#------------------------------------------------------------------------------ #$Date: 2025-07-01 14:07:03 +0300 (Tue, 01 Jul 2025) $ #$Revision: 1187 $ #$URL: svn://localhost/testcod/cif/1/00/00/1000016.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1000016 loop_ _publ_author_name 'Williams, P. Andrew' 'Hughes, Colan. E.' 'Buanz, Asma B. M.' 'Gaisford, Simon' 'Harris, Kenneth D. M.' _publ_section_title ; Expanding the Solid-State Landscape of l-Phenylalanine: Discovery of Polymorphism and New Hydrate Phases, with Rationalization of Hydration/Dehydration Processes ; _journal_issue 23 _journal_name_full 'The Journal of Physical Chemistry C' _journal_page_first 12136 _journal_page_last 12145 _journal_paper_doi 10.1021/jp401547f _journal_volume 117 _journal_year 2013 _chemical_formula_sum 'C18 H22 N2 O5' _chemical_formula_weight 346.38 _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _audit_creation_date 2013-05-09T16:47 _audit_creation_method 'from EXP file using GSAS2CIF' _audit_update_record ' 2013-05-09T16:47 Initial CIF as created by GSAS2CIF' _cell_angle_alpha 90.0 _cell_angle_beta 100.0115(35) _cell_angle_gamma 90.0 _cell_formula_units_Z 2 _cell_length_a 12.1112(5) _cell_length_b 5.42130(17) _cell_length_c 13.7691(5) _cell_volume 890.29(6) _computing_structure_refinement GSAS _diffrn_ambient_temperature 294 _diffrn_radiation_polarisn_ratio 0.55 _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 1.5406 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 No correction is applied. ; _pd_block_id 2013-05-09T16:47|PHEHH|| _pd_calc_method 'Rietveld Refinement' _pd_instr_location ' ?' _pd_meas_2theta_range_inc 0.01707 _pd_meas_2theta_range_max 70.00196 _pd_meas_2theta_range_min 4.0 _pd_meas_number_of_points 3868 _pd_phase_name 'Phenylalanine hemihydrate' _pd_proc_2theta_range_inc 0.01707 _pd_proc_2theta_range_max 70.00987 _pd_proc_2theta_range_min 4.00792 _pd_proc_info_datetime 2013-05-09T16:47:07 _pd_proc_info_excluded_regions ' ?' _pd_proc_ls_background_function ; GSAS Background function number 1 with 32 terms. Shifted Chebyshev function of 1st kind 1: 1649.92 2: -1766.58 3: 693.800 4: -179.157 5: 83.7192 6: -107.183 7: 136.613 8: -152.244 9: 154.939 10: -114.131 11: 29.2524 12: 56.7405 13: -82.2995 14: 34.8510 15: 25.6061 16: -37.8307 17: 24.4648 18: -21.2121 19: 13.5298 20: 11.9516 21: -30.2583 22: 24.0103 23: -7.96025 24: -5.21255 25: 11.9128 26: -9.22746 27: 0.900061 28: 4.41586 29: -8.62295 30: 7.86254 31: -3.63368 32: 2.71480 ; _pd_proc_ls_peak_cutoff 0.00500 _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) = 205.085 #2(GV) = 15.671 #3(GW) = 0.482 #4(GP) = 0.000 #5(LX) = 2.846 #6(LY) = 36.919 #7(S/L) = 0.0216 #8(H/L) = 0.0215 #9(trns) = 0.00 #10(shft)= 0.0000 #11(stec)= 0.00 #12(ptec)= 0.00 #13(sfec)= 0.00 #14(L11) = -0.159 #15(L22) = -1.356 #16(L33) = -0.154 #17(L12) = 0.024 #18(L13) = 0.015 #19(L23) = 0.018 Peak tails are ignored where the intensity is below 0.0050 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_prof_R_factor 0.0221 _pd_proc_ls_prof_wR_expected 0.0253 _pd_proc_ls_prof_wR_factor 0.0296 _pd_proc_number_of_points 3868 _pd_spec_mounting ' ?' _refine_ls_goodness_of_fit_all 1.22 _refine_ls_matrix_type full _refine_ls_number_parameters 160 _refine_ls_number_restraints 133 _refine_ls_R_Fsqd_factor 0.16533 _refine_ls_shift/su_max 0.08 _refine_ls_shift/su_mean 0.01 _reflns_d_resolution_high 1.344 _reflns_d_resolution_low 13.559 _reflns_limit_h_max 9 _reflns_limit_h_min 0 _reflns_limit_k_max 4 _reflns_limit_k_min 0 _reflns_limit_l_max 10 _reflns_limit_l_min -10 _reflns_number_total 445 _cod_data_source_file jp401547f_si_002.cif _cod_data_source_block PHEHH_publ _cod_original_cell_volume 890.29(8) _cod_database_code 1000016 _gsas_exptl_extinct_corr_t_min 1.00000 _gsas_exptl_extinct_corr_t_max 1.00000 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y+1/2,-z 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 O O1 -0.6076(9) 0.1623(18) -0.38044(16) 1.0 Uiso 0.0401(15) 2 O O2 -0.4298(9) 0.1327(22) -0.38981(18) 1.0 Uiso 0.0401(15) 2 C C3 -0.5137(6) 0.2613(12) -0.38219(9) 1.0 Uiso 0.0401(15) 2 C C4 -0.5013(6) 0.5399(13) -0.37506(13) 1.0 Uiso 0.0401(15) 2 H H5 -0.4510(9) 0.5949(18) -0.4193(4) 1.0 Uiso 0.0481(18) 2 N N6 -0.6171(9) 0.6537(18) -0.4086(7) 1.0 Uiso 0.0401(15) 2 H H7 -0.6725(18) 0.566(24) -0.378(11) 1.0 Uiso 0.0481(18) 2 H H8 -0.616(7) 0.828(9) -0.389(11) 1.0 Uiso 0.0481(18) 2 H H9 -0.638(7) 0.641(31) -0.4805(16) 1.0 Uiso 0.0481(18) 2 C C10 -0.4508(7) 0.6117(18) -0.26885(26) 1.0 Uiso 0.0401(15) 2 H H11 -0.3808(5) 0.5199(33) -0.2488(4) 1.0 Uiso 0.0481(18) 2 H H12 -0.4339(14) 0.7886(21) -0.2668(7) 1.0 Uiso 0.0481(18) 2 C C13 -0.5286(5) 0.5570(11) -0.19674(24) 1.0 Uiso 0.0401(15) 2 C C14 -0.6134(6) 0.7194(11) -0.1826(4) 1.0 Uiso 0.0401(15) 2 C C15 -0.6842(5) 0.6680(19) -0.1165(5) 1.0 Uiso 0.0401(15) 2 C C16 -0.6726(7) 0.4521(21) -0.0621(4) 1.0 Uiso 0.0401(15) 2 C C17 -0.5899(9) 0.2871(14) -0.0740(4) 1.0 Uiso 0.0401(15) 2 C C18 -0.5172(6) 0.3379(14) -0.1413(4) 1.0 Uiso 0.0401(15) 2 H H19 -0.6252(10) 0.8722(10) -0.2211(6) 1.0 Uiso 0.0481(18) 2 H H20 -0.7417(5) 0.7876(27) -0.1061(9) 1.0 Uiso 0.0481(18) 2 H H21 -0.7185(10) 0.4247(30) -0.0111(5) 1.0 Uiso 0.0481(18) 2 H H22 -0.5765(13) 0.1417(15) -0.0313(5) 1.0 Uiso 0.0481(18) 2 H H23 -0.4565(7) 0.2229(21) -0.1479(7) 1.0 Uiso 0.0481(18) 2 O O24 -0.8367(10) 0.5974(19) -0.38417(26) 1.0 Uiso 0.0401(15) 2 O O25 -1.0172(9) 0.6181(19) -0.38758(21) 1.0 Uiso 0.0401(15) 2 C C26 -0.9287(7) 0.4942(10) -0.37993(13) 1.0 Uiso 0.0401(15) 2 C C27 -0.9336(5) 0.2167(10) -0.36544(15) 1.0 Uiso 0.0401(15) 2 H H28 -1.0097(6) 0.1576(15) -0.3905(5) 1.0 Uiso 0.0481(18) 2 N N29 -0.8524(9) 0.0930(19) -0.4212(6) 1.0 Uiso 0.0401(15) 2 H H30 -0.7788(11) 0.172(8) -0.404(4) 1.0 Uiso 0.0481(18) 2 H H31 -0.846(4) -0.082(4) -0.403(5) 1.0 Uiso 0.0481(18) 2 H H32 -0.8797(24) 0.109(11) -0.4922(6) 1.0 Uiso 0.0481(18) 2 C C33 -0.9030(7) 0.1591(12) -0.25516(28) 1.0 Uiso 0.0401(15) 2 H H34 -0.8849(11) -0.0166(16) -0.2463(8) 1.0 Uiso 0.0481(18) 2 H H35 -0.8377(6) 0.2577(25) -0.22616(30) 1.0 Uiso 0.0481(18) 2 C C36 -1.0007(6) 0.2204(10) -0.20436(25) 1.0 Uiso 0.0401(15) 2 C C37 -1.0957(7) 0.0719(11) -0.21524(33) 1.0 Uiso 0.0401(15) 2 C C38 -1.1842(6) 0.1307(16) -0.1683(5) 1.0 Uiso 0.0401(15) 2 C C39 -1.1792(7) 0.3392(18) -0.1095(5) 1.0 Uiso 0.0401(15) 2 C C40 -1.0860(9) 0.4872(12) -0.09814(33) 1.0 Uiso 0.0401(15) 2 C C41 -0.9967(7) 0.4287(13) -0.1453(4) 1.0 Uiso 0.0401(15) 2 H H42 -1.1012(11) -0.0741(10) -0.2578(4) 1.0 Uiso 0.0481(18) 2 H H43 -1.2497(7) 0.0219(23) -0.1747(7) 1.0 Uiso 0.0481(18) 2 H H44 -1.2390(10) 0.3725(25) -0.0716(6) 1.0 Uiso 0.0481(18) 2 H H45 -1.0792(13) 0.6264(13) -0.0520(4) 1.0 Uiso 0.0481(18) 2 H H46 -0.9292(8) 0.5319(20) -0.1352(6) 1.0 Uiso 0.0481(18) 2 O O47 -1.2420(15) 0.4368(32) -0.4037(12) 1.0 Uiso 0.071(8) 2 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 O 10.0 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 C 36.0 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 H 44.0 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 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 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 ? ? ? ? ? ? ? ? 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 ? ? ? ? ? ? loop_ _pd_meas_counts_total _pd_proc_ls_weight _pd_proc_intensity_bkg_calc _pd_calc_intensity_total 5057.0 0.0001977 4942.10645 4942.10596 4943.0 0.0002023 4934.70117 4934.70166 4859.0 0.0002058 4926.01953 4926.01758 5026.0 0.0001990 4916.17676 4916.17578 5030.0 0.0001988 4905.28125 4905.28174 4765.0 0.0002099 4893.43652 4893.43555 4867.0 0.0002055 4880.73633 4880.73535 4914.0 0.0002035 4867.27002 4867.26953 4852.0 0.0002061 4853.12158 4853.12158 4868.0 0.0002054 4838.36914 4838.36816 4889.0 0.0002045 4823.08447 4823.08594 4703.0 0.0002126 4807.33643 4807.33545 4688.0 0.0002133 4791.18750 4791.18701 4912.0 0.0002036 4774.69580 4774.69580 4743.0 0.0002108 4757.91650 4757.91650 4710.0 0.0002123 4740.89893 4740.90039 4754.0 0.0002103 4723.69092 4723.69189 4644.0 0.0002153 4706.33447 4706.33594 4711.0 0.0002123 4688.86865 4688.86865 4677.0 0.0002138 4671.33154 4671.33008 4727.0 0.0002116 4653.75488 4653.75488 4657.0 0.0002147 4636.16992 4636.16895 4615.0 0.0002167 4618.60498 4618.60449 4437.0 0.0002254 4601.08301 4601.08252 4682.0 0.0002136 4583.63037 4583.62988 4693.0 0.0002131 4566.26514 4566.26367 4605.0 0.0002172 4549.00684 4549.00732 4627.0 0.0002161 4531.87305 4531.87305 4509.0 0.0002218 4514.87695 4514.87744 4507.0 0.0002219 4498.03271 4498.03076 4538.0 0.0002204 4481.35107 4481.35107 4545.0 0.0002200 4464.84375 4464.84375 4478.0 0.0002233 4448.51709 4448.51563 4491.0 0.0002227 4432.38037 4432.37939 4464.0 0.0002240 4416.43896 4416.43799 4452.0 0.0002246 4400.69727 4400.69727 4373.0 0.0002287 4385.16113 4385.16113 4370.0 0.0002288 4369.83105 4369.83105 4298.0 0.0002327 4354.71191 4354.71191 4406.0 0.0002270 4339.80371 4339.80420 4468.0 0.0002238 4325.10645 4325.10742 4384.0 0.0002281 4310.62158 4310.62158 4326.0 0.0002312 4296.34766 4296.34619 4383.0 0.0002282 4282.28320 4282.28369 4281.0 0.0002336 4268.42676 4268.42627 4261.0 0.0002347 4254.77637 4254.77539 4327.0 0.0002311 4241.33008 4241.32910 4275.0 0.0002339 4228.08350 4228.08398 4177.0 0.0002394 4215.03369 4215.03369 4185.0 0.0002389 4202.17773 4202.17920 4193.0 0.0002385 4189.51221 4189.51221 4233.0 0.0002362 4177.03174 4177.03027 4273.0 0.0002340 4164.73291 4164.73438 4236.0 0.0002361 4152.61182 4152.61230 4171.0 0.0002398 4140.66309 4140.66309 4061.0 0.0002462 4128.88232 4128.88184 4075.0 0.0002454 4117.26465 4117.26514 3986.0 0.0002509 4105.80664 4105.80713 4160.0 0.0002404 4094.50269 4094.50220 4030.0 0.0002481 4083.34766 4083.34814 4146.0 0.0002412 4072.33740 4072.33691 4045.0 0.0002472 4061.46680 4061.46655 4129.0 0.0002422 4050.73145 4050.73096 4118.0 0.0002428 4040.12671 4040.12695 4039.0 0.0002476 4029.64819 4029.64844 3990.0 0.0002506 4019.29150 4019.29102 4050.0 0.0002469 4009.05078 4009.05029 4014.0 0.0002491 3998.92310 3998.92261 3974.0 0.0002516 3988.90454 3988.90381 4061.0 0.0002462 3978.98999 3978.98999 3940.0 0.0002538 3969.17554 3969.17603 3883.0 0.0002575 3959.45801 3959.45850 3955.0 0.0002528 3949.83350 3949.83350 3899.0 0.0002565 3940.29810 3940.29834 3963.0 0.0002523 3930.84692 3930.84717 3884.0 0.0002575 3921.47925 3921.47998 3882.0 0.0002576 3912.18970 3912.18970 3952.0 0.0002530 3902.97681 3902.97632 3853.0 0.0002595 3893.83643 3893.83618 3874.0 0.0002581 3884.76563 3884.76587 3863.0 0.0002589 3875.76270 3875.76245 3889.0 0.0002571 3866.82397 3866.82349 3810.0 0.0002625 3857.94849 3857.94800 3798.0 0.0002633 3849.13208 3849.13184 3889.0 0.0002571 3840.37378 3840.37402 3859.0 0.0002591 3831.67139 3831.67163 3892.0 0.0002569 3823.02271 3823.02295 3735.0 0.0002677 3814.42627 3814.42627 3885.0 0.0002574 3805.88013 3805.87939 3806.0 0.0002627 3797.38257 3797.38232 3757.0 0.0002662 3788.93311 3788.93286 3804.0 0.0002629 3780.52979 3780.53027 3777.0 0.0002648 3772.17163 3772.17163 3909.0 0.0002558 3763.85645 3763.85620 3776.0 0.0002648 3755.58447 3755.58496 3749.0 0.0002667 3747.35474 3747.35474 3719.0 0.0002689 3739.16602 3739.16602 3792.0 0.0002637 3731.01807 3731.01807 3749.0 0.0002667 3722.90967 3722.90967 3738.0 0.0002675 3714.84082 3714.84106 3711.0 0.0002695 3706.81055 3706.81030 3718.0 0.0002690 3698.81958 3698.81860 3732.0 0.0002680 3690.86621 3690.86548 3689.0 0.0002711 3682.95093 3682.95093 3606.0 0.0002773 3675.07422 3690.94995 3609.0 0.0002771 3667.23486 3684.11011 3713.0 0.0002693 3659.43311 3677.41260 3638.0 0.0002749 3651.66943 3670.87915 3555.0 0.0002813 3643.94336 3664.52954 3730.0 0.0002681 3636.25562 3658.39282 3664.0 0.0002729 3628.60596 3652.50537 3671.0 0.0002724 3620.99512 3646.91602 3535.0 0.0002829 3613.42188 3641.69458 3593.0 0.0002783 3605.88818 3636.93555 3649.0 0.0002740 3598.39331 3632.79175 3648.0 0.0002741 3590.93848 3629.53638 3685.0 0.0002714 3583.52344 3627.81445 3607.0 0.0002772 3576.14819 3629.20508 3666.0 0.0002728 3568.81396 3636.55786 3790.0 0.0002639 3561.52124 3652.27417 3732.0 0.0002680 3554.26978 3675.54248 3746.0 0.0002670 3547.05908 3706.94434 3722.0 0.0002687 3539.89209 3741.18726 3750.0 0.0002667 3532.76782 3781.01611 3813.0 0.0002623 3525.68677 3823.49414 3789.0 0.0002639 3518.64941 3869.56763 3883.0 0.0002575 3511.65601 3922.20508 3881.0 0.0002577 3504.70752 3975.23242 4006.0 0.0002496 3497.80396 4038.93262 4039.0 0.0002476 3490.94604 4103.70557 4170.0 0.0002398 3484.13428 4177.33203 4081.0 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0.002203 443.44345 459.66959 465.0 0.002151 443.26770 459.75360 457.0 0.002188 443.09055 459.71457 414.0 0.002415 442.91202 459.55170 434.0 0.002304 442.73251 459.26740 469.0 0.002132 442.55200 458.88211 534.0 0.001873 442.37076 458.36487 449.0 0.002227 442.18915 457.75558 430.0 0.002326 442.00726 457.03323 475.0 0.002105 441.82556 456.23642 446.0 0.002242 441.64401 455.39377 437.0 0.002288 441.46301 454.54245 433.0 0.002309 441.28271 453.73175 476.0 0.002101 441.10361 452.97284 452.0 0.002212 440.92566 452.31073 418.0 0.002392 440.74933 451.77411 457.0 0.002188 440.57471 451.35641 460.0 0.002174 440.40237 451.13867 442.0 0.002262 440.23233 451.08734 473.0 0.002114 440.06494 451.20673 457.0 0.002188 439.90039 451.48633 404.0 0.002475 439.73917 451.90540 415.0 0.002410 439.58121 452.43423 422.0 0.002370 439.42709 453.03442 457.0 0.002188 439.27698 453.66153 438.0 0.002283 439.13104 454.26804 441.0 0.002268 438.98978 454.80783 458.0 0.002183 438.85312 455.24258 413.0 0.002421 438.72165 455.54233 446.0 0.002242 438.59525 455.68707 444.0 0.002252 438.47458 455.66333 451.0 0.002217 438.35959 455.46231 470.0 0.002128 438.25058 455.07932 417.0 0.002398 438.14767 454.51440 450.0 0.002222 438.05127 453.77997 445.0 0.002247 437.96136 452.89987 482.0 0.002075 437.87830 451.91351 461.0 0.002169 437.80215 450.86685 445.0 0.002247 437.73309 449.81189 467.0 0.002141 437.67126 448.79559 390.0 0.002564 437.61679 447.86139 434.0 0.002304 437.56976 447.04581 448.0 0.002232 437.53040 446.37930 398.0 0.002513 437.49860 445.90924 408.0 0.002451 437.47452 445.60764 446.0 0.002242 437.45816 445.50287 433.0 0.002309 437.44955 445.62045 442.0 0.002262 437.44867 445.93607 443.0 0.002257 437.45557 446.46286 440.0 0.002273 437.47006 447.14197 435.0 0.002299 437.49219 447.98651 440.0 0.002273 437.52179 448.97430 430.0 0.002326 437.55872 450.08167 424.0 0.002358 437.60294 451.27786 494.0 0.002024 437.65417 452.52786 457.0 0.002188 437.71219 453.78726 473.0 0.002114 437.77689 455.00900 454.0 0.002203 437.84787 456.13916 437.0 0.002288 437.92505 457.12851 416.0 0.002404 438.00784 457.93317 485.0 0.002062 438.09610 458.48691 476.0 0.002101 438.18939 458.89053 417.0 0.002398 438.28735 459.06342 440.0 0.002273 438.38953 459.05936 459.0 0.002179 438.49548 458.93179 460.0 0.002174 438.60477 458.69348 447.0 0.002237 438.71680 458.40320 449.0 0.002227 438.83118 458.10397 438.0 0.002283 438.94714 457.83490 476.0 0.002101 439.06430 457.62589 428.0 0.002336 439.18207 457.51031 454.0 0.002203 439.29977 457.50375 435.0 0.002299 439.41666 457.52274 443.0 0.002257 439.53229 457.58368 461.0 0.002169 439.64590 457.64896 436.0 0.002294 439.75690 457.67725 431.0 0.002320 439.86438 457.62463 470.0 0.002128 439.96790 457.46335 429.0 0.002331 440.06668 457.16623 415.0 0.002410 440.16010 456.73758 469.0 0.002132 440.24734 456.18289 438.0 0.002283 440.32800 455.52878 428.0 0.002336 440.40118 454.80423 400.0 0.002500 440.46637 454.04153 421.0 0.002375 440.52298 453.26938 464.0 0.002155 440.57043 452.51453 433.0 0.002309 440.60828 451.79675 454.0 0.002203 440.63596 451.13354 459.0 0.002179 440.65311 450.53745 470.0 0.002128 440.65939 450.02271 442.0 0.002262 440.65457 449.60092 413.0 0.002421 440.63840 449.30008 449.0 0.002227 440.61093 449.10947 393.0 0.002545 440.57211 449.03909 442.0 0.002262 440.52203 449.09714 398.0 0.002513 440.46109 449.26184 433.0 0.002309 440.38959 449.57089 420.0 0.002381 440.30823 449.97656 443.0 0.002257 440.21771 450.45383 428.0 0.002336 440.11899 451.01126 400.0 0.002500 440.01328 451.61212 453.0 0.002208 439.90186 452.23495 451.0 0.002217 439.78656 452.86041 440.0 0.002273 439.66916 453.47916 439.0 0.002278 439.55188 454.07382 453.0 0.002208 439.43716 454.64203 431.0 0.002320 439.32803 455.17773 431.0 0.002320 439.22751 455.67584 443.0 0.002257 439.13937 456.13043 451.0 0.002217 439.06754 456.55649 447.0 0.002237 439.01642 456.91431 421.0 0.002375 438.99103 457.16922 478.0 0.002092 438.99680 457.45810 443.0 0.002257 439.03979 457.73944 410.0 0.002439 439.12643 458.03851 443.0 0.002257 439.26407 458.39716 440.0 0.002273 439.46048 458.78738 457.0 0.002188 439.72437 459.26123 441.0 0.002268 440.06488 459.78714 488.0 0.002049 440.49222 460.38553 471.0 0.002123 441.01724 461.10001 435.0 0.002299 441.65182 461.82974 411.0 . . . 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 0 0 1 o 1258.572 1287.031 180.00 13.55943 100.00 1 0 0 o 20.998 70.148 180.00 11.92680 1.30 1 0 -1 o 580.997 531.675 180.00 9.84423 23.93 1 0 1 o 595.828 575.258 0.00 8.27071 17.29 0 0 2 o 361.713 360.672 180.00 6.77971 6.97 1 0 -2 o 251.480 283.971 0.00 6.39060 4.33 2 0 0 o 5668.106 6030.727 0.00 5.96340 84.66 2 0 -1 o 5.558 7.553 0.00 5.84617 0.08 1 0 2 o 1379.018 1466.719 180.00 5.49768 17.44 2 0 1 o 1715.177 1666.256 180.00 5.13946 18.87 0 1 1 o 3515.749 3401.825 47.47 5.03387 74.25 1 1 0 o 538.839 527.817 -18.23 4.93537 10.93 2 0 -2 o 1384.097 1377.415 0.00 4.92212 13.95 1 1 -1 o 190.057 304.511 177.21 4.74881 3.54 1 1 1 o 1908.594 2053.745 -46.12 4.53407 32.30 0 0 3 o 0.956 1.024 180.00 4.51981 0.01 1 0 -3 o 1761.164 1965.633 180.00 4.49327 14.70 0 1 2 o 3.266 56.671 42.55 4.23408 0.04 2 0 2 o 10840.902 11003.904 180.00 4.13536 76.12 1 1 -2 o 1079.494 1086.613 141.51 4.13412 15.28 1 0 3 o 329.369 332.640 0.00 4.00222 2.16 2 1 0 o 566.535 566.814 112.18 4.01143 7.46 3 0 -1 o 148.765 149.715 180.00 4.00775 0.98 3 0 0 o 365.079 366.631 180.00 3.97560 2.36 2 1 -1 o 136.553 137.643 -63.71 3.97516 1.75 2 0 -3 o 1167.247 1165.624 0.00 3.94758 7.43 1 1 2 o 546.175 539.108 -23.85 3.86016 6.72 2 1 1 o 2480.409 2364.578 39.24 3.72981 28.02 3 0 -2 o 1497.606 1419.363 0.00 3.72353 8.45 3 0 1 o 2565.026 2370.110 0.00 3.64763 13.85 2 1 -2 o 238.182 216.829 90.66 3.64419 2.55 0 1 3 o 3812.718 3827.648 66.09 3.47157 37.10 1 1 -3 o 1299.025 1331.198 -60.90 3.45949 12.60 1 0 -4 o 30.113 30.806 0.00 3.42085 0.14 0 0 4 o 12872.388 13061.915 180.00 3.38986 59.70 2 0 3 o 376.816 364.581 180.00 3.33388 1.67 2 1 2 o 1257.329 1244.888 73.86 3.28798 10.90 3 0 -3 o 808.477 827.157 180.00 3.28141 3.50 1 1 3 o 5165.887 5140.900 147.69 3.21986 42.85 3 1 0 o 869.261 868.306 -160.15 3.20595 7.14 3 1 -1 o 384.939 385.287 45.16 3.22274 3.21 3 0 2 o 191.216 187.270 180.00 3.19560 0.79 2 0 -4 o 376.120 350.856 180.00 3.19530 1.54 2 1 -3 o 17.088 16.460 -121.03 3.19120 0.14 1 0 4 o 13.832 52.652 0.00 3.12114 0.06 3 1 -2 o 178.104 158.751 -59.06 3.06930 1.33 3 1 1 o 506.579 615.289 134.01 3.02637 3.68 4 0 -1 o 65.196 78.646 180.00 3.02450 0.24 4 0 0 o 41.652 104.542 180.00 2.98170 0.15 4 0 -2 o 192.825 157.141 180.00 2.92308 0.65 1 1 -4 o 74.571 72.611 -114.34 2.89305 0.49 0 1 4 o 123.374 148.325 96.76 2.87423 0.80 2 1 3 o 357.634 300.785 -28.35 2.83987 2.26 4 0 1 o 331.484 291.826 0.00 2.81141 1.02 3 0 -4 o 832.320 656.356 0.00 2.83417 2.62 3 1 -3 o 204.315 197.998 -53.05 2.80723 1.26 3 0 3 o 817.614 792.896 0.00 2.75690 2.43 3 1 2 o 101.267 99.383 136.65 2.75293 0.59 2 0 4 o 472.500 481.965 180.00 2.74884 1.39 1 0 -5 o 26.871 27.349 180.00 2.74976 0.08 2 1 -4 o 8.389 8.177 114.64 2.75274 0.05 0 0 5 o 7204.380 6663.322 0.00 2.71189 20.65 1 1 4 o 1869.848 1729.282 161.52 2.70490 10.60 4 0 -3 o 30.814 28.036 180.00 2.71532 0.09 0 2 0 o 5384.118 5065.120 88.15 2.71065 15.42 0 2 1 o 3190.718 2733.998 -96.71 2.65806 17.48 4 1 -1 o 1306.972 1096.443 -83.59 2.64126 7.07 2 0 -5 o 715.364 584.901 0.00 2.64819 1.94 1 2 0 o 706.395 591.818 -3.62 2.64325 3.82 4 1 0 o 216.138 180.938 -172.48 2.61262 1.14 1 2 -1 o 430.744 368.339 -38.91 2.61339 2.27 4 0 2 o 4.563 4.789 180.00 2.56973 0.01 4 1 -2 o 233.048 226.812 118.07 2.57291 1.20 1 0 5 o 0.054 0.102 0.00 2.55027 0.00 1 2 1 o 603.984 538.717 123.45 2.57584 3.09 4 1 1 o 879.023 848.075 55.81 2.49577 4.18 0 2 2 o 246.008 270.442 -65.13 2.51694 1.20 3 1 -4 o 342.707 362.010 103.76 2.51166 1.66 1 2 -2 o 696.307 669.070 62.13 2.49545 3.33 3 1 3 o 1655.219 1500.953 158.29 2.45741 7.61 2 1 4 o 324.107 288.332 -102.54 2.45169 1.48 2 2 0 o 811.761 767.767 108.84 2.46768 3.78 1 1 -5 o 344.216 305.571 109.37 2.45234 1.58 4 0 -4 o 806.773 741.584 180.00 2.46106 1.85 2 2 -1 o 737.959 670.390 -87.73 2.45917 3.41 3 0 -5 o 20.798 18.261 0.00 2.44708 0.05 4 1 -3 o 143.014 137.493 -119.28 2.42782 0.64 0 1 5 o 255.316 249.447 -114.48 2.42536 1.14 5 0 -1 o 61.074 57.909 0.00 2.42224 0.14 1 2 2 o 652.051 585.039 -69.24 2.43120 2.94 5 0 0 o 250.970 227.707 0.00 2.38536 0.55 2 2 1 o 464.707 450.990 -41.01 2.39761 2.04 3 0 4 o 148.264 140.396 180.00 2.38303 0.32 5 0 -2 o 815.190 756.997 180.00 2.38362 1.76 2 1 -5 o 20.129 20.874 74.18 2.37947 0.09 2 2 -2 o 63.483 80.699 56.25 2.37441 0.27 4 1 2 o 502.517 503.630 -63.05 2.32207 2.05 2 0 5 o 902.411 910.112 0.00 2.32123 1.83 4 0 3 o 42.156 43.754 180.00 2.31107 0.09 1 1 5 o 1098.423 1119.657 -58.74 2.30769 4.40 0 2 3 o 230.802 225.900 72.25 2.32465 0.95 1 2 -3 o 812.433 818.476 -93.22 2.32101 3.30 1 0 -6 o 320.323 301.306 180.00 2.29456 0.63 5 0 1 o 1372.497 1254.523 180.00 2.28255 2.69 5 0 -3 o 725.657 650.156 0.00 2.27951 1.43 0 0 6 o 2869.309 2468.815 180.00 2.25991 5.48 2 2 2 o 318.621 262.441 -141.07 2.26703 1.23 2 0 -6 o 65.196 51.495 0.00 2.24663 0.12 3 2 -1 o 716.346 572.836 12.86 2.24531 2.69 1 2 3 o 751.588 603.690 102.55 2.24434 2.82 4 1 -4 o 1390.369 1142.396 18.90 2.24096 5.20 3 2 0 o 159.722 132.381 -153.89 2.23961 0.60 2 2 -3 o 800.945 712.420 150.49 2.23457 2.98 5 1 -1 o 24.616 9.360 136.69 2.21153 0.09 3 1 -5 o 1254.915 1086.325 -81.48 2.23039 4.65 4 0 -5 o 246.199 110.727 0.00 2.20619 0.44 5 1 0 o 452.487 404.406 158.24 2.18336 1.59 3 1 4 o 403.505 338.744 25.56 2.18157 1.42 3 2 -2 o 355.941 372.655 19.24 2.19147 1.27 5 1 -2 o 231.573 201.998 147.95 2.18203 0.81 3 2 1 o 3.908 2.341 -121.64 2.17568 0.01 1 0 6 o 352.860 262.313 0.00 2.15299 0.60 5 0 2 o 1691.797 1394.643 0.00 2.13685 2.85 2 1 5 o 1483.655 1278.528 -134.24 2.13386 4.96 4 1 3 o 15.937 15.267 143.16 2.12596 0.06 5 0 -4 o 1253.897 1108.065 180.00 2.13311 2.11 3 0 -6 o 287.410 269.530 180.00 2.13020 0.48 0 2 4 o 386.015 333.417 -87.49 2.11704 1.28 1 2 -4 o 1011.134 1014.668 153.96 2.12453 3.36 5 1 1 o 10.740 10.620 -123.80 2.10369 0.04 1 1 -6 o 547.115 479.092 -49.93 2.11308 1.80 2 2 3 o 696.131 708.736 74.96 2.10320 2.26 5 1 -3 o 596.124 626.399 112.90 2.10131 1.92 3 0 5 o 299.923 263.492 180.00 2.07841 0.47 0 1 6 o 283.325 212.209 18.71 2.08593 0.90 4 0 4 o 0.017 0.020 0.00 2.06768 0.00 3 2 -3 o 70.051 55.893 54.85 2.08983 0.22 3 2 2 o 24.576 27.061 120.36 2.06714 0.08 2 1 -6 o 220.022 198.228 -110.11 2.07548 0.69 2 2 -4 o 210.335 227.055 -50.35 2.06706 0.66 1 2 4 o 195.832 257.770 -175.32 2.04657 0.60 4 1 -5 o 155.675 209.091 109.92 2.04346 0.48 6 0 -1 o 1.869 10.857 0.00 2.01776 0.00 2 0 6 o 0.606 0.725 180.00 2.00111 0.00 4 2 -1 o 8.944 60.471 80.66 2.01859 0.03 6 0 -2 o 238.428 305.447 0.00 2.00387 0.35 1 1 6 o 131.709 157.984 -124.36 2.00097 0.38 5 1 2 o 452.102 427.096 2.85 1.98799 1.29 4 2 0 o 521.773 699.206 -74.64 2.00571 1.53 6 0 0 o 51.036 47.221 0.00 1.98780 0.07 5 0 3 o 586.122 667.532 180.00 1.97277 0.83 4 2 -2 o 180.818 158.757 -68.41 1.98758 0.52 5 1 -4 o 26.187 23.132 59.60 1.98498 0.07 3 1 -6 o 57.746 55.461 98.22 1.98264 0.16 1 0 -7 o 24.537 31.284 0.00 1.96688 0.03 4 0 -6 o 989.182 1122.343 0.00 1.97379 1.39 5 0 -5 o 1470.166 1643.435 0.00 1.96885 2.06 4 2 1 o 186.464 285.538 118.78 1.95137 0.52 3 1 5 o 320.182 496.029 -35.49 1.94068 0.87 3 2 -4 o 73.704 137.807 -50.20 1.95893 0.21 6 0 -3 o 102.440 183.865 180.00 1.94872 0.14 4 1 4 o 452.717 591.316 -98.63 1.93193 1.22 0 0 7 o 155.037 223.056 180.00 1.93706 0.21 2 0 -7 o 3.848 7.354 180.00 1.94430 0.01 3 2 3 o 22.101 29.626 -81.88 1.93287 0.06 2 2 4 o 141.653 176.441 126.24 1.93008 0.37 6 0 1 o 69.896 75.014 0.00 1.91947 0.09 1 2 -5 o 14.311 17.909 113.86 1.93040 0.04 4 2 -3 o 211.746 233.249 102.14 1.91837 0.56 0 2 5 o 1911.783 2152.083 85.19 1.91716 5.04 6 1 -1 o 164.900 238.429 -62.55 1.89103 0.43 2 1 6 o 215.424 373.058 -69.49 1.87730 0.55 2 2 -5 o 35.728 65.999 116.52 1.89425 0.09 6 1 -2 o 525.110 779.231 177.65 1.87958 1.33 3 0 -7 o 23.403 57.086 180.00 1.87439 0.03 6 1 0 o 16.747 78.444 41.73 1.86630 0.04 4 2 2 o 3.429 24.743 134.77 1.86490 0.01 5 1 3 o 14.608 35.065 -29.49 1.85384 0.04 1 0 7 o -0.977 95.349 180.00 1.86149 0.00 4 0 5 o 0.576 1.091 180.00 1.85232 0.00 1 2 5 o 0.001 2.373 -8.38 1.85743 0.00 6 0 -4 o -3.880 296.096 180.00 1.86177 0.00 1 1 -7 o 424.355 628.872 104.81 1.84895 1.04 4 1 -6 o 10.466 25.506 -141.96 1.85469 0.03 5 1 -5 o 143.642 205.448 -68.33 1.85059 0.35 3 0 6 o 19.464 412.850 0.00 1.83256 0.03 6 1 -3 o -0.306 7.672 -30.18 1.83385 0.00 6 0 2 o 112.971 175.089 180.00 1.82382 0.13 0 1 7 o 282.479 422.590 -110.74 1.82412 0.67 2 1 -7 o 6.698 14.365 148.32 1.83016 0.02 6 1 1 o 220.836 334.760 93.45 1.80941 0.51 5 0 4 o 31.932 59.158 180.00 1.80843 0.04 4 2 -4 o 125.495 186.838 135.71 1.82210 0.30 3 2 -5 o 130.773 173.444 -153.36 1.81640 0.31 5 2 -1 o 1.194 5.664 -132.03 1.80617 0.00 5 0 -6 o -1.982 98.158 0.00 1.80465 0.00 5 2 0 o 468.674 567.884 151.79 1.79073 1.05 3 2 4 o 162.130 210.806 -120.47 1.78974 0.36 5 2 -2 o 78.462 96.074 -113.53 1.78999 0.18 0 3 1 o 144.570 155.295 116.60 1.79126 0.32 1 3 0 o 72.254 133.579 6.84 1.78671 0.16 1 1 7 o 228.404 259.488 -15.45 1.76059 0.50 4 2 3 o 45.915 50.105 -52.18 1.75865 0.10 3 1 -7 o 11.260 40.119 -174.98 1.77149 0.03 1 3 -1 o -2.689 225.672 -152.59 1.77740 0.00 4 0 -7 o 52.545 180.893 0.00 1.77112 0.06 2 2 5 o 812.027 982.560 121.40 1.76311 1.76 2 0 7 o 523.857 512.029 180.00 1.75485 0.56 4 1 5 o 517.145 481.298 174.36 1.75283 1.10 6 1 -4 o 344.716 389.265 -26.08 1.76083 0.74 1 3 1 o 52.574 71.600 102.48 1.76545 0.11 6 0 -5 o 8.082 7.886 0.00 1.75532 0.01 5 2 1 o 1191.614 1119.542 -108.45 1.74598 2.52 1 2 -6 o 35.858 30.732 177.35 1.75134 0.08 3 1 6 o 305.987 342.899 -13.55 1.73606 0.64 5 2 -3 o 1051.166 1014.232 58.27 1.74462 2.22 0 2 6 o 201.361 221.468 -115.41 1.73578 0.42 6 1 2 o 171.548 301.735 -8.32 1.72862 0.36 0 3 2 o 705.706 656.880 -44.83 1.74614 1.49 7 0 -1 o 0.567 0.970 0.00 1.72811 0.00 1 3 -2 o 340.182 356.731 -127.82 1.73892 0.71 7 0 -2 o 3.393 8.440 180.00 1.72485 0.00 2 2 -6 o 84.411 141.240 -82.03 1.72975 0.18 5 1 4 o 78.825 219.518 -30.26 1.71550 0.16 1 0 -8 o 0.427 1.546 0.00 1.72024 0.00 6 0 3 o 64.082 216.157 180.00 1.71315 0.07 2 3 0 o 151.936 259.782 -61.38 1.72944 0.32 2 3 -1 o 247.391 530.592 -7.08 1.72650 0.52 7 0 0 o -0.135 1.783 0.00 1.70383 0.00 2 0 -8 o 3.280 42.692 0.00 1.71043 0.00 5 1 -6 o 0.852 3.064 -59.53 1.71227 0.00 1 3 2 o 139.218 358.299 68.69 1.71674 0.30 4 2 -5 o 9.038 75.441 -79.54 1.71108 0.02 2 3 1 o -2.911 201.997 130.18 1.70479 0.00 0 0 8 o 224.331 1194.564 0.00 1.69493 0.24 7 0 -3 o 6.937 36.783 180.00 1.69450 0.01 1 2 6 o -1.114 56.718 -176.34 1.68590 0.00 2 3 -2 o 84.904 377.200 173.56 1.69639 0.18 5 2 2 o 386.124 502.740 73.94 1.67812 0.75 4 0 6 o 13.063 28.723 0.00 1.66694 0.01 4 1 -7 o 17.707 49.473 115.31 1.68355 0.04 2 1 7 o 116.378 217.845 146.41 1.66956 0.23 5 2 -4 o 442.868 537.981 -75.23 1.67631 0.86 3 2 -6 o 13.831 18.996 -18.25 1.67489 0.03 5 0 5 o -2.122 47.130 0.00 1.65414 0.00 0 3 3 o 5.141 5.926 38.93 1.67796 0.01 1 3 -3 o 43.047 49.674 -39.02 1.67659 0.08 6 1 -5 o 145.866 265.107 91.27 1.66997 0.28 3 0 -8 o 170.278 285.180 180.00 1.66721 0.16 7 0 1 o -1.252 34.342 180.00 1.65531 0.00 3 2 5 o 197.469 299.875 -152.19 1.64937 0.37 7 1 -1 o 70.920 89.286 9.60 1.64648 0.13 2 3 2 o -0.099 3.267 -72.01 1.65590 0.00 4 2 4 o 139.991 188.548 98.74 1.64399 0.26 6 1 3 o 182.671 386.044 167.29 1.63353 0.34 3 0 7 o 37.335 80.399 180.00 1.63315 0.03 5 0 -7 o 137.060 239.539 180.00 1.65067 0.13 1 0 8 o 28.773 48.755 0.00 1.63885 0.03 7 1 -2 o 106.708 145.193 -118.86 1.64366 0.20 3 3 -1 o 74.396 85.400 95.98 1.64738 0.14 1 3 3 o 90.939 104.829 -94.92 1.64699 0.17 7 0 -4 o 3.586 5.365 0.00 1.64113 0.00 3 3 0 o 13.842 16.330 -64.15 1.64512 0.03 1 1 -8 o 53.793 87.134 -12.97 1.63968 0.10 6 0 -6 o 17.310 26.476 0.00 1.64071 0.02 2 3 -3 o 30.011 40.933 -6.35 1.64312 0.06 7 1 0 o 74.950 211.165 -84.94 1.62544 0.14 2 1 -8 o 68.950 197.400 -67.14 1.63117 0.13 0 1 8 o 27.984 43.508 110.89 1.61771 0.05 3 3 -2 o 2.532 7.832 130.14 1.62575 0.00 6 2 -1 o 123.049 190.841 -75.79 1.61856 0.22 7 1 -3 o 154.363 241.703 92.60 1.61734 0.27 2 2 6 o 166.012 379.996 -74.25 1.60993 0.30 3 3 1 o 108.198 165.556 44.22 1.61928 0.19 6 2 -2 o 80.531 167.076 90.68 1.61137 0.14 6 0 4 o 67.554 145.883 180.00 1.59780 0.06 6 2 0 o -0.062 1.123 11.85 1.60298 0.00 4 1 6 o 121.856 183.480 109.28 1.59332 0.21 5 2 3 o 84.563 127.723 -145.33 1.59506 0.15 7 0 2 o 30.883 74.861 0.00 1.58846 0.03 5 1 5 o 8.397 16.656 95.22 1.58213 0.01 3 1 -8 o 38.885 52.478 -122.89 1.59356 0.07 4 0 -8 o 0.007 0.011 180.00 1.59765 0.00 4 2 -6 o 197.943 278.390 100.51 1.59560 0.34 0 3 4 o 41.694 56.201 -161.27 1.59466 0.07 7 1 1 o 32.034 75.425 -55.88 1.58316 0.05 1 3 -4 o 51.502 92.985 -155.10 1.59785 0.09 5 2 -5 o 266.106 359.115 105.28 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