# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ; ? ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) loop_ _publ_author_name _publ_author_footnote _publ_author_address H.B.Yahia ; ? ; ; ? ; M.Shikano '' '' H.Sakaebe '' '' S.Koike '' '' M.Tabuchi '' '' H.Kobayashi '' '' ; H.Kawaji ; '' '' M.Avdeev '' '' _publ_contact_author_address # Address of author for correspondence ; ? ; _publ_contact_author_email benyahia.hamdi@voila.fr _publ_contact_author_fax ? _publ_contact_author_phone ? #============================================================================= # 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 'Hamdi Ben Yahia' #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; data_ECH0007212-13-97_BYH_publ _database_code_depnum_ccdc_archive 'CCDC 872881' #TrackingRef '- LiNaFePO4F-NPD.cif' _pd_block_id 2012-02-26T19:09|ECH0007212-13-97_BYH|y|Echidna _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2012-02-26T19:09 _audit_author_name y _audit_update_record ; 2012-02-26T19:09 Initial CIF as created by GSAS2CIF ; _publ_section_title_footnote ; ? ; #============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep # Details of the preparation of the sample(s) # should be given here. ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================= # 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 ? _refine_ls_extinction_method ? _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 300 _pd_char_colour black # use ICDD colour descriptions _refine_ls_shift/su_max 0.05 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 59 _refine_ls_goodness_of_fit_all 1.47 _refine_ls_number_restraints 0 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common BYH221LonG.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 3.317 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature 300 _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 BYH221LonG.cif _cell_length_a 10.9851(4) _cell_length_b 6.3686(3) _cell_length_c 11.4343(4) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 799.94(6) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' 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 3 +x,-y+1/2,+z 4 -x+1/2,-y,+z+1/2 -1 -x,-y,-z -2 +x+1/2,-y+1/2,-z+1/2 -3 -x,+y+1/2,-z -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 Na Na1 0.2273(11) 0.018(2) 0.3463(8) 1.0 Uiso 0.021(4) 8 Li Li2 0.286(3) 0.25 0.551(2) 1.0 Uiso 0.021(4) 4 Li Li3 0.444(3) 0.25 0.212(3) 1.0 Uiso 0.021(4) 4 Fe Fe1 0.0 0.0 0.0 1.0 Uiso 0.0130(16) 4 Fe Fe2 0.0 0.0 0.5 1.0 Uiso 0.0023(18) 4 P P1 0.0328(11) 0.25 0.7384(13) 1.0 Uiso 0.030(4) 4 P P2 0.2501(16) 0.25 0.0704(11) 1.0 Uiso 0.034(4) 4 O O1 0.1798(6) 0.0527(10) 0.0375(5) 1.0 Uiso 0.014(2) 8 O O2 0.2662(12) 0.25 0.2099(8) 1.0 Uiso 0.039(4) 4 O O3 0.1756(11) 0.25 0.7397(14) 1.0 Uiso 0.056(5) 4 O O4 0.3743(8) 0.25 0.0171(9) 1.0 Uiso 0.006(3) 4 O O5 0.4942(11) 0.25 0.6317(9) 1.0 Uiso 0.021(3) 4 O O6 0.0034(7) 0.5482(9) 0.3180(4) 1.0 Uiso 0.0023(19) 8 F F1 0.1316(9) 0.25 0.4668(10) 1.0 Uiso 0.026(4) 4 F F2 0.4345(9) 0.25 0.3987(9) 1.0 Uiso 0.006(3) 4 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'F Fe Li Na O4 P' _chemical_formula_weight 199.75 _cell_formula_units_Z 8 # 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 Na1 O1 2.455(12) . 4_555 N Na1 O2 2.190(13) . 1_555 N Na1 O3 2.353(14) . 2_544 N Na1 O4 2.824(16) . 2_545 N Na1 O6 2.517(14) . 3_555 N Na1 F1 2.278(13) . 1_555 N Na1 F2 2.779(16) . 1_555 N Li2 O1 1.970(8) . 2_555 N Li2 O1 1.970(8) . 4_555 N Li2 O3 2.47(3) . 1_555 N Li2 O5 2.46(3) . 1_555 N Li2 F1 1.96(3) . 1_555 N Li2 F2 2.39(3) . 1_555 N Li3 O2 1.95(3) . 1_555 N Li3 O4 2.36(3) . 1_555 N Li3 O6 2.037(12) . -2_555 N Li3 O6 2.037(12) . -4_555 N Li3 F1 2.91(3) . -2_555 N Li3 F2 2.14(3) . 1_555 N Fe1 O1 2.049(6) . 1_555 N Fe1 O1 2.049(6) . -1_555 N Fe1 O5 2.193(7) . 2_544 N Fe1 O5 2.193(7) . -2_455 N Fe1 F2 2.096(7) . 2_544 N Fe1 F2 2.096(7) . -2_455 N Fe2 O4 2.116(6) . 2_545 N Fe2 O4 2.116(6) . -2_455 N Fe2 O6 2.104(5) . 3_555 N Fe2 O6 2.104(5) . -3_546 N Fe2 F1 2.184(7) . 1_555 N Fe2 F1 2.184(7) . -1_556 N P1 O3 1.569(17) . 1_555 N P1 O5 1.544(17) . -2_456 N P1 O6 1.492(9) . -1_566 N P1 O6 1.492(9) . -3_546 N P2 O1 1.522(10) . 1_555 N P2 O1 1.522(10) . 3_555 N P2 O2 1.604(15) . 1_555 N P2 O4 1.495(16) . 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 O1 Fe1 O1 180.0 1_555 . -1_555 N O1 Fe1 F2 84.8(3) 1_555 . 2_544 N O1 Fe1 F2 95.2(3) -1_555 . 2_544 N O4 Fe2 O6 88.3(3) 2_545 . 3_555 N O4 Fe2 F1 97.6(3) 2_545 . 1_555 N O4 Fe2 F1 82.4(3) 2_545 . -1_556 N O6 Fe2 F1 85.6(4) 3_555 . 1_555 N O6 Fe2 F1 94.4(4) 3_555 . -1_556 N F1 Fe2 F1 180.0 1_555 . -1_556 N O3 P1 O6 105.7(7) 1_555 . -1_566 N O1 P2 O1 111.3(12) 1_555 . 3_555 N O1 P2 O2 107.6(6) 1_555 . 1_555 N O1 P2 O4 111.2(6) 1_555 . 1_555 N O1 P2 O2 107.6(6) 3_555 . 1_555 N O1 P2 O4 111.2(6) 3_555 . 1_555 N O2 P2 O4 107.8(11) 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 300 _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type Echidna _diffrn_detector ? _diffrn_detector_type ? # 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 ? _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 ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_length_neutron _atom_type_scat_source Na 8.0 0.3630 International_Tables_Vol_C Li 8.0 -0.1900 International_Tables_Vol_C Fe 8.0 0.9450 International_Tables_Vol_C P 8.0 0.5130 International_Tables_Vol_C O 32.0 0.5803 International_Tables_Vol_C F 8.0 0.5654 International_Tables_Vol_C _diffrn_radiation_probe neutron _diffrn_radiation_wavelength 2.4395 _pd_proc_ls_prof_R_factor 0.0192 _pd_proc_ls_prof_wR_factor 0.0241 _pd_proc_ls_prof_wR_expected 0.0166 _refine_ls_R_Fsqd_factor 0.05186 _pd_proc_ls_background_function ; GSAS Background function number 1 with 8 terms. Shifted Chebyshev function of 1st kind 1: 3182.24 2: -144.776 3: 131.390 4: -4.00489 5: 26.1631 6: 8.09793 7: -35.9162 8: -25.3581 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 Debye-Scherrer absorption correction Term (= MU.r/wave) = 0.10000 Correction is not refined. ; _exptl_absorpt_correction_T_min 0.66322 _exptl_absorpt_correction_T_max 0.68307 # 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 4 with 18 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. Microstrain broadening by P.W. Stephens, (1999). J. Appl. Cryst.,32,281-289. #1(GU) = 0.100 #2(GV) = -0.100 #3(GW) = 107.261 #4(GP) = 0.000 #5(LX) = 31.235 #6(ptec) = 0.00 #7(trns) = -13.37 #8(shft) = 0.0000 #9(sfec) = 0.00 #10(S/L) = 0.0660 #11(H/L) = 0.0660 #12(eta) = 0.0000 #13(S400 ) = 0.0E+00 #14(S040 ) = 0.0E+00 #15(S004 ) = 0.0E+00 #16(S220 ) = 0.0E+00 #17(S202 ) = 0.0E+00 #18(S022 ) = 0.0E+00 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00100 _pd_proc_info_datetime 2012-02-26T19:09:16 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 2.75 _pd_meas_2theta_range_max 163.95 _pd_meas_2theta_range_inc 0.05 _pd_proc_2theta_range_min 2.5091 _pd_proc_2theta_range_max 163.7091 _pd_proc_2theta_range_inc 0.05 loop_ _pd_meas_counts_total _pd_proc_ls_weight _pd_proc_intensity_bkg_calc _pd_calc_intensity_total 134.0 0.0 3798.84204 . 109.0 0.0 3796.27588 . 147.0 0.0 3793.72510 . 125.0 0.0 3791.18945 . 146.0 0.0 3788.66895 . 137.0 0.0 3786.16309 . 142.0 0.0 3783.67261 . 171.0 0.0 3781.19678 . 144.0 0.0 3778.73560 . 139.0 0.0 3776.28931 . 133.0 0.0 3773.85742 . 135.0 0.0 3771.44043 . 129.0 0.0 3769.03760 . 133.0 0.0 3766.64917 . 147.0 0.0 3764.27515 . 139.0 0.0 3761.91528 . 162.0 0.0 3759.56934 . 149.0 0.0 3757.23779 . 172.0 0.0 3754.92017 . 132.0 0.0 3752.61646 . 152.0 0.0 3750.32642 . 144.0 0.0 3748.05054 . 125.0 0.0 3745.78809 . 133.0 0.0 3743.53931 . 134.0 0.0 3741.30396 . 217.0 0.0 3739.08228 . 210.0 0.0 3736.87402 . 235.0 0.0 3734.67896 . 237.0 0.0 3732.49731 . 232.0 0.0 3730.32861 . 249.0 0.0 3728.17334 . 262.0 0.0 3726.03076 . 304.0 0.0 3723.90137 . 368.0 0.0 3721.78491 . 436.0 0.0 3719.68115 . 466.0 0.0 3717.59009 . 570.0 0.0 3715.51196 . 588.0 0.0 3713.44629 . 825.0 0.0 3711.39331 . 981.0 0.0 3709.35254 . 1174.0 0.0 3707.32446 . 1435.0 0.0 3705.30859 . 1717.0 0.0 3703.30493 . 2053.0 0.0 3701.31348 . 2357.0 0.0 3699.33423 . 2636.0 0.0 3697.36719 . 2866.0 0.0 3695.41187 . 3261.0 0.0 3693.46851 . 3618.0 0.0 3691.53711 . 3907.0 0.0 3689.61768 . 4565.0 0.0 3687.70972 . 4851.0 0.0 3685.81348 . 5235.0 0.0 3683.92871 . 5459.0 0.0 3682.05566 . 5537.0 0.0 3680.19409 . 5846.0 0.0 3678.34375 . 5928.0 0.0 3676.50488 . 5983.0 0.0 3674.67725 . 5892.0 0.0 3672.86084 . 5884.0 0.0 3671.05542 . 5965.0 0.0 3669.26123 . 5929.0 0.0 3667.47803 . 5867.0 0.0 3665.70581 . 5986.0 0.0 3663.94434 . 5817.0 0.0 3662.19385 . 5832.0 0.0 3660.45410 . 5754.0 0.0 3658.72510 . 5781.0 0.0 3657.00635 . 5556.0 0.0 3655.29858 . 5688.0 0.0 3653.60107 . 5587.0 0.0 3651.91406 . 5487.0 0.0 3650.23755 . 5593.0 0.0 3648.57129 . 5579.0 0.0 3646.91528 . 5395.0 0.0 3645.26953 . 5509.0 0.0 3643.63379 . 5518.0 0.0 3642.00830 . 5440.0 0.0 3640.39282 . 5391.0 0.0 3638.78711 . 5268.0 0.0 3637.19141 . 5228.0 0.0 3635.60547 . 5330.0 0.0 3634.02954 . 5195.0 0.0 3632.46313 . 5070.0 0.0 3630.90649 . 5041.0 0.0 3629.35938 . 5103.0 0.0 3627.82178 . 5160.0 0.0 3626.29370 . 5085.0 0.0 3624.77515 . 5034.0 0.0 3623.26587 . 5106.0 0.0 3621.76611 . 4958.0 0.0 3620.27539 . 5021.0 0.0 3618.79395 . 4823.0 0.0 3617.32153 . 5037.0 0.0 3615.85840 . 4962.0 0.0 3614.40430 . 4909.0 0.0 3612.95898 . 4869.0 0.0 3611.52271 . 4895.0 0.0 3610.09521 . 4817.0 0.0 3608.67676 . 4845.0 0.0 3607.26685 . 4678.0 0.0 3605.86572 . 4681.0 0.0 3604.47314 . 4871.0 0.0 3603.08936 . 4767.0 0.0 3601.71387 . 4795.0 0.0 3600.34717 . 4679.0 0.0 3598.98853 . 4730.0 0.0 3597.63867 . 4780.0 0.0 3596.29688 . 4718.0 0.0 3594.96338 . 4672.0 0.0 3593.63818 . 4589.0 0.0 3592.32104 . 4435.0 0.0 3591.01221 . 4771.0 0.0 3589.71118 . 4484.0 0.0 3588.41846 . 4526.0 0.0 3587.13354 . 4574.0 0.0 3585.85645 . 4418.0 0.0 3584.58740 . 4547.0 0.0 3583.32617 . 4436.0 0.0 3582.07251 . 4443.0 0.0 3580.82666 . 4461.0 0.0 3579.58838 . 4362.0 0.0 3578.35791 . 4363.0 0.0 3577.13477 . 4543.0 0.0 3575.91919 . 4356.0 0.0 3574.71118 . 4411.0 0.0 3573.51050 . 4374.0 0.0 3572.31714 . 4429.0 0.0 3571.13110 . 4309.0 0.0 3569.95239 . 4307.0 0.0 3568.78101 . 4277.0 0.0 3567.61670 . 4265.0 0.0 3566.45947 . 4406.0 0.0 3565.30933 . 4335.0 0.0 3564.16602 . 4280.0 0.0 3563.03003 . 4322.0 0.0 3561.90063 . 4261.0 0.0 3560.77832 . 4293.0 0.0 3559.66284 . 4248.0 0.0 3558.55420 . 4215.0 0.0 3557.45215 . 4138.0 0.0 3556.35693 . 4136.0 0.0 3555.26831 . 4109.0 0.0 3554.18628 . 4125.0 0.0 3553.11084 . 4185.0 0.0 3552.04175 . 4147.0 0.0 3550.97949 . 4059.0 0.0 3549.92334 . 4135.0 0.0 3548.87378 . 3998.0 0.0 3547.83032 . 4053.0 0.0 3546.79321 . 4118.0 0.0 3545.76245 . 4261.0 0.0 3544.73804 . 4096.0 0.0 3543.71948 . 4090.0 0.0 3542.70728 . 4047.0 0.0 3541.70093 . 4079.0 0.0 3540.70068 . 4092.0 0.0 3539.70654 . 4128.0 0.0 3538.71826 . 4018.0 0.0 3537.73584 . 4115.0 0.0 3536.75952 . 4007.0 0.0 3535.78882 . 4081.0 0.0 3534.82373 . 4052.0 0.0 3533.86475 . 4000.0 0.0 3532.91113 . 4001.0 0.0 3531.96338 . 4007.0 0.0 3531.02124 . 3956.0 0.0 3530.08447 . 3926.0 0.0 3529.15332 . 4038.0 0.0 3528.22778 . 3998.0 0.0 3527.30762 . 4075.0 0.0 3526.39282 . 3970.0 0.0 3525.48340 . 3926.0 0.0 3524.57935 . 3974.0 0.0 3523.68066 . 3964.0 0.0 3522.78711 . 3887.0 0.0 3521.89893 . 3978.0 0.0 3521.01563 . 3931.0 0.0 3520.13770 . 4004.0 0.0 3519.26489 . 3860.0 0.0 3518.39697 . 3892.0 0.0 3517.53418 . 3836.0 0.0 3516.67627 . 3796.0 0.0 3515.82349 . 3928.0 0.0 3514.97534 . 3909.0 0.0 3514.13232 . 3962.0 0.0 3513.29395 . 3867.0 0.0 3512.46045 . 3856.0 0.0 3511.63184 . 3789.0 0.0 3510.80762 . 3886.0 0.0 3509.98828 . 3833.0 0.0 3509.17358 . 3854.0 0.0 3508.36353 . 3856.0 0.0 3507.55786 . 3955.0 0.0 3506.75708 . 3970.0 0.0 3505.96045 . 3942.0 0.0 3505.16846 . 3807.0 0.0 3504.38086 . 3828.0 0.0 3503.59766 . 3778.0 0.0 3502.81885 . 3830.0 0.0 3502.04443 . 3857.0 0.0 3501.27417 . 3810.0 0.0 3500.50830 . 3815.0 0.0 3499.74658 . 3770.0 0.0 3498.98901 . 3721.0 0.0 3498.23560 . 3790.0 0.0 3497.48633 . 3797.0 0.0 3496.74121 . 3702.0 0.0 3496.00000 . 3683.0 0.0 3495.26294 . 3682.0 0.0 3494.52979 . 3643.0 0.0 3493.80054 . 3657.0 0.0 3493.07520 . 3629.0 0.0 3492.35400 . 3623.0 0.0 3491.63647 . 3672.0 0.0 3490.92261 . 3723.0 0.0 3490.21289 . 3628.0 0.0 3489.50659 . 3685.0 0.0 3488.80420 . 3608.0 0.0 3488.10547 . 3541.0 0.0 3487.41040 . 3677.0 0.0 3486.71899 . 3811.0 0.0 3486.03125 . 3635.0 0.0 3485.34692 . 3551.0 0.0 3484.66626 . 3675.0 0.0 3483.98901 . 3594.0 0.0 3483.31543 . 3648.0 0.0 3482.64502 . 3580.0 0.0 3481.97827 . 3594.0 0.0 3481.31470 . 3643.0 0.0 3480.65454 . 3601.0 0.0 3479.99780 . 3547.0 0.0 3479.34424 . 3633.0 0.0 3478.69409 . 3599.0 0.0 3478.04712 . 3574.0 0.0 3477.40332 . 3616.0 0.0 3476.76270 . 3563.0 0.0 3476.12524 . 3504.0 0.0 3475.49097 . 3550.0 0.0 3474.85962 . 3590.0 0.0 3474.23145 . 3598.0 0.0 3473.60645 . 3515.0 0.0 3472.98438 . 3510.0 0.0 3472.36523 . 3576.0 0.0 3471.74902 . 3452.0 0.0 3471.13574 . 3567.0 0.0 3470.52539 . 3540.0 0.0002825 3469.91797 3470.05200 3479.0 0.0002874 3469.31323 3469.45288 3476.0 0.0002877 3468.71143 3468.85718 3538.0 0.0002826 3468.11255 3468.26489 3469.0 0.0002883 3467.51611 3467.67529 3530.0 0.0002833 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3154.30054 3315.15259 3319.0 0.0003013 3153.44360 3314.86426 3370.0 0.0002967 3152.57300 3314.75659 3330.0 0.0003003 3151.68896 3314.82275 3314.0 0.0003018 3150.79102 3315.05762 3352.0 0.0002983 3149.87939 3315.45654 3372.0 0.0002966 3148.95410 3316.01929 3359.0 0.0002977 3148.01465 3316.74561 3412.0 0.0002931 3147.06128 3317.63696 3436.0 0.0002910 3146.09375 3318.69678 3410.0 0.0002933 3145.11182 3319.93506 3348.0 0.0002987 3144.11621 3321.35376 3404.0 0.0002938 3143.10596 3322.96313 3388.0 0.0002952 3142.08105 3324.76978 3344.0 0.0002990 3141.04175 3326.78027 3318.0 0.0003014 3139.98779 3329.00317 3375.0 0.0002963 3138.91943 3331.44214 3457.0 0.0002893 3137.83594 3334.09937 3364.0 . . . 3349.0 . . . 3388.0 . . . 3406.0 . . . 3441.0 . . . 3461.0 . . . 3496.0 . . . 3425.0 . . . 3313.0 . . . 3408.0 . . . 3417.0 . . . 3296.0 . . . 3391.0 . . . 3428.0 . . . 3426.0 . . . 3501.0 . . . 3489.0 . . . 3465.0 . . . 3444.0 . . . 3467.0 . . . 3511.0 . . . 3544.0 . . . 3491.0 . . . 3473.0 . . . 3396.0 . . . 3393.0 . . . 3407.0 . . . 3511.0 . . . 3480.0 . . . 3529.0 . . . 3557.0 . . . 3578.0 . . . 3558.0 . . . 3559.0 . . . 3549.0 . . . 3582.0 . . . 3523.0 . . . 3497.0 . . . 3544.0 . . . 3530.0 . . . 3477.0 . . . 3447.0 . . . 3502.0 . . . 3605.0 . . . 3597.0 . . . 3624.0 . . . 3575.0 . . . 3721.0 . . . 3736.0 . . . 3685.0 . . . 3715.0 . . . 3692.0 . . . 3657.0 . . . 3752.0 . . . 3666.0 . . . 3661.0 . . . 3744.0 . . . 3829.0 . . . 3769.0 . . . 3748.0 . . . 3726.0 . . . 3827.0 . . . 3765.0 . . . 3808.0 . . . 3812.0 . . . 3866.0 . . . 3738.0 . . . 3813.0 . . . 3855.0 . . . 3802.0 . . . 3930.0 . . . 3807.0 . . . 3708.0 . . . 3769.0 . . . 3838.0 . . . 1923.0 . . . 1952.0 . . . 2044.0 . . . 1992.0 . . . 1986.0 . . . 2008.0 . . . 1876.0 . . . 1997.0 . . . 1989.0 . . . 2015.0 . . . 2016.0 . . . 2022.0 . . . 2045.0 . . . 1970.0 . . . 2023.0 . . . 2176.0 . . . 2044.0 . . . 2126.0 . . . 2065.0 . . . 2093.0 . . . 2218.0 . . . 2088.0 . . . 2226.0 . . . 2176.0 . . . 2132.0 . . . _pd_meas_number_of_points 3225 _pd_proc_number_of_points 3225 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 0 1 o 0.696 0.158 180.00 7.92168 2.32 0 0 2 o 51.839 55.767 0.00 5.71715 45.53 0 1 1 o 3.626 3.850 0.00 5.56379 6.04 2 0 0 o 42.068 42.065 0.00 5.49255 34.18 1 0 2 o 0.187 0.215 180.00 5.07142 0.26 1 1 1 o 10.595 10.465 180.00 4.96346 28.29 2 0 1 o 2.712 2.682 0.00 4.95097 3.60 2 1 0 o 6.167 4.627 180.00 4.15934 5.87 1 1 2 o 0.616 0.591 180.00 3.96723 1.07 2 0 2 o 17.329 16.550 0.00 3.96084 15.03 2 1 1 o 46.817 45.388 0.00 3.90876 79.18 1 0 3 o 3.971 1.569 0.00 3.60085 2.88 3 0 1 o 0.732 0.287 0.00 3.48725 0.50 2 1 2 o 5.498 3.837 0.00 3.36341 7.03 0 1 3 o 97.621 91.416 180.00 3.27047 59.25 0 2 0 o 2.546 3.958 0.00 3.18429 0.74 1 1 3 o 2.720 3.667 180.00 3.13451 3.06 2 0 3 o 9.555 12.675 180.00 3.13135 5.36 3 0 2 o 5.788 6.873 0.00 3.08348 3.16 3 1 1 o 20.317 21.890 0.00 3.05872 21.84 1 2 1 o 0.008 0.084 180.00 2.95452 0.01 0 0 4 o 110.675 115.712 0.00 2.85857 26.36 2 1 3 o 0.054 0.051 0.00 2.81005 0.05 0 2 2 o 46.620 48.166 0.00 2.78189 21.17 3 1 2 o 0.050 0.052 180.00 2.77529 0.05 1 0 4 o 9.820 10.346 180.00 2.76644 4.42 2 2 0 o 35.794 38.011 0.00 2.75481 15.98 4 0 0 o 213.760 226.569 0.00 2.74628 47.45 1 2 2 o 5.262 5.036 0.00 2.69676 4.53 2 2 1 o 18.536 19.986 180.00 2.67818 15.76 4 0 1 o 0.626 0.722 0.00 2.67033 0.26 3 0 3 o 0.119 0.158 0.00 2.64056 0.05 1 1 4 o 2.448 4.010 0.00 2.53738 1.90 2 0 4 o 6.514 10.253 0.00 2.53571 2.52 4 1 0 o 13.717 16.584 0.00 2.52180 5.26 2 2 2 o 5.720 7.228 0.00 2.48173 4.27 4 0 2 o 7.249 8.699 180.00 2.47548 2.70 4 1 1 o 1.950 2.255 0.00 2.46262 1.44 3 1 3 o 4.509 3.578 180.00 2.43921 3.27 1 2 3 o 100.124 96.960 0.00 2.38537 70.07 2 1 4 o 14.191 13.854 180.00 2.35584 9.73 3 2 1 o 108.478 105.779 180.00 2.35146 74.17 1 1 1 o 7.890 7.606 180.00 2.32500 43.37 4 1 2 o 12.053 10.975 0.00 2.30731 7.99 3 0 4 o 8.485 9.173 0.00 2.25326 2.71 1 0 5 o 86.431 82.693 180.00 2.23886 27.33 2 2 3 o 0.987 0.903 180.00 2.23268 0.62 4 0 3 o 45.228 41.014 0.00 2.22813 14.20 3 2 2 o 34.405 32.760 180.00 2.21513 21.40 5 0 1 o 8.148 6.610 0.00 2.15755 2.43 0 1 5 o 37.743 28.983 180.00 2.15230 11.24 0 2 4 o 18.974 14.383 0.00 2.12718 5.55 3 1 4 o 1.526 1.183 0.00 2.12422 0.89 1 1 5 o 4.620 3.752 180.00 2.11214 2.67 2 0 5 o 0.264 0.214 180.00 2.11118 0.08 1 2 4 o 39.353 37.155 180.00 2.08838 22.40 4 1 3 o 2.909 2.337 0.00 2.10313 1.67 0 3 1 o 0.562 0.537 0.00 2.08719 0.16 4 2 0 o 126.899 125.368 0.00 2.07967 35.90 5 0 2 o 9.596 7.860 0.00 2.05081 2.66 1 3 1 o 0.822 0.674 180.00 2.05051 0.46 4 2 1 o 7.094 6.064 0.00 2.04610 3.92 5 1 1 o 0.412 0.361 0.00 2.04347 0.23 3 2 3 o 0.461 0.417 180.00 2.03261 0.25 2 0 0 o 1.560 1.768 0.00 2.01351 5.17 2 1 5 o 2.406 2.468 0.00 2.00394 1.29 2 2 4 o 122.741 120.767 0.00 1.98361 64.96 4 0 4 o 0.090 0.089 0.00 1.98042 0.02 2 3 0 o 6.057 6.014 180.00 1.98011 1.60 1 3 2 o 14.092 13.715 180.00 1.95822 7.33 4 2 2 o 81.272 81.124 0.00 1.95438 42.16 5 1 2 o 0.533 0.543 0.00 1.95209 0.28 2 3 1 o 0.000 0.000 0.00 1.95107 0.00 3 0 5 o 17.051 18.907 180.00 1.93966 4.38 0 0 6 o 113.572 117.560 0.00 1.90572 14.25 5 0 3 o 105.073 106.028 0.00 1.90343 26.33 4 1 4 o 2.374 2.339 180.00 1.89109 1.18 1 0 6 o 59.014 57.236 180.00 1.87767 14.53 2 3 2 o 25.222 27.262 180.00 1.87106 12.37 3 1 5 o 1.786 2.077 180.00 1.85551 0.87 0 3 3 o 12.303 14.308 0.00 1.85460 2.98 3 2 4 o 0.898 1.261 0.00 1.83934 0.43 1 2 5 o 5.975 7.051 0.00 1.83148 2.86 6 0 0 o 169.226 198.818 0.00 1.83085 20.21 1 3 3 o 5.190 6.105 180.00 1.82872 2.48 4 2 3 o 0.140 0.171 180.00 1.82559 0.07 5 1 3 o 0.017 0.021 180.00 1.82372 0.01 3 3 1 o 10.281 13.952 180.00 1.81330 4.86 6 0 1 o 0.588 0.745 0.00 1.80782 0.14 1 1 6 o 1.945 2.114 180.00 1.80102 0.91 2 0 6 o 69.365 75.177 0.00 1.80042 16.25 5 2 1 o 4.497 4.954 180.00 1.78616 2.09 6 1 0 o 2.119 2.564 180.00 1.75958 0.48 2 2 5 o 8.896 10.764 180.00 1.75958 4.07 4 0 5 o 2.575 3.224 0.00 1.75735 0.59 2 3 3 o 0.556 0.699 0.00 1.75713 0.25 3 3 2 o 2.544 2.880 180.00 1.74854 1.16 6 0 2 o 35.707 35.244 0.00 1.74363 8.08 5 0 4 o 0.242 0.234 0.00 1.74196 0.05 6 1 1 o 57.226 54.522 0.00 1.73911 25.85 2 1 6 o 3.442 3.076 0.00 1.73252 1.55 5 2 2 o 12.684 11.578 0.00 1.72417 5.68 4 1 5 o 0.399 0.520 180.00 1.69404 0.18 3 0 6 o 11.353 12.809 0.00 1.69047 2.50 1 3 4 o 1.569 1.616 0.00 1.68415 0.69 6 1 2 o 0.159 0.162 0.00 1.68173 0.07 4 2 4 o 76.407 77.843 0.00 1.68170 33.45 5 1 4 o 2.842 2.902 180.00 1.68024 1.24 4 3 0 o 4.040 4.137 0.00 1.67957 0.88 4 3 1 o 5.575 5.222 0.00 1.66174 2.42 3 2 5 o 33.916 32.007 180.00 1.65653 14.66 3 3 3 o 17.499 16.075 0.00 1.65449 7.56 6 0 3 o 4.954 4.026 180.00 1.65032 1.07 0 2 6 o 270.108 252.272 0.00 1.63524 57.83 3 1 6 o 14.075 13.359 180.00 1.63389 6.02 5 2 3 o 26.957 25.611 0.00 1.63379 11.54 2 3 4 o 1.590 1.439 0.00 1.62774 0.68 1 2 6 o 3.145 2.516 180.00 1.61741 1.34 1 0 7 o 0.527 0.414 0.00 1.61571 0.11 4 3 2 o 0.349 0.264 0.00 1.61147 0.15 6 1 3 o 0.113 0.106 0.00 1.59756 0.05 0 4 0 o 616.376 639.799 0.00 1.59214 64.88 6 2 0 o 139.754 143.022 0.00 1.58720 29.37 5 0 5 o 7.437 7.720 180.00 1.58434 1.56 0 1 7 o 33.361 34.897 180.00 1.58225 7.00 6 2 1 o 32.030 30.499 180.00 1.57213 13.40 2 2 6 o 62.993 60.623 0.00 1.56725 26.32 1 1 7 o 3.544 3.402 0.00 1.56609 1.48 2 0 7 o 48.793 46.818 180.00 1.56570 10.19 4 0 6 o 84.257 80.844 0.00 1.56568 17.60 1 4 1 o 0.635 0.603 180.00 1.56093 0.26 0 3 5 o 0.674 0.592 180.00 1.55584 0.14 7 0 1 o 18.579 16.332 180.00 1.55473 3.87 1 3 5 o 0.100 0.100 0.00 1.54046 0.04 4 2 5 o 6.732 6.867 0.00 1.53859 2.79 3 3 4 o 60.985 61.724 0.00 1.54513 25.35 5 1 5 o 0.953 0.978 180.00 1.53747 0.40 4 3 3 o 5.673 5.832 180.00 1.53696 2.35 6 0 4 o 127.457 128.133 0.00 1.54174 26.47 0 4 2 o 48.184 48.979 0.00 1.53378 9.99 6 2 2 o 98.532 95.670 0.00 1.52936 40.85 2 4 0 o 46.086 44.737 0.00 1.52919 9.55 5 2 4 o 0.092 0.089 180.00 1.52824 0.04 2 1 7 o 11.768 11.156 0.00 1.52042 4.87 4 1 6 o 1.985 1.881 180.00 1.52040 0.82 1 4 2 o 0.824 0.755 0.00 1.51904 0.34 2 4 1 o 3.686 3.053 0.00 1.51570 1.53 7 0 2 o 1.187 0.972 180.00 1.51332 0.25 5 3 1 o 5.488 4.496 0.00 1.51320 2.27 7 1 1 o 4.615 3.880 0.00 1.51037 1.91 6 1 4 o 24.023 19.909 180.00 1.49846 9.94 2 3 5 o 6.121 5.157 180.00 1.49694 2.53 3 2 6 o 0.728 0.619 0.00 1.49311 0.30 3 0 7 o 13.323 11.113 0.00 1.49177 2.76 7 1 2 o 12.325 13.288 0.00 1.47233 5.11 2 4 2 o 47.606 49.378 0.00 1.47726 19.72 5 3 2 o 27.746 29.316 180.00 1.47495 11.50 6 2 3 o 0.777 0.916 180.00 1.46523 0.32 1 4 3 o 5.767 7.304 180.00 1.45615 2.40 3 1 7 o 29.564 33.209 180.00 1.45245 12.31 7 0 3 o 2.593 2.848 180.00 1.45111 0.54 3 4 1 o 14.371 15.266 0.00 1.44833 5.99 4 3 4 o 13.984 14.814 0.00 1.44811 5.83 1 2 7 o 0.460 0.604 180.00 1.44084 0.19 5 0 6 o 0.614 0.906 180.00 1.43960 0.13 3 3 5 o 2.391 2.727 0.00 1.43194 1.00 0 0 8 o 44.287 44.686 0.00 1.42929 4.65 6 0 5 o 11.645 11.747 0.00 1.42924 2.45 2 2 0 o 1.170 1.386 0.00 1.42377 6.06 2 4 3 o 0.821 0.836 180.00 1.41923 0.35 5 2 5 o 9.488 9.385 180.00 1.41846 4.01 1 0 8 o 1.156 1.108 0.00 1.41734 0.24 5 3 3 o 3.928 3.754 0.00 1.41718 1.66 7 1 3 o 3.387 3.155 180.00 1.41485 1.44 3 4 2 o 3.979 3.706 0.00 1.41469 1.69 1 3 6 o 12.224 12.060 180.00 1.40645 5.21 2 2 7 o 0.001 0.001 0.00 1.40504 0.00 4 2 6 o 234.308 232.534 0.00 1.40502 100.00 5 1 6 o 41.167 41.185 180.00 1.40417 17.58 4 0 7 o 4.349 4.364 0.00 1.40390 0.93 7 2 1 o 3.430 3.316 0.00 1.39709 1.47 6 1 5 o 0.575 0.560 180.00 1.39455 0.25 6 2 4 o 61.938 61.640 0.00 1.38765 26.86 6 3 0 o 0.745 0.738 180.00 1.38645 0.16 0 4 4 o 64.134 64.684 0.00 1.39095 13.86 1 1 8 o 29.045 28.368 0.00 1.38349 12.65 2 0 8 o 59.079 57.675 0.00 1.38322 12.87 1 4 4 o 0.458 0.451 180.00 1.37993 0.20 4 4 0 o 122.694 121.232 0.00 1.37740 26.91 6 3 1 o 6.669 6.606 180.00 1.37636 2.93 7 0 4 o 3.141 3.122 180.00 1.37564 0.69 8 0 0 o 201.832 204.184 0.00 1.37314 22.25 2 3 6 o 4.549 4.603 180.00 1.37309 2.01 4 1 7 o 5.993 6.079 0.00 1.37099 2.65 4 4 1 o 0.430 0.460 0.00 1.36752 0.19 7 2 2 o 12.722 13.691 180.00 1.36682 5.66 3 4 3 o 0.030 0.033 0.00 1.36347 0.01 8 0 1 o 0.512 0.559 0.00 1.36334 0.11 4 3 5 o 0.128 0.132 180.00 1.35369 0.06 2 1 8 o 1.767 1.894 0.00 1.35171 0.81 3 2 7 o 0.280 0.303 180.00 1.35088 0.13 2 4 4 o 20.386 22.146 0.00 1.34838 9.35 6 3 2 o 4.675 5.066 180.00 1.34739 2.15 5 3 4 o 7.587 8.266 0.00 1.34663 3.49 7 1 4 o 24.725 27.790 0.00 1.34463 11.42 4 4 2 o 0.014 0.014 0.00 1.33909 0.01 8 1 0 o 8.917 10.118 180.00 1.34229 2.07 8 0 2 o 20.506 15.782 0.00 1.33517 4.83 8 1 1 o 0.017 0.014 0.00 1.33314 0.01 3 0 8 o 32.357 28.704 180.00 1.33145 7.70 3 3 6 o 27.744 28.340 0.00 1.32241 13.52 7 2 3 o 20.799 20.518 0.00 1.32046 10.19 6 0 6 o 134.872 132.838 0.00 1.32028 33.06 5 2 6 o 14.676 14.572 0.00 1.31177 7.39 5 0 7 o 13.192 13.195 0.00 1.31086 3.33 8 1 2 o 5.988 6.042 0.00 1.30676 3.07 0 2 8 o 4.491 4.535 180.00 1.30395 1.16 6 2 5 o 5.300 5.353 180.00 1.30392 2.75 3 1 8 o 0.161 0.163 0.00 1.30327 0.08 6 3 3 o 18.795 19.023 180.00 1.30292 9.78 1 4 5 o 45.383 45.458 180.00 1.29751 24.14 3 4 4 o 4.277 4.355 0.00 1.30029 2.25 4 4 3 o 13.129 11.987 0.00 1.29541 7.05 1 2 8 o 6.301 5.580 180.00 1.29486 3.39 0 3 7 o 27.895 24.322 0.00 1.29458 7.52 7 0 5 o 26.620 22.450 180.00 1.29394 7.19 6 1 6 o 0.258 0.207 180.00 1.29279 0.14 8 0 3 o 9.954 7.687 180.00 1.29186 2.72 1 3 7 o 0.100 0.086 180.00 1.28568 0.06 4 2 7 o 32.320 28.485 0.00 1.28459 18.33 5 1 7 o 9.554 8.424 0.00 1.28394 5.44 5 4 1 o 0.805 0.719 0.00 1.28109 0.47 2 4 5 o 1.243 1.689 0.00 1.27118 0.77 5 3 5 o 1.779 2.356 0.00 1.26971 1.11 8 1 3 o 7.063 7.730 0.00 1.26607 4.56 0 5 1 o 6.653 7.243 0.00 1.26588 2.15 2 2 8 o 0.282 0.354 180.00 1.26869 0.18 7 1 5 o 0.620 0.749 0.00 1.26803 0.39 1 0 9 o 8.633 9.005 0.00 1.26206 2.89 4 0 8 o 4.914 5.870 0.00 1.26786 1.56 8 2 0 o 10.605 10.946 0.00 1.26090 3.59 5 4 2 o 2.888 3.026 0.00 1.25763 2.02 1 5 1 o 18.292 19.162 180.00 1.25756 12.83 2 3 7 o 23.795 24.505 0.00 1.26005 16.25 4 3 6 o 7.378 7.598 0.00 1.26004 5.04 7 2 4 o 11.442 12.067 180.00 1.26283 7.60 8 2 1 o 0.576 0.606 0.00 1.25330 0.42 6 3 4 o 11.763 12.077 0.00 1.24746 9.43 7 3 1 o 44.908 46.223 180.00 1.25431 32.71 0 1 9 o 0.514 0.461 0.00 1.24593 0.21 4 1 8 o 0.460 0.380 0.00 1.24345 0.40 _reflns_number_total 251 _reflns_limit_h_min 0 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 5 _reflns_limit_l_min 0 _reflns_limit_l_max 9 _reflns_d_resolution_high 1.243 _reflns_d_resolution_low 7.922 #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#