uiso 0.0323(11) 4 C C2 0.1448(6) 0.7051(7) 0.5631(20) 1.0 Uiso 0.0323(11) 4 O O3 0.1349(4) 0.7712(5) 0.4793(12) 1.0 Uiso 0.0323(11) 4 O O4 0.0975(5) 0.6614(5) 0.6450(13) 1.0 Uiso 0.0323(11) 4 C C5 0.0292(5) 0.6932(8) 0.6166(18) 1.0 Uiso 0.0323(11) 4 C C6 -0.0185(5) 0.6353(9) 0.7137(19) 1.0 Uiso 0.0323(11) 4 C C7 0.2441(7) 0.7076(8) 0.7659(19) 1.0 Uiso 0.0323(11) 4 C C8 0.2528(7) 0.8081(8) 0.7616(18) 1.0 Uiso 0.0323(11) 4 C C9 0.2740(7) 0.8484(8) 0.9313(17) 1.0 Uiso 0.0323(11) 4 C C10 0.2389(6) 0.8358(8) 1.0858(23) 1.0 Uiso 0.0323(11) 4 C C11 0.2519(7) 0.8840(10) 1.2388(17) 1.0 Uiso 0.0323(11) 4 C C12 0.3033(7) 0.9485(9) 1.2348(17) 1.0 Uiso 0.0323(11) 4 C C13 0.3376(7) 0.9623(7) 1.0809(25) 1.0 Uiso 0.0323(11) 4 C C14 0.3257(7) 0.9112(10) 0.9347(18) 1.0 Uiso 0.0323(11) 4 C C15 0.5603(6) 0.5419(8) 0.8771(23) 1.0 Uiso 0.0323(11) 4 C C16 0.5629(5) 0.6165(10) 1.0126(17) 1.0 Uiso 0.0323(11) 4 C C17 0.5365(7) 0.7034(8) 0.9281(20) 1.0 Uiso 0.0323(11) 4 C C18 0.4908(6) 0.5336(8) 0.8053(18) 1.0 Uiso 0.0323(11) 4 C C19 0.4716(5) 0.4621(7) 0.6762(20) 1.0 Uiso 0.0323(11) 4 C C20 0.4718(6) 0.6162(8) 0.7170(17) 1.0 Uiso 0.0323(11) 4 C C21 0.4677(6) 0.6928(8) 0.8465(20) 1.0 Uiso 0.0323(11) 4 C C22 0.4028(5) 0.4977(7) 0.6132(17) 1.0 Uiso 0.0323(11) 4 N N23 0.4103(5) 0.5940(6) 0.6208(14) 1.0 Uiso 0.0323(11) 4 C C24 0.3741(6) 0.6528(6) 0.5255(16) 1.0 Uiso 0.0323(11) 4 C C25 0.3122(6) 0.6181(7) 0.4314(16) 1.0 Uiso 0.0323(11) 4 C C26 0.3466(6) 0.4547(6) 0.7212(18) 1.0 Uiso 0.0323(11) 4 O O27 0.31680(35) 0.5033(4) 0.8310(14) 1.0 Uiso 0.0323(11) 4 N N28 0.2536(6) 0.6816(7) 0.4334(15) 1.0 Uiso 0.0323(11) 4 O O29 0.3335(4) 0.3747(5) 0.7058(13) 1.0 Uiso 0.0323(11) 4 O O30 0.3833(4) 0.7340(5) 0.5354(13) 1.0 Uiso 0.0323(11) 4 C C31 0.3364(6) 0.6101(8) 0.2449(18) 1.0 Uiso 0.0323(11) 4 H H32 0.22058 0.59727 0.62272 1.0 Uiso 0.0420(14) 4 H H33 0.01662 0.68896 0.4802 1.0 Uiso 0.0420(14) 4 H H34 0.02421 0.76097 0.65613 1.0 Uiso 0.0420(14) 4 H H35 -0.01354 0.56947 0.67592 1.0 Uiso 0.0420(14) 4 H H36 -0.0692 0.6589 0.69629 1.0 Uiso 0.0420(14) 4 H H37 -0.00639 0.64179 0.85289 1.0 Uiso 0.0420(14) 4 H H38 0.29209 0.67951 0.79279 1.0 Uiso 0.0420(14) 4 H H39 0.20651 0.69597 0.86353 1.0 Uiso 0.0420(14) 4 H H40 0.20584 0.83718 0.72412 1.0 Uiso 0.0420(14) 4 H H41 0.29322 0.82091 0.67305 1.0 Uiso 0.0420(14) 4 H H42 0.20206 0.78749 1.091 1.0 Uiso 0.0420(14) 4 H H43 0.22589 0.87075 1.35417 1.0 Uiso 0.0420(14) 4 H H44 0.31128 0.99183 1.33849 1.0 Uiso 0.0420(14) 4 H H45 0.37697 1.00627 1.07653 1.0 Uiso 0.0420(14) 4 H H46 0.35374 0.91995 0.82236 1.0 Uiso 0.0420(14) 4 H H47 0.59413 0.55769 0.77172 1.0 Uiso 0.0420(14) 4 H H48 0.5745 0.47974 0.93354 1.0 Uiso 0.0420(14) 4 H H49 0.61426 0.62203 1.05829 1.0 Uiso 0.0420(14) 4 H H50 0.53205 0.59679 1.12257 1.0 Uiso 0.0420(14) 4 H H51 0.53522 0.75265 1.03048 1.0 Uiso 0.0420(14) 4 H H52 0.57286 0.72166 0.83094 1.0 Uiso 0.0420(14) 4 H H53 0.4649 0.51627 0.92335 1.0 Uiso 0.0420(14) 4 H H54 0.50774 0.45688 0.5752 1.0 Uiso 0.0420(14) 4 H H55 0.4697 0.39693 0.73301 1.0 Uiso 0.0420(14) 4 H H56 0.50772 0.64283 0.62621 1.0 Uiso 0.0420(14) 4 H H57 0.43179 0.67841 0.94645 1.0 Uiso 0.0420(14) 4 H H58 0.4542 0.75319 0.78413 1.0 Uiso 0.0420(14) 4 H H59 0.38972 0.48164 0.48178 1.0 Uiso 0.0420(14) 4 H H60 0.29391 0.55834 0.49387 1.0 Uiso 0.0420(14) 4 H H61 0.3281 0.56335 0.83876 1.0 Uiso 0.0420(14) 4 H H62 0.22277 0.66934 0.32738 1.0 Uiso 0.0420(14) 4 H H63 0.35292 0.67396 0.20079 1.0 Uiso 0.0420(14) 4 H H64 0.29621 0.58701 0.16448 1.0 Uiso 0.0420(14) 4 H H65 0.37788 0.56452 0.23939 1.0 Uiso 0.0420(14) 4 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum "C24 H34 N2 O5" _chemical_formula_weight 430.54 _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 C1 C2 1.548(13) . 1_555 N C1 C7 1.536(13) . 1_555 N C1 N28 1.467(14) . 1_555 N C2 C1 1.548(13) . 1_555 N C2 O3 1.201(11) . 1_555 N C2 O4 1.305(11) . 1_555 N O3 C2 1.201(11) . 1_555 N O4 C2 1.305(11) . 1_555 N O4 C5 1.449(10) . 1_555 N C5 O4 1.449(10) . 1_555 N C5 C6 1.486(14) . 1_555 N C6 C5 1.486(14) . 1_555 N C7 C1 1.536(13) . 1_555 N C7 C8 1.525(13) . 1_555 N C8 C7 1.525(13) . 1_555 N C8 C9 1.496(12) . 1_555 N C9 C8 1.496(12) . 1_555 N C9 C10 1.386(12) . 1_555 N C9 C14 1.395(10) . 1_555 N C10 C9 1.386(12) . 1_555 N C10 C11 1.404(12) . 1_555 N C11 C10 1.404(12) . 1_555 N C11 C12 1.406(12) . 1_555 N C12 C11 1.406(12) . 1_555 N C12 C13 1.378(14) . 1_555 N C13 C12 1.378(14) . 1_555 N C13 C14 1.382(12) . 1_555 N C14 C9 1.395(10) . 1_555 N C14 C13 1.382(12) . 1_555 N C15 C16 1.532(13) . 1_555 N C15 C18 1.485(11) . 1_555 N C16 C15 1.532(13) . 1_555 N C16 C17 1.553(15) . 1_555 N C17 C16 1.553(15) . 1_555 N C17 C21 1.505(11) . 1_555 N C18 C15 1.485(11) . 1_555 N C18 C19 1.512(15) . 1_555 N C18 C20 1.466(11) . 1_555 N C19 C18 1.512(15) . 1_555 N C19 C22 1.540(9) . 1_555 N C20 C18 1.466(11) . 1_555 N C20 C21 1.525(12) . 1_555 N C20 N23 1.461(9) . 1_555 N C21 C17 1.505(11) . 1_555 N C21 C20 1.525(12) . 1_555 N C22 C19 1.540(9) . 1_555 N C22 N23 1.461(9) . 1_555 N C22 C26 1.530(8) . 1_555 N N23 C20 1.461(9) . 1_555 N N23 C22 1.461(9) . 1_555 N N23 C24 1.355(9) . 1_555 N C24 N23 1.355(9) . 1_555 N C24 C25 1.514(10) . 1_555 N C24 O30 1.239(9) . 1_555 N C25 C24 1.514(10) . 1_555 N C25 N28 1.503(12) . 1_555 N C25 C31 1.514(14) . 1_555 N C26 C22 1.530(8) . 1_555 N C26 O27 1.263(11) . 1_555 N C26 O29 1.238(10) . 1_555 N O27 C26 1.263(11) . 1_555 N N28 C1 1.467(14) . 1_555 N N28 C25 1.503(12) . 1_555 N O29 C26 1.238(10) . 1_555 N O30 C24 1.239(9) . 1_555 N C31 C25 1.514(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 C2 C1 C7 108.6(12) 1_555 . 1_555 N C2 C1 N28 105.2(12) 1_555 . 1_555 N C7 C1 N28 119.0(13) 1_555 . 1_555 N C1 C2 O3 122.9(11) 1_555 . 1_555 N C1 C2 O4 112.9(10) 1_555 . 1_555 N O3 C2 O4 124.0(10) 1_555 . 1_555 N C2 O4 C5 115.4(8) 1_555 . 1_555 N O4 C5 C6 108.8(10) 1_555 . 1_555 N C1 C7 C8 114.6(11) 1_555 . 1_555 N C7 C8 C9 114.6(12) 1_555 . 1_555 N C8 C9 C10 123.4(13) 1_555 . 1_555 N C8 C9 C14 119.8(14) 1_555 . 1_555 N C10 C9 C14 116.3(8) 1_555 . 1_555 N C9 C10 C11 123.6(9) 1_555 . 1_555 N C10 C11 C12 118.1(9) 1_555 . 1_555 N C11 C12 C13 118.6(9) 1_555 . 1_555 N C12 C13 C14 121.9(8) 1_555 . 1_555 N C9 C14 C13 121.2(9) 1_555 . 1_555 N C16 C15 C18 110.2(9) 1_555 . 1_555 N C15 C16 C17 108.9(11) 1_555 . 1_555 N C16 C17 C21 112.8(10) 1_555 . 1_555 N C15 C18 C19 122.3(13) 1_555 . 1_555 N C15 C18 C20 109.6(10) 1_555 . 1_555 N C19 C18 C20 103.8(11) 1_555 . 1_555 N C18 C19 C22 100.3(9) 1_555 . 1_555 N C18 C20 C21 110.8(10) 1_555 . 1_555 N C18 C20 N23 104.5(10) 1_555 . 1_555 N C21 C20 N23 117.3(11) 1_555 . 1_555 N C17 C21 C20 107.7(9) 1_555 . 1_555 N C19 C22 N23 104.0(8) 1_555 . 1_555 N C19 C22 C26 108.9(11) 1_555 . 1_555 N N23 C22 C26 118.3(9) 1_555 . 1_555 N C20 N23 C22 109.5(9) 1_555 . 1_555 N C20 N23 C24 124.3(9) 1_555 . 1_555 N C22 N23 C24 125.1(10) 1_555 . 1_555 N N23 C24 C25 117.3(7) 1_555 . 1_555 N N23 C24 O30 122.4(9) 1_555 . 1_555 N C25 C24 O30 119.3(9) 1_555 . 1_555 N C24 C25 N28 113.5(9) 1_555 . 1_555 N C24 C25 C31 102.8(10) 1_555 . 1_555 N N28 C25 C31 107.7(10) 1_555 . 1_555 N C22 C26 O27 117.1(8) 1_555 . 1_555 N C22 C26 O29 120.8(8) 1_555 . 1_555 N O27 C26 O29 122.1(10) 1_555 . 1_555 N C1 N28 C25 107.5(10) 1_555 . 1_555 N # Powder diffraction data for histogram 1 #============================================================================== # 4. INSTRUMENT CHARACTERIZATION _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_target Cu _diffrn_source_type ? _diffrn_measurement_device_type 'Stoe StadiP' _diffrn_detector '18 deg PSD' _diffrn_detector_type 'Dectris® Mythen 1K' # make or model of detector _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) # Specimen size and mounting information _pd_spec_mounting '0.5 mm glass capillary' _pd_spec_mount_mode transmission _pd_spec_shape cylindrical #============================================================================== # 5. REFINEMENT DETAILS _refine_ls_shift/su_max 0.02 _refine_ls_shift/su_mean 0.00 _computing_structure_refinement GSAS _refine_ls_number_parameters 124 _refine_ls_goodness_of_fit_all 4.75 _refine_ls_number_restraints 80 _refine_ls_matrix_type full _refine_ls_hydrogen_treatment refU 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 96.0 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 20.0 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 N 8.0 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 H 136.0 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 ? _diffrn_radiation_wavelength 1.54059 _diffrn_radiation_type 'Cu K\a1' _pd_proc_ls_prof_R_factor 0.0242 _pd_proc_ls_prof_wR_factor 0.0328 _pd_proc_ls_prof_wR_expected 0.0071 _refine_ls_R_Fsqd_factor 0.04343 _pd_proc_ls_background_function ; GSAS Background function number 1 with 16 terms. Shifted Chebyshev function of 1st kind 1: 12846.5 2: -7988.08 3: -1032.51 4: 2829.42 5: -600.937 6: -1295.81 7: 1045.50 8: 490.883 9: -1031.70 10: 379.967 11: 423.002 12: -464.542 13: -18.8041 14: 371.633 15: -277.759 16: -14.0571 ; _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 3 with 19 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. #1(GU) = 173.053 #2(GV) = -30.719 #3(GW) = 8.618 #4(GP) = 0.000 #5(LX) = 0.008 #6(LY) = 3.990 #7(S/L) = 0.0207 #8(H/L) = 0.0204 #9(trns) = 0.00 #10(shft)= 0.0000 #11(stec)= 0.00 #12(ptec)= 0.00 #13(sfec)= 0.00 #14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000 #17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0001 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00010 _pd_proc_info_datetime 2016-01-14T13:02:00 _pd_calc_method "Rietveld Refinement" #---- raw/calc data loop ----- _pd_meas_2theta_range_min 5.0 _pd_meas_2theta_range_max 59.915 _pd_meas_2theta_range_inc 0.015 _pd_proc_2theta_range_min 4.99535 _pd_proc_2theta_range_max 59.91035 _pd_proc_2theta_range_inc 0.015 loop_ _pd_meas_counts_total _pd_proc_ls_weight _pd_proc_intensity_bkg_calc _pd_calc_intensity_total 17794.0 0.0000562 17043.87891 17043.93750 17964.0 0.0000557 17097.91406 17097.97070 17859.0 0.0000560 17150.39453 17150.44727 17735.0 0.0000564 17201.34766 17201.39648 17739.0 0.0000564 17250.80664 17250.85156 17792.0 0.0000562 17298.80078 17298.84180 17662.0 0.0000566 17345.36328 17345.39844 17907.0 0.0000558 17390.51563 17390.54883 17906.0 0.0000558 17434.29297 17434.32227 17730.0 0.0000564 17476.72461 17476.75000 18022.0 0.0000555 17517.83398 17517.85547 17889.0 0.0000559 17557.65039 17557.66992 17647.0 0.0000567 17596.20117 17596.21875 17890.0 0.0000559 17633.51758 17633.53125 17646.0 0.0000567 17669.61719 17669.62891 17739.0 0.0000564 17704.53320 17704.54297 17785.0 0.0000562 17738.28906 17738.29688 17777.0 0.0000563 17770.91211 17770.91602 17604.0 0.0000568 17802.42383 17802.42383 17775.0 0.0000563 17832.84961 17832.84766 17700.0 0.0000565 17862.21484 17862.21094 17805.0 0.0000562 17890.54102 17890.53711 17953.0 0.0000557 17917.85352 17917.84766 17817.0 0.0000561 17944.17578 17944.16797 17759.0 0.0000563 17969.53125 17969.51953 17982.0 0.0000556 17993.93750 17993.92578 17922.0 0.0000558 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5634.92627 9480.43359 9350.0 0.0001070 5633.51074 9556.59277 9211.0 0.0001086 5632.13867 9493.75781 9003.0 0.0001111 5630.80908 9306.93945 8822.0 0.0001134 5629.52344 9023.49902 8620.0 0.0001160 5628.28125 8676.45117 8152.0 0.0001227 5627.08350 8299.20898 7770.0 0.0001287 5625.93066 7921.38184 7275.0 0.0001375 5624.82275 7565.53516 6938.0 0.0001441 5623.76123 7245.69482 6858.0 0.0001458 5622.74463 6968.07031 6622.0 0.0001510 5621.77490 6733.24951 6511.0 0.0001536 5620.85205 6538.74561 6368.0 0.0001570 5619.97607 6381.05176 6393.0 0.0001564 5619.14697 6256.99951 6339.0 0.0001578 5618.36670 6164.17383 6195.0 0.0001614 5617.63330 6100.86475 6118.0 0.0001635 5616.94873 6065.72607 6209.0 0.0001611 5616.31348 6057.24561 6225.0 0.0001606 5615.72607 6073.56982 6192.0 0.0001615 5615.18848 6112.08594 6237.0 0.0001603 5614.70020 6169.38037 6281.0 0.0001592 5614.26221 6241.41455 6481.0 0.0001543 5613.87305 6324.03711 6596.0 0.0001516 5613.53467 6413.66504 6664.0 0.0001501 5613.24707 6508.11523 6586.0 0.0001518 5613.00928 6606.65967 6738.0 0.0001484 5612.82227 6709.61963 6876.0 0.0001454 5612.68652 6817.87646 6842.0 0.0001462 5612.60156 6932.56055 7213.0 0.0001386 5612.56738 7054.56934 7345.0 0.0001361 5612.58496 7183.19043 7604.0 0.0001315 5612.65332 7314.17578 7808.0 0.0001281 5612.77344 7438.65967 8028.0 0.0001246 5612.94482 7543.14795 7785.0 0.0001285 5613.16797 7612.40967 8016.0 0.0001248 5613.44238 7632.83838 7934.0 0.0001260 5613.76758 7596.39795 7628.0 0.0001311 5614.14502 7502.88721 7558.0 0.0001323 5614.57324 7360.00537 7381.0 0.0001355 5615.05273 7182.28564 7079.0 0.0001413 5615.58350 6988.65479 6966.0 0.0001436 5616.16553 6799.20898 6853.0 0.0001459 5616.79834 6632.13574 6491.0 0.0001541 5617.48145 6501.51807 6404.0 0.0001562 5618.21582 6416.16895 6306.0 0.0001586 5618.99951 6379.01611 6284.0 0.0001591 5619.83398 6387.26367 6357.0 0.0001573 5620.71826 6433.18652 6602.0 0.0001515 5621.65137 6505.21680 6549.0 0.0001527 5622.63428 6589.44727 6609.0 0.0001513 5623.66553 6671.46582 6564.0 0.0001523 5624.74561 6738.38037 6731.0 0.0001486 5625.87305 6781.51270 6699.0 0.0001493 5627.04883 6798.40234 6773.0 0.0001476 5628.27148 6793.16699 6632.0 0.0001508 5629.54053 6774.23438 6686.0 0.0001496 5630.85547 6751.04102 6834.0 0.0001463 5632.21582 6731.30615 6676.0 0.0001498 5633.62109 6719.48926 6700.0 0.0001493 5635.07129 6716.26514 6499.0 0.0001539 5636.56445 6719.17578 6452.0 0.0001550 5638.10059 6723.96729 6645.0 0.0001505 5639.67871 6726.77979 6573.0 0.0001521 5641.29834 6725.78467 6855.0 0.0001459 5642.95850 6721.51123 6788.0 0.0001473 5644.65820 6715.12842 6801.0 0.0001470 5646.39697 6706.93457 6803.0 0.0001470 5648.17383 6695.39941 6777.0 0.0001476 5649.98682 6677.09766 6678.0 0.0001497 5651.83643 6647.60596 6645.0 0.0001505 5653.72021 6603.22119 6634.0 0.0001507 5655.63818 6542.71875 6651.0 0.0001504 5657.58936 6468.16748 6476.0 0.0001544 5659.57129 6384.43604 6360.0 0.0001572 5661.58350 6298.03418 6319.0 0.0001583 5663.62451 6215.84424 6195.0 0.0001614 5665.69287 6144.07422 6122.0 0.0001633 5667.78809 6087.43750 6065.0 0.0001649 5669.90820 6048.72070 6050.0 0.0001653 5672.05176 6028.63623 5987.0 0.0001670 5674.21729 6025.86182 5909.0 0.0001692 5676.40283 6037.61719 5956.0 0.0001679 5678.60742 6059.85107 6053.0 0.0001652 5680.82861 6087.87646 6105.0 0.0001638 5683.06543 6116.72168 6133.0 0.0001631 5685.31641 6141.95361 6088.0 0.0001643 5687.57813 6160.53125 6236.0 0.0001604 5689.85059 6171.59180 6190.0 0.0001616 5692.13037 6176.73193 6190.0 0.0001616 5694.41650 6179.60547 6293.0 0.0001589 5696.70605 6184.72656 6298.0 0.0001588 5698.99854 6196.71680 6314.0 0.0001584 5701.29004 6219.62158 6295.0 0.0001589 5703.57861 6256.52490 6383.0 0.0001567 5705.86230 6309.02295 6420.0 0.0001558 5708.13916 6376.95166 6505.0 0.0001537 5710.40576 6458.32715 6557.0 0.0001525 5712.66113 6549.55859 6632.0 0.0001508 5714.90137 6645.33838 6646.0 0.0001505 5717.12402 6738.93457 6761.0 0.0001479 5719.32666 6821.98584 6806.0 0.0001469 5721.50635 6885.30371 6980.0 0.0001433 5723.66113 6920.07227 6971.0 0.0001435 5725.78662 6919.59570 6825.0 0.0001465 5727.88135 6881.07813 6894.0 0.0001451 5729.94092 6806.86572 6707.0 0.0001491 5731.96289 6704.35205 6698.0 0.0001493 5733.94385 6584.22168 6385.0 0.0001566 5735.88037 6458.19531 6298.0 0.0001588 5737.77002 6337.23096 6194.0 0.0001614 5739.60840 6230.47412 6052.0 0.0001652 5741.39209 6144.81006 5961.0 0.0001678 5743.11768 6084.76465 5921.0 0.0001689 5744.78125 6052.74561 5980.0 0.0001672 5746.37988 6049.42041 5796.0 0.0001725 5747.90820 6073.82813 6097.0 0.0001640 5749.36426 6123.89111 6118.0 0.0001635 5750.74219 6196.33887 6350.0 0.0001575 5752.03857 6286.77344 6433.0 0.0001554 5753.24902 6389.67725 6448.0 0.0001551 5754.36914 6498.63428 6386.0 0.0001566 5755.39502 6606.57227 6542.0 0.0001529 5756.32227 6706.43604 6555.0 0.0001526 5757.14551 6792.22607 6736.0 0.0001485 5757.86035 6860.09766 6857.0 0.0001458 5758.46240 6908.54395 6755.0 0.0001480 5758.94580 6937.42969 6829.0 0.0001464 5759.30664 6946.60059 6758.0 0.0001480 5759.53906 6935.04932 6721.0 0.0001488 5759.63818 6901.05713 6762.0 0.0001479 5759.59912 6843.34717 6627.0 0.0001509 5759.41553 6762.69531 6307.0 0.0001586 5759.08252 6662.93604 6113.0 0.0001636 5758.59375 6550.52295 6212.0 0.0001610 5757.94434 6433.06201 6115.0 0.0001635 5757.12744 6317.88721 6052.0 0.0001652 5756.13770 6211.15918 5991.0 0.0001669 5754.96973 6117.22266 6021.0 0.0001661 5753.61572 6038.57324 5946.0 0.0001682 5752.07031 5975.78223 5892.0 0.0001697 5750.32666 5927.87891 5933.0 0.0001685 5748.37793 5892.78662 5907.0 0.0001693 5746.21777 5867.88867 5967.0 0.0001676 5743.84033 5850.52002 5975.0 0.0001674 5741.23633 5838.39111 5823.0 0.0001717 5738.40088 5829.81543 5954.0 0.0001680 5735.32520 5823.85742 5880.0 0.0001701 5732.00195 5820.22070 5826.0 0.0001716 5728.42480 5819.06396 5999.0 0.0001667 5724.58545 5820.76172 6000.0 0.0001667 5720.47607 5825.72168 5880.0 0.0001701 5716.08838 5834.15234 5861.0 0.0001706 5711.41504 5845.96484 5886.0 0.0001699 5706.44727 5860.64844 5978.0 0.0001673 5701.17529 5877.24463 6145.0 0.0001627 5695.59375 5894.40820 5975.0 0.0001674 5689.69189 5910.53320 5991.0 0.0001669 5683.46191 5924.04541 6225.0 0.0001606 5676.89355 5933.76855 6154.0 0.0001625 5669.97900 5939.23242 6237.0 0.0001603 5662.70557 5940.82373 0.0 . . . _pd_meas_number_of_points 3662 _pd_proc_number_of_points 3662 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_observed_status _refln_F_squared_meas _refln_F_squared_calc _refln_phase_calc _refln_d_spacing _gsas_i100_meas 1 1 0 o 3790.536 3762.033 -90.00 11.98749 62.79 2 0 0 o 2988.939 2999.554 180.00 9.88600 17.71 2 1 0 o 196.226 256.085 0.00 8.26675 1.57 0 2 0 o 1012.537 1042.858 180.00 7.53696 3.28 1 0 1 o 8495.793 8264.774 90.00 7.15425 24.41 1 2 0 o 999.393 988.710 -90.00 7.04263 5.63 0 1 1 o 5233.367 5149.458 90.00 6.83896 14.37 1 1 1 o 187.297 174.587 -105.66 6.46325 0.95 2 0 1 o 371.776 357.988 90.00 6.06210 0.88 3 1 0 o 4616.980 4569.903 -90.00 6.03870 19.78 2 2 0 o 1290.288 1277.722 0.00 5.99374 5.26 2 1 1 o 4547.385 4515.648 -16.57 5.62432 19.74 0 2 1 o 6168.418 6216.012 0.00 5.37732 12.79 1 2 1 o 25311.043 25311.049 26.12 5.18884 100.00 3 0 1 o 777.749 776.307 90.00 4.99991 1.48 3 2 0 o 2167.933 2181.309 -90.00 4.96134 6.06 4 0 0 o 3654.621 3700.251 0.00 4.94300 5.29 1 3 0 o 1778.952 1836.026 90.00 4.86985 4.72 3 1 1 o 5689.921 5707.405 -14.31 4.74566 20.11 2 2 1 o 7434.018 7519.421 16.09 4.72374 25.86 4 1 0 o 366.922 416.546 0.00 4.69692 0.94 2 3 0 o 4295.153 4319.130 -180.00 4.47928 9.59 0 3 1 o 8716.406 8437.979 -90.00 4.20375 12.86 3 2 1 o 194.934 189.528 54.63 4.16647 0.57 4 0 1 o 10570.525 10460.446 90.00 4.15559 15.65 4 2 0 o 1765.669 1737.762 180.00 4.13337 3.42 1 3 1 o 10460.781 10351.225 115.91 4.11184 29.78 4 1 1 o 7610.807 7446.097 -97.44 4.00615 21.19 3 3 0 o 1621.983 1552.712 90.00 3.99583 2.87 2 3 1 o 4922.266 4748.648 8.89 3.86853 12.69 0 0 2 o 1196.227 1241.956 180.00 3.83713 0.46 5 1 0 o 3134.125 3124.241 90.00 3.82497 5.28 0 4 0 o 2305.595 2228.360 180.00 3.76848 1.80 1 0 2 o 2340.490 2236.037 -180.00 3.76685 1.75 0 1 2 o 1125.968 1102.059 -90.00 3.71854 0.83 1 4 0 o 5.075 6.636 -90.00 3.70184 0.01 1 1 2 o 5555.533 5576.320 23.26 3.65447 7.95 4 2 1 o 6299.466 6317.474 33.79 3.63910 14.86 2 0 2 o 0.000 86.741 0.00 3.57713 0.00 3 3 1 o 2395.646 2389.427 -138.69 3.54418 5.34 4 3 0 o 4154.015 4180.377 0.00 3.52374 5.67 2 4 0 o 1937.678 1935.731 0.00 3.52132 2.61 5 0 1 o 76.298 74.954 90.00 3.51518 0.09 5 2 0 o 3406.145 3406.409 90.00 3.50170 4.69 2 1 2 o 1005.971 1069.023 -83.07 3.48047 1.33 5 1 1 o 2670.285 2734.377 -80.19 3.42333 5.78 0 2 2 o 8770.095 8912.388 180.00 3.41948 5.74 0 4 1 o 1632.532 1844.235 -180.00 3.38265 1.68 1 2 2 o 1845.501 1777.148 -84.03 3.36946 2.37 1 4 1 o 4189.377 4251.164 130.25 3.33420 8.41 3 0 2 o 13068.509 12688.186 -180.00 3.31605 8.11 6 0 0 o 585.068 877.198 0.00 3.29533 0.36 3 1 2 o 1461.456 1513.468 80.06 3.23862 1.76 3 4 0 o 1084.710 1159.656 -90.00 3.27145 1.25 2 2 2 o 570.138 619.838 -106.69 3.23162 0.69 6 1 0 o 23.740 32.477 0.00 3.21930 0.03 4 3 1 o 5399.858 5524.547 138.67 3.20230 10.12 2 4 1 o 1895.569 1935.224 -140.63 3.20048 3.53 5 2 1 o 1781.219 1887.776 6.30 3.18573 3.36 5 3 0 o 1835.672 1777.457 -90.00 3.10747 1.93 0 3 2 o 4442.836 4366.942 90.00 3.04959 2.52 3 2 2 o 489.462 488.482 134.28 3.03527 0.55 4 0 2 o 9406.157 9421.908 -180.00 3.03105 5.24 6 0 1 o 0.023 0.022 90.00 3.02798 0.00 6 2 0 o 7230.565 6931.608 0.00 3.01935 7.30 1 3 2 o 312.114 306.477 93.74 3.01395 0.35 3 4 1 o 655.373 668.314 18.56 3.00942 1.09 4 4 0 o 3003.687 2914.559 -180.00 2.99687 2.88 1 5 0 o 1495.138 1438.694 -90.00 2.98034 1.41 4 1 2 o 2040.850 1985.546 49.15 2.97157 2.22 6 1 1 o 1104.535 1061.123 -7.33 2.96868 1.86 2 3 2 o 608.734 500.876 167.11 2.91409 0.65 2 5 0 o 286.919 196.600 -180.00 2.88368 0.25 5 3 1 o 83.734 61.354 -15.36 2.88030 0.13 4 2 2 o 1949.308 1997.617 28.58 2.81216 1.98 6 2 1 o 3171.212 3208.990 -177.70 2.80971 4.76 0 5 1 o 892.797 895.507 -90.00 2.80603 0.65 4 4 1 o 701.848 749.987 52.64 2.79157 1.01 1 5 1 o 1545.342 1563.157 25.51 2.77819 2.21 7 1 0 o 426.973 429.981 -90.00 2.77625 0.36 3 3 2 o 1054.842 963.610 -159.04 2.76766 1.05 6 3 0 o 603.138 649.618 -180.00 2.75558 0.49 5 0 2 o 67.746 72.010 -180.00 2.75378 0.03 3 5 0 o 8.967 4.497 90.00 2.74157 0.01 5 4 0 o 407.932 361.047 90.00 2.72808 0.32 5 1 2 o 3925.080 3777.393 -29.49 2.70895 3.81 2 5 1 o 283.440 254.755 -81.24 2.69940 0.38 0 4 2 o 1295.133 1449.472 0.00 2.68866 0.62 1 4 2 o 490.280 438.427 72.79 2.66414 0.47 7 0 1 o 242.196 182.763 90.00 2.65073 0.17 7 2 0 o 275.076 269.061 90.00 2.64494 0.21 7 1 1 o 2113.910 2240.046 128.00 2.61067 2.79 4 3 2 o 2955.807 3048.923 -51.85 2.59539 2.69 2 4 2 o 1175.953 1195.658 55.73 2.59442 1.07 6 3 1 o 877.836 883.316 -62.93 2.59346 1.12 5 2 2 o 913.467 930.639 152.54 2.58654 0.83 3 5 1 o 794.340 797.012 94.19 2.58177 0.98 4 5 0 o 1189.764 1113.871 0.00 2.57384 0.82 5 4 1 o 1493.229 1428.820 172.87 2.57049 1.84 0 1 3 o 1519.502 1618.697 90.00 2.52203 0.48 1 0 3 o 320.014 342.634 90.00 2.53694 0.10 0 6 0 o 4713.625 4709.253 0.00 2.51232 1.53 1 1 3 o 495.323 520.299 -120.94 2.50176 0.31 7 2 1 o 697.608 718.758 156.32 2.50059 0.84 6 0 2 o 2186.653 2231.476 -180.00 2.49995 0.96 1 6 0 o 0.001 0.001 -89.98 2.49228 0.00 3 4 2 o 205.741 257.686 -175.25 2.48948 0.18 6 4 0 o 370.245 391.396 0.00 2.48067 0.24 2 0 3 o 185.587 185.827 90.00 2.47652 0.06 8 0 0 o 2315.738 2344.940 0.00 2.47150 0.77 6 1 2 o 1537.811 1533.642 34.34 2.46627 1.32 7 3 0 o 7.098 7.284 90.00 2.46220 0.00 2 1 3 o 1382.032 1433.543 -120.04 2.44376 0.83 4 5 1 o 1867.097 1862.433 -156.29 2.44025 2.07 8 1 0 o 137.143 136.288 0.00 2.43894 0.09 2 6 0 o 995.265 1021.145 180.00 2.43492 0.60 0 2 3 o 722.882 935.789 0.00 2.42236 0.21 5 3 2 o 502.189 376.672 -18.11 2.41489 0.41 1 2 3 o 808.013 839.466 -7.31 2.40439 0.47 5 5 0 o 1411.599 1456.275 -90.00 2.39750 0.83 0 6 1 o 1737.622 1769.439 0.00 2.38763 0.92 3 0 3 o 16.471 17.516 90.00 2.38475 0.00 6 2 2 o 2087.192 2071.769 -174.12 2.37283 1.68 0 5 2 o 3266.319 3153.226 90.00 2.37061 1.31 1 6 1 o 163.983 158.043 -110.83 2.37041 0.17 4 4 2 o 2292.895 2160.492 137.56 2.36187 1.81 6 4 1 o 480.723 459.131 170.38 2.36042 0.50 3 1 3 o 3074.969 3116.958 -73.02 2.35546 1.73 1 5 2 o 136.216 136.620 -91.65 2.35375 0.11 2 2 3 o 357.843 355.307 -51.18 2.35276 0.20 8 0 1 o 1415.986 1402.590 -90.00 2.35251 0.76 8 2 0 o 10882.317 10783.260 -180.00 2.34846 6.37 3 6 0 o 1144.229 1144.908 -90.00 2.34754 0.64 7 3 1 o 716.606 757.484 67.05 2.34449 0.75 8 1 1 o 6811.524 6914.417 53.52 2.32438 7.13 2 6 1 o 505.578 532.979 -134.29 2.32090 0.51 2 5 2 o 76.846 65.078 -33.77 2.30526 0.06 5 5 1 o 2948.595 3016.620 5.13 2.28842 2.87 0 3 3 o 473.395 606.540 -90.00 2.27965 0.13 7 0 2 o 1061.288 1204.252 0.00 2.27473 0.40 3 2 3 o 86.442 95.844 158.40 2.27365 0.05 4 0 3 o 1.016 1.100 -90.00 2.27188 0.00 1 3 3 o 3715.277 3803.198 -68.43 2.26465 1.99 7 4 0 o 2320.419 2161.620 90.00 2.26017 1.22 7 1 2 o 3951.570 3993.427 106.76 2.24926 2.95 4 1 3 o 2018.599 1998.522 -46.44 2.24651 1.06 8 2 1 o 957.321 941.825 -9.27 2.24566 0.93 3 6 1 o 137.516 134.416 -119.62 2.24486 0.13 4 6 0 o 4135.367 3958.127 0.00 2.23964 2.08 6 3 2 o 1045.887 1005.527 64.19 2.23822 0.76 3 5 2 o 2795.917 2678.180 -21.90 2.23070 2.02 6 5 0 o 15.291 15.362 0.00 2.22436 0.01 5 4 2 o 543.959 546.747 -109.77 2.22341 0.39 2 3 3 o 1359.955 1330.821 -13.28 2.22136 0.71 8 3 0 o 734.159 628.181 -180.00 2.21774 0.37 7 2 2 o 549.673 520.556 15.35 2.17770 0.39 4 2 3 o 7074.323 6630.801 -135.08 2.17521 3.54 9 1 0 o 9.205 8.394 90.00 2.17392 0.00 7 4 1 o 1489.167 1406.159 1.31 2.16810 1.31 3 3 3 o 472.700 538.135 78.80 2.15442 0.23 4 6 1 o 673.234 730.642 -143.59 2.14996 0.57 5 0 3 o 817.934 805.841 -90.00 2.14785 0.20 1 7 0 o 701.695 605.540 -90.00 2.14076 0.32 5 6 0 o 201.256 189.467 90.00 2.12055 0.09 4 5 2 o 1803.708 1779.596 132.19 2.13750 1.21 6 5 1 o 442.311 445.394 -107.59 2.13642 0.37 0 4 3 o 1583.684 1722.211 180.00 2.11652 0.39 8 3 1 o 1276.115 1242.145 -133.02 2.13056 1.10 9 0 1 o 821.324 870.023 -90.00 2.11205 0.35 9 2 0 o 100.736 101.647 90.00 2.10912 0.05 5 1 3 o 3012.337 2945.191 115.60 2.12637 1.46 1 4 3 o 177.458 161.551 98.07 2.10449 0.09 2 7 0 o 1387.704 1259.802 0.00 2.10408 0.61 0 6 2 o 86.736 77.672 180.00 2.10187 0.03 9 1 1 o 180.613 144.238 -160.01 2.09162 0.15 1 6 2 o 84.639 70.393 122.56 2.09010 0.06 6 4 2 o 492.224 537.912 -4.29 2.08324 0.32 8 0 2 o 263.687 251.767 0.00 2.07780 0.09 0 7 1 o 822.967 782.296 -90.00 2.07334 0.32 7 3 2 o 277.938 273.164 -46.94 2.07226 0.18 4 3 3 o 885.597 903.605 120.92 2.07011 0.41 2 4 3 o 81.770 83.136 -141.99 2.06962 0.04 8 4 0 o 251.762 237.748 0.00 2.06669 0.11 5 2 3 o 215.520 199.815 -160.66 2.06561 0.10 1 7 1 o 429.126 408.961 -93.69 2.06203 0.33 7 5 0 o 282.688 273.129 90.00 2.06124 0.12 8 1 2 o 2280.376 2266.190 -30.84 2.05833 1.47 2 6 2 o 263.163 266.805 -138.92 2.05592 0.17 3 7 0 o 444.944 558.719 -90.00 2.04693 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