# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wright, P.' _publ_contact_author_email PAW2@ST-AND.AC.UK _publ_section_title ; A novel structural form of MIL-53 observed for the scandium analogue and its response to temperature variation and CO2 adsorption ; loop_ _publ_author_name J.Mowat V.Seymour J.Griffin S.Thompson A.Slawin ; D.Fairen-Jimenez ; T.Duren S.Ashbrook P.Wright data_100K_publ _database_code_depnum_ccdc_archive 'CCDC 844243' #TrackingRef '- MIL-53(Sc) Structures.cif' _pd_block_id 2011-09-07T20:45|100K|jpsm|i11 _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2011-09-07T20:45 _audit_author_name jpsm _audit_update_record ; 2011-09-07T20:45 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 ? # 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 92 _refine_ls_goodness_of_fit_all 7.68 _refine_ls_number_restraints 35 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common 'from C:/GSASSoln/MIL-53(Sc)/JMEX256-LT/Geomopt/p2c.cif' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _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 'from C:/GSASSoln/MIL-53(Sc)/JMEX256-LT/Geomopt/p2c.cif' _cell_length_a 20.29839(17) _cell_length_b 7.33083(8) _cell_length_c 11.69125(15) _cell_angle_alpha 90.0 _cell_angle_beta 104.9584(12) _cell_angle_gamma 90.0 _cell_volume 1680.752(29) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y+1/2,-z+1/2 -1 -x,-y,-z -2 +x,-y+1/2,+z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Sc Sc1 -0.00272(22) 0.9102(6) 0.2476(4) 1.0 Uiso 0.0264(6) 4 Sc Sc2 0.49515(21) 1.0817(6) 0.2431(4) 1.0 Uiso 0.0264(6) 4 O O3 0.5153(5) 0.8305(8) 0.1755(7) 1.0 Uiso 0.0169(10) 4 O O5 0.40115(34) 0.9769(14) 0.2534(11) 1.0 Uiso 0.0169(10) 4 O O6 0.0899(4) 0.9936(14) 0.3615(10) 1.0 Uiso 0.0169(10) 4 O O7 0.0125(5) 0.6621(8) 0.3388(6) 1.0 Uiso 0.0169(10) 4 O O9 0.4378(5) 1.3403(10) 0.5747(11) 1.0 Uiso 0.0169(10) 4 O O12 0.41548(34) 0.6824(16) 0.2909(9) 1.0 Uiso 0.0169(10) 4 O O14 0.0911(4) 1.2954(13) 0.3623(8) 1.0 Uiso 0.0169(10) 4 O O18 0.0698(4) 0.5035(14) 0.1562(8) 1.0 Uiso 0.0169(10) 4 O O24 0.0442(4) 0.8123(15) 0.1202(6) 1.0 Uiso 0.0169(10) 4 O O25 0.4457(5) 1.0282(10) 0.5978(7) 1.0 Uiso 0.0169(10) 4 C C4 0.41395(23) 1.1780(9) 0.5656(11) 1.0 Uiso 0.0008(10) 4 C C8 0.19000(18) 0.8831(5) 0.1605(12) 1.0 Uiso 0.0008(10) 4 C C10 0.25817(17) 0.9339(5) 0.1872(13) 1.0 Uiso 0.0008(10) 4 C C11 0.30070(21) 1.3034(9) 0.4834(13) 1.0 Uiso 0.0008(10) 4 C C13 0.12428(18) 1.1460(23) 0.3777(14) 1.0 Uiso 0.0008(10) 4 C C15 0.23271(18) 0.9701(5) 0.4405(16) 1.0 Uiso 0.0008(10) 4 C C16 0.20008(16) 1.1382(4) 0.4203(14) 1.0 Uiso 0.0008(10) 4 C C17 0.23052(20) 1.3094(5) 0.4355(15) 1.0 Uiso 0.0008(10) 4 C C19 0.34115(19) 1.1433(7) 0.5027(11) 1.0 Uiso 0.0008(10) 4 C C20 0.16548(15) 0.7067(5) 0.1652(11) 1.0 Uiso 0.0008(10) 4 C C21 0.30340(18) 0.9837(6) 0.4735(16) 1.0 Uiso 0.0008(10) 4 C C22 0.09129(20) 0.6707(21) 0.1477(14) 1.0 Uiso 0.0008(10) 4 C C23 0.21596(16) 0.5759(6) 0.2043(13) 1.0 Uiso 0.0008(10) 4 C C27 0.30302(16) 0.7877(5) 0.2135(11) 1.0 Uiso 0.0008(10) 4 C C28 0.28573(18) 0.6081(6) 0.2304(11) 1.0 Uiso 0.0008(10) 4 C C30 0.37702(21) 0.8309(20) 0.2568(14) 1.0 Uiso 0.0008(10) 4 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C8 O5 Sc' _chemical_formula_weight 221.04 _cell_formula_units_Z 8 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 Sc1 3.66706(25) . 2_545 N Sc1 Sc1 3.66706(25) . 2_555 N Sc1 O6 2.094(6) . 1_555 N Sc1 O7 2.091(5) . 1_555 N Sc1 O7 2.089(5) . 2_555 N Sc1 O14 2.094(6) . 2_545 N Sc1 O18 2.092(6) . 2_555 N Sc1 O24 2.091(5) . 1_555 N Sc2 Sc2 3.6720(5) . 2_645 N Sc2 Sc2 3.6720(5) . 2_655 N Sc2 O3 2.086(5) . 1_555 N Sc2 O3 2.094(5) . 2_655 N Sc2 O5 2.089(6) . 1_555 N Sc2 O9 2.092(11) . -2_574 N Sc2 O12 2.090(6) . 2_655 N Sc2 O25 2.097(6) . -1_676 N Sc2 C4 2.891(9) . -2_574 N O3 Sc2 2.086(5) . 1_555 N O3 Sc2 2.094(5) . 2_645 N O5 Sc2 2.089(6) . 1_555 N O5 C30 1.182(15) . 1_555 N O6 Sc1 2.094(6) . 1_555 N O6 C13 1.305(16) . 1_555 N O7 Sc1 2.091(5) . 1_555 N O7 Sc1 2.089(5) . 2_545 N O9 Sc2 2.092(11) . -2_575 N O9 C4 1.279(6) . 1_555 N O12 Sc2 2.090(6) . 2_645 N O12 C30 1.339(15) . 1_555 N O14 Sc1 2.094(6) . 2_555 N O14 C13 1.275(16) . 1_555 N O18 Sc1 2.092(6) . 2_545 N O18 C22 1.314(16) . 1_555 N O24 Sc1 2.091(5) . 1_555 N O24 C22 1.391(15) . 1_555 N O25 Sc2 2.097(6) . -1_676 N O25 C4 1.280(6) . 1_555 N C4 Sc2 2.891(9) . -2_575 N C4 O9 1.279(6) . 1_555 N C4 O25 1.280(6) . 1_555 N C4 C19 1.4929(33) . 1_555 N C8 C10 1.3887(27) . 1_555 N C8 C20 1.3918(29) . 1_555 N C10 C8 1.3887(27) . 1_555 N C10 C27 1.3886(27) . 1_555 N C11 C17 1.3903(31) . 1_555 N C11 C19 1.417(8) . 1_555 N C13 O6 1.305(16) . 1_555 N C13 O14 1.275(16) . 1_555 N C13 C16 1.4911(27) . 1_555 N C15 C16 1.3898(27) . 1_555 N C15 C21 1.3899(27) . 1_555 N C16 C13 1.4911(27) . 1_555 N C16 C15 1.3898(27) . 1_555 N C16 C17 1.3897(27) . 1_555 N C17 C11 1.3903(31) . 1_555 N C17 C16 1.3897(27) . 1_555 N C19 C4 1.4929(33) . 1_555 N C19 C11 1.417(8) . 1_555 N C19 C21 1.3920(31) . 1_555 N C20 C8 1.3918(29) . 1_555 N C20 C22 1.4900(31) . 1_555 N C20 C23 1.3916(29) . 1_555 N C21 C15 1.3899(27) . 1_555 N C21 C19 1.3920(31) . 1_555 N C22 O18 1.314(16) . 1_555 N C22 O24 1.391(15) . 1_555 N C22 C20 1.4900(31) . 1_555 N C23 C20 1.3916(29) . 1_555 N C23 C28 1.3896(27) . 1_555 N C27 C10 1.3886(27) . 1_555 N C27 C28 1.3898(32) . 1_555 N C27 C30 1.4900(30) . 1_555 N C28 C23 1.3896(27) . 1_555 N C28 C27 1.3898(32) . 1_555 N C30 O5 1.182(15) . 1_555 N C30 O12 1.339(15) . 1_555 N C30 C27 1.4900(30) . 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 O6 Sc1 O7 86.6(4) 1_555 . 1_555 N O6 Sc1 O7 90.4(4) 1_555 . 2_555 N O6 Sc1 O14 173.3(5) 1_555 . 2_545 N O6 Sc1 O18 99.5(5) 1_555 . 2_555 N O6 Sc1 O24 93.1(4) 1_555 . 1_555 N O7 Sc1 O7 176.90(24) 1_555 . 2_555 N O7 Sc1 O14 87.3(4) 1_555 . 2_545 N O7 Sc1 O18 92.4(4) 1_555 . 2_555 N O7 Sc1 O24 91.7(4) 1_555 . 1_555 N O7 Sc1 O14 95.7(4) 2_555 . 2_545 N O7 Sc1 O18 88.7(4) 2_555 . 2_555 N O7 Sc1 O24 87.8(4) 2_555 . 1_555 N O14 Sc1 O18 83.6(4) 2_545 . 2_555 N O14 Sc1 O24 84.3(4) 2_545 . 1_555 N O18 Sc1 O24 167.0(4) 2_555 . 1_555 N O3 Sc2 O3 173.96(24) 1_555 . 2_655 N O3 Sc2 O5 88.2(4) 1_555 . 1_555 N O3 Sc2 O9 90.0(4) 1_555 . -2_585 N O3 Sc2 O12 88.5(5) 1_555 . 2_655 N O3 Sc2 O25 82.74(33) 1_555 . -1_676 N O3 Sc2 O5 95.3(5) 2_655 . 1_555 N O3 Sc2 O9 95.31(33) 2_655 . -2_585 N O3 Sc2 O12 88.5(4) 2_655 . 2_655 N O3 Sc2 O25 91.9(4) 2_655 . -1_676 N O5 Sc2 O9 81.9(4) 1_555 . -2_585 N O5 Sc2 O12 172.6(5) 1_555 . 2_655 N O5 Sc2 O25 97.5(4) 1_555 . -1_676 N O9 Sc2 O12 91.4(4) -2_585 . 2_655 N O9 Sc2 O25 172.8(4) -2_585 . -1_676 N O12 Sc2 O25 88.7(4) 2_655 . -1_676 N Sc2 O3 Sc2 122.95(33) 1_555 . 2_645 N Sc2 O5 C30 136.7(9) 1_555 . 1_555 N Sc1 O6 C13 134.5(9) 1_555 . 1_555 N Sc1 O7 Sc1 122.65(32) 1_555 . 2_545 N Sc2 O9 C4 116.0(9) -2_586 . 1_555 N Sc2 O12 C30 134.3(9) 2_645 . 1_555 N Sc1 O14 C13 140.4(9) 2_555 . 1_555 N Sc1 O18 C22 128.4(9) 2_545 . 1_555 N Sc1 O24 C22 120.3(8) 1_555 . 1_555 N Sc2 O25 C4 136.1(8) -1_676 . 1_555 N O9 C4 O25 128.6(6) 1_555 . 1_555 N O9 C4 C19 120.3(7) 1_555 . 1_555 N O25 C4 C19 111.0(6) 1_555 . 1_555 N C10 C8 C20 125.9(4) 1_555 . 1_555 N C8 C10 C27 113.63(35) 1_555 . 1_555 N C17 C11 C19 125.5(5) 1_555 . 1_555 N O6 C13 O14 118.1(6) 1_555 . 1_555 N O6 C13 C16 118.9(11) 1_555 . 1_555 N O14 C13 C16 122.9(12) 1_555 . 1_555 N C16 C15 C21 113.4(4) 1_555 . 1_555 N C13 C16 C15 119.7(7) 1_555 . 1_555 N C13 C16 C17 113.2(7) 1_555 . 1_555 N C15 C16 C17 127.02(34) 1_555 . 1_555 N C11 C17 C16 113.5(4) 1_555 . 1_555 N C4 C19 C11 113.3(5) 1_555 . 1_555 N C4 C19 C21 132.6(5) 1_555 . 1_555 N C11 C19 C21 113.5(4) 1_555 . 1_555 N C8 C20 C22 121.2(7) 1_555 . 1_555 N C8 C20 C23 114.37(34) 1_555 . 1_555 N C22 C20 C23 123.8(6) 1_555 . 1_555 N C15 C21 C19 126.3(4) 1_555 . 1_555 N O18 C22 O24 119.5(6) 1_555 . 1_555 N O18 C22 C20 119.9(10) 1_555 . 1_555 N O24 C22 C20 120.6(11) 1_555 . 1_555 N C20 C23 C28 125.3(4) 1_555 . 1_555 N C10 C27 C28 126.0(4) 1_555 . 1_555 N C10 C27 C30 117.2(6) 1_555 . 1_555 N C28 C27 C30 115.0(7) 1_555 . 1_555 N C23 C28 C27 114.2(4) 1_555 . 1_555 N O5 C30 O12 122.1(6) 1_555 . 1_555 N O5 C30 C27 124.8(11) 1_555 . 1_555 N O12 C30 C27 112.8(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 100 _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection ? _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction ? # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator ? # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 10. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Sc 8.0 0.000 0.000 9.18900 9.02130 7.36790 0.57290 1.64090 136.108 1.46800 51.3531 1.33290 International_Tables_Vol_C O 40.0 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 64.0 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 0.93 _diffrn_radiation_wavelength 0.825028 _diffrn_radiation_type synchrotron _pd_proc_ls_prof_R_factor 0.0347 _pd_proc_ls_prof_wR_factor 0.0470 _pd_proc_ls_prof_wR_expected 0.0062 _refine_ls_R_Fsqd_factor 0.08622 _pd_proc_ls_background_function ; GSAS Background function number 7 with 36 terms. Linear interpolation 1: 198.106 2: 185.867 3: 168.110 4: 199.426 5: 219.999 6: 305.428 7: 332.348 8: 294.083 9: 236.819 10: 172.639 11: 172.373 12: 145.764 13: 133.157 14: 117.889 15: 107.139 16: 114.265 17: 108.312 18: 121.062 19: 114.903 20: 109.060 21: 114.785 22: 114.637 23: 118.746 24: 117.231 25: 118.197 26: 119.131 27: 118.791 28: 115.647 29: 117.542 30: 113.127 31: 115.218 32: 110.920 33: 98.4711 34: 90.6703 35: 82.9262 36: 79.7432 ; _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) = 0.000 #2(GV) = 1.715 #3(GW) = -0.022 #4(GP) = 0.000 #5(LX) = 0.296 #6(LY) = 2.220 #7(S/L) = 0.0094 #8(H/L) = 0.0037 #9(trns) = -0.07 #10(shft)= 0.0143 #11(stec)= 12.12 #12(ptec)= 0.00 #13(sfec)= 0.00 #14(L11) = -0.004 #15(L22) = 0.079 #16(L33) = 0.323 #17(L12) = 0.058 #18(L13) = -0.026 #19(L23) = 0.032 Peak tails are ignored where the intensity is below 0.0020 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00200 _pd_proc_info_datetime 2011-09-07T20:45:31 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 0.961 _pd_meas_2theta_range_max 60.001 _pd_meas_2theta_range_inc 0.005 _pd_proc_2theta_range_min 0.9667 _pd_proc_2theta_range_max 60.0067 _pd_proc_2theta_range_inc 0.005 _reflns_number_total 1399 _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 6 _reflns_limit_l_min -10 _reflns_limit_l_max 10 _reflns_d_resolution_high 1.078 _reflns_d_resolution_low 9.805 #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# data_298K_publ _database_code_depnum_ccdc_archive 'CCDC 844244' #TrackingRef '- MIL-53(Sc) Structures.cif' _pd_block_id 2011-09-07T20:21|298K|JPSM|I11 _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2011-09-07T20:21 _audit_author_name JPSM _audit_update_record ; 2011-09-07T20:21 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 ? # use ICDD colour descriptions _refine_ls_shift/su_max 0.06 _refine_ls_shift/su_mean 0.00 _computing_structure_refinement GSAS _refine_ls_number_parameters 99 _refine_ls_goodness_of_fit_all 6.73 _refine_ls_number_restraints 42 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common 'from C:/GSASSoln/MIL-53(Sc)/JMEX256/RT/Rebin/P21CNEW1F.cif' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _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 'from C:/GSASSoln/MIL-53(Sc)/JMEX256/RT/Rebin/P21CNEW1F.cif' _cell_length_a 20.32979(19) _cell_length_b 7.32576(8) _cell_length_c 11.83829(16) _cell_angle_alpha 90.0 _cell_angle_beta 105.2058(12) _cell_angle_gamma 90.0 _cell_volume 1701.365(34) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y+1/2,-z+1/2 -1 -x,-y,-z -2 +x,-y+1/2,+z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Sc Sc1 -0.00284(27) 0.9122(8) 0.2463(5) 1.0 Uiso 0.0204(7) 4 Sc Sc2 0.49384(26) 1.0781(8) 0.2460(6) 1.0 Uiso 0.0204(7) 4 O O3 0.5141(5) 0.8357(19) 0.1728(11) 1.0 Uiso 0.0197(11) 4 O O5 0.4014(6) 0.9747(17) 0.2545(13) 1.0 Uiso 0.0197(11) 4 O O6 0.0871(6) 0.9870(16) 0.3602(12) 1.0 Uiso 0.0197(11) 4 O O7 0.0153(5) 0.6672(18) 0.3423(11) 1.0 Uiso 0.0197(11) 4 O O9 0.4347(6) 1.3355(20) 0.5714(12) 1.0 Uiso 0.0197(11) 4 O O12 0.4151(6) 0.6778(23) 0.2938(11) 1.0 Uiso 0.0197(11) 4 O O14 0.0908(6) 1.2889(17) 0.3534(11) 1.0 Uiso 0.0197(11) 4 O O18 0.0712(6) 0.5050(16) 0.1569(12) 1.0 Uiso 0.0197(11) 4 O O24 0.0470(6) 0.8064(20) 0.1298(11) 1.0 Uiso 0.0197(11) 4 O O25 0.4442(6) 1.0246(17) 0.5935(12) 1.0 Uiso 0.0197(11) 4 C C4 0.4103(7) 1.1687(25) 0.5666(15) 1.0 Uiso 0.0036(13) 4 C C8 0.1903(7) 0.8819(22) 0.1600(15) 1.0 Uiso 0.0036(13) 4 C C10 0.2571(9) 0.9424(22) 0.1916(16) 1.0 Uiso 0.0036(13) 4 C C11 0.2995(8) 1.3309(22) 0.4882(16) 1.0 Uiso 0.0036(13) 4 C C13 0.1236(7) 1.1377(25) 0.3761(16) 1.0 Uiso 0.0036(13) 4 C C15 0.2350(8) 0.9732(19) 0.4392(18) 1.0 Uiso 0.0036(13) 4 C C16 0.2021(6) 1.1448(22) 0.4258(16) 1.0 Uiso 0.0036(13) 4 C C17 0.2283(8) 1.3251(22) 0.4503(17) 1.0 Uiso 0.0036(13) 4 C C19 0.3355(6) 1.1624(24) 0.4974(16) 1.0 Uiso 0.0036(13) 4 C C20 0.1682(7) 0.7015(24) 0.1701(16) 1.0 Uiso 0.0036(13) 4 C C21 0.3042(8) 0.9844(21) 0.4856(19) 1.0 Uiso 0.0036(13) 4 C C22 0.0933(7) 0.6707(28) 0.1539(17) 1.0 Uiso 0.0036(13) 4 C C23 0.2136(8) 0.5626(23) 0.2131(18) 1.0 Uiso 0.0036(13) 4 C C27 0.2983(7) 0.7825(24) 0.2231(16) 1.0 Uiso 0.0036(13) 4 C C28 0.2832(8) 0.5977(24) 0.2389(16) 1.0 Uiso 0.0036(13) 4 C C30 0.3750(7) 0.8140(27) 0.2583(18) 1.0 Uiso 0.0036(13) 4 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C8 O5 Sc' _chemical_formula_weight 221.04 _cell_formula_units_Z 8 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 Sc1 3.66501(34) . 2_545 N Sc1 Sc1 3.66501(34) . 2_555 N Sc1 O6 2.042(12) . 1_555 N Sc1 O7 2.104(13) . 1_555 N Sc1 O7 2.126(12) . 2_555 N Sc1 O14 2.073(12) . 2_545 N Sc1 O18 2.131(12) . 2_555 N Sc1 O24 2.065(11) . 1_555 N Sc2 Sc2 3.6710(7) . 2_645 N Sc2 Sc2 3.6710(7) . 2_655 N Sc2 O3 2.064(13) . 1_555 N Sc2 O3 2.143(14) . 2_655 N Sc2 O5 2.053(12) . 1_555 N Sc2 O9 2.194(14) . -2_574 N Sc2 O12 2.154(13) . 2_655 N Sc2 O25 2.124(12) . -1_676 N O3 Sc2 2.064(13) . 1_555 N O3 Sc2 2.143(14) . 2_645 N O5 Sc2 2.053(12) . 1_555 N O5 C30 1.300(17) . 1_555 N O6 Sc1 2.042(12) . 1_555 N O6 C13 1.316(15) . 1_555 N O7 Sc1 2.104(13) . 1_555 N O7 Sc1 2.126(12) . 2_545 N O9 Sc2 2.194(14) . -2_575 N O9 C4 1.314(18) . 1_555 N O12 Sc2 2.154(13) . 2_645 N O12 C30 1.286(17) . 1_555 N O14 Sc1 2.073(12) . 2_555 N O14 C13 1.285(16) . 1_555 N O18 Sc1 2.131(12) . 2_545 N O18 C22 1.298(17) . 1_555 N O24 Sc1 2.065(11) . 1_555 N O24 C22 1.347(17) . 1_555 N O25 Sc2 2.124(12) . -1_676 N O25 C4 1.255(16) . 1_555 N C4 O9 1.314(18) . 1_555 N C4 O25 1.255(16) . 1_555 N C4 C19 1.526(11) . 1_555 N C8 C10 1.383(11) . 1_555 N C8 C20 1.411(11) . 1_555 N C10 C8 1.383(11) . 1_555 N C10 C27 1.432(11) . 1_555 N C11 C17 1.399(10) . 1_555 N C11 C19 1.425(11) . 1_555 N C13 O6 1.316(15) . 1_555 N C13 O14 1.285(16) . 1_555 N C13 C16 1.550(11) . 1_555 N C15 C16 1.413(11) . 1_555 N C15 C21 1.373(11) . 1_555 N C16 C13 1.550(11) . 1_555 N C16 C15 1.413(11) . 1_555 N C16 C17 1.425(11) . 1_555 N C17 C11 1.399(10) . 1_555 N C17 C16 1.425(11) . 1_555 N C19 C4 1.526(11) . 1_555 N C19 C11 1.425(11) . 1_555 N C19 C21 1.442(11) . 1_555 N C20 C8 1.411(11) . 1_555 N C20 C22 1.502(11) . 1_555 N C20 C23 1.378(11) . 1_555 N C21 C15 1.373(11) . 1_555 N C21 C19 1.442(11) . 1_555 N C22 O18 1.298(17) . 1_555 N C22 O24 1.347(17) . 1_555 N C22 C20 1.502(11) . 1_555 N C23 C20 1.378(11) . 1_555 N C23 C28 1.391(11) . 1_555 N C27 C10 1.432(11) . 1_555 N C27 C28 1.412(11) . 1_555 N C27 C30 1.522(11) . 1_555 N C28 C23 1.391(11) . 1_555 N C28 C27 1.412(11) . 1_555 N C30 O5 1.300(17) . 1_555 N C30 O12 1.286(17) . 1_555 N C30 C27 1.522(11) . 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 O6 Sc1 O7 82.6(5) 1_555 . 1_555 N O6 Sc1 O7 93.5(5) 1_555 . 2_555 N O6 Sc1 O14 169.2(6) 1_555 . 2_545 N O6 Sc1 O18 99.0(6) 1_555 . 2_555 N O6 Sc1 O24 91.7(5) 1_555 . 1_555 N O7 Sc1 O7 176.1(4) 1_555 . 2_555 N O7 Sc1 O14 86.5(5) 1_555 . 2_545 N O7 Sc1 O18 91.6(5) 1_555 . 2_555 N O7 Sc1 O24 89.6(6) 1_555 . 1_555 N O7 Sc1 O14 97.3(5) 2_555 . 2_545 N O7 Sc1 O18 88.5(5) 2_555 . 2_555 N O7 Sc1 O24 90.9(6) 2_555 . 1_555 N O14 Sc1 O18 81.9(5) 2_545 . 2_555 N O14 Sc1 O24 87.6(5) 2_545 . 1_555 N O18 Sc1 O24 169.3(6) 2_555 . 1_555 N O3 Sc2 O3 173.03(30) 1_555 . 2_655 N O3 Sc2 O5 89.4(5) 1_555 . 1_555 N O3 Sc2 O9 88.5(6) 1_555 . -2_585 N O3 Sc2 O12 85.6(6) 1_555 . 2_655 N O3 Sc2 O25 86.2(5) 1_555 . -1_676 N O3 Sc2 O5 97.2(6) 2_655 . 1_555 N O3 Sc2 O9 94.7(5) 2_655 . -2_585 N O3 Sc2 O12 88.2(5) 2_655 . 2_655 N O3 Sc2 O25 90.4(6) 2_655 . -1_676 N O5 Sc2 O9 82.5(5) 1_555 . -2_585 N O5 Sc2 O12 170.4(7) 1_555 . 2_655 N O5 Sc2 O25 99.3(5) 1_555 . -1_676 N O9 Sc2 O12 89.2(5) -2_585 . 2_655 N O9 Sc2 O25 174.4(7) -2_585 . -1_676 N O12 Sc2 O25 88.5(5) 2_655 . -1_676 N Sc2 O3 Sc2 121.5(6) 1_555 . 2_645 N Sc2 O5 C30 136.7(12) 1_555 . 1_555 N Sc1 O6 C13 133.9(12) 1_555 . 1_555 N Sc1 O7 Sc1 120.1(6) 1_555 . 2_545 N Sc2 O9 C4 114.6(11) -2_586 . 1_555 N Sc2 O12 C30 134.3(13) 2_645 . 1_555 N Sc1 O14 C13 144.8(11) 2_555 . 1_555 N Sc1 O18 C22 126.3(12) 2_545 . 1_555 N Sc1 O24 C22 125.0(11) 1_555 . 1_555 N Sc2 O25 C4 133.0(13) -1_676 . 1_555 N O9 C4 O25 126.5(14) 1_555 . 1_555 N O9 C4 C19 111.3(15) 1_555 . 1_555 N O25 C4 C19 120.9(16) 1_555 . 1_555 N C10 C8 C20 126.1(15) 1_555 . 1_555 N C8 C10 C27 105.9(13) 1_555 . 1_555 N C17 C11 C19 117.8(14) 1_555 . 1_555 N O6 C13 O14 116.8(12) 1_555 . 1_555 N O6 C13 C16 124.6(15) 1_555 . 1_555 N O14 C13 C16 118.5(15) 1_555 . 1_555 N C16 C15 C21 113.4(13) 1_555 . 1_555 N C13 C16 C15 115.0(14) 1_555 . 1_555 N C13 C16 C17 113.7(14) 1_555 . 1_555 N C15 C16 C17 131.4(13) 1_555 . 1_555 N C11 C17 C16 113.2(14) 1_555 . 1_555 N C4 C19 C11 115.8(16) 1_555 . 1_555 N C4 C19 C21 115.6(16) 1_555 . 1_555 N C11 C19 C21 124.8(13) 1_555 . 1_555 N C8 C20 C22 117.7(16) 1_555 . 1_555 N C8 C20 C23 121.7(15) 1_555 . 1_555 N C22 C20 C23 119.6(15) 1_555 . 1_555 N C15 C21 C19 118.2(14) 1_555 . 1_555 N O18 C22 O24 118.0(14) 1_555 . 1_555 N O18 C22 C20 118.9(16) 1_555 . 1_555 N O24 C22 C20 123.0(17) 1_555 . 1_555 N C20 C23 C28 119.2(16) 1_555 . 1_555 N C10 C27 C28 133.3(14) 1_555 . 1_555 N C10 C27 C30 115.8(15) 1_555 . 1_555 N C28 C27 C30 110.6(16) 1_555 . 1_555 N C23 C28 C27 113.1(15) 1_555 . 1_555 N O5 C30 O12 118.8(14) 1_555 . 1_555 N O5 C30 C27 122.0(17) 1_555 . 1_555 N O12 C30 C27 119.2(16) 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 ? _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 Sc 8.0 0.000 0.000 9.18900 9.02130 7.36790 0.57290 1.64090 136.108 1.46800 51.3531 1.33290 International_Tables_Vol_C O 40.0 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 64.0 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 0.93 _diffrn_radiation_wavelength 0.825028 _diffrn_radiation_type synchrotron _pd_proc_ls_prof_R_factor 0.0347 _pd_proc_ls_prof_wR_factor 0.0449 _pd_proc_ls_prof_wR_expected 0.0068 _refine_ls_R_Fsqd_factor 0.05419 _pd_proc_ls_background_function ; GSAS Background function number 7 with 36 terms. Linear interpolation 1: 78.9722 2: 79.2729 3: 64.8986 4: 80.1455 5: 80.2982 6: 108.738 7: 136.607 8: 140.002 9: 127.343 10: 98.0676 11: 77.9252 12: 64.7886 13: 59.6771 14: 49.4836 15: 48.7388 16: 42.1868 17: 39.7367 18: 41.1836 19: 40.0763 20: 41.4494 21: 42.1264 22: 39.0258 23: 40.0383 24: 42.1301 25: 41.8449 26: 42.7051 27: 42.7083 28: 43.9318 29: 42.2198 30: 43.9696 31: 43.2586 32: 42.5459 33: 43.3402 34: 42.7592 35: 42.5044 36: 42.6773 ; _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) = 0.334 #2(GV) = -0.058 #3(GW) = 0.060 #4(GP) = 0.000 #5(LX) = 0.155 #6(LY) = 2.222 #7(S/L) = 0.0093 #8(H/L) = 0.0039 #9(trns) = -0.07 #10(shft)= 0.0143 #11(stec)= 12.12 #12(ptec)= 0.00 #13(sfec)= 0.00 #14(L11) = 0.004 #15(L22) = 0.159 #16(L33) = 0.347 #17(L12) = 0.057 #18(L13) = -0.021 #19(L23) = 0.029 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00400 _pd_proc_info_datetime 2011-09-07T20:21:57 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 0.962 _pd_meas_2theta_range_max 149.99701 _pd_meas_2theta_range_inc 0.005 _pd_proc_2theta_range_min 0.96877 _pd_proc_2theta_range_max 150.00377 _pd_proc_2theta_range_inc 0.005 _pd_meas_number_of_points 29808 _pd_proc_number_of_points 29808 _reflns_number_total 1009 _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 6 _reflns_limit_l_min -9 _reflns_limit_l_max 9 _reflns_d_resolution_high 1.206 _reflns_d_resolution_low 9.809 #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# data_573K_publ _database_code_depnum_ccdc_archive 'CCDC 844245' #TrackingRef '- MIL-53(Sc) Structures.cif' _pd_block_id 2011-09-07T20:43|573K|jpsm|I11 _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2011-09-07T20:43 _audit_author_name jpsm _audit_update_record ; 2011-09-07T20:43 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 ? # use ICDD colour descriptions _refine_ls_shift/su_max 0.03 _refine_ls_shift/su_mean 0.00 _computing_structure_refinement GSAS _refine_ls_number_parameters 93 _refine_ls_goodness_of_fit_all 6.21 _refine_ls_number_restraints 42 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common 'from C:/GSASSoln/MIL-53(Sc)/JMEX256/300C/Rebin/P21CNEW1F.cif' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature 573 _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 'from C:/GSASSoln/MIL-53(Sc)/JMEX256/300C/Rebin/P21CNEW1F.cif' _cell_length_a 20.53822(25) _cell_length_b 7.29921(12) _cell_length_c 12.56044(25) _cell_angle_alpha 90.0 _cell_angle_beta 106.5514(17) _cell_angle_gamma 90.0 _cell_volume 1804.95(5) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y+1/2,-z+1/2 -1 -x,-y,-z -2 +x,-y+1/2,+z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Sc Sc1 -0.00468(20) 0.9350(5) 0.24040(34) 1.0 Uiso 0.0182(6) 4 Sc Sc2 0.49878(22) 1.0719(6) 0.2626(4) 1.0 Uiso 0.0182(6) 4 O O3 0.5087(5) 0.8342(7) 0.1744(5) 1.0 Uiso 0.0275(11) 4 O O5 0.40892(32) 0.9446(9) 0.2702(11) 1.0 Uiso 0.0275(11) 4 O O6 0.0834(4) 1.0147(10) 0.3602(8) 1.0 Uiso 0.0275(11) 4 O O7 0.0075(6) 0.6931(7) 0.3343(5) 1.0 Uiso 0.0275(11) 4 O O9 0.4400(5) 1.3363(11) 0.6025(9) 1.0 Uiso 0.0275(11) 4 O O12 0.41912(33) 0.6432(10) 0.2966(7) 1.0 Uiso 0.0275(11) 4 O O14 0.09616(33) 1.3281(9) 0.3575(8) 1.0 Uiso 0.0275(11) 4 O O18 0.0717(4) 0.5047(8) 0.1682(7) 1.0 Uiso 0.0275(11) 4 O O24 0.05237(31) 0.7985(10) 0.1512(5) 1.0 Uiso 0.0275(11) 4 O O25 0.4349(5) 1.0397(10) 0.5939(6) 1.0 Uiso 0.0275(11) 4 C C4 0.40710(14) 1.1929(8) 0.5592(11) 1.0 Uiso 0.0148(14) 4 C C8 0.19505(12) 0.8888(4) 0.1852(10) 1.0 Uiso 0.0148(14) 4 C C10 0.26408(13) 0.9292(4) 0.2155(11) 1.0 Uiso 0.0148(14) 4 C C11 0.29532(14) 1.32743(34) 0.5002(11) 1.0 Uiso 0.0148(14) 4 C C13 0.11716(15) 1.1636(8) 0.3736(11) 1.0 Uiso 0.0148(14) 4 C C15 0.22358(14) 1.00079(33) 0.4504(13) 1.0 Uiso 0.0148(14) 4 C C16 0.19202(11) 1.17063(34) 0.4262(10) 1.0 Uiso 0.0148(14) 4 C C17 0.22570(15) 1.33769(33) 0.4500(11) 1.0 Uiso 0.0148(14) 4 C C19 0.33228(10) 1.16482(35) 0.5149(12) 1.0 Uiso 0.0148(14) 4 C C20 0.16868(9) 0.7139(4) 0.1890(9) 1.0 Uiso 0.0148(14) 4 C C21 0.29406(13) 1.00480(33) 0.4905(16) 1.0 Uiso 0.0148(14) 4 C C22 0.09590(15) 0.6674(8) 0.1741(11) 1.0 Uiso 0.0148(14) 4 C C23 0.21635(13) 0.5741(4) 0.2210(11) 1.0 Uiso 0.0148(14) 4 C C27 0.30753(10) 0.7803(4) 0.2483(8) 1.0 Uiso 0.0148(14) 4 C C28 0.28585(13) 0.6040(4) 0.2634(8) 1.0 Uiso 0.0148(14) 4 C C30 0.38218(15) 0.7852(8) 0.2630(11) 1.0 Uiso 0.0148(14) 4 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C8 O5 Sc' _chemical_formula_weight 221.04 _cell_formula_units_Z 8 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 Sc1 3.6590(5) . 2_545 N Sc1 Sc1 3.6590(5) . 2_555 N Sc1 O6 2.079(5) . 1_555 N Sc1 O7 2.099(5) . 1_555 N Sc1 O7 2.098(5) . 2_555 N Sc1 O14 2.082(5) . 2_545 N Sc1 O18 2.090(5) . 2_555 N Sc1 O24 2.091(4) . 1_555 N Sc1 C22 2.947(8) . 2_555 N Sc2 Sc2 3.6649(9) . 2_645 N Sc2 Sc2 3.6649(9) . 2_655 N Sc2 O3 2.100(5) . 1_555 N Sc2 O3 2.094(5) . 2_655 N Sc2 O5 2.093(5) . 1_555 N Sc2 O9 2.137(10) . -2_574 N Sc2 O12 2.093(5) . 2_655 N Sc2 O25 2.090(5) . -1_676 N O3 Sc2 2.100(5) . 1_555 N O3 Sc2 2.094(5) . 2_645 N O5 Sc2 2.093(5) . 1_555 N O5 C30 1.279(5) . 1_555 N O6 Sc1 2.079(5) . 1_555 N O6 C13 1.274(5) . 1_555 N O7 Sc1 2.099(5) . 1_555 N O7 Sc1 2.098(5) . 2_545 N O9 Sc2 2.137(10) . -2_575 N O9 O25 2.169(10) . 1_555 N O9 C4 1.280(6) . 1_555 N O12 Sc2 2.093(5) . 2_645 N O12 C30 1.283(5) . 1_555 N O14 Sc1 2.082(5) . 2_555 N O14 C13 1.272(5) . 1_555 N O18 Sc1 2.090(5) . 2_545 N O18 O24 2.180(8) . 1_555 N O18 C22 1.281(5) . 1_555 N O24 Sc1 2.091(4) . 1_555 N O24 O18 2.180(8) . 1_555 N O24 C22 1.285(5) . 1_555 N O25 Sc2 2.090(5) . -1_676 N O25 O9 2.169(10) . 1_555 N O25 C4 1.274(5) . 1_555 N C4 O9 1.280(6) . 1_555 N C4 O25 1.274(5) . 1_555 N C4 C19 1.4919(22) . 1_555 N C8 C10 1.3908(21) . 1_555 N C8 C20 1.3927(23) . 1_555 N C10 C8 1.3908(21) . 1_555 N C10 C27 1.3919(22) . 1_555 N C11 C17 1.3907(25) . 1_555 N C11 C19 1.3926(21) . 1_555 N C13 O6 1.274(5) . 1_555 N C13 O14 1.272(5) . 1_555 N C13 C16 1.4913(24) . 1_555 N C15 C16 1.3918(21) . 1_555 N C15 C21 1.3908(22) . 1_555 N C16 C13 1.4913(24) . 1_555 N C16 C15 1.3918(21) . 1_555 N C16 C17 1.3918(21) . 1_555 N C17 C11 1.3907(25) . 1_555 N C17 C16 1.3918(21) . 1_555 N C19 C4 1.4919(22) . 1_555 N C19 C11 1.3926(21) . 1_555 N C19 C21 1.3918(21) . 1_555 N C20 C8 1.3927(23) . 1_555 N C20 C22 1.4920(25) . 1_555 N C20 C23 1.3922(21) . 1_555 N C21 C15 1.3908(22) . 1_555 N C21 C19 1.3918(21) . 1_555 N C22 Sc1 2.947(8) . 2_545 N C22 O18 1.281(5) . 1_555 N C22 O24 1.285(5) . 1_555 N C22 C20 1.4920(25) . 1_555 N C23 C20 1.3922(21) . 1_555 N C23 C28 1.3914(22) . 1_555 N C27 C10 1.3919(22) . 1_555 N C27 C28 1.3922(25) . 1_555 N C27 C30 1.4914(24) . 1_555 N C28 C23 1.3914(22) . 1_555 N C28 C27 1.3922(25) . 1_555 N C30 O5 1.279(5) . 1_555 N C30 O12 1.283(5) . 1_555 N C30 C27 1.4914(24) . 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 O6 Sc1 O7 83.63(34) 1_555 . 1_555 N O6 Sc1 O7 88.84(34) 1_555 . 2_555 N O6 Sc1 O14 170.0(5) 1_555 . 2_545 N O6 Sc1 O18 96.2(4) 1_555 . 2_555 N O6 Sc1 O24 90.9(4) 1_555 . 1_555 N O7 Sc1 O7 172.15(23) 1_555 . 2_555 N O7 Sc1 O14 87.7(4) 1_555 . 2_545 N O7 Sc1 O18 83.6(4) 1_555 . 2_555 N O7 Sc1 O24 84.54(33) 1_555 . 1_555 N O7 Sc1 O14 99.6(4) 2_555 . 2_545 N O7 Sc1 O18 95.07(34) 2_555 . 2_555 N O7 Sc1 O24 97.8(4) 2_555 . 1_555 N O14 Sc1 O18 78.0(4) 2_545 . 2_555 N O14 Sc1 O24 93.1(4) 2_545 . 1_555 N O18 Sc1 O24 165.4(4) 2_555 . 1_555 N O3 Sc2 O3 169.61(31) 1_555 . 2_655 N O3 Sc2 O5 82.9(4) 1_555 . 1_555 N O3 Sc2 O9 82.9(4) 1_555 . -2_585 N O3 Sc2 O12 78.99(34) 1_555 . 2_655 N O3 Sc2 O25 89.76(34) 1_555 . -1_676 N O3 Sc2 O5 103.2(4) 2_655 . 1_555 N O3 Sc2 O9 89.23(34) 2_655 . -2_585 N O3 Sc2 O12 93.4(4) 2_655 . 2_655 N O3 Sc2 O25 97.5(4) 2_655 . -1_676 N O5 Sc2 O9 85.0(4) 1_555 . -2_585 N O5 Sc2 O12 159.5(5) 1_555 . 2_655 N O5 Sc2 O25 98.9(4) 1_555 . -1_676 N O9 Sc2 O12 83.3(4) -2_585 . 2_655 N O9 Sc2 O25 171.2(5) -2_585 . -1_676 N O12 Sc2 O25 90.6(4) 2_655 . -1_676 N Sc2 O3 Sc2 121.83(30) 1_555 . 2_645 N Sc2 O5 C30 140.1(6) 1_555 . 1_555 N Sc1 O6 C13 131.5(6) 1_555 . 1_555 N Sc1 O7 Sc1 121.38(27) 1_555 . 2_545 N Sc2 O9 C4 138.1(10) -2_586 . 1_555 N Sc2 O12 C30 123.0(6) 2_645 . 1_555 N Sc1 O14 C13 131.0(5) 2_555 . 1_555 N Sc1 O18 C22 120.0(7) 2_545 . 1_555 N Sc1 O24 C22 134.0(8) 1_555 . 1_555 N Sc2 O25 C4 139.1(8) -1_676 . 1_555 N O9 C4 O25 116.2(7) 1_555 . 1_555 N O9 C4 C19 129.3(7) 1_555 . 1_555 N O25 C4 C19 108.7(6) 1_555 . 1_555 N C10 C8 C20 124.12(24) 1_555 . 1_555 N C8 C10 C27 115.68(23) 1_555 . 1_555 N C17 C11 C19 123.86(29) 1_555 . 1_555 N O6 C13 O14 129.6(5) 1_555 . 1_555 N O6 C13 C16 122.8(5) 1_555 . 1_555 N O14 C13 C16 107.3(4) 1_555 . 1_555 N C16 C15 C21 115.62(23) 1_555 . 1_555 N C13 C16 C15 115.06(30) 1_555 . 1_555 N C13 C16 C17 120.78(31) 1_555 . 1_555 N C15 C16 C17 124.15(25) 1_555 . 1_555 N C11 C17 C16 115.73(23) 1_555 . 1_555 N C4 C19 C11 113.39(31) 1_555 . 1_555 N C4 C19 C21 130.82(31) 1_555 . 1_555 N C11 C19 C21 115.73(21) 1_555 . 1_555 N C8 C20 C22 126.17(32) 1_555 . 1_555 N C8 C20 C23 115.70(22) 1_555 . 1_555 N C22 C20 C23 117.78(34) 1_555 . 1_555 N C15 C21 C19 124.12(23) 1_555 . 1_555 N O18 C22 O24 116.3(5) 1_555 . 1_555 N O18 C22 C20 125.3(5) 1_555 . 1_555 N O24 C22 C20 117.8(5) 1_555 . 1_555 N C20 C23 C28 123.76(24) 1_555 . 1_555 N C10 C27 C28 123.97(25) 1_555 . 1_555 N C10 C27 C30 124.6(4) 1_555 . 1_555 N C28 C27 C30 111.27(33) 1_555 . 1_555 N C23 C28 C27 115.22(28) 1_555 . 1_555 N O5 C30 O12 120.7(6) 1_555 . 1_555 N O5 C30 C27 115.9(5) 1_555 . 1_555 N O12 C30 C27 120.8(5) 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 573 _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection ? _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction ? # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator ? # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 10. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Sc 8.0 0.000 0.000 9.18900 9.02130 7.36790 0.57290 1.64090 136.108 1.46800 51.3531 1.33290 International_Tables_Vol_C O 40.0 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 64.0 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 0.93 _diffrn_radiation_wavelength 0.825028 _diffrn_radiation_type synchrotron _pd_proc_ls_prof_R_factor 0.0315 _pd_proc_ls_prof_wR_factor 0.0413 _pd_proc_ls_prof_wR_expected 0.0067 _refine_ls_R_Fsqd_factor 0.05549 _pd_proc_ls_background_function ; GSAS Background function number 7 with 36 terms. Linear interpolation 1: 86.0893 2: 81.7415 3: 71.5056 4: 82.3220 5: 82.6855 6: 120.362 7: 141.095 8: 149.773 9: 135.826 10: 100.406 11: 88.6197 12: 66.7253 13: 62.8764 14: 52.7821 15: 54.0688 16: 46.0901 17: 42.6797 18: 46.6047 19: 42.0990 20: 43.3423 21: 45.7149 22: 42.2218 23: 43.4069 24: 45.9704 25: 43.2524 26: 45.1549 27: 45.2076 28: 45.2108 29: 45.7655 30: 47.9726 31: 46.5589 32: 46.0799 33: 46.2510 34: 45.3972 35: 44.4492 36: 44.1557 ; _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) = 5.724 #2(GV) = -1.251 #3(GW) = 0.100 #4(GP) = 0.000 #5(LX) = 0.030 #6(LY) = 2.222 #7(S/L) = 0.0092 #8(H/L) = 0.0040 #9(trns) = -0.07 #10(shft)= 0.0143 #11(stec)= 13.10 #12(ptec)= -0.03 #13(sfec)= 0.00 #14(L11) = 0.008 #15(L22) = 0.265 #16(L33) = 0.545 #17(L12) = 0.070 #18(L13) = -0.045 #19(L23) = 0.070 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00400 _pd_proc_info_datetime 2011-09-07T20:43:36 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 0.962 _pd_meas_2theta_range_max 149.99701 _pd_meas_2theta_range_inc 0.005 _pd_proc_2theta_range_min 0.96855 _pd_proc_2theta_range_max 150.00356 _pd_proc_2theta_range_inc 0.005 _pd_meas_number_of_points 29808 _pd_proc_number_of_points 29808 _reflns_number_total 1068 _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 6 _reflns_limit_l_min -10 _reflns_limit_l_max 10 _reflns_d_resolution_high 1.206 _reflns_d_resolution_low 9.844 #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# data_623K_publ _database_code_depnum_ccdc_archive 'CCDC 844246' #TrackingRef '- MIL-53(Sc) Structures.cif' _pd_block_id 2011-09-07T20:29|623K|jpsm|I11 _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2011-09-07T20:29 _audit_author_name jpsm _audit_update_record ; 2011-09-07T20:29 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 ? # use ICDD colour descriptions _refine_ls_shift/su_max 0.07 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 39 _refine_ls_goodness_of_fit_all 5.03 _refine_ls_number_restraints 28 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ;from C:/GSASSoln/Diamond-i11-2010/JM-DATA/MIL-53- JMEX256/350C/Fe-M ; _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature 623 _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 'from C:/GSASSoln/Diamond-i11-2010/JM-DATA/MIL-53-JMEX256/350C/Fe-M' _cell_length_a 21.50501(26) _cell_length_b 6.63008(7) _cell_length_c 7.27431(20) _cell_angle_alpha 90.0 _cell_angle_beta 113.5427(14) _cell_angle_gamma 90.0 _cell_volume 950.839(26) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y,-z+1/2 -1 -x,-y,-z -2 +x,-y,+z+1/2 101 +x+1/2,+y+1/2,+z 102 -x+1/2,+y+1/2,-z+1/2 -101 -x+1/2,-y+1/2,-z -102 +x+1/2,-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 Sc Sc 0.0 0.0 0.0 1.0 Uiso 0.0480(6) 4 O O1 0.0 -0.1484(7) 0.75 1.0 Uiso 0.0125(20) 4 O O11 0.43482(19) 0.2988(6) 0.3214(7) 1.0 Uiso 0.1102(23) 8 O O12 0.41559(16) 0.3239(6) -0.0012(6) 1.0 Uiso 0.0595(19) 8 C C11 0.31458(20) 0.2527(9) 0.0433(10) 1.0 Uiso 0.0317(22) 8 C C12 0.29526(24) 0.2404(9) 0.2090(8) 1.0 Uiso 0.0200(25) 8 C C13 0.22200(28) 0.1998(10) 0.1457(9) 1.0 Uiso 0.0576(29) 8 C C17 0.39435(23) 0.3006(9) 0.1398(10) 1.0 Uiso 0.0785(33) 8 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C8 O5 Sc' _chemical_formula_weight 221.04 _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 Sc Sc 3.63715(10) . 2_554 N Sc Sc 3.63715(10) . 2_555 N Sc O1 2.0678(21) . 1_554 N Sc O1 2.0678(21) . -1_556 N Sc O11 1.994(4) . 102_545 N Sc O11 1.994(4) . -102_344 N Sc O12 2.155(4) . 101_445 N Sc O12 2.155(4) . -101_445 N O1 Sc 2.0678(21) . 1_556 N O1 Sc 2.0678(21) . 2_555 N O11 Sc 1.994(4) . 102_555 N O11 C17 1.258(6) . 1_555 N O12 Sc 2.155(4) . 101_555 N O12 C17 1.288(7) . 1_555 N C11 C12 1.425(7) . 1_555 N C11 C13 1.321(6) . -101_445 N C11 C17 1.605(6) . 1_555 N C12 C11 1.425(7) . 1_555 N C12 C13 1.479(5) . 1_555 N C13 C11 1.321(6) . -101_445 N C13 C12 1.479(5) . 1_555 N C17 O11 1.258(6) . 1_555 N C17 O12 1.288(7) . 1_555 N C17 C11 1.605(6) . 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 Sc O1 179.9802 1_554 . -1_556 N O1 Sc O11 90.45(15) 1_554 . 102_545 N O1 Sc O11 89.55(15) 1_554 . -102_344 N O1 Sc O12 91.98(13) 1_554 . 101_445 N O1 Sc O12 88.02(13) 1_554 . -101_555 N O1 Sc O11 89.55(15) -1_556 . 102_545 N O1 Sc O11 90.45(15) -1_556 . -102_344 N O1 Sc O12 88.02(13) -1_556 . 101_445 N O1 Sc O12 91.98(13) -1_556 . -101_555 N O11 Sc O11 179.9802 102_545 . -102_344 N O11 Sc O12 90.69(13) 102_545 . 101_445 N O11 Sc O12 89.31(13) 102_545 . -101_555 N O11 Sc O12 89.31(13) -102_455 . 101_445 N O11 Sc O12 90.69(13) -102_455 . -101_555 N O12 Sc O12 180.0 101_445 . -101_555 N Sc O1 Sc 123.16(21) 1_556 . 2_555 N Sc O11 C17 133.6(5) 102_555 . 1_555 N Sc O12 C17 128.9(4) 101_555 . 1_555 N C12 C11 C13 129.8(5) 1_555 . -101_555 N C12 C11 C17 105.3(5) 1_555 . 1_555 N C13 C11 C17 119.8(6) -101_555 . 1_555 N C11 C12 C13 112.4(5) 1_555 . 1_555 N C11 C13 C12 113.5(5) -101_555 . 1_555 N O11 C17 O12 121.4(5) 1_555 . 1_555 N O11 C17 C11 128.9(6) 1_555 . 1_555 N O12 C17 C11 109.4(5) 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 623 _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection ? _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction ? # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator ? # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 10. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Sc 4.0 0.000 0.000 9.18900 9.02130 7.36790 0.57290 1.64090 136.108 1.46800 51.3531 1.33290 International_Tables_Vol_C O 20.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C C 32.0 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 0.93 _diffrn_radiation_wavelength 0.825 _diffrn_radiation_type synchrotron _pd_proc_ls_prof_R_factor 0.0409 _pd_proc_ls_prof_wR_factor 0.0538 _pd_proc_ls_prof_wR_expected 0.0109 _refine_ls_R_Fsqd_factor 0.10722 _pd_proc_ls_background_function ; GSAS Background function number 7 with 36 terms. Linear interpolation 1: 36.4543 2: 33.5418 3: 30.5000 4: 30.8521 5: 38.0161 6: 45.4017 7: 62.0788 8: 63.8913 9: 57.9179 10: 44.3113 11: 35.5427 12: 29.1875 13: 28.5665 14: 24.2315 15: 23.7185 16: 19.0245 17: 18.4713 18: 20.7427 19: 19.1670 20: 21.7900 21: 19.0404 22: 18.8322 23: 19.3911 24: 19.8200 25: 20.2952 26: 20.6734 27: 20.8593 28: 20.0638 29: 20.5978 30: 20.6267 31: 20.7774 32: 19.9372 33: 20.5151 34: 19.7540 35: 20.0146 36: 18.6888 ; _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) = 0.000 #2(GV) = 2.542 #3(GW) = -0.008 #4(GP) = 0.000 #5(LX) = 0.351 #6(LY) = 1.804 #7(S/L) = 0.0066 #8(H/L) = 0.0066 #9(trns) = 0.24 #10(shft)= -0.0371 #11(stec)= 19.57 #12(ptec)= -0.09 #13(sfec)= 0.00 #14(L11) = -0.018 #15(L22) = 1.250 #16(L33) = 0.976 #17(L12) = 0.112 #18(L13) = 0.041 #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 2011-09-07T20:29:57 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 0.962 _pd_meas_2theta_range_max 75.04 _pd_meas_2theta_range_inc 0.002 _pd_proc_2theta_range_min 0.968135 _pd_proc_2theta_range_max 75.04613 _pd_proc_2theta_range_inc 0.002 _pd_meas_number_of_points 37040 _pd_proc_number_of_points 37040 _reflns_number_total 283 _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 5 _reflns_limit_l_min -6 _reflns_limit_l_max 5 _reflns_d_resolution_high 1.207 _reflns_d_resolution_low 9.857 #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# data_MIL-53NO2 _database_code_depnum_ccdc_archive 'CCDC 844247' _vrf_PLAT_078_global ; PROBLEM: No H-atoms, but _solution_hydrogens reported as geom RESPONSE: Disordered -NO2 functionalised phenyl ring in the structure H-atoms not added for clarity ; _vrf_PLAT_079_global ; PROBLEM: No H-atoms, but _hydrogen_treatment reported as mixed RESPONSE: Disordered -NO2 functionalised phenyl ring in the structure H-atoms not added for clarity ; _vrf_PLAT_242_global ; PROBLEM: Structure Contains Solvent Accessible VOIDS of 202 A**3 RESPONSE: Porous framework material ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 N1 O8 Sc1' _chemical_formula_weight 283.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Imma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' 'x, -y, -z' '-x, y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z' '-x, y, z' 'x, -y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y, z+1/2' _cell_length_a 18.279(7) _cell_length_b 7.330(3) _cell_length_c 11.601(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1554.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 93 _cell_measurement_reflns_used 2418 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.5 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.20 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 526 _exptl_absorpt_coefficient_mu 0.497 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.833 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4879 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.34 _reflns_number_total 800 _reflns_number_gt 669 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1332P)^2^+2.3533P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 800 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.2253 _refine_ls_wR_factor_gt 0.2135 _refine_ls_goodness_of_fit_ref 1.211 _refine_ls_restrained_S_all 1.211 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc1 Sc 0.5000 0.0000 0.5000 0.0185(6) Uani 1 4 d S . . O1 O 0.5000 -0.2500 0.5820(4) 0.0271(12) Uani 1 4 d S . . O2 O 0.58196(14) 0.0984(3) 0.6108(3) 0.0414(9) Uani 1 1 d . . . C1 C 0.6099(3) 0.2500 0.6338(5) 0.0379(14) Uani 1 2 d S . . C2 C 0.6827(3) 0.2500 0.6946(6) 0.0472(18) Uani 1 2 d S . . C3 C 0.7160(3) 0.4090(6) 0.7236(7) 0.091(3) Uani 1 1 d . . . N1 N 0.6904(14) 0.578(4) 0.691(2) 0.092(7) Uiso 0.25 1 d P . . O3A O 0.7096(13) 0.653(4) 0.590(2) 0.138(9) Uiso 0.25 1 d P . . O3B O 0.6503(16) 0.641(4) 0.779(2) 0.150(9) Uiso 0.25 1 d P . . OW1 O 0.5000 0.7500 0.825(3) 0.155(11) Uiso 0.50 4 d SP . . OW2 O 0.565(2) 0.7500 0.813(3) 0.115(10) Uiso 0.25 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc1 0.0144(8) 0.0133(8) 0.0278(9) -0.0011(4) 0.000 0.000 O1 0.038(3) 0.016(2) 0.027(3) 0.000 0.000 0.000 O2 0.0393(17) 0.0250(16) 0.060(2) 0.0027(13) -0.0284(13) -0.0038(12) C1 0.040(3) 0.020(3) 0.054(4) 0.000 -0.026(3) 0.000 C2 0.044(4) 0.023(3) 0.075(5) 0.000 -0.036(3) 0.000 C3 0.075(4) 0.026(3) 0.171(6) 0.004(3) -0.088(4) 0.001(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 O1 2.065(2) 9_656 ? Sc1 O1 2.065(2) . ? Sc1 O2 2.101(2) 9_656 ? Sc1 O2 2.101(2) . ? Sc1 O2 2.101(2) 11_655 ? Sc1 O2 2.101(2) 3_556 ? Sc1 Sc1 3.6650(15) 2_655 ? Sc1 Sc1 3.6650(15) 2_645 ? O1 Sc1 2.065(2) 2_645 ? O2 C1 1.252(3) . ? C1 O2 1.252(3) 12_565 ? C1 C2 1.507(8) . ? C2 C3 1.357(6) . ? C2 C3 1.357(6) 12_565 ? C3 N1 1.38(3) . ? C3 C3 1.387(9) 8_646 ? N1 O3B 1.34(3) . ? N1 O3A 1.34(3) . ? O3A O3A 1.43(6) 12_575 ? O3B O3B 1.60(6) 12_575 ? O3B OW2 1.80(4) . ? OW1 OW2 1.19(4) 2_665 ? OW1 OW2 1.19(4) . ? OW2 O3B 1.80(4) 12_575 ? 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_3 _geom_angle_publ_flag O1 Sc1 O1 180.0 9_656 . ? O1 Sc1 O2 91.32(11) 9_656 9_656 ? O1 Sc1 O2 88.68(11) . 9_656 ? O1 Sc1 O2 88.68(11) 9_656 . ? O1 Sc1 O2 91.32(11) . . ? O2 Sc1 O2 180.00(10) 9_656 . ? O1 Sc1 O2 88.68(11) 9_656 11_655 ? O1 Sc1 O2 91.32(11) . 11_655 ? O2 Sc1 O2 89.05(17) 9_656 11_655 ? O2 Sc1 O2 90.95(17) . 11_655 ? O1 Sc1 O2 91.32(11) 9_656 3_556 ? O1 Sc1 O2 88.68(11) . 3_556 ? O2 Sc1 O2 90.95(17) 9_656 3_556 ? O2 Sc1 O2 89.05(17) . 3_556 ? O2 Sc1 O2 180.00(13) 11_655 3_556 ? O1 Sc1 Sc1 27.42(12) 9_656 2_655 ? O1 Sc1 Sc1 152.58(12) . 2_655 ? O2 Sc1 Sc1 110.07(7) 9_656 2_655 ? O2 Sc1 Sc1 69.93(7) . 2_655 ? O2 Sc1 Sc1 69.93(7) 11_655 2_655 ? O2 Sc1 Sc1 110.07(7) 3_556 2_655 ? O1 Sc1 Sc1 152.58(12) 9_656 2_645 ? O1 Sc1 Sc1 27.42(12) . 2_645 ? O2 Sc1 Sc1 69.93(7) 9_656 2_645 ? O2 Sc1 Sc1 110.07(7) . 2_645 ? O2 Sc1 Sc1 110.07(7) 11_655 2_645 ? O2 Sc1 Sc1 69.93(7) 3_556 2_645 ? Sc1 Sc1 Sc1 180.0 2_655 2_645 ? Sc1 O1 Sc1 125.2(2) 2_645 . ? C1 O2 Sc1 136.5(3) . . ? O2 C1 O2 125.2(5) . 12_565 ? O2 C1 C2 117.4(2) . . ? O2 C1 C2 117.4(2) 12_565 . ? C3 C2 C3 118.4(6) . 12_565 ? C3 C2 C1 120.8(3) . . ? C3 C2 C1 120.8(3) 12_565 . ? C2 C3 N1 123.6(12) . . ? C2 C3 C3 120.8(3) . 8_646 ? N1 C3 C3 115.2(11) . 8_646 ? O3B N1 O3A 132(3) . . ? O3B N1 C3 106(2) . . ? O3A N1 C3 121(2) . . ? N1 O3A O3A 114.0(18) . 12_575 ? N1 O3B O3B 110.0(18) . 12_575 ? N1 O3B OW2 143(3) . . ? O3B O3B OW2 63.6(10) 12_575 . ? OW2 OW1 OW2 166(5) 2_665 . ? OW1 OW2 O3B 152.6(13) . 12_575 ? OW1 OW2 O3B 152.6(13) . . ? O3B OW2 O3B 53(2) 12_575 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.726 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.116