# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Wharmby, Michael' Michael T. 'Miller, Stuart' ; School of Chemistry, University of St Andrews, Purdie Building, North Haugh, St Andrews, Fife, KY16 9ST, UK ; Miller, 'Margiolaki, Irene' R. ? 'Wright, P.' Groves, John _publ_contact_author_name 'Wright, P.' _publ_contact_author_email PAW2@ST-AND.AC.UK _publ_section_title ; Yttrium Bisphosphonate STA-13: A Racemic Phosphonate Metal Organic Framework with Permanent Microporosity ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ; ? ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_data_validation_number ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_name_full ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_volume ? _journal_year ? _publ_contact_author_address ; School of Chemistry, University of St Andrews, Purdie Building, North Haugh, St Andrews, KY16 9ST, UK ; _publ_contact_author_fax '+44 (0)1334 463808' _publ_contact_author_phone '+44 (0)1334 463791' _publ_contact_letter ; ? ; _publ_requested_category ? # Acta C: one of CI/CM/CO/FI/FM/FO _publ_requested_coeditor_name ? _publ_requested_journal ? # Attachment '- Structure-1.cif' data_Y2(LH2)3.5H2O-AP_publ _database_code_depnum_ccdc_archive 'CCDC 771870' #TrackingRef '- Structure-1.cif' _pd_block_id 2010-03-08T18:39|Y2(LH2)3.5H2O-AP||Stoe_STADIP _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2010-03-08T18:39 _audit_author_name 'Michael T. Wharmby' _audit_update_record ; 2010-03-08T18:39 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 ? _pd_char_colour white # 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 95 _refine_ls_goodness_of_fit_all 1.34 _refine_ls_number_restraints 77 _refine_ls_matrix_type full _refine_diff_density_max 0.675 _refine_diff_density_min -0.677 #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C9 N3 O9 P3 Y, 2(O)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall 'P 2bc 2' _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _cell_measurement_temperature 298 _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 'Y2(LH2)3.5H2O - As prepared' _cell_length_a 8.67363(29) _cell_length_b 9.78127(29) _cell_length_c 22.7964(9) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 1934.02(13) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 2 21 21' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 +x,-y,-z 3 -x,+y+1/2,-z+1/2 4 -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 Y Y1 0.0400(5) 0.1409(5) 0.25576(20) 1.0 Uiso 0.0113(5) 4 P P1 0.0186(16) 0.3898(15) 0.3702(4) 1.0 Uiso 0.0113(5) 4 P P4 0.6953(13) 0.3601(13) 0.2204(5) 1.0 Uiso 0.0113(5) 4 P P11 -0.2185(14) -0.0990(14) 0.3337(5) 1.0 Uiso 0.0113(5) 4 O O1 0.0747(27) 0.2722(20) 0.3386(9) 1.0 Uiso 0.0113(5) 4 O O2 0.0124(28) 0.5100(19) 0.3275(8) 1.0 Uiso 0.0113(5) 4 O O3 -0.1377(20) 0.3813(28) 0.3983(9) 1.0 Uiso 0.0113(5) 4 O O4 0.8282(21) 0.2620(19) 0.2253(10) 1.0 Uiso 0.0113(5) 4 O O5 0.7523(22) 0.5021(15) 0.2235(10) 1.0 Uiso 0.0113(5) 4 O O6 0.6160(21) 0.3314(24) 0.1611(7) 1.0 Uiso 0.0113(5) 4 O O11 -0.1169(22) 0.0146(21) 0.3166(10) 1.0 Uiso 0.0113(5) 4 O O12 -0.2173(20) -0.2072(19) 0.2863(8) 1.0 Uiso 0.0113(5) 4 O O13 -0.3784(19) -0.0519(21) 0.3481(9) 1.0 Uiso 0.0113(5) 4 N N1 0.3278(26) 0.4263(27) 0.4110(12) 1.0 Uiso 0.0113(5) 4 N N4 0.6015(23) 0.3642(29) 0.3464(10) 1.0 Uiso 0.0113(5) 4 N N11A -0.0849(35) -0.0889(25) 0.4500(10) 0.5 Uiso 0.0113(5) 4 C C1 0.1643(22) 0.4381(27) 0.4301(8) 1.0 Uiso 0.0113(5) 4 C C2 0.3746(32) 0.5083(25) 0.3585(15) 1.0 Uiso 0.0113(5) 4 C C3 0.545(4) 0.5132(21) 0.3569(11) 1.0 Uiso 0.0113(5) 4 C C5 0.549(4) 0.2744(26) 0.3935(10) 1.0 Uiso 0.0113(5) 4 C C6 0.3794(34) 0.2779(21) 0.3999(16) 1.0 Uiso 0.0113(5) 4 C C4 0.5562(25) 0.3244(26) 0.2833(7) 1.0 Uiso 0.0113(5) 4 C C11 -0.1433(32) -0.1843(19) 0.4031(7) 1.0 Uiso 0.0113(5) 4 O O103 0.566(5) 0.383(5) 0.0326(16) 0.66667 Uiso 0.06 4 O O104 0.736(10) 0.354(11) 0.058(4) 0.33333 Uiso 0.06 4 O O101 0.239(5) 0.0 0.0 1.0 Uiso 0.06 2 O O102 0.542(6) 0.0 0.0 1.0 Uiso 0.06 2 C C12 -0.117(4) -0.1463(9) 0.5095(8) 1.0 Uiso 0.0113(5) 4 C C14 -0.074(5) 0.0483(23) 0.4424(8) 0.5 Uiso 0.0113(5) 4 C C13 -0.137(5) 0.0533(21) 0.4420(8) 0.5 Uiso 0.0113(5) 4 N N11B -0.146(4) -0.0876(25) 0.4503(10) 0.5 Uiso 0.0113(5) 4 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C9 N3 O11 P3 Y' _chemical_formula_weight 507.94 _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 Y1 O1 2.304(16) . 1_555 N Y1 O2 2.334(14) . 3_545 N Y1 O4 2.293(15) . 1_455 N Y1 O5 2.305(14) . 3_645 N Y1 O11 2.303(15) . 1_555 N Y1 O12 2.343(8) . 3_555 N P1 O1 1.442(19) . 1_555 N P1 O3 1.501(19) . 1_555 N P1 O2 1.528(19) . 1_555 N P1 C1 1.920(16) . 1_555 N P4 O4 1.504(18) . 1_555 N P4 O5 1.475(11) . 1_555 N P4 O6 1.543(14) . 1_555 N P4 C4 1.907(14) . 1_555 N P11 O11 1.471(18) . 1_555 N P11 O12 1.513(17) . 1_555 N P11 O13 1.498(18) . 1_555 N P11 C11 1.903(20) . 1_555 N O1 Y1 2.304(16) . 1_555 N O1 P1 1.442(19) . 1_555 N O3 P1 1.501(19) . 1_555 N O2 Y1 2.334(14) . 3_555 N O2 P1 1.528(19) . 1_555 N O4 Y1 2.293(15) . 1_655 N O4 P4 1.504(18) . 1_555 N O5 Y1 2.305(14) . 3_655 N O5 P4 1.475(11) . 1_555 N O6 P4 1.543(14) . 1_555 N O11 Y1 2.303(15) . 1_555 N O11 P11 1.471(18) . 1_555 N O12 Y1 2.343(8) . 3_545 N O12 P11 1.513(17) . 1_555 N O13 P11 1.498(18) . 1_555 N N1 C1 1.488(22) . 1_555 N N1 C2 1.497(24) . 1_555 N N1 C6 1.540(25) . 1_555 N N4 C3 1.558(25) . 1_555 N N4 C5 1.459(22) . 1_555 N N4 C4 1.540(26) . 1_555 N N11A C11 1.507(24) . 1_555 N N11A C12 1.495(27) . 1_555 N N11A C14 1.356(28) . 1_555 N N11A C13 1.472(25) . 1_555 N N11A N11B 0.533(21) . 1_555 N C1 P1 1.920(16) . 1_555 N C1 N1 1.488(22) . 1_555 N C2 N1 1.497(24) . 1_555 N C2 C3 1.476(34) . 1_555 N C3 N4 1.558(25) . 1_555 N C3 C2 1.476(34) . 1_555 N C5 N4 1.459(22) . 1_555 N C5 C6 1.480(32) . 1_555 N C6 N1 1.540(25) . 1_555 N C6 C5 1.480(32) . 1_555 N C4 P4 1.907(14) . 1_555 N C4 N4 1.540(26) . 1_555 N C11 P11 1.903(20) . 1_555 N C11 N11A 1.507(24) . 1_555 N C11 N11B 1.433(21) . 1_555 N O103 O104 1.61(8) . 1_555 N O104 O103 1.61(8) . 1_555 N C12 N11A 1.495(27) . 1_555 N C12 C14 1.504(26) . 2_556 N C12 C13 1.442(22) . 2_556 N C12 N11B 1.489(27) . 1_555 N C14 N11A 1.356(28) . 1_555 N C14 C12 1.504(26) . 2_556 N C14 C13 0.545(21) . 1_555 N C14 N11B 1.480(26) . 1_555 N C13 N11A 1.472(25) . 1_555 N C13 C12 1.442(22) . 2_556 N C13 C14 0.545(21) . 1_555 N C13 N11B 1.393(28) . 1_555 N N11B N11A 0.533(21) . 1_555 N N11B C11 1.433(21) . 1_555 N N11B C12 1.489(27) . 1_555 N N11B C14 1.480(26) . 1_555 N N11B C13 1.393(28) . 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 Y1 O2 176.3(9) 1_555 . 3_545 N O1 Y1 O4 93.7(8) 1_555 . 1_455 N O1 Y1 O5 93.3(7) 1_555 . 3_645 N O1 Y1 O11 83.2(8) 1_555 . 1_555 N O1 Y1 O12 84.1(7) 1_555 . 3_555 N O2 Y1 O4 83.2(7) 3_545 . 1_455 N O2 Y1 O5 89.8(8) 3_545 . 3_645 N O2 Y1 O11 94.6(8) 3_545 . 1_555 N O2 Y1 O12 98.2(8) 3_545 . 3_555 N O4 Y1 O5 172.9(9) 1_455 . 3_645 N O4 Y1 O11 89.2(8) 1_455 . 1_555 N O4 Y1 O12 94.3(8) 1_455 . 3_555 N O5 Y1 O11 91.3(8) 3_645 . 1_555 N O5 Y1 O12 86.8(7) 3_645 . 3_555 N O11 Y1 O12 167.0(8) 1_555 . 3_555 N O1 P1 O3 118.2(15) 1_555 . 1_555 N O1 P1 O2 107.9(11) 1_555 . 1_555 N O1 P1 C1 109.2(13) 1_555 . 1_555 N O3 P1 O2 106.4(14) 1_555 . 1_555 N O3 P1 C1 107.8(10) 1_555 . 1_555 N O2 P1 C1 106.7(13) 1_555 . 1_555 N O4 P4 O5 109.9(13) 1_555 . 1_555 N O4 P4 O6 106.9(12) 1_555 . 1_555 N O4 P4 C4 108.2(11) 1_555 . 1_555 N O5 P4 O6 111.2(13) 1_555 . 1_555 N O5 P4 C4 110.4(12) 1_555 . 1_555 N O6 P4 C4 110.1(10) 1_555 . 1_555 N O11 P11 O12 109.6(12) 1_555 . 1_555 N O11 P11 O13 112.4(14) 1_555 . 1_555 N O11 P11 C11 110.2(12) 1_555 . 1_555 N O12 P11 O13 112.2(14) 1_555 . 1_555 N O12 P11 C11 106.5(11) 1_555 . 1_555 N O13 P11 C11 105.7(12) 1_555 . 1_555 N Y1 O1 P1 144.1(15) 1_555 . 1_555 N Y1 O2 P1 161.4(14) 3_555 . 1_555 N Y1 O4 P4 165.0(15) 1_655 . 1_555 N Y1 O5 P4 145.7(14) 3_655 . 1_555 N Y1 O11 P11 156.8(16) 1_555 . 1_555 N Y1 O12 P11 137.8(12) 3_545 . 1_555 N C1 N1 C2 116.8(19) 1_555 . 1_555 N C1 N1 C6 113.5(18) 1_555 . 1_555 N C2 N1 C6 107.2(18) 1_555 . 1_555 N C3 N4 C5 110.6(14) 1_555 . 1_555 N C3 N4 C4 107.4(17) 1_555 . 1_555 N C5 N4 C4 117.1(21) 1_555 . 1_555 N C11 N11A C12 110.3(21) 1_555 . 1_555 N C11 N11A C14 123.1(24) 1_555 . 1_555 N C11 N11A C13 113.2(20) 1_555 . 1_555 N C11 N11A N11B 71.7(33) 1_555 . 1_555 N C12 N11A C14 120.0(17) 1_555 . 1_555 N C12 N11A C13 114.2(15) 1_555 . 1_555 N C12 N11A N11B 79(5) 1_555 . 1_555 N C14 N11A C13 21.7(9) 1_555 . 1_555 N C14 N11A N11B 93(4) 1_555 . 1_555 N C13 N11A N11B 71(4) 1_555 . 1_555 N P1 C1 N1 113.6(15) 1_555 . 1_555 N N1 C2 C3 107.9(20) 1_555 . 1_555 N N4 C3 C2 106.9(18) 1_555 . 1_555 N N4 C5 C6 111.6(17) 1_555 . 1_555 N N1 C6 C5 109.1(19) 1_555 . 1_555 N P4 C4 N4 119.6(14) 1_555 . 1_555 N P11 C11 N11A 115.7(13) 1_555 . 1_555 N P11 C11 N11B 109.2(15) 1_555 . 1_555 N N11A C11 N11B 20.7(8) 1_555 . 1_555 N N11A C12 C14 112.0(18) 1_555 . 2_556 N N11A C12 C13 118.7(12) 1_555 . 2_556 N N11A C12 N11B 20.6(8) 1_555 . 1_555 N C14 C12 C13 21.2(9) 2_556 . 2_556 N C14 C12 N11B 117.2(12) 2_556 . 1_555 N C13 C12 N11B 115.6(16) 2_556 . 1_555 N N11A C14 C12 121.4(19) 1_555 . 2_556 N N11A C14 C13 91.2(28) 1_555 . 1_555 N N11A C14 N11B 21.1(9) 1_555 . 1_555 N C12 C14 C13 73(4) 2_556 . 1_555 N C12 C14 N11B 112.3(20) 2_556 . 1_555 N C13 C14 N11B 70.1(26) 1_555 . 1_555 N N11A C13 C12 117.8(16) 1_555 . 2_556 N N11A C13 C14 67.1(26) 1_555 . 1_555 N N11A C13 N11B 21.2(9) 1_555 . 1_555 N C12 C13 C14 86(4) 2_556 . 1_555 N C12 C13 N11B 121.9(19) 2_556 . 1_555 N C14 C13 N11B 88.3(28) 1_555 . 1_555 N N11A N11B C11 88(4) 1_555 . 1_555 N N11A N11B C12 80(5) 1_555 . 1_555 N N11A N11B C14 66(4) 1_555 . 1_555 N N11A N11B C13 88(4) 1_555 . 1_555 N C11 N11B C12 115.0(20) 1_555 . 1_555 N C11 N11B C14 119.7(20) 1_555 . 1_555 N C11 N11B C13 123.4(24) 1_555 . 1_555 N C12 N11B C14 112.6(16) 1_555 . 1_555 N C12 N11B C13 119.6(16) 1_555 . 1_555 N C14 N11B C13 21.6(9) 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 298 _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type 'STOE STADI P' _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 Y 4.0 0.000 0.000 17.7760 1.40290 10.2946 12.8006 5.72629 0.12560 3.26588 104.354 1.91213 International_Tables_Vol_C P 12.0 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 44.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C N 12.0 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 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 _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 0.55 _diffrn_radiation_wavelength 1.54056 _diffrn_radiation_type 'Cu K\a~1~' _pd_proc_ls_prof_R_factor 0.0303 _pd_proc_ls_prof_wR_factor 0.0388 _pd_proc_ls_prof_wR_expected 0.0294 _refine_ls_R_Fsqd_factor 0.09876 _pd_proc_ls_background_function ; GSAS Background function number 2 with 36 terms. Cosine Fourier series 1: -13193.3 2: 12089.2 3: 19495.2 4: -32932.6 5: 19351.8 6: 2317.04 7: -9766.22 8: 1113.48 9: 6865.48 10: -3746.99 11: -7041.01 12: 14710.9 13: -14564.1 14: 9929.44 15: -5268.92 16: 3777.55 17: -4646.78 18: 5845.04 19: -4341.50 20: 99.1158 21: 3532.25 22: -3477.81 23: 584.995 24: 924.233 25: 645.004 26: -2665.08 27: 1743.76 28: 1383.99 29: -2839.47 30: 317.443 31: 4147.88 32: -6881.65 33: 6273.50 34: -3729.66 35: 1407.97 36: -278.295 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 No correction is applied. ; _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_correction_T_max 1.00000 # Extinction correction _gsas_exptl_extinct_corr_T_min 1.00000 _gsas_exptl_extinct_corr_T_max 1.00000 _pd_proc_ls_profile_function ; CW Profile function number 3 with 19 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. #1(GU) = 231.403 #2(GV) = -31.987 #3(GW) = 7.551 #4(GP) = 9.299 #5(LX) = 1.865 #6(LY) = 4.529 #7(S/L) = 0.0281 #8(H/L) = 0.0221 #9(trns) = 27.73 #10(shft)= -5.4000 #11(stec)= -1.07 #12(ptec)= 0.11 #13(sfec)= 0.00 #14(L11) = -0.032 #15(L22) = -0.107 #16(L33) = -0.003 #17(L12) = 0.123 #18(L13) = -0.009 #19(L23) = -0.003 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_peak_cutoff 0.00500 _pd_proc_info_datetime 2010-03-08T18:39:30 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 5.0 _pd_meas_2theta_range_max 89.98 _pd_meas_2theta_range_inc 0.02 _pd_proc_2theta_range_min 5.0711 _pd_proc_2theta_range_max 90.05109 _pd_proc_2theta_range_inc 0.02 loop_ _pd_meas_counts_total _pd_proc_ls_weight _pd_proc_intensity_bkg_calc _pd_calc_intensity_total 1199.0 0.000834 1243.62268 1243.62305 1172.0 0.000853 1243.51465 1243.51392 1158.0 0.000864 1243.40430 1243.40430 1196.0 0.000836 1243.28040 1243.28088 1200.0 0.000833 1243.15283 1243.15430 1144.0 0.000874 1243.01917 1243.01855 1174.0 0.000852 1242.87671 1242.87646 1125.0 0.000889 1242.72559 1242.72595 1202.0 0.000832 1242.56873 1242.56946 1223.0 0.000818 1242.40430 1242.40454 1217.0 0.000822 1242.23413 1242.23352 1220.0 0.000820 1242.05420 1242.05457 1170.0 0.000855 1241.86584 1241.86584 1222.0 0.000818 1241.67261 1241.67249 1222.0 0.000818 1241.47168 1241.47217 1241.0 0.000806 1241.26404 1241.26343 1257.0 0.000796 1241.04358 1241.04492 1210.0 0.000826 1240.82178 1240.82129 1230.0 0.000813 1240.59265 1240.59155 1217.0 0.000822 1240.35266 1240.35291 1205.0 0.000830 1240.10632 1240.10608 1209.0 0.000827 1239.85437 1239.85376 1205.0 0.000830 1239.59045 1239.59192 1250.0 0.000800 1239.32495 1239.32556 1191.0 0.000840 1239.04980 1239.04956 1223.0 0.000818 1238.76562 1238.76501 1251.0 0.000799 1238.47192 1238.47241 1292.0 0.000774 1238.17468 1238.17468 1295.0 0.000772 1237.87073 1237.87097 1179.0 0.000848 1237.55603 1237.55701 1206.0 0.000829 1237.23865 1237.23682 1228.0 0.000814 1236.90906 1236.90833 1284.0 0.000779 1236.56909 1236.57019 1277.0 0.000783 1236.22449 1236.22437 1248.0 0.000801 1235.87561 1235.87512 1216.0 0.000822 1235.51343 1235.51453 1209.0 0.000827 1235.15112 1235.15112 1277.0 0.000783 1234.77771 1234.77710 1249.0 0.000801 1234.39636 1234.39551 1260.0 0.000794 1234.00928 1234.00806 1223.0 0.000818 1233.61316 1233.61365 1276.0 0.000784 1233.20801 1233.20874 1222.0 0.000818 1232.79724 1232.79651 1262.0 0.000792 1232.37549 1232.37708 1216.0 0.000822 1231.95251 1231.95251 1255.0 0.000797 1231.51758 1231.51892 1230.0 0.000813 1231.07715 1231.07751 1228.0 0.000814 1230.62854 1230.62781 1212.0 0.000825 1230.17554 1230.17542 1223.0 0.000818 1229.71216 1229.71240 1199.0 0.000834 1229.23975 1229.23938 1205.0 0.000830 1228.75977 1228.75977 1240.0 0.000806 1228.27527 1228.27563 1260.0 0.000794 1227.78674 1227.78723 1230.0 0.000813 1227.28503 1227.28564 1263.0 0.000792 1226.77795 1226.77820 1226.0 0.000816 1226.26367 1226.26489 1222.0 0.000818 1225.74219 1225.74231 1252.0 0.000799 1225.21240 1225.21313 1251.0 0.000799 1224.67737 1224.67590 1275.0 0.000784 1224.13293 1224.13269 1237.0 0.000808 1223.58301 1223.58215 1259.0 0.000794 1223.02417 1223.02515 1339.0 0.000747 1222.46204 1222.46204 1242.0 0.000805 1221.88794 1221.88745 1233.0 0.000811 1221.31067 1221.31152 1282.0 0.000780 1220.72266 1220.72302 1257.0 0.000796 1220.13074 1220.13049 1262.0 0.000792 1219.53247 1219.53247 1226.0 0.000816 1218.92322 1218.92163 1196.0 0.000836 1218.31006 1218.31091 1218.0 0.000821 1217.69006 1217.68994 1253.0 0.000798 1217.06433 1217.06287 1216.0 0.000822 1216.43115 1216.43140 1204.0 0.000831 1215.78796 1215.78918 1270.0 0.000787 1215.14136 1215.14038 1284.0 0.000779 1214.48352 1214.48279 1265.0 0.000791 1213.82349 1213.82300 1224.0 0.000817 1213.15894 1213.15906 1226.0 0.000816 1212.48096 1212.48145 1198.0 0.000835 1211.80115 1211.80151 1212.0 0.000825 1211.11523 1211.11438 1226.0 0.000816 1210.41931 1210.41846 1198.0 0.000835 1209.71973 1209.71985 1238.0 0.000808 1209.01282 1209.01294 1261.0 0.000793 1208.29907 1208.29834 1237.0 0.000808 1207.57935 1207.57971 1214.0 0.000824 1206.85413 1206.85315 1230.0 0.000813 1206.12195 1206.12195 1236.0 0.000809 1205.38354 1205.38318 1271.0 0.000787 1204.64282 1204.64185 1237.0 0.000808 1203.88696 1203.88745 1237.0 0.000808 1203.13013 1203.13037 1279.0 0.000782 1202.36877 1202.36865 1262.0 0.000792 1201.59973 1201.59900 1249.0 0.000801 1200.82800 1200.82837 1268.0 0.000789 1200.04700 1200.04553 1336.0 0.000749 1199.25720 1199.25793 1267.0 0.000789 1198.47070 1235.96252 1376.0 0.000727 1197.67212 1238.20776 1350.0 0.000741 1196.86987 1240.92456 1370.0 0.000730 1196.05591 1244.31555 1341.0 0.000746 1195.24255 1248.84705 1382.0 0.000724 1194.42639 1255.55481 1449.0 0.000690 1193.59949 1266.49731 1382.0 0.000724 1192.76929 1285.12219 1441.0 0.000694 1191.93347 1316.02393 1515.0 0.000660 1191.09119 1363.77820 1575.0 0.000635 1190.24658 1431.15625 1696.0 0.000590 1189.39270 1518.00793 1756.0 0.000569 1188.53369 1621.97595 1833.0 0.000546 1187.67224 1740.19043 1905.0 0.000525 1186.80835 1870.56750 2051.0 0.000488 1185.93542 2012.25391 2086.0 0.000479 1185.05786 2165.46899 2307.0 0.000433 1184.17798 2331.17871 2395.0 0.000418 1183.29004 2510.83643 2608.0 0.000383 1182.39807 2706.32861 2687.0 0.000372 1181.50452 2919.99219 2926.0 0.0003418 1180.60144 3154.71924 3216.0 0.0003109 1179.69824 3414.14404 3516.0 0.0002844 1178.78845 3702.88330 3813.0 0.0002623 1177.87634 4026.93115 4186.0 0.0002389 1176.96289 4394.26953 4664.0 0.0002144 1176.04077 4815.89990 5185.0 0.0001929 1175.11304 5307.75439 5891.0 0.0001698 1174.17883 5894.41895 6629.0 0.0001509 1173.24622 6616.02393 7640.0 0.0001309 1172.31006 7537.68604 8916.0 0.0001122 1171.36731 8751.00879 10476.0 0.0000955 1170.42285 10337.59277 12450.0 0.0000803 1169.47400 12258.70508 14360.0 0.0000696 1168.52014 14195.39551 15598.0 0.0000641 1167.56213 15483.56641 15090.0 0.0000663 1166.59924 15326.73828 12899.0 0.0000775 1165.63586 13348.91797 9711.0 0.0001030 1164.67053 10146.30371 6349.0 0.0001575 1163.69800 6881.64941 4061.0 0.0002462 1162.72351 4372.22412 2720.0 0.000368 1161.74585 2822.02026 2004.0 0.000499 1160.77209 2024.13281 1644.0 0.000608 1159.78528 1663.61182 1555.0 0.000643 1158.79773 1505.12329 1366.0 0.000732 1157.80859 1426.19775 1364.0 0.000733 1156.81238 1377.56018 1390.0 0.000719 1155.82031 1342.41028 1309.0 0.000764 1154.82141 1315.02405 1274.0 0.000785 1153.82104 1292.97144 1197.0 0.000835 1152.82239 1274.86243 1156.0 0.000865 1151.81628 1259.75513 1180.0 0.000847 1150.80798 1246.98328 1193.0 0.000838 1149.79944 1236.05701 1124.0 0.000890 1148.78308 1226.59924 1195.0 0.000837 1147.77112 1218.33972 1210.0 0.000826 1146.75854 1211.05981 1162.0 0.000861 1145.73755 1204.58020 1161.0 0.000861 1144.72034 1198.77856 1113.0 0.000898 1143.69739 1193.53735 1191.0 0.000840 1142.67261 1188.77539 1125.0 0.000889 1141.64795 1184.42200 1142.0 0.000876 1140.61829 1140.61938 1145.0 0.000873 1139.59119 1139.59070 1150.0 0.000870 1138.56384 1138.56287 1132.0 0.000883 1137.53345 1137.53394 1143.0 0.000875 1136.50134 1136.50073 1162.0 0.000861 1135.46802 1135.46814 1120.0 0.000893 1134.43188 1134.43213 1133.0 0.000883 1133.39465 1133.39453 1132.0 0.000883 1132.35742 1132.35681 1055.0 0.000948 1131.32031 1131.31958 1143.0 0.000875 1130.28479 1130.28418 1137.0 0.000880 1129.24609 1129.24524 1186.0 0.000843 1128.20544 1128.20618 1151.0 0.000869 1127.16711 1127.16638 1163.0 0.000860 1126.12500 1126.12390 1190.0 0.000840 1125.08264 1125.08252 1118.0 0.000894 1124.04126 1124.04150 1128.0 0.000887 1123.00134 1123.00012 1074.0 0.000931 1121.95618 1121.95569 1131.0 0.000884 1120.91785 1120.91699 1094.0 0.000914 1119.87244 1119.87390 1129.0 0.000886 1118.83508 1118.83447 1125.0 0.000889 1117.79541 1117.79602 1087.0 0.000920 1116.75342 1116.75220 1099.0 0.000910 1115.71057 1115.71045 1175.0 0.000851 1114.67017 1114.66956 1111.0 0.000900 1113.63062 1113.63049 1123.0 0.000890 1112.59033 1112.59009 1102.0 0.000907 1111.55701 1111.55652 1105.0 0.000905 1110.51831 1110.51782 1070.0 0.000935 1109.47913 1109.47949 1110.0 0.000901 1108.44348 1108.44287 1062.0 0.000942 1107.40906 1107.40979 1061.0 0.000943 1106.37317 1106.37439 1080.0 0.000926 1105.34241 1105.34192 1100.0 0.000909 1104.31396 1104.31458 1095.0 0.000913 1103.28442 1103.28381 1038.0 0.000963 1102.25586 1102.25659 1099.0 0.000910 1101.23157 1101.23047 1115.0 0.000897 1100.20422 1100.20435 1090.0 0.000917 1099.18176 1099.18188 1067.0 0.000937 1098.15894 1098.15894 1141.0 0.000876 1097.14014 1097.13916 1148.0 0.000871 1096.11987 1096.11975 1106.0 0.000904 1095.10828 1095.10889 1138.0 0.000879 1094.09204 1094.09290 1144.0 0.000874 1093.08325 1093.08362 1217.0 0.000822 1092.07690 1092.07678 1158.0 0.000864 1091.06848 1091.06885 1170.0 0.000855 1090.06482 1090.06482 1224.0 0.000817 1089.06226 1089.35400 1257.0 0.000796 1088.06299 1088.38928 1211.0 0.000826 1087.06458 1087.43396 1226.0 0.000816 1086.07666 1086.51282 1241.0 0.000806 1085.08459 1085.63403 1176.0 0.000850 1084.09485 1084.84863 1183.0 0.000845 1083.11035 1084.21948 1086.0 0.000921 1082.12964 1083.80286 1059.0 0.000944 1081.14954 1083.63232 1115.0 0.000897 1080.17615 1083.71362 1054.0 0.000949 1079.20642 1084.02087 1039.0 0.000962 1078.23889 1084.52209 1029.0 0.000972 1077.27673 1085.20898 1094.0 0.000914 1076.31201 1086.07910 1088.0 0.000919 1075.35449 1087.16394 1095.0 0.000913 1074.40332 1088.49292 1045.0 0.000957 1073.45203 1090.11682 1093.0 0.000915 1072.50562 1092.10669 1041.0 0.000961 1071.56470 1111.36829 1081.0 0.000925 1070.63013 1116.19934 1107.0 0.000903 1069.69348 1122.29736 1087.0 0.000920 1068.76831 1130.41321 1125.0 0.000889 1067.84399 1141.93652 1130.0 0.000885 1066.92224 1159.17249 1136.0 0.000880 1066.00623 1184.95190 1234.0 0.000810 1065.09412 1221.10205 1232.0 0.000812 1064.18506 1266.19165 1199.0 0.000834 1063.28357 1314.71252 1327.0 0.000754 1062.39062 1360.12122 1342.0 0.000745 1061.49927 1401.06970 1337.0 0.000748 1060.60889 1444.43713 1445.0 0.000692 1059.72571 1499.41235 1514.0 0.000661 1058.85034 1571.48975 1579.0 0.000633 1057.97766 1661.94849 1678.0 0.000596 1057.11060 1770.40027 1843.0 0.000543 1056.25073 1897.43457 1971.0 0.000507 1055.39417 2045.99792 2197.0 0.000455 1054.54480 2222.12158 2292.0 0.000436 1053.70203 2436.27295 2617.0 0.000382 1052.86096 2706.03442 3015.0 0.0003317 1052.02710 3058.51782 3447.0 0.0002901 1051.19666 3525.46338 4116.0 0.0002430 1050.37646 4118.46240 4708.0 0.0002124 1049.55920 4780.15039 5224.0 0.0001914 1048.75269 5341.64453 5365.0 0.0001864 1047.94336 5547.38574 5072.0 0.0001972 1047.14819 5188.84668 4165.0 0.0002401 1046.35840 4314.88135 3109.0 0.0003216 1045.57263 3256.26514 2248.0 0.000445 1044.79407 2345.59790 1715.0 0.000583 1044.01892 1730.54504 1414.0 0.000707 1043.25049 1390.48999 1319.0 0.000758 1042.49036 1230.14478 1191.0 0.000840 1041.74377 1160.47766 1123.0 0.000890 1040.99695 1129.86572 1084.0 0.000923 1040.25562 1112.02991 1030.0 0.000971 1039.52234 1099.87903 1060.0 0.000943 1038.79761 1090.66833 1051.0 0.000951 1038.07495 1083.39539 1072.0 0.000933 1037.36768 1077.63342 1032.0 0.000969 1036.66113 1073.19470 1036.0 0.000965 1035.96204 1070.08472 1037.0 0.000964 1035.27466 1068.42273 1065.0 0.000939 1034.59326 1068.32959 1050.0 0.000952 1033.91602 1048.65198 1063.0 0.000941 1033.24561 1053.61377 981.0 0.001019 1032.58667 1059.67981 1030.0 0.000971 1031.93127 1066.77747 1052.0 0.000951 1031.28784 1074.93262 1024.0 0.000977 1030.65076 1084.24988 1066.0 0.000938 1030.01965 1094.94653 1030.0 0.000971 1029.39526 1107.35425 1043.0 0.000959 1028.78308 1121.96790 1108.0 0.000903 1028.17456 1139.55017 1125.0 0.000889 1027.57495 1161.37146 1170.0 0.000855 1026.98462 1189.49988 1142.0 0.000876 1026.39917 1226.88806 1237.0 0.000808 1025.82434 1276.26282 1287.0 0.000777 1025.26135 1336.66711 1308.0 0.000765 1024.70349 1398.39380 1302.0 0.000768 1024.15112 1440.87903 1366.0 0.000732 1023.60919 1439.40234 1343.0 0.000745 1023.07526 1382.24658 1250.0 0.000800 1022.54889 1287.36633 1120.0 0.000893 1022.03253 1189.91467 1031.0 0.000970 1021.52435 1114.81567 1047.0 0.000955 1021.02930 1068.44067 1063.0 0.000941 1020.54065 1044.57178 1021.0 0.000979 1020.05725 1033.70984 1064.0 0.000940 1019.58301 1028.79688 1076.0 0.000929 1019.11926 1026.19312 1014.0 0.000986 1018.66119 1024.45117 1016.0 0.000984 1018.21588 1023.09155 993.0 0.001007 1017.78009 1021.95490 1035.0 0.000966 1017.34930 1020.96472 1005.0 0.000995 1016.93433 1020.09650 1000.0 0.001000 1016.52380 1019.31256 1047.0 0.000955 1016.12274 1018.60223 1045.0 0.000957 1015.72968 1017.94836 973.0 0.001028 1015.34686 1017.34473 1008.0 0.000992 1014.97168 1014.97278 1007.0 0.000993 1014.60718 1014.60669 1016.0 0.000984 1014.25348 1014.25385 1006.0 0.000994 1013.90894 1013.90802 1021.0 0.000979 1013.57159 1014.56415 985.0 0.001015 1013.24701 1014.33069 1013.0 0.000987 1012.92456 1014.11835 1051.0 0.000951 1012.62128 1013.93982 1049.0 0.000953 1012.32043 1013.79431 1045.0 0.000957 1012.03699 1013.70624 951.0 0.001052 1011.75439 1013.70459 987.0 0.001013 1011.49261 1013.90228 1023.0 0.000978 1011.23029 1014.44891 1003.0 0.000997 1010.98389 1015.63696 1026.0 0.000975 1010.74255 1017.77582 997.0 0.001003 1010.51361 1021.15759 1049.0 0.000953 1010.29504 1025.91028 1094.0 0.000914 1010.08405 1032.01526 1047.0 0.000955 1009.88580 1039.40027 1109.0 0.000902 1009.69611 1048.03198 1082.0 0.000924 1009.52173 1058.00586 1045.0 0.000957 1009.34735 1069.54004 1091.0 0.000917 1009.18988 1083.04895 1070.0 0.000935 1009.04120 1099.18054 1112.0 0.000899 1008.90210 1119.01941 1140.0 0.000877 1008.77551 1144.39600 1096.0 0.000912 1008.65491 1178.11011 1219.0 0.000820 1008.54620 1223.28748 1277.0 0.000783 1008.44922 1280.45898 1364.0 0.000733 1008.36163 1342.38672 1374.0 0.000728 1008.28497 1390.61255 1350.0 0.000741 1008.22009 1400.32776 1326.0 0.000754 1008.16101 1356.17798 1302.0 0.000768 1008.11523 1270.33606 1177.0 0.000850 1008.07971 1176.13147 1140.0 0.000877 1008.05457 1100.95630 1022.0 0.000978 1008.04480 1053.89539 1029.0 0.000972 1008.03906 1029.92944 1036.0 0.000965 1008.04529 1019.55914 1036.0 0.000965 1008.06097 1015.38971 1028.0 0.000973 1008.09174 1013.56659 997.0 0.001003 1008.13141 1012.56720 1036.0 0.000965 1008.17670 1011.89349 1037.0 0.000964 1008.23950 1011.41101 1026.0 0.000975 1008.30725 1011.04486 1022.0 0.000978 1008.39337 1010.78259 1038.0 0.000963 1008.48541 1010.58722 1014.0 0.000986 1008.58765 1010.45239 1034.0 0.000967 1008.70062 1010.36603 1017.0 0.000983 1008.82239 1018.96893 1004.0 0.000996 1008.95984 1018.40051 1035.0 0.000966 1009.10474 1019.45917 1052.0 0.000951 1009.26208 1020.67566 1069.0 0.000935 1009.42877 1022.09009 1046.0 0.000956 1009.60583 1023.77277 1005.0 0.000995 1009.79791 1025.87292 1049.0 0.000953 1009.99756 1028.72278 1076.0 0.000929 1010.20459 1033.05811 1070.0 0.000935 1010.42859 1040.27136 1092.0 0.000916 1010.65979 1052.52051 1135.0 0.000881 1010.90320 1072.52100 1175.0 0.000851 1011.16034 1102.81140 1167.0 0.000857 1011.42560 1144.92651 1238.0 0.000808 1011.70203 1199.19910 1364.0 0.000733 1011.98785 1265.39331 1351.0 0.000740 1012.28937 1343.65332 1425.0 0.000702 1012.59772 1435.19604 1500.0 0.000667 1012.91559 1542.84912 1656.0 0.000604 1013.24719 1671.74963 1915.0 0.000522 1013.58746 1830.70691 2061.0 0.000485 1013.94598 2034.30408 2370.0 0.000422 1014.30872 2303.35522 2745.0 0.000364 1014.68073 2657.36230 3220.0 0.0003106 1015.07080 3090.88770 3573.0 0.0002799 1015.46527 3538.66724 3907.0 0.0002560 1015.87433 3860.29175 3903.0 0.0002562 1016.29443 3883.88062 3541.0 0.0002824 1016.72382 3521.34863 2994.0 0.0003340 1017.16199 2885.52490 2275.0 0.000440 1017.61627 2215.86890 1768.0 0.000566 1018.07825 1690.59534 1474.0 0.000678 1018.55463 1361.81775 1310.0 0.000763 1019.03491 1191.75818 1224.0 0.000817 1019.53143 1115.72913 1159.0 0.000863 1020.04315 1083.61951 1113.0 0.000898 1020.55841 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2145.0 0.000466 1178.59216 2223.64673 2311.0 0.000433 1180.38574 2411.09473 2352.0 0.000425 1182.18359 2510.34033 2404.0 0.000416 1183.98926 2458.12793 2160.0 0.000463 1185.80615 2248.51831 1954.0 0.000512 1187.62329 1957.69507 1653.0 0.000605 1189.45154 1681.48535 1454.0 0.000688 1191.28381 1475.05090 1347.0 0.000742 1193.12549 1347.49756 1323.0 0.000756 1194.97400 1280.44055 1276.0 0.000784 1196.83105 1249.26807 1233.0 0.000811 1198.69287 1235.52576 1171.0 0.000854 1200.56494 1229.23926 1287.0 0.000777 1202.44092 1226.02148 1243.0 0.000805 1204.32312 1224.24231 1209.0 0.000827 1206.21106 1223.30115 1226.0 0.000816 1208.10938 1222.94104 1234.0 0.000810 1210.00793 1223.00098 1261.0 0.000793 1211.92029 1223.39685 1196.0 0.000836 1213.83850 1224.05017 1264.0 0.000791 1215.75806 1224.90430 1214.0 0.000824 1217.68945 1225.82178 1213.0 0.000824 1219.62341 1226.98401 1245.0 0.000803 1221.56384 1228.25720 1179.0 0.000848 1223.51282 1229.62720 1233.0 0.000811 1225.46704 1231.07300 1174.0 0.000852 1227.42908 1232.58923 1266.0 0.000790 1229.39148 1234.15613 1221.0 0.000819 1231.36487 1235.77759 1209.0 0.000827 1233.34509 1233.34558 1202.0 0.000832 1235.32983 1235.33008 1289.0 0.000776 1237.32104 1237.32104 1220.0 0.000820 1239.31543 1239.31531 1245.0 0.000803 1241.32031 1241.31995 1249.0 0.000801 1243.32837 1243.32910 1212.0 0.000825 1245.34351 1245.34363 1224.0 0.000817 1247.36597 1247.36487 1245.0 0.000803 1249.39185 1249.39172 1183.0 0.000845 1251.42029 1251.42029 1213.0 0.000824 1253.45972 1253.45911 1233.0 0.000811 1255.49902 1255.49902 1264.0 0.000791 1257.54724 1257.54822 1273.0 0.000786 1259.60132 1259.60156 1294.0 0.000773 1261.66492 1261.66504 1207.0 0.000829 1263.72937 1263.72852 1189.0 0.000841 1265.79810 1265.79797 1306.0 0.000766 1267.87341 1267.87378 1264.0 0.000791 1269.95435 1269.95544 1308.0 0.000765 1272.04150 1272.04187 1254.0 0.000797 1274.13025 1274.13049 1243.0 0.000805 1276.22937 1276.22986 1327.0 0.000754 1278.33105 1278.33069 1269.0 0.000788 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1336.82288 1374.0 0.000728 1339.04590 1339.04590 1331.0 0.000751 1341.27515 1341.27515 1315.0 0.000760 1343.51038 1343.50964 1330.0 0.000752 1345.74219 1345.74280 1305.0 0.000766 1347.98267 1347.98267 1299.0 0.000770 1350.22522 1350.22498 1329.0 0.000752 1352.47058 1352.47021 1328.0 0.000753 1354.72205 1354.72083 1367.0 0.000732 1356.97485 1356.97534 1365.0 0.000733 1359.22766 1360.58777 1314.0 0.000761 1361.49194 1362.96582 1350.0 0.000741 1363.75269 1365.35437 1375.0 0.000727 1366.01770 1367.76709 1315.0 0.000760 1368.29065 1370.20679 1332.0 0.000751 1370.56104 1372.67200 1347.0 0.000742 1372.84253 1375.17712 1354.0 0.000739 1375.11694 1377.71704 1358.0 0.000736 1377.39893 1380.31213 1382.0 0.000724 1379.68713 1385.01196 1361.0 0.000735 1381.97168 1388.01611 1391.0 0.000719 1384.25867 1391.22961 1348.0 0.000742 1386.55920 1394.81580 1417.0 0.000706 1388.85364 1399.06067 1404.0 0.000712 1391.14844 1404.52551 1422.0 0.000703 1393.45251 1412.11682 1376.0 0.000727 1395.75635 1423.48889 1383.0 0.000723 1398.06384 1439.49084 1395.0 0.000717 1400.37256 1462.17346 1501.0 0.000666 1402.68030 1493.30640 1539.0 0.000650 1404.99756 1534.92468 1479.0 0.000676 1407.31042 1589.76501 1550.0 0.000645 1409.62952 1661.64709 1622.0 0.000617 1411.95105 1754.61841 1683.0 0.000594 1414.27405 1869.93713 1696.0 0.000590 1416.59534 2000.95056 1894.0 0.000528 1418.92419 2128.30005 1943.0 0.000515 1421.25269 2220.08911 2024.0 0.000494 1423.58118 2243.37109 1900.0 0.000526 1425.91602 2185.43555 1825.0 0.000548 1428.25220 2063.20874 1826.0 0.000548 1430.59058 1917.11890 1711.0 0.000584 1432.92700 1794.45068 1777.0 0.000563 1435.26404 1712.20850 1728.0 0.000579 1437.60913 1668.72241 1656.0 0.000604 1439.95386 1643.07019 1599.0 0.000625 1442.29724 1619.02808 1614.0 0.000620 1444.64563 1582.30396 1637.0 0.000611 1446.99487 1543.65393 1512.0 0.000661 1449.34131 1512.73718 1463.0 0.000684 1451.69470 1494.03809 1504.0 0.000665 1454.04846 1486.46436 1460.0 0.000685 1456.40283 1486.98474 1525.0 0.000656 1458.75684 1493.99878 1597.0 0.000626 1461.11060 1508.64551 1583.0 0.000632 1463.47095 1534.45239 1647.0 0.000607 1465.82922 1576.29053 1689.0 0.000592 1468.18896 1639.47961 1909.0 0.000524 1470.54834 1729.84900 1925.0 0.000519 1472.91150 1855.30261 2165.0 0.000462 1475.27271 2028.18555 2354.0 0.000425 1477.63904 2266.28442 2738.0 0.000365 1480.00012 2587.48193 3160.0 0.0003165 1482.36389 2992.28223 3597.0 0.0002780 1484.72888 3435.51050 4025.0 0.0002484 1487.09546 3826.27051 4165.0 0.0002401 1489.46631 4045.38135 4114.0 0.0002431 1491.83301 4027.23584 3858.0 0.0002592 1494.19934 3808.64697 3491.0 0.0002865 1496.56873 3479.15405 3119.0 0.0003206 1498.93848 3097.75464 2784.0 0.000359 1501.30603 2694.49756 2374.0 0.000421 1503.67749 2313.83618 2117.0 0.000472 1506.04749 2003.93469 1845.0 0.000542 1508.41602 1787.89026 1714.0 0.000583 1510.78662 1659.40491 1720.0 0.000581 1513.15808 1593.91577 1587.0 0.000630 1515.53162 1564.62122 1570.0 0.000637 1517.89917 1552.47485 1610.0 0.000621 1520.26843 1547.40601 1556.0 0.000643 1522.63977 1545.15918 1505.0 0.000664 1525.00818 1544.19006 1575.0 0.000635 1527.38416 1543.96338 1597.0 0.000626 1529.74731 1544.23083 1485.0 0.000673 1532.12024 1544.88354 1483.0 0.000674 1534.48840 1545.82239 1536.0 0.000651 1536.86060 1546.99451 1562.0 0.000640 1539.22766 1548.34167 1523.0 0.000657 1541.59155 1549.83484 1477.0 0.000677 1543.96094 1543.96155 1481.0 0.000675 1546.32922 1546.33008 1477.0 0.000677 1548.69165 1548.69214 1580.0 0.000633 1551.06067 1551.06055 1589.0 0.000629 1553.42261 1553.42261 1560.0 0.000641 1555.78882 1555.78918 1575.0 0.000635 1558.15149 1558.15149 1605.0 0.000623 1560.51501 1560.51416 1566.0 0.000639 1562.87549 1562.87561 1536.0 0.000651 1565.23584 1565.23584 1600.0 0.000625 1567.59473 1567.59497 1598.0 0.000626 1569.95044 1569.95093 1637.0 0.000611 1572.30981 1572.30945 1614.0 0.000620 1574.66711 1574.66785 1495.0 0.000669 1577.01868 1577.01843 1531.0 0.000653 1579.36914 1579.36902 1602.0 0.000624 1581.72620 1581.72571 1531.0 0.000653 1584.07397 1585.16907 1695.0 0.000590 1586.42603 1587.65527 1574.0 0.000635 1588.76917 1590.15796 1579.0 0.000633 1591.11865 1592.70752 1606.0 0.000623 1593.46106 1595.31750 1585.0 0.000631 1595.80566 1598.07397 1610.0 0.000621 1598.14539 1601.15955 1548.0 0.000646 1600.48169 1604.97571 1637.0 0.000611 1602.82275 1610.24548 1571.0 0.000637 1605.15662 1618.01025 1624.0 0.000616 1607.48535 1629.54431 1638.0 0.000611 1609.82141 1646.17224 1656.0 0.000604 1612.14758 1669.24927 1746.0 0.000573 1614.47522 1700.62634 1743.0 0.000574 1616.80212 1743.22083 1862.0 0.000537 1619.12402 1800.79919 1868.0 0.000535 1621.44666 1875.30713 1991.0 0.000502 1623.76086 1961.15137 2028.0 0.000493 1626.07983 2039.96704 2099.0 0.000476 1628.39185 2083.13745 2122.0 0.000471 1630.70410 2066.44946 2065.0 0.000484 1633.01233 1990.32056 1919.0 0.000521 1635.31165 1884.61182 1849.0 0.000541 1637.61841 1786.08716 1732.0 0.000577 1639.92175 1716.23718 1616.0 0.000619 1642.21631 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0.001880 470.74274 530.33557 517.0 0.001934 470.62244 529.77148 558.0 0.001792 470.49738 529.35248 547.0 0.001828 470.43500 529.09882 545.0 0.001835 470.30432 528.81622 518.0 0.001931 470.18546 528.52039 505.0 0.001980 470.10510 528.22021 501.0 0.001996 469.99106 527.73370 512.0 0.001953 469.85175 527.07776 527.0 0.001898 469.81241 526.35858 526.0 0.001901 469.66348 525.50232 527.0 0.001898 469.55014 524.44763 531.0 0.001883 469.46585 523.34015 541.0 0.001848 469.34183 522.15192 489.0 0.002045 469.24384 520.98260 505.0 0.001980 469.11612 519.79865 502.0 0.001992 468.99017 518.68292 518.0 0.001931 468.88708 517.37000 484.0 0.002066 468.75992 516.29919 491.0 0.002037 468.67343 515.29810 518.0 0.001931 468.54819 514.35309 523.0 0.001912 468.39740 513.39771 509.0 0.001965 468.34396 512.61340 522.0 0.001916 468.18958 511.78040 560.0 0.001786 468.06561 511.17404 499.0 0.002004 467.97647 510.78061 518.0 0.001931 467.83609 510.55908 517.0 0.001934 467.69086 510.59808 557.0 0.001795 467.61218 511.01257 523.0 0.001912 467.46558 511.71237 585.0 0.001709 467.32690 512.80420 540.0 0.001852 467.23303 514.34381 564.0 0.001773 467.10651 516.33069 538.0 0.001859 466.95151 518.59039 522.0 0.001916 466.88354 521.26892 531.0 0.001883 466.72513 524.11316 555.0 0.001802 466.59464 527.12640 542.0 0.001845 466.50226 530.22369 541.0 0.001848 466.36401 533.16418 537.0 0.001862 466.25479 535.89606 528.0 0.001894 466.11487 538.22589 539.0 0.001855 465.97934 540.06134 557.0 0.001795 465.86652 541.32056 554.0 0.001805 465.73416 541.88971 529.0 0.001890 465.63556 541.79572 534.0 0.001873 465.50888 540.96729 487.0 0.002053 465.34921 539.43408 484.0 0.002066 465.27551 537.41089 543.0 0.001842 465.11829 534.72125 499.0 0.002004 464.99081 531.65149 503.0 0.001988 464.89685 528.32166 492.0 0.002033 464.75833 524.54071 519.0 0.001927 464.60840 520.64197 508.0 0.001969 464.52823 516.77277 509.0 0.001965 464.38013 512.89984 478.0 0.002092 464.24591 509.31363 503.0 0.001988 464.15240 505.92072 502.0 0.001992 464.03012 502.83502 517.0 0.001934 463.87662 499.91660 493.0 0.002028 463.80161 497.73874 488.0 0.002049 463.64365 495.97656 519.0 0.001927 463.52521 494.80963 506.0 0.001976 463.43661 494.20972 509.0 0.001965 463.30875 494.15161 527.0 0.001898 463.20441 494.70340 541.0 0.001848 463.07727 495.82083 532.0 0.001880 462.95004 497.60410 534.0 0.001873 462.84863 499.86761 524.0 0.001908 462.72437 502.65555 570.0 0.001754 462.64767 505.87344 527.0 0.001898 462.53439 509.42422 489.0 0.002045 462.38596 513.18597 548.0 0.001825 462.31659 517.17310 534.0 0.001873 462.17459 521.11737 530.0 0.001887 462.07352 525.00153 510.0 0.001961 461.99738 528.68866 520.0 0.001923 461.87738 531.93878 512.0 0.001953 461.75134 534.75592 515.0 0.001942 461.69302 537.15558 492.0 0.002033 461.57043 538.92084 510.0 0.001961 461.45966 540.11389 550.0 0.001818 461.39124 540.78894 558.0 0.001792 461.30109 540.93646 569.0 0.001757 461.17386 540.61737 553.0 0.001808 461.11606 540.01520 513.0 0.001949 460.98804 539.08044 512.0 0.001953 460.89786 538.00665 520.0 0.001923 460.84213 536.84497 513.0 0.001949 460.75153 535.65210 539.0 0.001855 460.67731 534.52386 540.0 0.001852 460.58328 533.51282 544.0 0.001838 460.49698 532.64270 548.0 0.001825 460.42651 531.99811 527.0 0.001898 460.34448 531.57434 582.0 0.001718 460.30560 531.43848 549.0 0.001821 460.23196 531.55536 527.0 0.001898 460.12445 531.82770 532.0 0.001880 460.08121 532.41058 555.0 0.001802 459.98447 533.08704 559.0 0.001789 459.93042 533.88837 548.0 0.001825 459.89404 534.75781 519.0 0.001927 459.82471 535.58954 525.0 0.001905 459.74731 536.35992 521.0 0.001919 459.73315 537.10016 503.0 0.001988 459.66153 537.64148 546.0 0.001832 459.59982 538.05957 531.0 0.001883 459.57864 538.34314 527.0 0.001898 459.54153 538.40808 526.0 0.001901 459.47064 538.12634 553.0 0.001808 459.45026 537.71979 507.0 0.001972 459.37500 536.96631 525.0 0.001905 459.34177 535.93188 528.0 0.001894 459.34152 534.58563 524.0 0.001908 459.30411 532.84711 537.0 0.001862 459.28293 530.77258 490.0 0.002041 459.25101 528.33899 505.0 0.001980 459.21777 525.59351 529.0 0.001890 459.20541 522.58972 498.0 0.002008 459.18237 519.34247 469.0 0.002132 459.20087 515.98462 511.0 0.001957 459.19025 512.46881 485.0 0.002062 459.14301 508.88950 547.0 0.001828 459.15082 505.42810 479.0 0.002088 459.11652 502.07385 489.0 0.002045 459.12045 498.99399 483.0 0.002070 459.14850 496.23874 542.0 0.001845 459.14484 493.83606 474.0 0.002110 459.12851 491.78885 474.0 0.002110 459.17206 490.19809 482.0 0.002075 459.15945 489.02551 532.0 0.001880 459.16470 488.12695 452.0 0.002212 459.21204 487.71341 478.0 0.002092 459.23853 487.65967 527.0 0.001898 459.22922 487.94525 497.0 0.002012 459.25980 488.45444 494.0 0.002024 459.24622 489.15344 510.0 0.001961 459.28076 490.15356 484.0 0.002066 459.34122 491.40060 465.0 0.002151 459.37021 492.66074 508.0 0.001969 459.41064 494.05261 484.0 0.002066 459.43710 495.49069 497.0 0.002012 459.46786 496.98575 487.0 0.002053 459.51489 498.53799 512.0 0.001953 459.55252 500.07288 509.0 0.001965 459.63278 501.63031 528.0 0.001894 459.68524 503.13742 514.0 0.001946 459.69696 504.57458 532.0 0.001880 459.74716 506.02115 557.0 0.001795 459.77267 507.45245 490.0 0.002041 459.83472 508.87140 505.0 0.001980 459.92169 510.29703 539.0 0.001855 459.97415 511.66052 518.0 0.001931 460.01480 512.95996 539.0 0.001855 460.10156 514.22424 509.0 0.001965 460.14709 515.32391 501.0 0.001996 460.20685 516.28186 510.0 0.001961 460.29904 517.08185 483.0 0.002070 460.37289 517.66156 462.0 0.002165 460.41150 517.95758 505.0 0.001980 460.47867 518.05750 515.0 0.001942 460.50897 517.91943 527.0 0.001898 460.58209 517.66791 505.0 0.001980 460.68393 517.34406 519.0 0.001927 460.75208 516.96515 543.0 0.001842 460.82806 516.63983 510.0 0.001961 460.88919 516.42535 534.0 0.001873 460.94885 516.42963 545.0 0.001835 461.02432 516.69452 528.0 0.001894 461.09213 517.24689 537.0 0.001862 461.19186 518.15875 552.0 0.001812 461.26941 519.38397 535.0 0.001869 461.30371 520.80792 518.0 0.001931 461.36060 522.47162 518.0 0.001931 461.40225 524.25183 526.0 0.001901 461.48056 526.18750 514.0 0.001946 461.57108 528.02716 486.0 0.002058 461.63342 529.64532 521.0 0.001919 461.67438 531.09924 572.0 0.001748 461.75970 532.32892 537.0 0.001862 461.80002 533.21149 490.0 0.002041 461.85010 533.81274 528.0 0.001894 461.93353 534.11554 481.0 0.002079 461.99536 534.08978 530.0 0.001887 462.01321 533.86682 509.0 0.001965 462.04776 533.51562 553.0 0.001808 462.05133 533.06488 553.0 0.001808 462.09912 532.70013 549.0 0.001821 462.16333 532.36932 516.0 0.001938 462.19223 532.10254 524.0 . . . _pd_meas_number_of_points 4250 _pd_proc_number_of_points 4250 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 2 o 70210.35 71116.43 180.00 11.39818 100.00 0 1 1 o 567.822 380.005 0.00 8.98878 1.00 1 0 0 o 32872.113 34635.836 0.00 8.67363 26.83 1 0 1 o 1226.692 1780.239 90.00 8.10667 1.79 0 1 2 o 1996.447 1923.657 0.00 7.42282 2.36 1 0 2 o 17714.662 16576.775 180.00 6.90240 17.93 1 1 0 o 1642.826 1659.378 -90.00 6.48961 1.53 1 1 1 o 942.119 670.837 -146.90 6.24162 1.52 0 1 3 o 281.023 116.873 0.00 6.00075 0.23 1 0 3 o 59.327 43.215 -90.00 5.71561 0.05 0 0 4 o 933.418 744.447 0.00 5.69909 0.30 1 1 2 o 5549.189 5571.170 -64.07 5.63959 7.63 1 1 3 o 1123.900 2056.249 -140.65 4.93486 1.29 0 1 4 o 2999.063 4408.866 0.00 4.92421 1.64 0 2 0 o 3087.647 2940.624 0.00 4.89064 0.81 1 0 4 o 15496.945 14337.101 0.00 4.76294 7.17 0 2 1 o 19363.891 17490.588 0.00 4.78183 9.98 0 2 2 o 5505.433 5222.763 0.00 4.49439 2.34 2 0 0 o 9799.083 9933.390 0.00 4.33682 1.87 1 1 4 o 13694.039 13480.736 108.89 4.28223 10.74 1 2 0 o 1.018 1.013 180.00 4.26010 0.00 2 0 1 o 12882.184 12848.560 90.00 4.26041 4.96 1 2 1 o 21995.016 20997.021 171.05 4.18760 15.88 0 1 5 o 24033.977 24410.268 180.00 4.13240 8.79 0 2 3 o 48507.71 44599.93 0.00 4.11249 17.04 2 0 2 o 3136.101 2082.957 -180.00 4.05333 1.01 1 0 5 o 40.346 13.162 90.00 4.03569 0.01 1 2 2 o 1890.168 1309.163 54.81 3.99049 1.26 2 1 0 o 3619.545 4448.463 -90.00 3.96460 1.26 2 1 1 o 16539.475 17550.766 -69.08 3.90597 10.69 0 0 6 o 574.499 2135.655 180.00 3.79939 0.06 2 1 2 o 12555.919 12996.331 -11.78 3.74455 7.49 2 0 3 o 1383.815 1578.651 90.00 3.76655 0.40 1 1 5 o 1989.765 1900.003 152.33 3.73063 1.20 1 2 3 o 34442.113 31727.941 -9.08 3.71596 19.75 0 2 4 o 3205.248 2858.973 180.00 3.71141 0.93 0 1 6 o 10812.103 12785.406 -180.00 3.54159 2.92 2 1 3 o 21715.609 22036.986 157.46 3.51495 11.36 1 0 6 o 15400.124 14856.800 180.00 3.48015 3.75 2 0 4 o -48.423 12.912 180.00 3.45120 0.00 1 2 4 o 1777.189 2648.935 -132.37 3.41216 0.86 0 2 5 o 31682.152 29503.000 -180.00 3.33489 7.23 1 1 6 o 5427.597 4880.456 -92.28 3.27880 2.46 2 2 0 o 188.127 188.038 180.00 3.24481 0.04 2 1 4 o 8769.579 9645.364 179.25 3.25456 3.89 2 2 1 o 24316.373 23430.461 172.69 3.21243 10.24 0 3 1 o 3608.471 3105.927 0.00 3.22758 0.77 2 0 5 o 7.844 25.542 -90.00 3.14229 0.00 2 2 2 o 1938.814 1887.623 83.33 3.12081 0.78 1 2 5 o 22164.297 21450.475 167.37 3.11274 8.74 0 3 2 o 19.703 20.478 -180.00 3.13470 0.00 0 1 7 o 15995.328 13640.348 0.00 3.08986 3.14 1 3 0 o 5038.844 5554.392 -90.00 3.05193 0.96 1 0 7 o 9567.001 10298.041 90.00 3.04881 1.86 1 3 1 o 1019.419 1559.981 -123.30 3.02494 0.39 2 1 5 o 2215.334 2299.461 -8.35 2.99170 0.82 0 2 6 o 10844.803 11952.306 0.00 3.00038 1.99 2 2 3 o 21940.203 22016.785 -4.60 2.98412 7.93 0 3 3 o 218.770 231.790 0.00 2.99626 0.04 1 3 2 o 9543.108 8181.752 36.50 2.94808 3.40 1 1 7 o 1392.777 1712.370 7.51 2.91069 0.48 3 0 0 o 7684.268 6631.413 0.00 2.89121 0.65 3 0 1 o 7.114 54.231 90.00 2.86824 0.00 0 0 8 o 12583.384 16045.511 0.00 2.84954 1.01 2 0 6 o 404.567 796.913 -180.00 2.85781 0.06 1 2 6 o 2727.746 1963.580 -90.86 2.83552 0.90 1 3 3 o 84.489 58.608 -36.08 2.83204 0.03 2 2 4 o 389.901 419.700 140.48 2.81980 0.12 0 3 4 o 2844.454 2104.391 0.00 2.83003 0.47 3 0 2 o 19467.670 17748.109 180.00 2.80246 3.04 3 1 0 o 116.008 130.173 -90.00 2.77262 0.02 3 1 1 o 2973.433 2801.507 -45.96 2.75234 0.90 2 1 6 o 6082.989 6546.870 -60.98 2.74312 1.82 0 1 8 o 326.012 363.364 -180.00 2.73581 0.04 1 0 8 o 4216.883 4448.497 0.00 2.70719 0.61 3 0 3 o 507.633 504.796 90.00 2.70222 0.08 0 2 7 o 10585.972 11708.735 0.00 2.71065 1.51 3 1 2 o 5917.802 4935.596 -59.37 2.69406 1.70 1 3 4 o 221.332 173.270 16.11 2.69044 0.07 2 2 5 o 21034.441 19730.447 163.95 2.64364 5.78 0 3 5 o 8533.136 8136.791 0.00 2.65207 1.22 2 3 0 o 2272.230 2021.638 90.00 2.60608 0.32 1 1 8 o 9686.507 8773.773 57.48 2.60910 2.63 3 1 3 o 5065.940 4486.249 127.54 2.60465 1.36 2 0 7 o 1769.797 1534.459 -90.00 2.60414 0.25 2 3 1 o 1347.438 1394.290 -125.34 2.58922 0.37 1 2 7 o 5426.036 5570.027 37.10 2.58725 1.39 3 0 4 o 50.913 239.776 0.00 2.57839 0.01 2 3 2 o 476.012 1175.482 53.16 2.54053 0.13 1 3 5 o 314.157 690.432 21.17 2.53616 0.09 2 1 7 o -59.708 1523.911 -16.90 2.51648 0.00 3 2 0 o 135.366 191.179 0.00 2.48883 0.02 3 1 4 o 105.082 129.242 160.23 2.49322 0.02 3 2 1 o 2663.024 2622.126 163.75 2.47413 0.59 2 3 3 o 3183.031 3210.458 73.40 2.46514 0.76 2 2 6 o 2694.911 2651.506 42.44 2.46743 0.64 0 3 6 o 24.091 20.370 -180.00 2.47427 0.00 0 2 8 o 2468.781 2514.412 180.00 2.46210 0.29 0 1 9 o 671.916 863.437 0.00 2.45205 0.09 3 2 2 o 747.066 518.050 -157.82 2.43154 0.18 3 0 5 o 565.163 694.894 -90.00 2.44166 0.06 1 0 9 o 9001.817 6541.496 -90.00 2.43138 1.07 0 4 0 o 10295.553 15203.376 180.00 2.44532 0.62 0 4 1 o 68.398 50.541 180.00 2.43137 0.01 2 0 8 o 20731.670 20888.846 0.00 2.38147 2.28 2 3 4 o 4191.467 3990.663 -130.46 2.37004 0.91 1 3 6 o 784.523 786.064 128.15 2.37936 0.18 3 2 3 o 9728.973 8905.072 -41.52 2.36520 2.07 0 4 2 o 5229.270 4602.867 0.00 2.39092 0.58 3 1 5 o 5590.130 5407.965 -100.29 2.36897 1.21 1 2 8 o 7993.197 7735.020 153.02 2.36853 1.76 1 1 9 o 472.207 389.913 167.03 2.35957 0.10 1 4 0 o 16935.908 12273.273 -180.00 2.35357 1.79 1 4 1 o 4539.503 4029.262 -19.64 2.34113 0.96 2 1 8 o 12430.618 12670.051 119.44 2.31388 2.55 0 4 3 o 108.727 150.414 0.00 2.32776 0.02 3 0 6 o 2586.835 2346.858 -180.00 2.30080 0.26 2 2 7 o 5391.652 5014.952 -14.79 2.29859 1.04 1 4 2 o 1660.921 1480.660 23.12 2.30495 0.33 0 3 7 o 179.590 156.263 180.00 2.30412 0.02 3 2 4 o 691.094 823.834 152.09 2.28083 0.14 0 0 10 o 14932.720 17663.756 180.00 2.27964 0.74 2 3 5 o 3899.434 4327.687 -77.95 2.26255 0.75 0 2 9 o 7785.951 7404.203 -180.00 2.24917 0.72 1 4 3 o 2063.022 1936.385 142.29 2.24820 0.39 3 1 6 o 1651.452 1440.397 -100.63 2.23967 0.30 0 4 4 o 5850.895 5447.304 180.00 2.24719 0.54 1 3 7 o 1776.129 3099.084 -167.60 2.22689 0.34 0 1 10 o 44.555 204.803 0.00 2.22014 0.00 1 0 10 o 11926.835 9708.631 180.00 2.20476 1.09 3 2 5 o 13404.931 11699.527 168.38 2.18454 2.38 2 0 9 o 122.148 99.126 90.00 2.18721 0.01 1 2 9 o 12310.044 11583.234 -149.07 2.17717 2.15 3 3 0 o 23288.053 23491.596 -90.00 2.16320 2.04 4 0 0 o 593.696 577.629 0.00 2.16841 0.03 1 4 4 o 4050.569 3840.508 -129.21 2.17537 0.71 3 3 1 o 411.909 395.871 -125.85 2.15353 0.07 3 0 7 o 4460.622 4606.921 -90.00 2.16209 0.41 4 0 1 o 3154.753 3259.944 -90.00 2.15866 0.29 2 3 6 o 10187.704 9444.323 104.36 2.14911 1.76 1 1 10 o 1509.188 1388.329 29.32 2.15080 0.28 0 4 5 o 835.061 816.712 0.00 2.15494 0.07 2 2 8 o 4813.220 4762.501 -109.70 2.14112 0.83 2 4 0 o 4090.212 4395.212 180.00 2.13005 0.33 0 3 8 o 12730.709 12195.034 -180.00 2.14559 1.11 2 1 9 o 3093.104 3350.712 -96.78 2.13449 0.52 3 3 2 o 10741.795 11502.737 82.89 2.12527 1.80 4 0 2 o 11184.092 12081.562 180.00 2.13020 0.95 2 4 1 o 1710.464 1976.077 -51.75 2.12081 0.29 4 1 0 o 1437.462 1662.116 90.00 2.11701 0.12 4 1 1 o 8607.065 8387.393 -67.06 2.10794 1.39 3 1 7 o 8811.328 8690.376 61.31 2.11113 1.49 2 4 2 o 6424.921 6444.831 -23.75 2.09380 1.01 3 2 6 o 539.492 551.608 90.77 2.08192 0.09 4 1 2 o 6533.747 6738.357 -93.42 2.08141 1.06 3 3 3 o 4496.979 4707.243 129.65 2.08054 0.72 4 0 3 o 19174.725 19093.305 90.00 2.08517 1.60 1 4 5 o 1811.102 1917.481 26.61 2.09136 0.29 1 3 8 o 3315.725 3329.551 177.10 2.08281 0.54 0 2 10 o 1075.272 986.829 180.00 2.06620 0.09 2 4 3 o 4017.794 3830.562 179.82 2.05099 0.62 4 1 3 o 2185.313 1494.811 90.22 2.03935 0.32 0 4 6 o 13272.232 12613.535 0.00 2.05625 1.02 2 3 7 o 180.952 185.134 56.60 2.03477 0.03 3 3 4 o 4577.391 4395.264 -83.36 2.02242 0.67 3 0 8 o 12069.507 11911.668 0.00 2.02950 0.93 0 1 11 o 4223.736 4013.064 0.00 2.02739 0.32 4 0 4 o 11305.672 10710.950 0.00 2.02667 0.84 2 0 10 o 17471.607 16075.091 -180.00 2.01785 1.30 1 0 11 o 8367.353 7634.771 90.00 2.01566 0.65 1 2 10 o 3066.173 2741.965 -33.27 2.00996 0.47 2 4 4 o 11248.104 12437.193 172.85 1.99524 1.59 1 4 6 o 14396.263 15138.500 -5.60 2.00079 2.08 4 2 0 o 252.079 260.993 0.00 1.98230 0.02 2 2 9 o 1059.610 1154.179 -165.96 1.99663 0.14 0 3 9 o 1017.400 1078.274 0.00 2.00025 0.07 4 1 4 o 9040.029 9028.394 92.15 1.98452 1.31 4 2 1 o 2811.097 2860.149 163.94 1.97485 0.38 3 1 8 o 1323.309 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5 11 o 8135.852 9961.170 -46.38 1.18945 0.38 5 6 1 o 1061.060 976.666 -17.51 1.18636 0.05 1 8 3 o 3635.362 3651.790 15.54 1.19561 0.16 0 1 19 o 132.813 149.557 180.00 1.19088 0.00 3 5 13 o 461.758 541.778 71.66 1.19002 0.02 3 3 16 o 451.778 540.311 -113.55 1.18987 0.02 0 6 13 o 7113.282 6688.620 0.00 1.19396 0.16 7 2 3 o 53.118 48.204 103.11 1.18641 0.00 0 8 4 o 2451.615 2431.106 0.00 1.19546 0.05 1 0 19 o 2011.831 2440.699 90.00 1.18849 0.05 6 4 6 o 1087.626 1242.260 -46.84 1.18260 0.05 4 0 16 o 3045.802 3386.899 0.00 1.19074 0.07 4 6 8 o 292.611 261.051 39.16 1.18502 0.01 5 6 2 o 163.949 190.990 71.12 1.18156 0.01 2 6 12 o 6433.048 7998.741 21.66 1.18968 0.31 6 2 10 o 349.149 324.168 106.81 1.18448 0.01 7 1 5 o 828.774 795.841 -99.43 1.18688 0.03 0 7 10 o 625.878 650.564 -180.00 1.19133 0.02 1 5 15 o 4689.874 5952.209 -126.76 1.18882 0.22 5 0 14 o 369.559 372.083 -180.00 1.18723 0.01 2 4 16 o 7468.653 7030.328 -179.95 1.18426 0.35 5 5 8 o 451.591 518.614 18.45 1.18117 0.02 6 0 11 o 153.094 130.049 90.00 1.18565 0.00 4 1 16 o 448.511 528.287 117.41 1.18201 0.02 3 2 17 o 407.066 440.192 -173.52 1.18052 0.02 1 1 19 o 1169.531 1156.452 71.84 1.17981 0.05 2 2 18 o 131.069 128.661 -99.44 1.17979 0.01 1 8 4 o 1683.950 1570.538 43.32 1.18426 0.08 5 6 3 o 2588.613 2461.265 177.48 1.17371 0.12 3 4 15 o 1513.370 1283.076 -109.69 1.17865 0.07 5 1 14 o 884.925 736.248 -152.24 1.17858 0.04 1 6 13 o 3052.011 3606.268 -19.19 1.18281 0.14 0 3 18 o 3585.146 3948.978 0.00 1.18053 0.08 7 2 4 o 0.979 0.796 134.91 1.17532 0.00 4 7 0 o 5965.906 5734.899 90.00 1.17457 0.13 6 1 11 o 657.061 539.437 78.87 1.17703 0.03 1 7 10 o 1591.888 1698.165 -150.54 1.18025 0.08 4 7 1 o 376.511 350.120 60.15 1.17302 0.02 7 0 6 o 1331.854 1048.458 -180.00 1.17803 0.03 2 7 9 o 788.444 624.448 107.38 1.17753 0.04 0 8 5 o 414.504 482.694 -180.00 1.18093 0.01 2 8 0 o 3838.701 3156.053 0.00 1.17679 0.09 6 3 9 o 3007.789 2622.864 -83.63 1.17165 0.14 3 7 7 o 3300.104 3173.382 -6.17 1.17357 0.15 0 4 17 o 4666.235 4226.162 0.00 1.17578 0.11 2 8 1 o 2881.239 2750.061 177.28 1.17522 0.13 3 6 11 o 5498.105 4744.556 174.17 1.17142 0.25 5 4 11 o 3420.565 2709.197 -118.15 1.16851 0.15 4 7 2 o 7531.126 5924.428 -82.13 1.16839 0.33 1 3 18 o 1831.238 1550.224 13.91 1.16975 0.08 7 1 6 o 1458.021 1227.666 -119.34 1.16957 0.07 5 6 4 o 1000.483 800.975 82.11 1.16297 0.04 2 8 2 o 761.910 656.651 -148.47 1.17056 0.03 6 5 0 o 95.713 73.197 90.00 1.16261 0.00 6 4 7 o 71.739 61.100 -156.84 1.16244 0.00 6 5 1 o 7438.907 6950.549 111.19 1.16110 0.33 1 8 5 o 2212.071 1901.054 -134.92 1.17014 0.10 4 3 15 o 3225.510 2656.668 132.76 1.16270 0.14 0 2 19 o 10936.101 7432.123 0.00 1.16525 0.25 7 2 5 o 2260.723 2101.634 22.21 1.16151 0.10 7 3 0 o 6612.614 5322.486 -90.00 1.15827 0.14 4 7 3 o 291.426 278.646 89.89 1.16079 0.01 1 4 17 o 763.062 525.362 -0.67 1.16512 0.03 7 3 1 o 4259.072 3269.188 -91.13 1.15677 0.19 6 5 2 o 237.089 187.238 105.99 1.15661 0.01 4 6 9 o 2186.715 1800.467 -78.92 1.15871 0.10 2 8 3 o 1119.684 907.698 4.18 1.16292 0.05 5 5 9 o 6116.461 4962.030 120.23 1.15510 0.27 0 8 6 o 506.274 372.853 180.00 1.16388 0.01 3 0 18 o 4883.339 4686.282 -180.00 1.16005 0.11 7 3 2 o 7386.272 7496.035 55.41 1.15233 0.33 4 2 16 o 1566.461 1183.473 -139.78 1.15694 0.07 2 5 15 o 907.076 676.249 176.70 1.15668 0.04 4 5 12 o 2121.860 1868.535 -83.52 1.15387 0.10 2 0 19 o 2873.416 2156.635 90.00 1.15637 0.06 5 3 13 o 2084.511 1903.903 -97.19 1.15349 0.09 7 0 7 o 500.583 391.531 90.00 1.15810 0.01 5 6 5 o 3424.040 4772.240 -10.31 1.14958 0.16 1 2 19 o 3220.299 2644.142 9.99 1.15488 0.14 6 2 11 o 1371.812 1407.519 31.21 1.15227 0.06 6 5 3 o 6240.195 8518.188 -85.31 1.14924 0.27 0 7 11 o 289.846 229.492 0.00 1.15857 0.01 5 2 14 o 4320.155 3858.458 82.54 1.15372 0.19 4 7 4 o 5280.837 6826.959 99.18 1.15040 0.23 3 1 18 o 1794.726 1904.180 -43.83 1.15198 0.08 4 4 14 o 823.869 1176.092 -25.15 1.14930 0.03 3 7 8 o 2544.196 3114.196 129.52 1.15091 0.11 7 3 3 o 265.803 209.433 15.74 1.14504 0.01 2 8 4 o 360.025 361.424 -96.21 1.15247 0.02 7 1 7 o 1724.773 2372.549 57.16 1.15006 0.08 1 8 6 o 1820.668 1647.361 -134.40 1.15354 0.08 2 6 13 o 5071.589 6040.664 9.16 1.15113 0.22 3 5 14 o 1274.531 1847.387 78.17 1.14852 0.06 2 1 19 o 597.530 832.330 9.83 1.14837 0.02 6 0 12 o 224.463 315.575 180.00 1.15040 0.01 0 6 14 o 39.478 41.219 180.00 1.15206 0.00 7 2 6 o 855.747 671.843 68.45 1.14527 0.04 0 5 16 o 241.226 264.060 0.00 1.15169 0.00 2 7 10 o 1451.979 2187.726 -92.86 1.14878 0.06 6 3 10 o 11686.876 10155.343 89.51 1.14331 0.50 6 4 8 o 2026.980 2107.386 130.55 1.14041 0.09 6 5 4 o 1494.878 1382.000 -75.92 1.13915 0.07 1 7 11 o 1283.808 1929.750 -49.04 1.14837 0.06 6 1 12 o 3461.711 3336.283 79.06 1.14253 0.15 5 0 15 o 1052.171 938.592 90.00 1.14312 0.02 0 8 7 o 1852.997 1351.885 0.00 1.14465 0.04 7 3 4 o 14284.121 14572.964 -97.43 1.13506 0.61 4 7 5 o 192.418 156.260 48.65 1.13743 0.01 1 6 14 o 6111.069 6344.704 -169.54 1.14203 0.26 0 0 20 o 986.153 990.608 0.00 1.13982 0.01 3 3 17 o 3095.698 3084.063 -46.39 1.13974 0.13 1 5 16 o 2547.917 2724.339 -4.65 1.14167 0.11 2 3 18 o 4706.949 4316.272 47.99 1.13908 0.21 5 6 6 o 286.269 324.228 -134.19 1.13383 0.01 4 0 17 o 287.118 309.235 -90.00 1.14050 0.01 3 6 12 o 3056.413 2460.491 39.89 1.13739 0.13 2 8 5 o 2264.773 2185.565 166.28 1.13944 0.10 5 4 12 o 1842.447 1981.978 147.06 1.13472 0.08 5 1 15 o 3339.360 3284.007 40.39 1.13539 0.14 2 4 17 o 1210.668 1314.447 19.88 1.13481 0.05 7 0 8 o 185.801 153.787 0.00 1.13631 0.00 4 6 10 o 186.648 156.201 -172.93 1.13127 0.01 5 5 10 o 2325.189 1618.739 138.73 1.12792 0.10 4 1 17 o 1846.719 2034.406 -82.74 1.13282 0.08 3 4 16 o 2477.388 2627.554 154.98 1.13265 0.10 0 1 20 o 3349.525 3256.765 -180.00 1.13216 0.07 6 5 5 o 13065.779 11408.348 72.87 1.12656 0.55 1 8 7 o 1531.295 1719.551 60.03 1.13481 0.07 1 0 20 o 274.210 195.064 0.00 1.13010 0.01 7 2 7 o 4799.312 3909.805 -165.36 1.12693 0.21 3 2 18 o 120.392 79.201 24.68 1.12873 0.00 7 1 8 o 2288.044 1478.459 64.09 1.12872 0.09 3 8 0 o 3546.600 3382.682 0.00 1.12611 0.08 7 3 5 o 855.786 894.712 -79.12 1.12261 0.03 3 8 1 o 183.150 193.510 -137.90 1.12473 0.01 3 7 9 o 3653.561 3094.821 175.66 1.12676 0.16 0 3 19 o 487.972 480.879 180.00 1.12599 0.01 2 2 19 o 500.794 521.250 -36.55 1.12534 0.02 4 7 6 o 7096.080 7476.769 -95.10 1.12217 0.30 3 8 2 o 3266.808 3267.964 147.88 1.12065 0.14 1 1 20 o 1209.037 1280.359 -175.97 1.12263 0.05 0 4 18 o 1617.422 1733.494 0.00 1.12459 0.03 6 2 12 o 3661.913 3345.721 -73.73 1.11984 0.15 2 8 6 o 572.734 610.666 -179.67 1.12410 0.02 6 4 9 o 2512.924 2067.581 93.40 1.11690 0.11 0 7 12 o 28.456 30.379 -180.00 1.12562 0.00 4 5 13 o 3615.726 2907.861 70.82 1.11860 0.15 5 6 7 o 2879.554 2598.521 128.91 1.11603 0.12 4 3 16 o 1260.334 1011.065 -59.40 1.11848 0.05 0 8 8 o 7197.146 7702.930 0.00 1.12360 0.15 5 3 14 o 6685.999 6428.507 107.36 1.11557 0.28 2 7 11 o 599.609 510.966 -91.80 1.11932 0.03 1 3 19 o 409.126 345.071 -164.95 1.11662 0.02 6 5 6 o 2329.311 1920.331 78.86 1.11173 0.10 6 3 11 o 1887.431 2027.547 97.84 1.11426 0.08 5 2 15 o 256.141 259.647 38.72 1.11312 0.01 1 4 18 o 6243.677 6328.503 -7.78 1.11525 0.26 3 8 3 o 162.502 174.891 -24.79 1.11394 0.01 2 6 14 o 2777.565 2978.811 -155.78 1.11344 0.12 6 0 13 o 81.683 80.309 90.00 1.11544 0.00 2 5 16 o 402.368 410.954 8.26 1.11311 0.02 7 4 0 o 316.240 307.557 180.00 1.10529 0.01 7 3 6 o 10765.673 10232.219 111.00 1.10793 0.45 1 7 12 o 317.229 277.277 121.52 1.11626 0.01 7 4 1 o 1307.381 1300.467 122.15 1.10399 0.06 4 4 15 o 2740.342 2280.940 -125.50 1.10914 0.11 7 0 9 o 994.058 1010.400 -90.00 1.11305 0.02 3 5 15 o 5274.696 4805.833 -116.11 1.10845 0.22 4 2 17 o 102.349 73.899 67.03 1.11070 0.00 1 8 8 o 2670.297 3056.656 -12.66 1.11429 0.11 0 2 20 o 497.468 374.049 180.00 1.11007 0.01 7 2 8 o 217.383 216.885 -143.57 1.10683 0.01 6 1 13 o 1655.311 1548.901 -92.20 1.10826 0.07 3 0 19 o 1470.954 1389.209 90.00 1.10818 0.03 7 1 9 o 5161.166 5082.880 -109.82 1.10591 0.21 0 6 15 o 1215.008 960.559 -180.00 1.11163 0.02 7 4 2 o 1361.844 1504.403 -111.26 1.10013 0.06 4 7 7 o 1117.637 1084.368 -47.31 1.10490 0.05 4 6 11 o 2889.497 3007.957 110.14 1.10311 0.12 2 8 7 o 4241.265 4291.736 2.03 1.10675 0.18 3 8 4 o 2854.437 2764.287 -52.46 1.10475 0.12 5 5 11 o 6230.941 6905.765 -46.80 1.10000 0.26 0 5 17 o 620.395 614.884 0.00 1.10605 0.01 3 6 13 o 7360.975 7450.048 3.15 1.10357 0.31 5 4 13 o 41.631 45.807 86.21 1.10113 0.00 2 0 20 o 3970.106 4331.739 0.00 1.10238 0.08 3 7 10 o 5737.817 6513.872 -93.61 1.10149 0.24 3 1 19 o 1389.182 1591.972 100.91 1.10113 0.06 5 6 8 o 312.511 287.384 -88.05 1.09649 0.01 1 2 20 o 721.663 829.549 -177.00 1.10109 0.03 7 4 3 o 1201.402 1130.863 -72.69 1.09378 0.05 1 6 15 o 1038.653 1125.648 116.61 1.10261 0.04 6 5 7 o 7765.121 7091.074 -104.71 1.09493 0.32 5 0 16 o 126.903 149.428 0.00 1.10102 0.00 0 8 9 o 2493.355 2934.733 -180.00 1.10109 0.05 6 4 10 o 2244.411 2209.631 -104.32 1.09227 0.10 7 3 7 o 3502.940 3407.721 100.20 1.09130 0.14 2 1 20 o 2007.158 1804.235 89.25 1.09544 0.08 5 7 0 o 4813.164 5033.791 90.00 1.08820 0.10 1 5 17 o 2713.085 2537.974 64.69 1.09717 0.11 3 3 18 o 1083.231 1060.664 28.94 1.09293 0.04 5 7 1 o 1849.317 1968.371 58.89 1.08696 0.08 5 1 16 o 832.121 771.646 81.78 1.09411 0.03 4 0 18 o 227.632 217.387 -180.00 1.09360 0.00 3 8 5 o 775.163 750.542 161.18 1.09325 0.03 3 4 17 o 2427.229 2457.401 56.55 1.08916 0.10 2 3 19 o 2612.085 2556.052 -168.04 1.08985 0.11 6 2 13 o 979.475 1051.042 143.47 1.08751 0.04 0 7 13 o 1454.648 1445.923 180.00 1.09281 0.03 1 8 9 o 5817.255 5808.808 -147.34 1.09232 0.24 7 0 10 o 2025.053 2108.004 0.00 1.08866 0.04 2 4 18 o 6838.792 7133.711 -3.48 1.08858 0.29 2 7 12 o 849.132 843.241 51.67 1.08952 0.04 4 1 18 o 906.306 972.251 6.21 1.08683 0.04 2 8 8 o 2665.393 2868.493 -20.23 1.08769 0.11 _reflns_number_total 942 _reflns_limit_h_min 0 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 9 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _reflns_d_resolution_high 1.087 _reflns_d_resolution_low 11.398 # start Validation Reply Form _vrf_PLAT306_Y2LH23.5H2O-AP_publ ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O101 RESPONSE: Solvent water molecule in pore; powder data, H-atoms cannot be found ; _vrf_PLAT040_Y2LH23.5H2O-AP_publ ; PROBLEM: No H-atoms in this Carbon Containing Compound .. RESPONSE: Powder data: could not identify protons ; # end Validation Reply Form #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# # Attachment '- Structure-2.cif' data_STA-13(Y)-AP_publ _database_code_depnum_ccdc_archive 'CCDC 771871' #TrackingRef '- Structure-2.cif' _pd_block_id 2010-03-08T14:00|STA-13(Y)-AP||ID31 _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2010-03-08T14:00 _audit_author_name 'Michael T. Wharmby' _audit_update_record ; 2010-03-08T14:00 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 ? _pd_char_colour white # use ICDD colour descriptions _refine_ls_shift/su_max 0.03 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 71 _refine_ls_goodness_of_fit_all 2.11 _refine_ls_number_restraints 67 _refine_ls_matrix_type full _refine_diff_density_max 0.338 _refine_diff_density_min -0.371 #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C21 N6 O18 P6 Y2, 7.75(O)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall '-P 3' _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_meas 1.806 _exptl_crystal_density_method 'helium pycnometry' _cell_measurement_temperature 100 _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 'STA-13(Y) - As prepared' _cell_length_a 16.18945(26) _cell_length_b 16.18945 _cell_length_c 10.00355(16) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 2270.64(4) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P -3' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -y,x-y,+z 3 y-x,-x,+z -1 -x,-y,-z -2 +y,y-x,-z -3 x-y,+x,-z # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Y Y1 0.6667 0.3333 0.3081(5) 1.0 Uiso 0.01273(33) 2 Y Y2 0.6667 0.3333 -0.2053(5) 1.0 Uiso 0.01273(33) 2 P P1 0.6042(5) 0.4511(5) 0.0632(6) 1.0 Uiso 0.01273(33) 6 P P4 0.2036(5) 0.4715(5) 0.4505(7) 1.0 Uiso 0.01273(33) 6 O O1 0.6584(7) 0.4414(8) 0.1740(8) 1.0 Uiso 0.01273(33) 6 O O2 0.6359(5) 0.4274(5) -0.0627(7) 1.0 Uiso 0.01273(33) 6 O O3 0.6219(9) 0.5518(8) 0.0591(14) 1.0 Uiso 0.01273(33) 6 O O4 0.2158(7) 0.5405(6) 0.5600(10) 1.0 Uiso 0.01273(33) 6 O O5 0.2507(5) 0.5245(6) 0.3290(8) 1.0 Uiso 0.01273(33) 6 O O6 0.1013(6) 0.4018(6) 0.4278(10) 1.0 Uiso 0.01273(33) 6 O O101 0.0 0.0 0.1040(26) 1.0 Uiso 0.06 2 O O102 0.2841(13) -0.0012(18) 0.2277(16) 1.0 Uiso 0.06 6 O O103 0.0300(17) 0.1918(12) 0.0191(26) 0.75 Uiso 0.06 6 O O104 0.1174(14) 0.0258(13) 0.3952(21) 0.5 Uiso 0.06 6 N N1 0.4159(7) 0.3839(10) 0.1771(12) 1.0 Uiso 0.01273(33) 6 N N4 0.3221(8) 0.3835(9) 0.4174(12) 1.0 Uiso 0.01273(33) 6 C C1 0.4750(7) 0.3600(10) 0.0890(15) 1.0 Uiso 0.01273(33) 6 C C2 0.3306(10) 0.2946(9) 0.2258(15) 1.0 Uiso 0.01273(33) 6 C C3 0.2693(8) 0.3169(10) 0.3074(14) 1.0 Uiso 0.01273(33) 6 C C4 0.2593(10) 0.3999(10) 0.5101(13) 1.0 Uiso 0.01273(33) 6 C C5 0.4118(9) 0.4681(9) 0.3796(16) 1.0 Uiso 0.01273(33) 6 C C6 0.4690(7) 0.4553(10) 0.2787(17) 1.0 Uiso 0.01273(33) 6 C C7 0.2781(21) 0.2409(25) 0.1036(26) 0.25 Uiso 0.01273(33) 6 C C8 0.1891(11) 0.2301(10) 0.3665(19) 0.75 Uiso 0.01273(33) 6 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C21 N6 O25.75 P6 Y2' _chemical_formula_weight 1111.90 _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 Y1 O1 2.261(9) . 1_555 N Y1 O1 2.260(9) . 2_655 N Y1 O1 2.260(9) . 3_665 N Y1 O4 2.376(8) . -1_666 N Y1 O4 2.377(8) . -2_556 N Y1 O4 2.375(8) . -3_656 N Y2 O2 2.316(7) . 1_555 N Y2 O2 2.315(7) . 2_655 N Y2 O2 2.315(7) . 3_665 N Y2 O5 2.354(7) . -1_665 N Y2 O5 2.354(7) . -2_555 N Y2 O5 2.353(7) . -3_655 N P1 O1 1.470(6) . 1_555 N P1 O2 1.481(5) . 1_555 N P1 O3 1.508(10) . 1_555 N P1 C1 1.880(8) . 1_555 N P4 O4 1.506(8) . 1_555 N P4 O5 1.463(7) . 1_555 N P4 O6 1.483(9) . 1_555 N P4 C4 1.887(8) . 1_555 N O1 Y1 2.261(9) . 1_555 N O1 P1 1.470(6) . 1_555 N O2 Y2 2.316(7) . 1_555 N O2 P1 1.481(5) . 1_555 N O3 P1 1.508(10) . 1_555 N O4 Y1 2.376(8) . -1_666 N O4 P4 1.506(8) . 1_555 N O5 Y2 2.354(7) . -1_665 N O5 P4 1.463(7) . 1_555 N C1 P1 1.880(8) . 1_555 N C1 N1 1.487(6) . 1_555 N O6 P4 1.483(9) . 1_555 N N1 C1 1.487(6) . 1_555 N N1 C2 1.497(13) . 1_555 N N1 C6 1.454(10) . 1_555 N C2 N1 1.497(13) . 1_555 N C2 C3 1.462(13) . 1_555 N C2 C7 1.494(10) . 1_555 N C6 N1 1.454(10) . 1_555 N C6 C5 1.453(9) . 1_555 N C3 C2 1.462(13) . 1_555 N C3 C8 1.479(9) . 1_555 N C3 N4 1.477(13) . 1_555 N C8 C3 1.479(9) . 1_555 N C5 C6 1.453(9) . 1_555 N C5 N4 1.462(12) . 1_555 N O101 O101 2.08(5) . -1_555 N C4 P4 1.887(8) . 1_555 N C4 N4 1.494(8) . 1_555 N O103 C7 1.820(22) . -3_555 N C7 C2 1.494(10) . 1_555 N C7 O103 1.820(22) . -2_555 N N4 C3 1.477(13) . 1_555 N N4 C5 1.462(12) . 1_555 N N4 C4 1.494(8) . 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 Y1 O1 88.4(4) 1_555 . 2_655 N O1 Y1 O1 88.4(4) 1_555 . 3_665 N O1 Y1 O4 89.8(4) 1_555 . -1_666 N O1 Y1 O4 89.6(4) 1_555 . -2_556 N O1 Y1 O4 177.4(4) 1_555 . -3_656 N O1 Y1 O1 88.4(4) 2_655 . 3_665 N O1 Y1 O4 177.3(4) 2_655 . -1_666 N O1 Y1 O4 89.8(4) 2_655 . -2_556 N O1 Y1 O4 89.6(4) 2_655 . -3_656 N O1 Y1 O4 89.6(4) 3_665 . -1_666 N O1 Y1 O4 177.3(4) 3_665 . -2_556 N O1 Y1 O4 89.8(4) 3_665 . -3_656 N O4 Y1 O4 92.1(4) -1_666 . -2_556 N O4 Y1 O4 92.2(4) -1_666 . -3_656 N O4 Y1 O4 92.2(4) -2_556 . -3_656 N O2 Y2 O2 86.0(4) 1_555 . 2_655 N O2 Y2 O2 86.0(4) 1_555 . 3_665 N O2 Y2 O5 83.37(26) 1_555 . -1_665 N O2 Y2 O5 96.00(30) 1_555 . -2_555 N O2 Y2 O5 169.06(30) 1_555 . -3_655 N O2 Y2 O2 86.0(4) 2_655 . 3_665 N O2 Y2 O5 169.00(30) 2_655 . -1_665 N O2 Y2 O5 83.38(26) 2_655 . -2_555 N O2 Y2 O5 96.05(30) 2_655 . -3_655 N O2 Y2 O5 96.03(30) 3_665 . -1_665 N O2 Y2 O5 169.06(30) 3_665 . -2_555 N O2 Y2 O5 83.42(26) 3_665 . -3_655 N O5 Y2 O5 94.88(33) -1_665 . -2_555 N O5 Y2 O5 94.92(33) -1_665 . -3_655 N O5 Y2 O5 94.91(33) -2_555 . -3_655 N O1 P1 O2 108.1(6) 1_555 . 1_555 N O1 P1 O3 109.6(7) 1_555 . 1_555 N O1 P1 C1 107.6(8) 1_555 . 1_555 N O2 P1 O3 110.7(7) 1_555 . 1_555 N O2 P1 C1 107.9(5) 1_555 . 1_555 N O3 P1 C1 112.8(7) 1_555 . 1_555 N O4 P4 O5 109.4(7) 1_555 . 1_555 N O4 P4 O6 111.0(6) 1_555 . 1_555 N O4 P4 C4 107.5(7) 1_555 . 1_555 N O5 P4 O6 112.0(6) 1_555 . 1_555 N O5 P4 C4 110.7(6) 1_555 . 1_555 N O6 P4 C4 106.1(8) 1_555 . 1_555 N Y1 O1 P1 143.1(7) 1_555 . 1_555 N Y2 O2 P1 155.6(6) 1_555 . 1_555 N Y1 O4 P4 142.5(6) -1_666 . 1_555 N Y2 O5 P4 152.2(6) -1_665 . 1_555 N P1 C1 N1 119.0(8) 1_555 . 1_555 N C1 N1 C2 110.1(10) 1_555 . 1_555 N C1 N1 C6 114.8(9) 1_555 . 1_555 N C2 N1 C6 115.7(9) 1_555 . 1_555 N N1 C2 C3 110.8(8) 1_555 . 1_555 N N1 C2 C7 106.1(9) 1_555 . 1_555 N C3 C2 C7 110.0(16) 1_555 . 1_555 N N1 C6 C5 115.6(8) 1_555 . 1_555 N C2 C3 C8 111.7(14) 1_555 . 1_555 N C2 C3 N4 112.3(9) 1_555 . 1_555 N C8 C3 N4 108.0(9) 1_555 . 1_555 N C6 C5 N4 116.8(8) 1_555 . 1_555 N P4 C4 N4 119.3(10) 1_555 . 1_555 N C3 N4 C5 115.6(8) 1_555 . 1_555 N C3 N4 C4 113.2(10) 1_555 . 1_555 N C5 N4 C4 116.1(10) 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 100 _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type 'ID31, ESRF' _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 Y 4.0 0.000 0.000 17.7760 1.40290 10.2946 12.8006 5.72629 0.12560 3.26588 104.354 1.91213 International_Tables_Vol_C P 12.0 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 51.5 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 42.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C N 12.0 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 _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 0.95 _diffrn_radiation_wavelength 0.800178 _diffrn_radiation_type synchrotron _pd_proc_ls_prof_R_factor 0.0409 _pd_proc_ls_prof_wR_factor 0.0523 _pd_proc_ls_prof_wR_expected 0.0256 _refine_ls_R_Fsqd_factor 0.04521 _pd_proc_ls_background_function ; GSAS Background function number 7 with 36 terms. Linear interpolation 1: 1984.59 2: 1872.62 3: 1366.28 4: 1222.75 5: 1080.07 6: 1031.29 7: 1066.03 8: 1221.17 9: 1450.49 10: 1554.57 11: 1379.40 12: 1114.25 13: 933.410 14: 794.499 15: 681.719 16: 578.365 17: 578.990 18: 512.592 19: 475.685 20: 466.528 21: 479.849 22: 456.979 23: 464.517 24: 473.970 25: 444.109 26: 426.630 27: 424.906 28: 463.004 29: 457.295 30: 472.870 31: 465.664 32: 459.435 33: 448.412 34: 424.120 35: 418.383 36: 440.601 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 No correction is applied. ; _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_correction_T_max 1.00000 # Extinction correction _gsas_exptl_extinct_corr_T_min 1.00000 _gsas_exptl_extinct_corr_T_max 1.00000 _pd_proc_ls_profile_function ; CW Profile function number 3 with 19 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. #1(GU) = 73.518 #2(GV) = 4.756 #3(GW) = -1.881 #4(GP) = 0.590 #5(LX) = 2.777 #6(LY) = 76.303 #7(S/L) = 0.0021 #8(H/L) = 0.0026 #9(trns) = -4.07 #10(shft)= -0.5645 #11(stec)= -38.34 #12(ptec)= -0.53 #13(sfec)= 0.00 #14(L11) = -0.174 #15(L22) = -0.230 #16(L33) = -0.153 #17(L12) = -0.105 #18(L13) = 0.003 #19(L23) = -0.043 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_peak_cutoff 0.00500 _pd_proc_info_datetime 2010-03-08T14:00:52 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 0.003 _pd_meas_2theta_range_max 42.969 _pd_meas_2theta_range_inc 0.003 _pd_proc_2theta_range_min 0.005793 _pd_proc_2theta_range_max 42.97179 _pd_proc_2theta_range_inc 0.003 _pd_meas_number_of_points 14323 _pd_proc_number_of_points 14323 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 0 o 35024.152 34865.172 180.00 14.02048 100.00 0 0 1 o 1158.819 1964.430 180.00 10.00355 0.56 1 0 1 o 27.519 13.918 0.00 8.14327 0.03 1 0 -1 o 33.312 16.930 180.00 8.14327 0.03 1 1 0 o 23794.631 23630.580 0.00 8.09473 22.66 2 0 0 o 1127.105 1156.843 180.00 7.01024 0.81 1 1 -1 o 671.342 618.736 180.00 6.29263 0.39 1 1 1 o 8276.164 7646.827 0.00 6.29263 4.76 2 0 -1 o 11122.428 11287.743 0.00 5.74092 5.33 2 0 1 o 2279.630 2313.562 0.00 5.74092 1.09 2 1 0 o 2044.136 1769.806 180.00 5.29924 0.83 3 -1 0 o 2727.807 2354.805 180.00 5.29924 1.11 0 0 2 o 733.973 1458.592 0.00 5.00178 0.09 3 -1 1 o 14538.380 14576.891 180.00 4.68278 4.64 3 0 0 o 31607.535 31598.600 0.00 4.67349 10.05 1 0 2 o 3888.905 3860.842 0.00 4.71097 1.26 1 0 -2 o 617.717 613.143 180.00 4.71097 0.20 2 1 -1 o 44.597 44.821 0.00 4.68278 0.01 3 -1 -1 o 10837.963 10892.396 180.00 4.68278 3.46 2 1 1 o 4785.390 4807.188 180.00 4.68278 1.53 3 0 1 o 3024.057 2458.476 0.00 4.23420 0.79 3 0 -1 o 4722.230 3840.884 180.00 4.23420 1.23 1 1 2 o 6358.003 5756.710 180.00 4.25501 1.68 1 1 -2 o 591.787 529.880 180.00 4.25501 0.16 2 2 0 o 4.199 4.466 0.00 4.04736 0.00 2 0 2 o 25792.779 27233.314 0.00 4.07163 6.23 2 0 -2 o 3934.342 4152.329 180.00 4.07163 0.95 3 1 0 o 2601.142 1729.730 180.00 3.88858 0.57 4 -1 0 o 1566.119 1040.359 180.00 3.88858 0.34 2 2 -1 o 1646.708 1720.637 0.00 3.75191 0.34 2 2 1 o 4014.804 4237.976 180.00 3.75191 0.82 3 -1 2 o 965.001 944.392 180.00 3.63741 0.19 3 1 1 o 2559.949 2570.614 0.00 3.62438 0.49 3 1 -1 o 203.549 204.422 180.00 3.62438 0.04 4 -1 1 o 13935.443 13999.147 0.00 3.62438 2.67 4 -1 -1 o 58499.80 58754.74 0.00 3.62438 11.20 2 1 2 o 1233.913 1206.312 180.00 3.63741 0.24 2 1 -2 o 60338.56 59044.41 0.00 3.63741 11.64 3 -1 -2 o 45261.30 44266.22 0.00 3.63741 8.73 4 0 0 o 87.561 97.564 0.00 3.50512 0.02 3 0 -2 o 45199.35 44745.26 180.00 3.41482 7.69 3 0 2 o 35856.59 35487.86 180.00 3.41482 6.10 4 0 -1 o 3784.174 3590.792 180.00 3.30794 0.60 4 0 1 o 11918.099 11317.104 180.00 3.30794 1.90 0 0 3 o 72.575 70.489 0.00 3.33452 0.00 3 2 0 o 2361.997 2872.535 180.00 3.21652 0.36 5 -2 0 o 810.003 989.464 180.00 3.21652 0.12 1 0 3 o 439.943 729.089 0.00 3.24403 0.07 1 0 -3 o 50.425 83.710 0.00 3.24403 0.01 2 2 -2 o 20238.660 20209.197 180.00 3.14631 2.92 2 2 2 o 23687.758 23625.691 180.00 3.14631 3.42 5 -2 1 o 4612.847 4599.967 180.00 3.06212 0.63 5 -1 0 o 1213.602 1214.685 0.00 3.05952 0.17 4 1 0 o 21819.662 21857.322 0.00 3.05952 2.98 1 1 -3 o 1344.065 1226.072 0.00 3.08317 0.19 4 -1 2 o 21212.432 20404.320 0.00 3.06996 2.92 3 1 -2 o 541.911 521.007 0.00 3.06996 0.07 4 -1 -2 o 577.885 555.501 180.00 3.06996 0.08 3 1 2 o 9066.211 8712.701 0.00 3.06996 1.25 5 -2 -1 o 4355.544 4343.075 180.00 3.06212 0.60 3 2 1 o 6387.368 6379.740 0.00 3.06212 0.87 3 2 -1 o 8569.475 8550.613 0.00 3.06212 1.17 1 1 3 o 4.647 4.213 180.00 3.08317 0.00 2 0 3 o 653.855 632.519 180.00 3.01122 0.09 2 0 -3 o 5511.736 5325.287 0.00 3.01122 0.73 5 -1 1 o 9154.482 7690.631 0.00 2.92574 1.14 4 1 1 o 83.636 69.286 180.00 2.92574 0.01 5 -1 -1 o 972.112 811.378 180.00 2.92574 0.12 4 1 -1 o 520.576 432.772 180.00 2.92574 0.07 4 0 2 o 484.142 1099.027 180.00 2.87046 0.06 4 0 -2 o 100.084 227.268 180.00 2.87046 0.01 5 0 0 o 422.692 290.973 180.00 2.80410 0.05 3 -1 3 o 13868.398 12691.463 180.00 2.82227 1.61 3 -1 -3 o 2998.252 2744.392 180.00 2.82227 0.35 2 1 -3 o 1031.878 944.379 180.00 2.82227 0.12 2 1 3 o 0.590 0.540 180.00 2.82227 0.00 5 -2 2 o 929.416 939.227 180.00 2.70540 0.10 5 0 1 o 4319.230 4353.925 0.00 2.70003 0.46 5 0 -1 o 14557.506 14675.014 0.00 2.70003 1.55 3 3 0 o 10055.015 10121.376 0.00 2.69824 1.07 3 0 3 o 2239.035 2271.260 0.00 2.71442 0.24 3 0 -3 o 7481.695 7590.734 180.00 2.71442 0.81 3 2 2 o 1176.544 1191.249 180.00 2.70540 0.13 5 -2 -2 o 59444.09 60208.57 0.00 2.70540 6.36 3 2 -2 o 1515.895 1535.520 0.00 2.70540 0.16 6 -2 0 o 292.131 341.075 0.00 2.64962 0.03 4 2 0 o 7793.728 9201.680 180.00 2.64962 0.80 5 -1 2 o 14750.579 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9 -4 -3 o 842.427 870.519 180.00 1.58064 0.03 5 4 -3 o 2081.438 2150.092 180.00 1.58064 0.08 9 -4 3 o 371.529 381.772 180.00 1.58064 0.01 2 1 6 o 12339.687 12543.009 180.00 1.59040 0.46 2 1 -6 o 7897.185 8024.378 0.00 1.59040 0.30 3 -1 -6 o 3043.947 3094.097 0.00 1.59040 0.11 3 -1 6 o 15698.017 15948.342 180.00 1.59040 0.59 4 4 -4 o 30.300 28.303 180.00 1.57316 0.00 5 4 3 o 788.746 819.243 0.00 1.58064 0.03 10 -3 1 o 1298.363 1322.211 0.00 1.55817 0.05 7 3 -1 o 550.833 562.182 180.00 1.55817 0.02 10 -3 -1 o 2818.137 2871.934 0.00 1.55817 0.10 9 0 0 o 7929.906 8078.924 0.00 1.55783 0.29 6 -1 5 o 636.210 581.567 0.00 1.56647 0.02 8 -3 4 o 13174.616 12617.121 180.00 1.56335 0.48 7 0 4 o 3320.906 3177.626 0.00 1.56335 0.12 7 0 -4 o 798.675 764.054 180.00 1.56335 0.03 5 3 -4 o 5884.796 5629.845 0.00 1.56335 0.21 4 4 4 o 1291.886 1202.390 0.00 1.57316 0.05 9 -3 -3 o 9.495 9.464 0.00 1.56093 0.00 9 -3 3 o 855.959 851.707 0.00 1.56093 0.03 6 3 3 o 1964.965 1961.436 0.00 1.56093 0.07 6 3 -3 o 418.484 417.133 0.00 1.56093 0.02 3 0 6 o 25.255 22.493 0.00 1.57032 0.00 3 0 -6 o 2285.977 2034.347 0.00 1.57032 0.08 9 -1 2 o 323.818 328.252 180.00 1.55920 0.01 9 -1 -2 o 17646.180 17900.277 0.00 1.55920 0.64 8 1 2 o 47.382 48.089 0.00 1.55920 0.00 8 1 -2 o 14310.322 14521.072 0.00 1.55920 0.52 7 3 1 o 1766.509 1804.320 180.00 1.55817 0.06 5 1 5 o 295.411 269.356 180.00 1.56647 0.01 5 1 -5 o 397.027 362.420 0.00 1.56647 0.01 6 -1 -5 o 686.935 626.441 180.00 1.56647 0.03 8 -3 -4 o 8865.335 8479.021 0.00 1.56335 0.32 5 3 4 o 16995.350 16241.804 180.00 1.56335 0.62 8 0 -3 o 117.683 121.227 0.00 1.55134 0.00 8 0 3 o 731.875 753.730 180.00 1.55134 0.03 9 0 1 o 375.240 383.035 0.00 1.53928 0.01 9 0 -1 o 185.724 189.588 180.00 1.53928 0.01 10 -4 2 o 13261.654 13736.882 0.00 1.53106 0.46 2 2 -6 o 2986.198 3059.417 0.00 1.54158 0.11 8 2 0 o 18878.043 19534.537 0.00 1.52976 0.66 10 -2 0 o 14448.123 14936.479 0.00 1.52976 0.50 5 5 -2 o 19863.320 20340.016 180.00 1.54027 0.70 5 5 2 o 12045.153 12351.066 180.00 1.54027 0.42 8 -2 -4 o 10369.386 10557.775 180.00 1.53498 0.36 8 -2 4 o 1541.076 1570.185 0.00 1.53498 0.05 6 2 -4 o 6841.756 6967.351 180.00 1.53498 0.24 4 -1 6 o 1277.375 1320.847 0.00 1.53235 0.04 2 2 6 o 2753.042 2826.073 0.00 1.54158 0.10 6 4 2 o 11249.924 11692.563 0.00 1.53106 0.39 6 4 -2 o 7.304 7.582 180.00 1.53106 0.00 10 -4 -2 o 1764.109 1829.594 180.00 1.53106 0.06 6 2 4 o 2233.885 2274.120 0.00 1.53498 0.08 7 2 -3 o 3006.424 3099.017 0.00 1.52361 0.10 9 -2 -3 o 372.796 384.260 180.00 1.52361 0.01 9 -2 3 o 1188.428 1223.962 0.00 1.52361 0.04 7 2 3 o 763.389 787.274 180.00 1.52361 0.03 10 -2 1 o 2326.157 2266.906 180.00 1.51218 0.08 8 2 -1 o 9.586 9.335 0.00 1.51218 0.00 8 2 1 o 763.008 742.913 0.00 1.51218 0.03 10 -2 -1 o 27.325 26.622 0.00 1.51218 0.00 3 1 6 o 962.345 996.101 0.00 1.53235 0.03 3 1 -6 o 11224.223 11611.479 180.00 1.53235 0.39 4 -1 -6 o 24130.201 24976.471 180.00 1.53235 0.84 6 0 5 o 364.137 369.523 180.00 1.51976 0.01 6 0 -5 o 554.223 562.714 0.00 1.51976 0.02 10 -3 2 o 819.450 836.221 180.00 1.50439 0.03 7 -3 5 o 54.037 53.037 180.00 1.51091 0.00 4 3 -5 o 764.042 749.990 0.00 1.51091 0.03 4 0 6 o 2922.319 2952.094 180.00 1.50561 0.10 7 3 2 o 19.764 20.219 180.00 1.50439 0.00 10 -3 -2 o 4562.791 4660.802 0.00 1.50439 0.15 7 3 -2 o 12888.540 13174.429 0.00 1.50439 0.43 4 3 5 o 1479.688 1452.932 180.00 1.51091 0.05 7 -3 -5 o 605.528 594.436 180.00 1.51091 0.02 9 0 2 o 6196.486 5937.747 180.00 1.48736 0.20 4 0 -6 o 5750.106 5810.050 0.00 1.50561 0.19 7 -2 5 o 6083.715 6255.957 180.00 1.49367 0.20 5 2 -5 o 300.094 309.084 180.00 1.49367 0.01 11 -5 0 o 32.296 28.159 180.00 1.46975 0.00 8 -1 -4 o 698.806 701.380 0.00 1.49095 0.02 8 -1 4 o 281.999 282.764 180.00 1.49095 0.01 7 1 -4 o 126.873 127.319 0.00 1.49095 0.00 7 1 4 o 460.881 462.661 0.00 1.49095 0.02 9 0 -2 o 7116.376 6819.837 180.00 1.48736 0.23 5 2 5 o 2967.079 3061.908 180.00 1.49367 0.10 7 -2 -5 o 6205.336 6399.221 0.00 1.49367 0.21 5 -2 6 o 15839.371 14336.399 180.00 1.48022 0.52 3 2 -6 o 4638.341 4194.758 0.00 1.48022 0.15 6 5 0 o 1545.382 1336.073 180.00 1.46975 0.05 10 -1 0 o 3523.365 3068.178 180.00 1.46975 0.11 9 1 0 o 700.447 608.922 180.00 1.46975 0.02 11 -4 0 o 3040.001 3204.249 0.00 1.45386 0.10 10 -2 -2 o 4332.864 4253.417 180.00 1.46287 0.14 10 -2 2 o 766.467 751.838 180.00 1.46287 0.02 9 -1 3 o 3569.502 3018.371 0.00 1.47234 0.12 8 1 3 o 1475.076 1242.834 180.00 1.47234 0.05 9 -1 -3 o 56.466 47.623 0.00 1.47234 0.00 8 1 -3 o 374.207 315.532 180.00 1.47234 0.01 3 2 6 o 1536.424 1386.519 180.00 1.48022 0.05 5 -2 -6 o 5944.744 5366.521 0.00 1.48022 0.19 6 5 -1 o 2165.891 2294.406 0.00 1.45413 0.07 9 1 1 o 149.750 158.325 180.00 1.45413 0.00 11 -5 -1 o 168.933 178.514 180.00 1.45413 0.01 10 -1 1 o 238.220 251.622 180.00 1.45413 0.01 10 -1 -1 o 33.694 35.600 0.00 1.45413 0.00 11 -5 1 o 5638.556 5951.944 180.00 1.45413 0.18 9 1 -1 o 6188.262 6542.125 0.00 1.45413 0.19 4 1 -6 o 5.558 5.403 0.00 1.46399 0.00 5 -1 6 o 3807.260 3698.881 0.00 1.46399 0.12 7 4 0 o 13019.814 13765.865 0.00 1.45386 0.41 8 2 -2 o 9286.674 9121.250 180.00 1.46287 0.30 8 2 2 o 9335.881 9173.698 180.00 1.46287 0.30 6 1 -5 o 77.724 78.015 180.00 1.46087 0.00 7 -1 -5 o 2041.528 2049.845 180.00 1.46087 0.06 7 -1 5 o 3692.694 3704.149 0.00 1.46087 0.12 6 1 5 o 2.121 2.130 180.00 1.46087 0.00 10 -4 3 o 1346.585 1436.370 180.00 1.44858 0.04 9 -4 4 o 4472.031 4557.646 0.00 1.45834 0.14 9 -4 -4 o 10917.001 11126.646 180.00 1.45834 0.35 5 4 -4 o 6133.056 6251.141 180.00 1.45834 0.19 5 5 3 o 336.347 351.422 180.00 1.45637 0.01 5 5 -3 o 9282.264 9678.496 0.00 1.45637 0.29 5 -1 -6 o 1951.228 1898.206 0.00 1.46399 0.06 4 1 6 o 245.121 238.463 180.00 1.46399 0.01 6 5 1 o 492.340 522.095 0.00 1.45413 0.02 5 4 4 o 866.185 882.467 0.00 1.45834 0.03 6 4 3 o 875.941 935.332 180.00 1.44858 0.03 10 -4 -3 o 2545.037 2716.581 0.00 1.44858 0.08 6 4 -3 o 1143.633 1220.758 180.00 1.44858 0.04 11 -4 -1 o 3250.703 3679.732 180.00 1.43874 0.10 11 -4 1 o 4.901 5.542 0.00 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180.00 1.32481 0.07 4 -1 -7 o 131.944 120.633 180.00 1.34136 0.00 4 -1 7 o 14278.201 13084.581 180.00 1.34136 0.38 3 1 7 o 2355.582 2153.767 180.00 1.34136 0.06 3 1 -7 o 747.260 684.242 0.00 1.34136 0.02 7 4 -3 o 1009.956 1077.318 0.00 1.33269 0.03 11 -4 3 o 4236.465 4511.149 0.00 1.33269 0.11 11 -4 -3 o 4772.115 5089.046 180.00 1.33269 0.13 11 -2 2 o 1363.223 1492.801 0.00 1.33162 0.04 9 2 2 o 2808.625 3083.042 180.00 1.33162 0.07 9 2 -2 o 11897.669 13052.987 0.00 1.33162 0.32 11 -2 -2 o 305.168 334.530 0.00 1.33162 0.01 12 -5 -1 o 277.231 308.018 0.00 1.33098 0.01 7 5 -1 o 173.876 193.891 180.00 1.33098 0.00 7 5 1 o 757.354 845.511 0.00 1.33098 0.02 5 2 -6 o 691.120 635.807 0.00 1.33853 0.02 7 -2 -6 o 619.636 568.332 0.00 1.33853 0.02 7 -2 6 o 3915.157 3612.137 0.00 1.33853 0.11 5 2 6 o 78.527 71.949 0.00 1.33853 0.00 11 -1 1 o 422.042 473.419 0.00 1.31914 0.01 5 4 -5 o 2.189 2.114 0.00 1.33614 0.00 9 -4 -5 o 9.968 9.608 180.00 1.33614 0.00 5 4 5 o 738.815 710.777 0.00 1.33614 0.02 7 3 -4 o 583.540 595.655 180.00 1.33420 0.02 10 -3 -4 o 8726.897 8907.963 180.00 1.33420 0.23 7 3 4 o 2061.965 2104.656 0.00 1.33420 0.05 7 4 3 o 316.166 337.451 0.00 1.33269 0.01 9 -3 5 o 70.960 82.721 180.00 1.32417 0.00 12 -4 1 o 352.806 377.640 0.00 1.31334 0.01 12 -4 -1 o 1759.487 1886.959 0.00 1.31334 0.05 10 1 1 o 463.302 520.179 180.00 1.31914 0.01 11 -1 -1 o 119.287 133.873 0.00 1.31914 0.00 10 1 -1 o 0.002 0.003 0.00 1.31914 0.00 6 3 5 o 399.909 468.541 180.00 1.32417 0.01 9 -3 -5 o 16.011 18.739 180.00 1.32417 0.00 6 3 -5 o 701.435 820.161 180.00 1.32417 0.02 4 0 -7 o 577.603 666.794 0.00 1.32332 0.02 4 0 7 o 2008.380 2318.296 0.00 1.32332 0.05 9 0 -4 o 3181.856 3636.545 0.00 1.32228 0.08 9 0 4 o 812.734 928.680 180.00 1.32228 0.02 8 4 1 o 61.066 65.981 180.00 1.31334 0.00 8 4 -1 o 2560.685 2762.442 0.00 1.31334 0.07 8 0 -5 o 4680.701 5298.902 180.00 1.31830 0.12 8 0 5 o 21.861 24.739 0.00 1.31830 0.00 11 -3 3 o 1.285 1.163 180.00 1.30924 0.00 11 -3 -3 o 2368.538 2134.489 0.00 1.30924 0.06 8 3 -3 o 11.989 10.792 180.00 1.30924 0.00 7 -1 6 o 1960.837 2228.416 0.00 1.31477 0.05 6 1 6 o 1294.086 1478.724 0.00 1.31477 0.03 6 1 -6 o 4891.332 5576.742 180.00 1.31477 0.13 7 -1 -6 o 10284.903 11751.756 180.00 1.31477 0.27 10 -2 4 o 2609.315 2245.425 0.00 1.30498 0.07 12 -3 0 o 16079.136 15047.941 0.00 1.29619 0.41 9 3 0 o 5571.847 5213.225 0.00 1.29619 0.14 6 6 -2 o 6558.500 5750.152 180.00 1.30257 0.17 8 3 3 o 1520.807 1364.474 0.00 1.30924 0.04 9 -2 5 o 1253.236 1111.715 0.00 1.30116 0.03 3 2 7 o 63.906 53.803 0.00 1.30598 0.00 5 -2 7 o 2332.302 1979.937 0.00 1.30598 0.06 5 -2 -7 o 1296.086 1091.935 0.00 1.30598 0.03 3 2 -7 o 564.004 477.648 180.00 1.30598 0.01 8 2 -4 o 129.135 110.819 180.00 1.30498 0.00 8 2 4 o 22.200 19.016 180.00 1.30498 0.00 10 -2 -4 o 1089.771 934.966 0.00 1.30498 0.03 12 -5 -2 o 1975.645 1838.565 0.00 1.29698 0.05 12 -5 2 o 22172.523 20635.246 0.00 1.29698 0.56 7 5 -2 o 284.911 265.154 180.00 1.29698 0.01 7 5 2 o 4157.828 3870.019 0.00 1.29698 0.10 6 6 2 o 2323.213 2031.818 180.00 1.30257 0.06 12 -3 1 o 1.880 1.993 180.00 1.28545 0.00 12 -3 -1 o 1249.651 1325.721 0.00 1.28545 0.03 7 2 5 o 1155.031 1021.300 180.00 1.30116 0.03 9 -2 -5 o 1339.974 1185.679 180.00 1.30116 0.03 7 2 -5 o 831.051 735.845 0.00 1.30116 0.02 10 0 3 o 1859.694 1756.894 180.00 1.29245 0.05 10 0 -3 o 33.653 31.781 180.00 1.29245 0.00 5 -1 7 o 32.729 30.683 0.00 1.29480 0.00 4 1 -7 o 1756.712 1646.724 180.00 1.29480 0.04 5 -1 -7 o 820.908 769.420 180.00 1.29480 0.02 4 1 7 o 0.037 0.035 180.00 1.29480 0.00 10 1 2 o 3528.736 3694.611 180.00 1.28603 0.09 10 1 -2 o 10127.073 10602.793 180.00 1.28603 0.25 11 -1 -2 o 1264.972 1324.247 180.00 1.28603 0.03 11 -1 2 o 92.489 96.805 180.00 1.28603 0.00 9 3 -1 o 679.175 721.117 180.00 1.28545 0.02 9 3 1 o 252.345 268.014 0.00 1.28545 0.01 11 0 0 o 368.493 359.180 180.00 1.27459 0.01 8 -3 6 o 8419.619 9744.637 0.00 1.28140 0.21 8 4 -2 o 3017.797 3429.552 0.00 1.28065 0.07 12 -4 2 o 416.815 468.835 180.00 1.28065 0.01 12 -4 -2 o 2281.617 2580.206 0.00 1.28065 0.06 8 4 2 o 13.329 15.213 0.00 1.28065 0.00 4 4 -6 o 551.998 566.883 180.00 1.28679 0.01 4 4 6 o 55.767 57.143 0.00 1.28679 0.00 9 2 -3 o 379.133 375.594 0.00 1.27628 0.01 11 -2 3 o 176.423 175.166 0.00 1.27628 0.00 9 2 3 o 174.354 172.566 180.00 1.27628 0.00 11 -2 -3 o 521.960 517.328 180.00 1.27628 0.01 7 0 6 o 9919.887 11574.064 180.00 1.28140 0.24 7 0 -6 o 4369.497 5109.138 0.00 1.28140 0.11 5 3 -6 o 3734.201 4355.165 180.00 1.28140 0.09 5 3 6 o 961.743 1136.028 0.00 1.28140 0.02 8 -3 -6 o 1756.154 2065.102 180.00 1.28140 0.04 11 0 1 o 790.887 814.509 0.00 1.26437 0.02 11 0 -1 o 24.777 25.520 180.00 1.26437 0.00 9 -1 5 o 1105.784 1200.479 180.00 1.26879 0.03 12 -2 0 o 9999.209 9792.541 180.00 1.25908 0.24 10 2 0 o 95.124 93.224 0.00 1.25908 0.00 11 -5 4 o 891.705 973.462 0.00 1.26713 0.02 9 1 4 o 289.814 319.398 180.00 1.26713 0.01 9 1 -4 o 1777.853 1957.583 180.00 1.26713 0.04 10 -1 4 o 8808.137 9664.049 180.00 1.26713 0.21 10 -1 -4 o 4475.346 4928.318 0.00 1.26713 0.11 5 0 7 o 2881.796 2712.265 180.00 1.27326 0.07 5 0 -7 o 286.841 269.590 0.00 1.27326 0.01 12 -3 2 o 102.551 94.296 0.00 1.25475 0.00 9 -1 -5 o 337.945 368.772 180.00 1.26879 0.01 8 1 -5 o 4803.064 5236.977 0.00 1.26879 0.12 8 1 5 o 1109.605 1211.229 180.00 1.26879 0.03 6 5 -4 o 2363.213 2610.850 180.00 1.26713 0.06 6 5 4 o 197.392 220.510 0.00 1.26713 0.00 11 -5 -4 o 1362.971 1508.435 180.00 1.26713 0.03 8 -2 6 o 21054.609 22703.582 180.00 1.26564 0.51 8 -2 -6 o 1946.860 2112.469 0.00 1.26564 0.05 6 2 6 o 952.221 1034.556 180.00 1.26564 0.02 6 2 -6 o 1881.544 2035.949 0.00 1.26564 0.05 12 -2 -1 o 1090.429 975.396 0.00 1.24922 0.03 10 2 -1 o 670.639 599.414 180.00 1.24922 0.02 12 -2 1 o 431.889 386.450 180.00 1.24922 0.01 10 2 1 o 40.911 36.560 180.00 1.24922 0.00 7 4 -4 o 501.392 494.644 0.00 1.25690 0.01 11 -4 -4 o 295.541 291.755 180.00 1.25690 0.01 11 -4 4 o 3101.555 3040.642 0.00 1.25690 0.07 3 3 7 o 450.960 443.381 180.00 1.26289 0.01 3 3 -7 o 717.454 708.596 180.00 1.26289 0.02 9 3 -2 o 2347.087 2152.878 180.00 1.25475 0.06 12 -3 -2 o 102.767 94.375 180.00 1.25475 0.00 9 3 2 o 2344.481 2148.622 180.00 1.25475 0.06 10 -4 5 o 471.902 418.519 180.00 1.25349 0.01 13 -6 0 o 1180.873 1069.019 180.00 1.24412 0.03 7 6 0 o 1573.649 1418.197 180.00 1.24412 0.04 5 5 -5 o 1291.835 1283.879 0.00 1.25853 0.03 5 5 5 o 5575.167 5578.939 180.00 1.25853 0.13 6 6 -3 o 6928.158 6105.114 0.00 1.25064 0.16 6 -2 7 o 768.450 766.628 0.00 1.25779 0.02 4 2 7 o 1176.243 1183.110 0.00 1.25779 0.03 6 -2 -7 o 979.651 984.520 0.00 1.25779 0.02 4 2 -7 o 18.200 18.206 0.00 1.25779 0.00 7 4 4 o 924.695 918.026 0.00 1.25690 0.02 10 -4 -5 o 86.246 75.737 0.00 1.25349 0.00 6 4 5 o 66.682 58.278 0.00 1.25349 0.00 6 4 -5 o 127.091 111.951 180.00 1.25349 0.00 12 -5 3 o 1692.938 1525.278 180.00 1.24569 0.04 7 5 -3 o 1538.648 1383.963 180.00 1.24569 0.04 12 -5 -3 o 116.546 104.862 180.00 1.24569 0.00 6 6 3 o 3178.107 2788.646 180.00 1.25064 0.07 0 0 8 o 45921.06 40319.53 180.00 1.25044 0.36 13 -6 -1 o 1275.981 1325.948 0.00 1.23460 0.03 13 -6 1 o 864.493 897.430 0.00 1.23460 0.02 13 -5 0 o 949.039 983.331 0.00 1.23443 0.02 8 5 0 o 15270.004 15870.742 0.00 1.23443 0.35 10 -3 5 o 1335.262 1344.599 180.00 1.23872 0.03 7 5 3 o 59.050 53.019 180.00 1.24569 0.00 1 0 -8 o 1738.840 1558.647 0.00 1.24550 0.04 1 0 8 o 21906.494 19637.090 0.00 1.24550 0.51 11 -3 -4 o 13711.620 14223.534 0.00 1.23717 0.32 11 -3 4 o 24257.238 25054.703 180.00 1.23717 0.56 8 3 -4 o 171.925 178.313 0.00 1.23717 0.00 10 1 3 o 176.659 183.959 0.00 1.23597 0.00 11 -1 -3 o 160.183 166.726 180.00 1.23597 0.00 10 1 -3 o 1260.584 1312.411 180.00 1.23597 0.03 11 -1 3 o 11.229 11.676 180.00 1.23597 0.00 5 1 -7 o 769.524 686.275 0.00 1.24288 0.02 6 -1 -7 o 0.096 0.086 0.00 1.24288 0.00 5 1 7 o 80.559 71.733 0.00 1.24288 0.00 6 -1 7 o 89.581 80.014 0.00 1.24288 0.00 11 0 -2 o 68.703 71.553 0.00 1.23512 0.00 11 0 2 o 4947.213 5151.173 0.00 1.23512 0.11 7 6 1 o 0.865 0.902 0.00 1.23460 0.00 7 6 -1 o 213.566 222.658 0.00 1.23460 0.00 8 -1 -6 o 2286.298 2147.686 0.00 1.24062 0.05 8 -1 6 o 2234.401 2101.772 0.00 1.24062 0.05 7 1 -6 o 986.196 926.840 0.00 1.24062 0.02 7 1 6 o 270.824 254.401 180.00 1.24062 0.01 7 3 -5 o 979.952 990.823 0.00 1.23872 0.02 10 -3 -5 o 3013.667 3051.952 0.00 1.23872 0.07 7 3 5 o 22.365 22.709 180.00 1.23872 0.00 8 4 -3 o 730.672 768.469 0.00 1.23120 0.02 12 -4 -3 o 831.861 874.397 0.00 1.23120 0.02 12 -4 3 o 816.377 856.489 180.00 1.23120 0.02 8 4 3 o 415.437 437.556 180.00 1.23120 0.01 8 3 4 o 4796.922 4989.388 180.00 1.23717 0.11 1 1 -8 o 8777.415 9192.080 180.00 1.23579 0.20 1 1 8 o 6477.703 6793.591 180.00 1.23579 0.15 2 0 8 o 125.392 132.690 180.00 1.23101 0.00 2 0 -8 o 6193.153 6554.828 0.00 1.23101 0.14 _reflns_number_total 861 _reflns_limit_h_min 0 _reflns_limit_h_max 13 _reflns_limit_k_min -6 _reflns_limit_k_max 6 _reflns_limit_l_min -8 _reflns_limit_l_max 8 _reflns_d_resolution_high 1.231 _reflns_d_resolution_low 14.020 # start Validation Reply Form _vrf_PLAT306_STA-13Y-AP_publ ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O101 RESPONSE: Solvent water molecule in pore; powder data, H-atoms cannot be found ; _vrf_PLAT040_STA-13Y-AP_publ ; PROBLEM: No H-atoms in this Carbon Containing Compound .. RESPONSE: Powder data: could not identify protons ; # end Validation Reply Form #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# # Attachment '- Structure-2(Deh).cif' data_STA-13(Y)-DH_publ _database_code_depnum_ccdc_archive 'CCDC 771872' #TrackingRef '- Structure-2(Deh).cif' _pd_block_id 2010-03-22T10:31|STA-13(Y)-DH||ID31 _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2010-03-22T10:31 _audit_author_name 'Michael T. Wharmby' _audit_update_record ; 2010-03-22T10:31 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 ? _pd_char_colour white # 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 61 _refine_ls_goodness_of_fit_all 3.38 _refine_ls_number_restraints 73 _refine_ls_matrix_type full _refine_diff_density_max 0.322 _refine_diff_density_min -0.289 #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C21 N6 O18 P6 Y2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall '-P 3' _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _cell_measurement_temperature 100 _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 'STA-13(Y) - Dehydrated' _cell_length_a 16.1352(4) _cell_length_b 16.1352 _cell_length_c 10.02957(22) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 2261.32(6) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P -3' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -y,x-y,+z 3 y-x,-x,+z -1 -x,-y,-z -2 +y,y-x,-z -3 x-y,+x,-z # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Y Y1 0.6667 0.3333 0.3030(4) 1.0 Uiso 0.02517(31) 2 Y Y2 0.6667 0.3333 -0.2174(4) 1.0 Uiso 0.02517(31) 2 P P1 0.6008(5) 0.4455(4) 0.0509(6) 1.0 Uiso 0.02517(31) 6 P P4 0.2087(4) 0.4692(4) 0.4636(7) 1.0 Uiso 0.02517(31) 6 O O1 0.6594(4) 0.4511(5) 0.1718(5) 1.0 Uiso 0.02517(31) 6 O O2 0.64115(32) 0.42619(35) -0.0673(5) 1.0 Uiso 0.02517(31) 6 O O3 0.6142(7) 0.5465(5) 0.0343(9) 1.0 Uiso 0.02517(31) 6 O O4 0.2174(5) 0.5378(5) 0.5709(7) 1.0 Uiso 0.02517(31) 6 O O5 0.2442(5) 0.5253(5) 0.3347(7) 1.0 Uiso 0.02517(31) 6 O O6 0.1017(5) 0.3997(6) 0.4455(9) 1.0 Uiso 0.02517(31) 6 N N1 0.4253(7) 0.3893(8) 0.1690(8) 1.0 Uiso 0.02517(31) 6 N N4 0.3370(7) 0.3858(7) 0.4146(7) 1.0 Uiso 0.02517(31) 6 C C1 0.47402(32) 0.3572(7) 0.0758(9) 1.0 Uiso 0.02517(31) 6 C C2 0.3365(7) 0.2999(7) 0.2192(10) 1.0 Uiso 0.02517(31) 6 C C3 0.2788(5) 0.3397(7) 0.2867(9) 1.0 Uiso 0.02517(31) 6 C C4 0.2738(9) 0.4074(8) 0.5017(9) 1.0 Uiso 0.02517(31) 6 C C5 0.4265(7) 0.4764(7) 0.3648(11) 1.0 Uiso 0.02517(31) 6 C C6 0.4831(5) 0.4423(8) 0.2899(12) 1.0 Uiso 0.02517(31) 6 C C7 0.2821(11) 0.2410(12) 0.1012(16) 0.25 Uiso 0.02517(31) 6 C C8 0.1836(6) 0.2599(10) 0.3268(17) 0.75 Uiso 0.02517(31) 6 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C21 N6 O18 P6 Y2' _chemical_formula_weight 987.91 _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 Y1 O1 2.362(7) . 1_555 N Y1 O1 2.361(7) . 2_655 N Y1 O1 2.361(7) . 3_665 N Y1 O4 2.352(6) . -1_666 N Y1 O4 2.353(6) . -2_556 N Y1 O4 2.352(6) . -3_656 N Y2 O2 2.302(4) . 1_555 N Y2 O2 2.301(4) . 2_655 N Y2 O2 2.301(4) . 3_665 N Y2 O5 2.318(6) . -1_665 N Y2 O5 2.319(6) . -2_555 N Y2 O5 2.317(6) . -3_655 N P1 O1 1.513(7) . 1_555 N P1 O2 1.459(5) . 1_555 N P1 O3 1.543(5) . 1_555 N P1 C1 1.833(7) . 1_555 N P4 O4 1.500(8) . 1_555 N P4 O5 1.517(8) . 1_555 N P4 O6 1.528(7) . 1_555 N P4 C4 1.813(7) . 1_555 N O1 Y1 2.362(7) . 1_555 N O1 P1 1.513(7) . 1_555 N O2 Y2 2.302(4) . 1_555 N O2 P1 1.459(5) . 1_555 N O3 P1 1.543(5) . 1_555 N O4 Y1 2.352(6) . -1_666 N O4 P4 1.500(8) . 1_555 N O5 Y2 2.318(6) . -1_665 N O5 P4 1.517(8) . 1_555 N C1 P1 1.833(7) . 1_555 N C1 N1 1.472(6) . 1_555 N O6 P4 1.528(7) . 1_555 N N1 C1 1.472(6) . 1_555 N N1 C2 1.522(8) . 1_555 N N1 C6 1.508(8) . 1_555 N C2 N1 1.522(8) . 1_555 N C2 C3 1.529(6) . 1_555 N C2 C7 1.4966(34) . 1_555 N C6 N1 1.508(8) . 1_555 N C6 C5 1.484(6) . 1_555 N C3 C2 1.529(6) . 1_555 N C3 C8 1.4835(33) . 1_555 N C3 N4 1.543(6) . 1_555 N C8 C3 1.4835(33) . 1_555 N C5 C6 1.484(6) . 1_555 N C5 N4 1.536(8) . 1_555 N C4 P4 1.813(7) . 1_555 N C4 N4 1.510(9) . 1_555 N C7 C2 1.4966(34) . 1_555 N N4 C3 1.543(6) . 1_555 N N4 C5 1.536(8) . 1_555 N N4 C4 1.510(9) . 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 Y1 O1 91.95(28) 1_555 . 2_655 N O1 Y1 O1 91.97(28) 1_555 . 3_665 N O1 Y1 O4 85.76(23) 1_555 . -1_666 N O1 Y1 O4 88.45(23) 1_555 . -2_556 N O1 Y1 O4 177.74(28) 1_555 . -3_656 N O1 Y1 O1 91.99(28) 2_655 . 3_665 N O1 Y1 O4 177.67(27) 2_655 . -1_666 N O1 Y1 O4 85.76(23) 2_655 . -2_556 N O1 Y1 O4 88.50(23) 2_655 . -3_656 N O1 Y1 O4 88.50(23) 3_665 . -1_666 N O1 Y1 O4 177.72(28) 3_665 . -2_556 N O1 Y1 O4 85.80(23) 3_665 . -3_656 N O4 Y1 O4 93.77(31) -1_666 . -2_556 N O4 Y1 O4 93.80(31) -1_666 . -3_656 N O4 Y1 O4 93.79(31) -2_556 . -3_656 N O2 Y2 O2 81.85(20) 1_555 . 2_655 N O2 Y2 O2 81.86(20) 1_555 . 3_665 N O2 Y2 O5 85.20(21) 1_555 . -1_665 N O2 Y2 O5 95.99(23) 1_555 . -2_555 N O2 Y2 O5 167.10(25) 1_555 . -3_655 N O2 Y2 O2 81.87(20) 2_655 . 3_665 N O2 Y2 O5 167.04(25) 2_655 . -1_665 N O2 Y2 O5 85.21(21) 2_655 . -2_555 N O2 Y2 O5 96.05(23) 2_655 . -3_655 N O2 Y2 O5 96.03(23) 3_665 . -1_665 N O2 Y2 O5 167.08(25) 3_665 . -2_555 N O2 Y2 O5 85.25(21) 3_665 . -3_655 N O5 Y2 O5 96.48(29) -1_665 . -2_555 N O5 Y2 O5 96.52(29) -1_665 . -3_655 N O5 Y2 O5 96.51(29) -2_555 . -3_655 N O1 P1 O2 109.3(4) 1_555 . 1_555 N O1 P1 O3 105.7(4) 1_555 . 1_555 N O1 P1 C1 111.0(4) 1_555 . 1_555 N O2 P1 O3 107.2(4) 1_555 . 1_555 N O2 P1 C1 112.9(4) 1_555 . 1_555 N O3 P1 C1 110.4(4) 1_555 . 1_555 N O4 P4 O5 107.6(5) 1_555 . 1_555 N O4 P4 O6 106.3(5) 1_555 . 1_555 N O4 P4 C4 112.9(5) 1_555 . 1_555 N O5 P4 O6 106.7(5) 1_555 . 1_555 N O5 P4 C4 111.0(4) 1_555 . 1_555 N O6 P4 C4 111.9(5) 1_555 . 1_555 N Y1 O1 P1 132.8(4) 1_555 . 1_555 N Y2 O2 P1 156.1(4) 1_555 . 1_555 N Y1 O4 P4 141.0(5) -1_666 . 1_555 N Y2 O5 P4 152.0(6) -1_665 . 1_555 N P1 C1 N1 113.5(6) 1_555 . 1_555 N C1 N1 C2 107.0(7) 1_555 . 1_555 N C1 N1 C6 114.9(7) 1_555 . 1_555 N C2 N1 C6 107.1(6) 1_555 . 1_555 N N1 C2 C3 103.4(5) 1_555 . 1_555 N N1 C2 C7 108.4(5) 1_555 . 1_555 N C3 C2 C7 109.2(4) 1_555 . 1_555 N N1 C6 C5 107.2(5) 1_555 . 1_555 N C2 C3 C8 109.9(4) 1_555 . 1_555 N C2 C3 N4 102.7(4) 1_555 . 1_555 N C8 C3 N4 108.1(4) 1_555 . 1_555 N C6 C5 N4 105.8(5) 1_555 . 1_555 N P4 C4 N4 130.4(7) 1_555 . 1_555 N C3 N4 C5 104.2(5) 1_555 . 1_555 N C3 N4 C4 105.9(7) 1_555 . 1_555 N C5 N4 C4 113.0(8) 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 100 _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type 'ID31, ESRF' _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 Y 4.0 0.000 0.000 17.7760 1.40290 10.2946 12.8006 5.72629 0.12560 3.26588 104.354 1.91213 International_Tables_Vol_C P 12.0 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 36.0 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 42.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C N 12.0 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 _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 0.95 _diffrn_radiation_wavelength 0.800178 _diffrn_radiation_type synchrotron _pd_proc_ls_prof_R_factor 0.0540 _pd_proc_ls_prof_wR_factor 0.0677 _pd_proc_ls_prof_wR_expected 0.0220 _refine_ls_R_Fsqd_factor 0.06473 _pd_proc_ls_background_function ; GSAS Background function number 2 with 36 terms. Cosine Fourier series 1: 29976.3 2: -36287.4 3: -9963.12 4: 8675.36 5: -8470.04 6: 54753.7 7: 1534.87 8: -34281.1 9: -97064.7 10: 109133. 11: 13500.1 12: -5338.23 13: -50506.4 14: 29848.6 15: 755.425 16: -7747.81 17: -1599.38 18: 704.607 19: 14098.3 20: -9856.13 21: 590.563 22: 731.146 23: -4735.73 24: 3356.60 25: 5722.18 26: -10042.9 27: 2046.59 28: 1591.33 29: 8796.21 30: -5379.14 31: 1627.11 32: -15730.0 33: 676.227 34: 39403.3 35: -40337.9 36: 12778.2 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 No correction is applied. ; _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_correction_T_max 1.00000 # Extinction correction _gsas_exptl_extinct_corr_T_min 1.00000 _gsas_exptl_extinct_corr_T_max 1.00000 _pd_proc_ls_profile_function ; CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 179.944 #2(GV) = -22.810 #3(GW) = 0.441 #4(LX) = 3.480 #5(LY) = 51.124 #6(trns) = -1.723 #7(asym) = 0.0228 #8(shft) = 0.4634 #9(GP) = 0.000 #10(stec)= -27.26 #11(ptec)= 0.04 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.004 #15(L33) = 0.000 #16(L12) = -0.001 #17(L13) = 0.001 #18(L23) = -0.007 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 2010-03-22T10:31:06 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 0.003 _pd_meas_2theta_range_max 47.976 _pd_meas_2theta_range_inc 0.003 _pd_proc_2theta_range_min -0.002145 _pd_proc_2theta_range_max 47.97086 _pd_proc_2theta_range_inc 0.003 _pd_meas_number_of_points 15992 _pd_proc_number_of_points 15992 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 0 o 70316.52 68267.77 180.00 13.97347 100.00 0 0 1 o 3262.672 4533.617 180.00 10.02957 0.80 1 0 1 o 92.887 101.220 180.00 8.14799 0.04 1 1 0 o 18459.002 19854.760 0.00 8.06759 8.75 1 0 -1 o 302.086 345.154 180.00 8.14799 0.15 2 0 0 o 2109.843 1325.773 180.00 6.98674 0.75 1 1 -1 o 6426.242 5164.341 180.00 6.28627 1.85 1 1 1 o 18638.008 15773.939 0.00 6.28627 5.37 2 0 1 o 1815.804 2221.182 0.00 5.73286 0.44 2 0 -1 o 9916.642 11729.946 0.00 5.73286 2.38 3 -1 0 o 783.494 1657.843 180.00 5.28148 0.16 2 1 0 o 788.395 1438.910 180.00 5.28148 0.16 0 0 2 o 1322.708 2110.022 0.00 5.01478 0.08 3 -1 1 o 17519.652 18708.859 180.00 4.67315 2.79 3 0 0 o 17006.350 17920.061 0.00 4.65782 2.69 1 0 2 o 675.562 716.872 0.00 4.72003 0.11 2 1 1 o 4361.708 4623.845 180.00 4.67315 0.70 2 1 -1 o 21.353 22.644 0.00 4.67315 0.00 3 -1 -1 o 6429.825 6815.291 180.00 4.67315 1.02 1 0 -2 o 1492.607 1566.949 180.00 4.72003 0.24 1 1 -2 o 5313.484 4995.699 180.00 4.25903 0.70 3 0 1 o 1328.622 1226.139 0.00 4.22449 0.17 3 0 -1 o 3776.463 3573.140 180.00 4.22449 0.49 1 1 2 o 7679.387 7665.846 180.00 4.25903 1.02 2 2 0 o 1321.438 906.128 0.00 4.03379 0.16 2 0 2 o 25689.209 23090.559 0.00 4.07400 3.11 2 0 -2 o 3782.007 3493.663 180.00 4.07400 0.46 4 -1 0 o 4767.206 3150.469 180.00 3.87554 0.52 3 1 0 o 3672.921 2496.548 180.00 3.87554 0.40 2 2 -1 o 2592.028 2189.873 0.00 3.74245 0.27 2 2 1 o 6951.092 6101.508 180.00 3.74245 0.71 4 -1 1 o 13429.640 13404.693 0.00 3.61504 1.28 3 -1 2 o 72.577 71.892 180.00 3.63662 0.01 2 1 -2 o 42093.50 41889.80 0.00 3.63662 4.07 3 1 1 o 3912.019 3939.917 0.00 3.61504 0.37 3 1 -1 o 2.014 2.027 180.00 3.61504 0.00 2 1 2 o 0.004 0.004 180.00 3.63662 0.00 4 -1 -1 o 45737.86 46227.00 0.00 3.61504 4.37 3 -1 -2 o 43103.98 43446.97 0.00 3.63662 4.17 4 0 0 o 983.281 1036.530 180.00 3.49337 0.09 3 0 2 o 21831.576 23413.146 180.00 3.41280 1.86 3 0 -2 o 32142.494 34362.418 180.00 3.41280 2.74 4 0 -1 o 5094.302 5582.733 180.00 3.29898 0.41 4 0 1 o 12817.636 14151.380 180.00 3.29898 1.02 0 0 3 o 311.614 454.751 0.00 3.34319 0.01 3 2 0 o 405.962 521.400 180.00 3.20573 0.03 5 -2 0 o 335.153 431.901 180.00 3.20573 0.03 1 0 3 o 8.220 11.983 0.00 3.25143 0.00 1 0 -3 o 511.859 741.063 180.00 3.25143 0.04 2 2 -2 o 22963.645 22217.613 180.00 3.14314 1.66 4 -1 2 o 22067.271 23801.754 0.00 3.06652 1.52 2 2 2 o 30273.943 28537.049 180.00 3.14314 2.19 3 2 -1 o 6328.687 6968.667 0.00 3.05355 0.43 5 -2 1 o 4933.647 5447.555 180.00 3.05355 0.34 5 -1 0 o 417.877 463.764 0.00 3.04926 0.03 4 1 0 o 15087.564 16722.271 0.00 3.04926 1.03 1 1 -3 o 2249.493 2518.281 0.00 3.08850 0.16 3 1 -2 o 387.675 415.310 0.00 3.06652 0.03 3 1 2 o 7322.084 7824.175 0.00 3.06652 0.50 5 -2 -1 o 7202.977 7919.292 180.00 3.05355 0.49 3 2 1 o 4388.958 4822.281 0.00 3.05355 0.30 1 1 3 o 63.410 70.632 180.00 3.08850 0.00 4 -1 -2 o 87.546 93.140 0.00 3.06652 0.01 2 0 3 o 0.296 0.355 180.00 3.01572 0.00 2 0 -3 o 4973.481 5954.187 0.00 3.01572 0.33 5 -1 1 o 1149.684 1292.674 0.00 2.91741 0.07 5 -1 -1 o 1042.914 1172.845 180.00 2.91741 0.07 4 1 -1 o 695.900 782.584 180.00 2.91741 0.04 4 1 1 o 168.949 189.997 180.00 2.91741 0.01 4 0 -2 o 333.131 369.990 0.00 2.86643 0.02 4 0 2 o 6.072 6.718 0.00 2.86643 0.00 5 0 0 o 1982.485 1537.745 180.00 2.79469 0.11 2 1 -3 o 337.057 324.594 180.00 2.82481 0.02 3 -1 3 o 8402.866 8030.876 180.00 2.82481 0.49 3 -1 -3 o 9382.595 9144.990 180.00 2.82481 0.55 2 1 3 o 290.195 281.368 180.00 2.82481 0.02 3 2 -2 o 1856.918 1688.750 0.00 2.70101 0.10 5 -2 2 o 56.493 51.430 180.00 2.70101 0.00 5 0 -1 o 9982.756 9075.771 0.00 2.69213 0.53 5 0 1 o 2663.833 2422.790 0.00 2.69213 0.14 3 3 0 o 11995.110 10965.966 0.00 2.68920 0.64 3 0 -3 o 3459.966 3291.584 180.00 2.71600 0.19 3 0 3 o 3509.677 3318.134 0.00 2.71600 0.19 6 -2 0 o 27.476 27.163 0.00 2.64074 0.00 5 -2 -2 o 40650.30 36859.15 0.00 2.70101 2.17 3 2 2 o 1705.391 1546.580 180.00 2.70101 0.09 4 2 0 o 7138.749 7079.117 180.00 2.64074 0.37 5 -1 2 o 17902.539 18381.994 180.00 2.60542 0.89 3 3 -1 o 1647.527 1691.443 180.00 2.59745 0.08 3 3 1 o 556.947 573.938 180.00 2.59745 0.03 4 1 2 o 3942.210 4078.323 180.00 2.60542 0.20 4 1 -2 o 10.612 10.972 180.00 2.60542 0.00 5 -1 -2 o 8608.203 8922.500 180.00 2.60542 0.43 4 2 -1 o 9793.618 8027.561 180.00 2.55370 0.47 4 2 1 o 1133.272 927.525 180.00 2.55370 0.05 6 -2 1 o 606.885 499.236 0.00 2.55370 0.03 6 -2 -1 o 305.047 249.912 0.00 2.55370 0.01 6 -1 0 o 1174.172 1051.701 180.00 2.50971 0.05 2 2 -3 o 443.341 437.628 0.00 2.57404 0.02 2 2 3 o 3222.590 3232.282 0.00 2.57404 0.16 4 -1 3 o 1.224 0.961 180.00 2.53145 0.00 5 1 0 o 5162.640 4636.937 180.00 2.50971 0.24 3 1 3 o 1173.346 911.997 0.00 2.53145 0.06 3 1 -3 o 1448.975 1129.231 0.00 2.53145 0.07 4 -1 -3 o 1743.331 1349.841 0.00 2.53145 0.08 0 0 4 o 8280.703 7697.286 0.00 2.50739 0.13 5 0 2 o 26563.727 22138.367 0.00 2.44120 1.16 1 0 4 o 2900.222 2634.827 0.00 2.46797 0.13 1 0 -4 o 12420.913 11324.906 180.00 2.46797 0.56 6 -1 -1 o 1093.433 869.227 180.00 2.43464 0.05 5 1 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180.00 1.87522 0.14 2 1 -5 o 611.730 555.385 0.00 1.87522 0.02 8 -3 2 o 7954.537 8064.912 0.00 1.85467 0.20 8 -3 -2 o 18.239 18.549 180.00 1.85467 0.00 5 3 2 o 643.243 654.346 0.00 1.85467 0.02 7 0 -2 o 9513.019 9675.659 0.00 1.85467 0.24 7 0 2 o 94.341 95.858 0.00 1.85467 0.00 5 3 -2 o 683.199 694.063 0.00 1.85467 0.02 5 0 -4 o 7596.774 6724.748 0.00 1.86633 0.20 5 0 4 o 21117.949 18753.980 180.00 1.86633 0.54 5 2 3 o 558.495 526.672 180.00 1.85950 0.01 7 -2 -3 o 13004.982 12255.976 0.00 1.85950 0.33 2 1 5 o 990.633 898.132 180.00 1.87522 0.03 3 -1 -5 o 2963.117 2684.075 0.00 1.87522 0.08 3 0 -5 o 1814.234 1961.729 180.00 1.84233 0.05 3 0 5 o 8069.152 8712.748 0.00 1.84233 0.20 8 -1 1 o 2864.195 2800.320 180.00 1.82010 0.07 8 -1 -1 o 442.952 433.090 0.00 1.82010 0.01 7 1 1 o 1009.159 986.688 180.00 1.82010 0.02 7 1 -1 o 19.182 18.755 180.00 1.82010 0.00 6 -2 4 o 13160.228 12853.166 180.00 1.81831 0.32 3 3 4 o 5503.695 5680.830 0.00 1.83390 0.14 3 3 -4 o 6002.779 6189.096 0.00 1.83390 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0.00 1.68509 0.00 9 -4 -2 o 7731.590 7993.688 0.00 1.68509 0.16 4 3 4 o 5490.316 5340.148 0.00 1.69382 0.12 7 -3 -4 o 24523.143 23844.664 180.00 1.69382 0.52 9 -3 2 o 14410.765 17525.799 180.00 1.66111 0.30 6 3 -2 o 4261.489 5194.604 180.00 1.66111 0.09 8 -2 -3 o 26.144 28.378 180.00 1.67651 0.00 8 -2 3 o 6418.297 6950.822 0.00 1.67651 0.13 6 2 3 o 41.015 44.501 0.00 1.67651 0.00 6 2 -3 o 1898.895 2059.288 180.00 1.67651 0.04 5 -1 5 o 5272.171 5741.506 180.00 1.67582 0.11 5 2 -4 o 3106.570 3330.150 0.00 1.66947 0.06 5 2 4 o 5941.385 6356.421 0.00 1.66947 0.12 7 -2 4 o 1134.992 1220.824 0.00 1.66947 0.02 8 0 2 o 10224.839 13531.498 0.00 1.64949 0.21 6 3 2 o 1002.000 1222.630 180.00 1.66111 0.02 9 -3 -2 o 4274.869 5214.483 180.00 1.66111 0.09 4 1 5 o 967.676 1055.571 0.00 1.67582 0.02 5 -1 -5 o 323.927 353.786 0.00 1.67582 0.01 4 1 -5 o 1072.788 1169.930 180.00 1.67582 0.02 0 0 6 o 6.801 7.215 0.00 1.67160 0.00 7 -2 -4 o 1294.308 1381.901 0.00 1.66947 0.03 9 -1 0 o 1000.721 1202.315 180.00 1.63547 0.02 8 1 0 o 1998.218 2401.495 180.00 1.63547 0.04 8 0 -2 o 218.261 289.186 180.00 1.64949 0.00 1 0 6 o 415.428 519.710 180.00 1.65976 0.01 1 0 -6 o 529.556 662.777 0.00 1.65976 0.01 10 -4 0 o 1278.883 1262.336 180.00 1.60287 0.02 7 2 -2 o 1020.057 1022.439 180.00 1.61606 0.02 9 -2 2 o 7023.573 7046.057 0.00 1.61606 0.14 9 -2 -2 o 320.601 321.282 180.00 1.61606 0.01 7 2 2 o 1217.730 1220.390 0.00 1.61606 0.02 5 0 5 o 1826.698 1990.421 0.00 1.62960 0.04 9 -1 1 o 12024.737 12039.301 0.00 1.61415 0.23 8 1 1 o 2076.637 2078.354 180.00 1.61415 0.04 8 1 -1 o 1446.195 1447.253 180.00 1.61415 0.03 9 -1 -1 o 1428.263 1429.397 0.00 1.61415 0.03 5 5 0 o 1918.929 1923.262 0.00 1.61352 0.04 7 -1 4 o 42.037 43.418 0.00 1.62375 0.00 6 1 -4 o 2226.536 2297.122 0.00 1.62375 0.04 7 -1 -4 o 432.093 445.541 0.00 1.62375 0.01 6 1 4 o 8573.110 8846.381 180.00 1.62375 0.17 1 1 6 o 41.569 52.283 0.00 1.63683 0.00 1 1 -6 o 0.199 0.250 180.00 1.63683 0.00 8 -1 3 o 5124.764 5174.628 180.00 1.61925 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634.799 0.00 1.56692 0.01 8 0 3 o 147.203 144.370 180.00 1.54813 0.00 7 0 -4 o 974.191 883.637 180.00 1.56172 0.02 8 -3 4 o 16370.931 14900.260 180.00 1.56172 0.30 8 -3 -4 o 6008.329 5446.305 0.00 1.56172 0.11 5 3 4 o 14758.965 13384.145 180.00 1.56172 0.27 7 0 4 o 458.299 416.238 0.00 1.56172 0.01 5 3 -4 o 1952.413 1773.640 0.00 1.56172 0.04 3 0 6 o 504.406 486.822 180.00 1.57334 0.01 3 0 -6 o 6.442 6.219 180.00 1.57334 0.00 9 -3 -3 o 194.207 186.199 0.00 1.55772 0.00 6 3 3 o 3894.033 3733.181 0.00 1.55772 0.07 6 -1 -5 o 28.781 25.289 0.00 1.56692 0.00 10 -2 0 o 10601.739 10116.820 0.00 1.52463 0.18 8 2 0 o 11747.654 11210.116 0.00 1.52463 0.20 5 5 -2 o 23235.805 21334.250 180.00 1.53597 0.41 5 5 2 o 11708.505 10740.229 180.00 1.53597 0.21 8 0 -3 o 76.404 75.003 180.00 1.54813 0.00 9 0 1 o 197.615 182.346 0.00 1.53433 0.00 9 0 -1 o 269.631 248.762 180.00 1.53433 0.00 2 2 -6 o 590.054 557.806 0.00 1.54425 0.01 10 -4 2 o 12564.503 11840.452 0.00 1.52677 0.22 6 4 2 o 4453.018 4192.696 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6 6 2 o 2616.657 2140.050 180.00 1.29872 0.03 6 6 -2 o 3652.122 2993.576 180.00 1.29872 0.05 11 -3 -3 o 2217.306 2026.782 0.00 1.30605 0.03 8 3 3 o 677.112 618.950 0.00 1.30605 0.01 6 1 6 o 1677.534 1765.152 0.00 1.31522 0.02 7 -1 -6 o 5742.056 6049.284 180.00 1.31522 0.07 6 1 -6 o 3192.336 3359.943 180.00 1.31522 0.04 7 5 -2 o 530.516 459.119 180.00 1.29315 0.01 12 -5 2 o 13540.198 11727.270 0.00 1.29315 0.17 7 5 2 o 1287.660 1113.881 0.00 1.29315 0.02 12 -5 -2 o 2193.981 1898.428 0.00 1.29315 0.03 10 -2 4 o 2978.653 2524.128 0.00 1.30271 0.04 8 2 -4 o 66.736 56.455 0.00 1.30271 0.00 10 -2 -4 o 6262.152 5292.686 0.00 1.30271 0.08 8 2 4 o 267.464 226.211 0.00 1.30271 0.00 9 -2 5 o 1120.331 910.455 0.00 1.30006 0.01 9 -2 -5 o 3520.342 2846.681 180.00 1.30006 0.04 7 2 -5 o 788.215 638.731 0.00 1.30006 0.01 7 2 5 o 121.225 98.166 180.00 1.30006 0.00 10 0 3 o 1946.451 1750.363 180.00 1.28926 0.02 10 0 -3 o 94.630 85.059 180.00 1.28926 0.00 5 -2 7 o 1388.166 1348.463 0.00 1.30809 0.02 3 2 -7 o 708.504 688.613 180.00 1.30809 0.01 3 2 7 o 528.664 514.189 0.00 1.30809 0.01 5 -2 -7 o 194.460 189.197 0.00 1.30809 0.00 11 -1 -2 o 1059.295 1064.145 180.00 1.28222 0.01 10 1 -2 o 5921.854 5948.917 180.00 1.28222 0.07 10 1 2 o 2864.759 2877.715 180.00 1.28222 0.04 11 -1 2 o 2.085 2.094 180.00 1.28222 0.00 11 0 0 o 1109.555 1284.418 180.00 1.27032 0.01 9 3 1 o 4.985 5.092 180.00 1.28126 0.00 12 -3 1 o 7.075 7.223 0.00 1.28126 0.00 12 -3 -1 o 29.709 30.339 0.00 1.28126 0.00 9 3 -1 o 9.238 9.435 180.00 1.28126 0.00 5 -1 7 o 1252.399 1017.641 0.00 1.29677 0.02 4 1 7 o 0.033 0.027 180.00 1.29677 0.00 5 -1 -7 o 2578.594 2088.748 180.00 1.29677 0.03 4 1 -7 o 532.136 431.702 180.00 1.29677 0.01 12 -4 2 o 1220.262 1333.425 180.00 1.27685 0.01 8 4 2 o 79.954 87.485 180.00 1.27685 0.00 8 4 -2 o 3695.672 4042.189 0.00 1.27685 0.05 12 -4 -2 o 1831.968 2004.004 0.00 1.27685 0.02 4 4 -6 o 372.178 344.737 180.00 1.28702 0.00 9 2 3 o 478.473 551.634 180.00 1.27311 0.01 11 -2 3 o 59.157 68.094 0.00 1.27311 0.00 11 -2 -3 o 697.465 804.443 180.00 1.27311 0.01 9 2 -3 o 106.490 122.765 180.00 1.27311 0.00 7 0 6 o 5433.466 5539.282 180.00 1.28160 0.07 5 3 -6 o 2504.028 2552.632 180.00 1.28160 0.03 7 0 -6 o 7509.044 7657.971 0.00 1.28160 0.09 8 -3 6 o 5517.904 5622.444 0.00 1.28160 0.07 4 4 6 o 17.633 16.325 0.00 1.28702 0.00 12 -2 0 o 6865.442 7028.058 180.00 1.25485 0.08 10 2 0 o 0.220 0.225 0.00 1.25485 0.00 10 -1 4 o 9255.994 10709.011 180.00 1.26480 0.11 6 5 -4 o 3003.416 3474.459 180.00 1.26480 0.04 11 -5 4 o 585.759 676.768 0.00 1.26480 0.01 5 3 6 o 399.456 407.546 0.00 1.28160 0.00 8 -3 -6 o 1318.229 1345.172 180.00 1.28160 0.02 11 0 -1 o 93.779 105.668 180.00 1.26025 0.00 11 0 1 o 299.816 337.724 0.00 1.26025 0.00 9 -1 5 o 513.671 598.027 180.00 1.26756 0.01 9 -1 -5 o 196.708 229.277 0.00 1.26756 0.00 8 1 -5 o 3101.286 3613.614 0.00 1.26756 0.04 8 1 5 o 1641.673 1912.366 180.00 1.26756 0.02 5 0 7 o 1591.862 1804.672 180.00 1.27500 0.02 5 0 -7 o 798.565 905.928 0.00 1.27500 0.01 6 2 6 o 953.810 1107.779 180.00 1.26573 0.01 6 2 -6 o 2036.829 2364.977 0.00 1.26573 0.02 8 -2 6 o 8620.581 10002.346 180.00 1.26573 0.10 8 -2 -6 o 1472.840 1711.226 0.00 1.26573 0.02 12 -2 1 o 499.862 482.834 180.00 1.24515 0.01 9 1 -4 o 45.407 52.594 180.00 1.26480 0.00 11 -5 -4 o 661.443 766.345 180.00 1.26480 0.01 9 1 4 o 175.198 202.869 0.00 1.26480 0.00 10 -1 -4 o 581.816 674.055 0.00 1.26480 0.01 6 5 4 o 170.056 197.036 0.00 1.26480 0.00 7 4 -4 o 347.897 353.648 0.00 1.25456 0.00 11 -4 4 o 1460.819 1485.438 0.00 1.25456 0.02 12 -3 2 o 42.947 41.394 180.00 1.25101 0.00 9 3 2 o 2571.106 2474.383 180.00 1.25101 0.03 9 3 -2 o 3867.403 3722.975 180.00 1.25101 0.05 12 -3 -2 o 854.097 822.104 180.00 1.25101 0.01 13 -6 0 o 1190.946 1133.803 180.00 1.23995 0.01 7 6 0 o 2115.428 2013.048 180.00 1.23995 0.02 6 -2 7 o 0.414 0.467 0.00 1.25937 0.00 5 5 -5 o 468.647 502.981 0.00 1.25725 0.01 5 5 5 o 3183.571 3419.477 180.00 1.25725 0.04 6 6 3 o 3541.653 3422.063 180.00 1.24748 0.04 6 6 -3 o 2914.245 2816.160 0.00 1.24748 0.03 3 3 7 o 629.814 734.241 180.00 1.26451 0.01 3 3 -7 o 125.118 145.664 180.00 1.26451 0.00 10 2 -1 o 8.613 8.317 180.00 1.24515 0.00 10 2 1 o 4.964 4.794 0.00 1.24515 0.00 12 -2 -1 o 537.821 519.377 0.00 1.24515 0.01 11 -4 -4 o 148.646 151.045 180.00 1.25456 0.00 7 4 4 o 98.237 99.824 0.00 1.25456 0.00 6 4 -5 o 7.506 7.280 0.00 1.25220 0.00 10 -4 -5 o 2057.040 1991.337 0.00 1.25220 0.02 6 4 5 o 58.519 56.667 0.00 1.25220 0.00 10 -4 5 o 45.733 44.426 0.00 1.25220 0.00 12 -5 3 o 648.213 617.838 180.00 1.24254 0.01 12 -5 -3 o 459.918 437.956 0.00 1.24254 0.01 7 5 3 o 46.404 44.183 0.00 1.24254 0.00 7 5 -3 o 1394.281 1328.149 180.00 1.24254 0.02 13 -6 1 o 280.181 266.471 0.00 1.23058 0.00 13 -6 -1 o 186.918 177.733 0.00 1.23058 0.00 7 6 -1 o 282.542 268.629 0.00 1.23058 0.00 7 6 1 o 32.373 30.775 0.00 1.23058 0.00 4 2 7 o 32.144 36.330 0.00 1.25937 0.00 4 2 -7 o 89.013 100.494 0.00 1.25937 0.00 6 -2 -7 o 186.947 211.448 0.00 1.25937 0.00 13 -5 0 o 1558.880 1481.896 0.00 1.23030 0.02 8 5 0 o 11793.559 11208.158 0.00 1.23030 0.13 0 0 8 o 17849.662 17776.836 180.00 1.25370 0.07 8 3 -4 o 17.660 16.942 0.00 1.23482 0.00 8 3 4 o 2924.396 2805.700 180.00 1.23482 0.03 11 -3 4 o 16499.068 15828.221 180.00 1.23482 0.19 6 -1 7 o 542.931 522.274 0.00 1.24430 0.01 10 1 3 o 279.050 267.293 0.00 1.23283 0.00 10 1 -3 o 568.092 544.160 180.00 1.23283 0.01 11 -1 -3 o 393.005 376.450 0.00 1.23283 0.00 11 -1 3 o 628.550 602.065 0.00 1.23283 0.01 11 0 -2 o 186.437 177.831 0.00 1.23142 0.00 11 0 2 o 3121.560 2977.689 0.00 1.23142 0.04 8 -1 -6 o 583.454 550.663 0.00 1.24054 0.01 8 -1 6 o 213.801 202.009 0.00 1.24054 0.00 7 1 -6 o 66.195 62.498 180.00 1.24054 0.00 7 1 6 o 135.942 128.374 180.00 1.24054 0.00 1 0 8 o 21159.111 20163.008 0.00 1.24868 0.25 1 0 -8 o 2418.155 2304.018 180.00 1.24868 0.03 10 -3 -5 o 3020.267 2891.423 0.00 1.23738 0.03 7 3 -5 o 0.206 0.198 180.00 1.23738 0.00 7 3 5 o 949.742 909.212 180.00 1.23738 0.01 10 -3 5 o 1989.864 1904.869 180.00 1.23738 0.02 6 -1 -7 o 558.715 537.756 180.00 1.24430 0.01 5 1 -7 o 105.968 101.993 0.00 1.24430 0.00 5 1 7 o 1061.796 1021.969 0.00 1.24430 0.01 11 -3 -4 o 8204.417 7876.013 0.00 1.23482 0.09 1 1 -8 o 3596.932 3416.201 180.00 1.23883 0.04 1 1 8 o 2186.176 2075.967 180.00 1.23883 0.03 2 0 -8 o 4410.372 4236.450 0.00 1.23399 0.05 2 0 8 o 1051.494 1009.989 180.00 1.23399 0.01 _reflns_number_total 857 _reflns_limit_h_min 0 _reflns_limit_h_max 13 _reflns_limit_k_min -6 _reflns_limit_k_max 6 _reflns_limit_l_min -8 _reflns_limit_l_max 8 _reflns_d_resolution_high 1.230 _reflns_d_resolution_low 13.973 # start Validation Reply Form _vrf_PLAT601_STA-13Y-DH_publ ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 521.00 A**3 RESPONSE: Data collected under vacuum and after dehydration at 473K ; _vrf_PLAT040_STA-13Y-DH_publ ; PROBLEM: No H-atoms in this Carbon Containing Compound .. RESPONSE: Powder data: could not identify protons ; # end Validation Reply Form #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#