Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Aurelio Cabeza' 'Miguel Aranda' 'Premysl Beran' 'J. L. Garcia-Munoz' 'M. M. Gomez-Alcantara' 'Pascual Olivera-Pastor' _publ_contact_author_name 'Aurelio Cabeza' _publ_contact_author_address ; Departamento de Quimica Inorganica Universidad de Malaga Teatinos s/n Malaga 29071 SPAIN ; _publ_contact_author_email AURELIO@UMA.ES _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Layered and pillared metal carboxyethylphosphonate hybrid compounds ; data_MN3ACEF4_3F2_publ _database_code_depnum_ccdc_archive 'CCDC 279120' _pd_block_id 2005-07-12T17:35|MN3ACEF4_3F2|mez-Alcantara_et_al.|Siemens_D5000 _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2005-07-12T17:35 _audit_author_name 'M.Mar G?mez-Alcantara et al.' _audit_update_record ; 2005-07-12T17:35 Initial CIF as created by GSAS2CIF ; #============================================================================= # 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 ? _pd_char_colour ? # use ICDD colour descriptions _refine_ls_shift/su_max 0.04 _refine_ls_shift/su_mean 0.00 _computing_structure_refinement GSAS _refine_ls_number_parameters 78 _refine_ls_goodness_of_fit_all 2.19 _refine_ls_number_restraints 19 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature ? _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 Mn3Acef4 _cell_length_a 10.38287(22) _cell_length_b 7.15915(19) _cell_length_c 10.21950(29) _cell_angle_alpha 90.0 _cell_angle_beta 108.7229(16) _cell_angle_gamma 90.0 _cell_volume 719.44(4) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y+1/2,-z+1/2 -1 -x,-y,-z -2 +x,-y+1/2,+z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity O OW1 0.1344(7) -0.0901(15) 0.4699(9) 1.0 Uiso 0.0416(16) 4 Mn Mn 0.01304(29) 0.1366(8) 0.77494(28) 1.0 Uiso 0.0479(14) 4 P P 0.18796(33) 0.3718(7) 0.6343(5) 1.0 Uiso 0.0405(21) 4 O OH1 0.0754(7) -0.1342(24) 0.7646(8) 1.0 Uiso 0.0416(16) 4 O O2 0.1724(7) 0.2232(9) 0.7372(7) 1.0 Uiso 0.0416(16) 4 O O3 0.1087(6) 0.3172(13) 0.4843(6) 1.0 Uiso 0.0416(16) 4 O O4 0.1314(6) 0.5647(8) 0.6620(9) 1.0 Uiso 0.0416(16) 4 C C3 0.5621(6) 0.2747(15) 0.5930(11) 1.0 Uiso 0.035(4) 4 C C1 0.3662(5) 0.3983(12) 0.6548(10) 1.0 Uiso 0.035(4) 4 C C2 0.4160(5) 0.2487(14) 0.5824(11) 1.0 Uiso 0.035(4) 4 O OC1 0.6417(7) 0.3687(11) 0.6859(9) 1.0 Uiso 0.0416(16) 4 O OC2 0.6126(6) 0.1608(12) 0.5283(8) 1.0 Uiso 0.0416(16) 4 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C3 Mn O7 P' _chemical_formula_weight 233.94 _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 OW1 Mn 2.501(8) . -1_556 N Mn OW1 2.501(8) . -1_556 N Mn Mn 3.6136(7) . 2_546 N Mn Mn 3.6136(7) . 2_556 N Mn P 3.143(5) . 1_555 N Mn P 3.170(5) . 2_546 N Mn OH1 2.057(13) . 1_555 N Mn OH1 1.861(13) . 2_556 N Mn O2 1.919(6) . 1_555 N Mn O3 2.076(6) . -2_555 N Mn O4 1.884(7) . 2_546 N P Mn 3.143(5) . 1_555 N P Mn 3.170(5) . 2_556 N P O2 1.540(4) . 1_555 N P O3 1.539(4) . 1_555 N P O4 1.561(5) . 1_555 N P C1 1.804(4) . 1_555 N OH1 Mn 2.057(13) . 1_555 N OH1 Mn 1.861(13) . 2_546 N O2 Mn 1.919(6) . 1_555 N O2 P 1.540(4) . 1_555 N O3 Mn 2.076(6) . -2_554 N O3 P 1.539(4) . 1_555 N O4 Mn 1.884(7) . 2_556 N O4 P 1.561(5) . 1_555 N C3 C2 1.498(5) . 1_555 N C3 OC1 1.238(5) . 1_555 N C3 OC2 1.265(5) . 1_555 N C1 P 1.804(4) . 1_555 N C1 C2 1.486(5) . 1_555 N C2 C3 1.498(5) . 1_555 N C2 C1 1.486(5) . 1_555 N OC1 C3 1.238(5) . 1_555 N OC1 OC2 2.142(5) . 1_555 N OC2 C3 1.265(5) . 1_555 N OC2 OC1 2.142(5) . 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 OW1 Mn OH1 85.69(33) -1_556 . 1_555 N OW1 Mn OH1 78.4(4) -1_556 . 2_556 N OW1 Mn O2 97.60(33) -1_556 . 1_555 N OW1 Mn O3 171.49(35) -1_556 . -2_566 N OW1 Mn O4 90.40(33) -1_556 . 2_546 N OH1 Mn OH1 164.06(28) 1_555 . 2_556 N OH1 Mn O2 89.3(5) 1_555 . 1_555 N OH1 Mn O3 98.6(4) 1_555 . -2_566 N OH1 Mn O4 93.3(4) 1_555 . 2_546 N OH1 Mn O2 93.9(4) 2_556 . 1_555 N OH1 Mn O3 97.0(5) 2_556 . -2_566 N OH1 Mn O4 85.6(4) 2_556 . 2_546 N O2 Mn O3 89.85(30) 1_555 . -2_566 N O2 Mn O4 171.7(5) 1_555 . 2_546 N O3 Mn O4 82.02(29) -2_566 . 2_546 N O2 P O3 111.4(4) 1_555 . 1_555 N O2 P O4 111.1(4) 1_555 . 1_555 N O2 P C1 108.76(33) 1_555 . 1_555 N O3 P O4 107.0(5) 1_555 . 1_555 N O3 P C1 110.03(33) 1_555 . 1_555 N O4 P C1 108.54(34) 1_555 . 1_555 N Mn OH1 Mn 134.5(4) 1_555 . 2_546 N Mn O2 P 130.3(5) 1_555 . 1_555 N Mn O3 P 155.7(7) -2_565 . 1_555 N Mn O4 P 133.7(5) 2_556 . 1_555 N C2 C3 OC1 122.3(5) 1_555 . 1_555 N C2 C3 OC2 117.5(5) 1_555 . 1_555 N OC1 C3 OC2 117.7(5) 1_555 . 1_555 N P C1 C2 112.0(4) 1_555 . 1_555 N C3 C2 C1 112.4(4) 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 ? _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # 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_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 Mn 4.0 0.000 0.000 11.2819 5.34090 7.35730 0.34320 3.01930 17.8674 2.24410 83.7543 1.08960 International_Tables_Vol_C P 4.0 0.000 0.000 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080 68.1645 1.11490 International_Tables_Vol_C O 28.0 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 12.0 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 _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 0.58 loop_ _diffrn_radiation_wavelength _diffrn_radiation_wavelength_wt _diffrn_radiation_type _diffrn_radiation_wavelength_id 1.540598 1.000 K\a~1~ 1 1.544398 0.450 K\a~2~ 2 _pd_proc_ls_prof_R_factor 0.0428 _pd_proc_ls_prof_wR_factor 0.0540 _pd_proc_ls_prof_wR_expected 0.0262 _refine_ls_R_Fsqd_factor 0.08244 _pd_proc_ls_background_function ; GSAS Background function number 7 with 26 terms. Linear interpolation 1: 29.1448 2: -57.0238 3: 21.9899 4: 95.9790 5: 218.888 6: 305.030 7: 355.193 8: 347.138 9: 203.008 10: 283.158 11: 171.064 12: 288.101 13: 209.242 14: 86.1774 15: 54.2251 16: 47.3104 17: 43.3947 18: 48.4272 19: -11.7332 20: -25.3936 21: -18.4834 22: -15.3310 23: -47.1548 24: -73.0108 25: -78.4139 26: -59.2970 ; _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_pref_orient_corr ; March-Dollase AXIS 1 Ratio= 0.850 Frac 0.897 h= 1.000 k= 0.000 l= 0.000 AXIS 2 Ratio= 0.578 Frac 0.103 h= 0.000 k= 0.000 l= 1.000 **** Spherical Harmonic ODF **** Spherical harmonic order= 2 The sample symmetry is: cylindrical (fiber texture) Index = 2 0 -2 Coeff= 0.0000 Index = 2 0 0 Coeff= 0.0000 Index = 2 0 2 Coeff= 0.0000 Prefered orientation correction range: Min= 0.74834, Max= 1.51111 ; _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) = 0.000 #2(GV) = 0.000 #3(GW) = 7.167 #4(GP) = 0.000 #5(LX) = 3.201 #6(LY) = 3.765 #7(S/L) = 0.0488 #8(H/L) = 0.0301 #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 0.0030 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00300 _pd_proc_info_datetime 2005-07-12T17:35:59 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 14.0 _pd_meas_2theta_range_max 80.0 _pd_meas_2theta_range_inc 0.02 _pd_proc_2theta_range_min 13.82818 _pd_proc_2theta_range_max 79.82819 _pd_proc_2theta_range_inc 0.02 _reflns_number_total 802 _reflns_limit_h_min 0 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 5 _reflns_limit_l_min -8 _reflns_limit_l_max 7 _reflns_d_resolution_high 1.232 _reflns_d_resolution_low 5.788 #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# data_MN3ACEF1_publ _database_code_depnum_ccdc_archive 'CCDC 279121' _pd_block_id 2005-07-12T17:16|MN3ACEF1|ez-Alcantara,_et_al.|Siemens_D5000 _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2005-07-12T17:16 _audit_author_name 'M.Mar Gomez-Alcantara, et al.' _audit_update_record ; 2005-07-12T17:16 Initial CIF as created by GSAS2CIF ; # 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 ? _pd_char_colour ? # use ICDD colour descriptions _refine_ls_shift/su_max 0.16 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 53 _refine_ls_goodness_of_fit_all 2.21 _refine_ls_number_restraints 19 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature ? _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 Mn3ACEF _cell_length_a 24.5597(16) _cell_length_b 4.9197(4) _cell_length_c 5.7769(4) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 698.01(10) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' 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+1/2,-y+1/2,+z 4 -x,-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 Mn MN 0.75870(16) 0.5291(9) 0.0890(20) 1.0 Uiso 0.0163(17) 4 P P 0.81901(23) 0.4729(13) 0.5909(11) 1.0 Uiso 0.0330(32) 4 O O1 0.7956(5) 0.325(4) 0.3756(26) 1.0 Uiso 0.0241(22) 4 O O2 0.7943(6) 0.347(4) 0.8151(24) 1.0 Uiso 0.0241(22) 4 O O3 0.8104(6) 0.7800(14) 0.585(4) 1.0 Uiso 0.0241(22) 4 C C1 0.89251(28) 0.4022(30) 0.5934(20) 1.0 Uiso 0.0241(22) 4 C C2 0.9129(5) 0.4324(30) 0.8367(21) 1.0 Uiso 0.0241(22) 4 C c3 0.9518(10) 0.666(4) 0.8535(15) 1.0 Uiso 0.0241(22) 4 O OC1 0.9655(6) 0.7840(21) 0.6726(17) 1.0 Uiso 0.0241(22) 4 O OC2 0.9665(6) 0.7435(20) 0.0485(16) 1.0 Uiso 0.0241(22) 4 O OW1 0.8264(6) 0.8658(25) 0.073(5) 1.0 Uiso 0.0241(22) 4 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C3 Mn O6 P' _chemical_formula_weight 217.94 _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 MN MN 3.8180(9) . 2_644 N MN MN 3.8180(9) . 2_645 N MN MN 3.8180(9) . 2_654 N MN MN 3.8180(9) . 2_655 N MN P 3.248(12) . 1_554 N MN P 3.268(11) . 1_555 N MN P 3.336(7) . 2_644 N MN P 2.900(7) . 2_654 N MN O1 2.137(16) . 1_555 N MN O1 2.330(20) . 2_654 N MN O2 2.017(14) . 1_554 N MN O2 2.418(21) . 2_654 N MN O3 2.094(13) . 2_644 N MN OW1 2.348(13) . 1_555 N P MN 3.268(11) . 1_555 N P MN 3.248(12) . 1_556 N P MN 2.900(7) . 2_645 N P MN 3.336(7) . 2_655 N P O1 1.550(7) . 1_555 N P O2 1.558(7) . 1_555 N P O3 1.526(6) . 1_555 N P C1 1.838(6) . 1_555 N O1 MN 2.137(16) . 1_555 N O1 MN 2.330(20) . 2_645 N O1 P 1.550(7) . 1_555 N O2 MN 2.017(14) . 1_556 N O2 MN 2.418(21) . 2_645 N O2 P 1.558(7) . 1_555 N O3 MN 2.094(13) . 2_655 N O3 P 1.526(6) . 1_555 N C1 P 1.838(6) . 1_555 N C1 C2 1.500(8) . 1_555 N C2 C1 1.500(8) . 1_555 N C2 c3 1.498(6) . 1_555 N c3 C2 1.498(6) . 1_555 N c3 OC1 1.241(4) . 1_555 N c3 OC2 1.242(4) . 1_556 N OC1 c3 1.241(4) . 1_555 N OC2 c3 1.242(4) . 1_554 N OW1 MN 2.348(13) . 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 MN O1 161.2(6) 1_555 . 2_654 N O1 MN O2 102.5(4) 1_555 . 1_554 N O1 MN O2 96.5(6) 1_555 . 2_654 N O1 MN O3 94.5(6) 1_555 . 2_644 N O1 MN OW1 93.5(9) 1_555 . 1_555 N O1 MN O2 96.4(6) 2_654 . 1_554 N O1 MN O2 64.70(23) 2_654 . 2_654 N O1 MN O3 84.0(7) 2_654 . 2_644 N O1 MN OW1 86.8(5) 2_654 . 1_555 N O2 MN O2 160.7(7) 1_554 . 2_654 N O2 MN O3 94.7(5) 1_554 . 2_644 N O2 MN OW1 88.6(10) 1_554 . 1_555 N O2 MN O3 87.0(7) 2_654 . 2_644 N O2 MN OW1 86.9(5) 2_654 . 1_555 N O3 MN OW1 170.5(7) 2_644 . 1_555 N O1 P O2 109.7(5) 1_555 . 1_555 N O1 P O3 113.2(6) 1_555 . 1_555 N O1 P C1 106.3(5) 1_555 . 1_555 N O2 P O3 111.0(6) 1_555 . 1_555 N O2 P C1 107.5(5) 1_555 . 1_555 N O3 P C1 108.8(5) 1_555 . 1_555 N MN O1 MN 117.4(5) 1_555 . 2_645 N MN O1 P 124.0(12) 1_555 . 1_555 N MN O1 P 94.6(9) 2_645 . 1_555 N MN O2 MN 118.5(6) 1_556 . 2_645 N MN O2 P 130.1(12) 1_556 . 1_555 N MN O2 P 91.0(8) 2_645 . 1_555 N MN O3 P 133.7(7) 2_655 . 1_555 N P C1 C2 108.5(6) 1_555 . 1_555 N C1 C2 c3 110.5(6) 1_555 . 1_555 N C2 c3 OC1 118.4(6) 1_555 . 1_555 N C2 c3 OC2 118.6(6) 1_555 . 1_556 N OC1 c3 OC2 122.8(7) 1_555 . 1_556 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 ? _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # 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_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 Mn 4.0 0.000 0.000 11.2819 5.34090 7.35730 0.34320 3.01930 17.8674 2.24410 83.7543 1.08960 International_Tables_Vol_C P 4.0 0.000 0.000 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080 68.1645 1.11490 International_Tables_Vol_C O 24.0 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 12.0 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 _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 0.58 loop_ _diffrn_radiation_wavelength _diffrn_radiation_wavelength_wt _diffrn_radiation_type _diffrn_radiation_wavelength_id 1.540500 1.000 K\a~1~ 1 1.544300 0.450 K\a~2~ 2 _pd_proc_ls_prof_R_factor 0.0663 _pd_proc_ls_prof_wR_factor 0.0889 _pd_proc_ls_prof_wR_expected 0.0412 _refine_ls_R_Fsqd_factor 0.07817 _pd_proc_ls_background_function ; GSAS Background function number 7 with 10 terms. Linear interpolation 1: -39.8034 2: -80.7380 3: -24.4264 4: -71.3973 5: -42.7767 6: -65.6595 7: -74.0261 8: -48.7394 9: -45.0509 10: -64.1089 ; _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_pref_orient_corr ; March-Dollase AXIS 1 Ratio= 0.98469 h= 1.000 k= 0.000 l= 0.000 Prefered orientation correction range: Min= 0.97713, Max= 1.04736 ; _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) = 0.000 #2(GV) = 0.000 #3(GW) = 3.456 #4(GP) = 0.000 #5(LX) = 5.959 #6(LY) = 33.281 #7(S/L) = 0.0417 #8(H/L) = 0.0400 #9(trns) = 0.00 #10(shft)= -12.1036 #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 0.0050 times the peak Aniso. broadening axis 0.0 1.0 0.0 ; _pd_proc_ls_peak_cutoff 0.00500 _pd_proc_info_datetime 2005-07-12T17:16:41 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 11.0 _pd_meas_2theta_range_max 80.0 _pd_meas_2theta_range_inc 0.02 _pd_proc_2theta_range_min 11.0 _pd_proc_2theta_range_max 80.0 _pd_proc_2theta_range_inc 0.02 _reflns_number_total 476 _reflns_limit_h_min 0 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 4 _reflns_limit_l_min 0 _reflns_limit_l_max 4 _reflns_d_resolution_high 1.206 _reflns_d_resolution_low 5.227 #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# data_ALACEF15_SIN_publ _database_code_depnum_ccdc_archive 'CCDC 279122' _pd_block_id ; 2005-07-12T17:45|ALACEF15_SIN|mez-Alcantara_et_al.| Synchrotron_line_ID-31_Grenobl ; _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2005-07-12T17:45 _audit_author_name 'M.Mar G?mez-Alcantara et al.' _audit_update_record ; 2005-07-12T17:45 Initial CIF as created by GSAS2CIF ; #============================================================================= # 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 ? _pd_char_colour ? # use ICDD colour descriptions _refine_ls_shift/su_max 0.12 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 55 _refine_ls_goodness_of_fit_all 0.96 _refine_ls_number_restraints 19 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature ? _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 Alacef15_SIN _cell_length_a 10.54073(22) _cell_length_b 7.89512(16) _cell_length_c 10.32709(22) _cell_angle_alpha 90.0 _cell_angle_beta 109.8186(13) _cell_angle_gamma 90.0 _cell_volume 808.52(4) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 2/C' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y,-z+1/2 -1 -x,-y,-z -2 +x,-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 Al Al1 0.3194(5) 0.4298(6) 0.7093(5) 1.0 Uiso 0.0183(14) 4 Al Al2 0.0 0.5 0.0 1.0 Uiso 0.0142(21) 2 P p 0.2463(4) 0.3085(4) 0.96519(30) 1.0 Uiso 0.0166(13) 4 O O1 0.1062(4) 0.3904(7) 0.9128(5) 1.0 Uiso 0.0055(8) 4 O O2 0.3026(6) 0.2847(7) 0.8460(5) 1.0 Uiso 0.0055(8) 4 O O3 0.3467(5) 0.5831(6) 0.5809(5) 1.0 Uiso 0.0055(8) 4 O OC1 0.2636(6) 0.2510(8) 0.5688(6) 1.0 Uiso 0.0055(8) 4 O OC2 -0.0524(5) 0.2742(7) 1.0492(7) 1.0 Uiso 0.0055(8) 4 O OH1 0.1376(8) 0.5032(8) 0.6667(7) 1.0 Uiso 0.0055(8) 4 O OW1 0.3892(7) 0.6237(8) 0.8486(7) 1.0 Uiso 0.0055(8) 4 O OH2 0.5 0.3526(12) 0.75 1.0 Uiso 0.0055(8) 2 C C1 0.2357(8) 0.1026(5) 0.0378(5) 1.0 Uiso 0.0097(27) 4 C C2 0.1590(9) 0.0173(6) 0.4277(6) 1.0 Uiso 0.0097(27) 4 C C3 0.1581(6) 0.1913(6) 0.4868(9) 1.0 Uiso 0.0097(27) 4 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C6 Al3 O15 P2' _chemical_formula_weight 454.94 _cell_formula_units_Z 2 # 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 Al1 Al2 3.373(5) . 2_555 N Al1 p 3.142(5) . 1_555 N Al1 p 3.146(5) . -2_564 N Al1 O2 1.872(6) . 1_555 N Al1 O3 1.888(6) . 1_555 N Al1 OC1 1.966(6) . 1_555 N Al1 OH1 1.905(7) . 1_555 N Al1 OW1 2.058(7) . 1_555 N Al1 OH2 1.905(6) . 1_555 N Al2 Al1 3.373(5) . 2_555 N Al2 Al1 3.373(5) . -2_564 N Al2 p 3.129(4) . 1_554 N Al2 p 3.129(4) . -1_566 N Al2 O1 1.870(5) . 1_554 N Al2 O1 1.870(5) . -1_566 N Al2 OC2 1.983(5) . 1_554 N Al2 OC2 1.983(5) . -1_566 N Al2 OH1 1.837(7) . 2_555 N Al2 OH1 1.837(7) . -2_564 N p Al1 3.142(5) . 1_555 N p Al1 3.146(5) . -2_565 N p Al2 3.129(4) . 1_556 N p O1 1.5335(33) . 1_555 N p O2 1.5485(32) . 1_555 N p O3 1.5567(32) . -2_565 N p C1 1.8102(31) . 1_556 N p C2 2.7157(35) . -2_555 N O1 Al2 1.870(5) . 1_556 N O1 p 1.5335(33) . 1_555 N O2 Al1 1.872(6) . 1_555 N O2 p 1.5485(32) . 1_555 N O3 Al1 1.888(6) . 1_555 N O3 p 1.5567(32) . -2_564 N OC1 Al1 1.966(6) . 1_555 N OC1 OC2 2.153(4) . 2_556 N OC1 C3 1.240(4) . 1_555 N OC2 Al2 1.983(5) . 1_556 N OC2 OC1 2.153(4) . 2_556 N OC2 C3 1.2361(34) . 2_556 N OH1 Al1 1.905(7) . 1_555 N OH1 Al2 1.837(7) . 2_555 N OW1 Al1 2.058(7) . 1_555 N OH2 Al1 1.905(6) . 1_555 N OH2 Al1 1.905(6) . 2_656 N C1 p 1.8102(31) . 1_554 N C1 C2 1.490(4) . -2_554 N C2 p 2.7157(35) . -2_554 N C2 C1 1.490(4) . -2_555 N C2 C3 1.5044(35) . 1_555 N C3 OC1 1.240(4) . 1_555 N C3 OC2 1.2361(34) . 2_556 N C3 C2 1.5044(35) . 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 O2 Al1 O3 176.0(4) 1_555 . 1_555 N O2 Al1 OC1 92.07(34) 1_555 . 1_555 N O2 Al1 OH1 90.89(32) 1_555 . 1_555 N O2 Al1 OW1 91.79(31) 1_555 . 1_555 N O2 Al1 OH2 88.89(33) 1_555 . 1_555 N O3 Al1 OC1 91.19(33) 1_555 . 1_555 N O3 Al1 OH1 91.38(33) 1_555 . 1_555 N O3 Al1 OW1 84.84(32) 1_555 . 1_555 N O3 Al1 OH2 88.91(30) 1_555 . 1_555 N OC1 Al1 OH1 91.25(32) 1_555 . 1_555 N OC1 Al1 OW1 175.1(4) 1_555 . 1_555 N OC1 Al1 OH2 87.69(34) 1_555 . 1_555 N OH1 Al1 OW1 91.6(4) 1_555 . 1_555 N OH1 Al1 OH2 178.9(5) 1_555 . 1_555 N OW1 Al1 OH2 89.4(4) 1_555 . 1_555 N O1 Al2 O1 180.0 1_554 . -1_566 N O1 Al2 OC2 88.36(27) 1_554 . 1_554 N O1 Al2 OC2 91.64(27) 1_554 . -1_566 N O1 Al2 OH1 88.06(25) 1_554 . 2_555 N O1 Al2 OH1 91.94(25) 1_554 . -2_565 N O1 Al2 OC2 91.64(27) -1_566 . 1_554 N O1 Al2 OC2 88.36(27) -1_566 . -1_566 N O1 Al2 OH1 91.94(25) -1_566 . 2_555 N O1 Al2 OH1 88.06(25) -1_566 . -2_565 N OC2 Al2 OC2 180.0 1_554 . -1_566 N OC2 Al2 OH1 93.00(24) 1_554 . 2_555 N OC2 Al2 OH1 87.00(24) 1_554 . -2_565 N OC2 Al2 OH1 87.00(24) -1_566 . 2_555 N OC2 Al2 OH1 93.00(24) -1_566 . -2_565 N OH1 Al2 OH1 180.0 2_555 . -2_565 N O1 p O2 110.70(28) 1_555 . 1_555 N O1 p O3 111.23(26) 1_555 . -2_566 N O1 p C1 109.71(25) 1_555 . 1_556 N O2 p O3 109.48(28) 1_555 . -2_566 N O2 p C1 108.34(24) 1_555 . 1_556 N O3 p C1 107.28(26) -2_566 . 1_556 N Al2 O1 p 133.43(34) 1_556 . 1_555 N Al1 O2 p 133.2(4) 1_555 . 1_555 N Al1 O3 p 131.7(4) 1_555 . -2_565 N Al1 OC1 C3 138.8(5) 1_555 . 1_555 N Al2 OC2 C3 134.4(4) 1_556 . 2_556 N Al1 OH1 Al2 128.7(4) 1_555 . 2_555 N Al1 OH2 Al1 142.7(7) 1_555 . 2_656 N p C1 C2 110.39(29) 1_554 . -2_555 N C1 C2 C3 110.3(4) -2_556 . 1_555 N OC1 C3 OC2 120.8(4) 1_555 . 2_556 N OC1 C3 C2 119.8(4) 1_555 . 1_555 N OC2 C3 C2 119.4(4) 2_556 . 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 ? _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # 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_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 P 4.0 0.026 0.034 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080 68.1645 1.11490 International_Tables_Vol_C Al 6.0 0.014 0.018 6.42020 3.03870 1.90020 0.74260 1.59360 31.5472 1.96460 85.0886 1.11510 International_Tables_Vol_C O 30.0 -0.001 0.002 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C C 12.0 -0.001 0.001 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 1.0 _diffrn_radiation_wavelength 0.429697 _diffrn_radiation_type ? _pd_proc_ls_prof_R_factor 0.0549 _pd_proc_ls_prof_wR_factor 0.0702 _pd_proc_ls_prof_wR_expected 0.0739 _refine_ls_R_Fsqd_factor 0.07413 _pd_proc_ls_background_function ; GSAS Background function number 7 with 1 terms. Linear interpolation 1: -7.78418 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 1 Linear absorption correction Term = 0.0000 Correction is not refined. ; _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_pref_orient_corr ; March-Dollase AXIS 1 Ratio= 0.99261 h= 0.000 k= 0.000 l= 1.000 Prefered orientation correction range: Min= 0.98893, Max= 1.02250 ; _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) = 0.000 #2(GV) = 0.000 #3(GW) = 0.010 #4(GP) = 0.000 #5(LX) = 0.817 #6(LY) = 18.760 #7(S/L) = 0.0025 #8(H/L) = 0.0031 #9(trns) = 0.00 #10(shft)= 0.0000 #11(stec)= 4.22 #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 0.0050 times the peak Aniso. broadening axis 1.0 1.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00500 _pd_proc_info_datetime 2005-07-12T17:45:20 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 1.002 _pd_meas_2theta_range_max 38.022 _pd_meas_2theta_range_inc 0.003 _pd_proc_2theta_range_min 0.997817 _pd_proc_2theta_range_max 38.01782 _pd_proc_2theta_range_inc 0.003 _reflns_number_total 690 _reflns_limit_h_min 0 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min -9 _reflns_limit_l_max 9 _reflns_d_resolution_high 1.074 _reflns_d_resolution_low 6.177 #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#