Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Paul A. Wright' _publ_contact_author_address ; School of Chemistry University of St. Andrews Purdie Building, North Haugh St. Andrews, Fife, KY16 9ST ; _publ_contact_author_email paw2@st-andrews.ac.uk _publ_contact_author_fax '(0044) (0)1334 463808' _publ_contact_author_phone ? # Definition of non standard CIF items (Reliability indices used in FULLPROF) loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_info _publ_manuscript_incl_extra_defn # Name Explanation Standard? # ------ ----------- --------- '_pd_proc_ls_prof_cR_factor' 'Prof. R-factor CORRECTED for background' no '_pd_proc_ls_prof_cwR_factor' 'wProf.R-factor CORRECTED for background' no '_pd_proc_ls_prof_cwR_expected' 'wProf.Expected CORRECTED for background' no '_pd_proc_ls_prof_chi2' 'Chi-square for all considered points' no '_pd_proc_ls_prof_echi2' 'Chi-2 for points with Bragg contribution' no #============================================================================= # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and structure of the framework scandium methylphosphonates ScF(H2O)MePO3 and NaSc(CH3PO3)2*0.5H2O ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Stuart R. Miller' ; School of Chemistry University of St. Andrews Purdie Building, North Haugh St. Andrews, Fife, KY16 9ST ; 'Emily Lear' ; School of Chemistry University of St. Andrews Purdie Building, North Haugh St. Andrews, Fife, KY16 9ST ; 'Jorge Gonzalez' ; School of Chemistry University of St. Andrews Purdie Building, North Haugh St. Andrews, Fife, KY16 9ST ; 'Alexandra M. Z. Slawin' ; School of Chemistry University of St. Andrews Purdie Building, North Haugh St. Andrews, Fife, KY16 9ST ; 'Paul A. Wright' ; School of Chemistry University of St. Andrews Purdie Building, North Haugh St. Andrews, Fife, KY16 9ST ; ; N.Guillou ; ; Institut Lavoisier, UMR CNRS C8637 Universite de Versailles St-Quntin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles cedex France ; 'Gerard Ferey' ; Institut Lavoisier, UMR CNRS C8637 Universite de Versailles St-Quntin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles cedex France ; data_smpw5 _database_code_depnum_ccdc_archive 'CCDC 263646' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' ScF(H2O)C H3PO3' _chemical_formula_sum 'C H5 F O4 P Sc' _chemical_formula_weight 175.98 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.532(2) _cell_length_b 8.081(3) _cell_length_c 8.721(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 530.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 1810 _cell_measurement_theta_min 2.3355 _cell_measurement_theta_max 25.3491 _exptl_crystal_description needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.1500 _exptl_crystal_size_mid 0.0300 _exptl_crystal_size_min 0.0100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 352 _exptl_absorpt_coefficient_mu 1.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9330 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3156 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0174 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 25.34 _reflns_number_total 908 _reflns_number_gt 881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2sigma(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^)+(0.0191P)^2^+0.2088P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.53(4) _refine_ls_number_reflns 908 _refine_ls_number_parameters 82 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0169 _refine_ls_R_factor_gt 0.0157 _refine_ls_wR_factor_ref 0.0375 _refine_ls_wR_factor_gt 0.0369 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.052 _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 0.86787(4) 0.74549(4) 0.50941(4) 0.00432(10) Uani 1 1 d . . . P1 P 0.61681(6) 1.04235(6) 0.67048(5) 0.00577(12) Uani 1 1 d . . . O1 O 0.77541(18) 0.92506(16) 0.65650(15) 0.0092(3) Uani 1 1 d . . . O2 O 0.44473(17) 0.96026(18) 0.61386(15) 0.0087(3) Uani 1 1 d . . . O3 O 0.59117(17) 1.09616(16) 0.83581(15) 0.0090(3) Uani 1 1 d . . . C1 C 0.6588(3) 1.2189(2) 0.5540(2) 0.0109(4) Uani 1 1 d . . . H1A H 0.7683 1.2731 0.5882 0.016 Uiso 1 1 calc R . . H1B H 0.5594 1.2966 0.5627 0.016 Uiso 1 1 calc R . . H1C H 0.6719 1.1843 0.4469 0.016 Uiso 1 1 calc R . . F4 F 1.12015(14) 0.79427(13) 0.57389(12) 0.0085(2) Uani 1 1 d . . . O5 O 0.8567(2) 0.57667(17) 0.70983(15) 0.0121(3) Uani 1 1 d D . . H5A H 0.754(2) 0.541(3) 0.771(2) 0.014(6) Uiso 1 1 d D . . H5B H 0.956(3) 0.515(3) 0.755(3) 0.038(9) Uiso 1 1 d D . . 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 0.00425(16) 0.00433(18) 0.00439(17) -0.00012(12) -0.00002(12) 0.00018(14) P1 0.0061(2) 0.0053(2) 0.0059(2) -0.00088(18) 0.0004(2) 0.0002(2) O1 0.0119(7) 0.0085(7) 0.0073(6) -0.0029(6) 0.0002(5) 0.0013(6) O2 0.0093(7) 0.0077(7) 0.0091(7) -0.0028(6) -0.0004(5) -0.0018(6) O3 0.0103(7) 0.0077(6) 0.0088(6) -0.0018(5) 0.0003(5) 0.0009(5) C1 0.0126(10) 0.0080(9) 0.0120(10) 0.0003(8) 0.0020(8) -0.0003(8) F4 0.0060(5) 0.0110(5) 0.0085(5) -0.0024(4) -0.0013(4) 0.0005(5) O5 0.0159(7) 0.0101(7) 0.0103(7) 0.0029(5) 0.0025(6) 0.0013(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 O3 2.0062(14) 2_674 ? Sc1 F4 2.0205(12) . ? Sc1 F4 2.0279(12) 4_466 ? Sc1 O1 2.0582(14) . ? Sc1 O2 2.0628(15) 4_566 ? Sc1 O5 2.2189(15) . ? P1 O3 1.5183(14) . ? P1 O1 1.5298(15) . ? P1 O2 1.5374(14) . ? P1 C1 1.780(2) . ? O2 Sc1 2.0628(15) 4_466 ? O3 Sc1 2.0062(14) 2_675 ? F4 Sc1 2.0279(12) 4_566 ? 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 O3 Sc1 F4 86.62(5) 2_674 . ? O3 Sc1 F4 88.41(5) 2_674 4_466 ? F4 Sc1 F4 174.83(2) . 4_466 ? O3 Sc1 O1 94.17(6) 2_674 . ? F4 Sc1 O1 90.41(5) . . ? F4 Sc1 O1 91.36(5) 4_466 . ? O3 Sc1 O2 94.45(6) 2_674 4_566 ? F4 Sc1 O2 92.20(5) . 4_566 ? F4 Sc1 O2 86.78(5) 4_466 4_566 ? O1 Sc1 O2 171.12(6) . 4_566 ? O3 Sc1 O5 172.97(6) 2_674 . ? F4 Sc1 O5 86.36(5) . . ? F4 Sc1 O5 98.62(5) 4_466 . ? O1 Sc1 O5 85.96(6) . . ? O2 Sc1 O5 85.74(6) 4_566 . ? O3 P1 O1 110.64(8) . . ? O3 P1 O2 108.75(7) . . ? O1 P1 O2 111.43(8) . . ? O3 P1 C1 109.58(9) . . ? O1 P1 C1 108.20(9) . . ? O2 P1 C1 108.20(9) . . ? P1 O1 Sc1 138.65(9) . . ? P1 O2 Sc1 138.74(9) . 4_466 ? P1 O3 Sc1 151.61(9) . 2_675 ? Sc1 F4 Sc1 137.28(5) . 4_566 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 Sc1 157.76(12) . . . . ? O2 P1 O1 Sc1 36.64(16) . . . . ? C1 P1 O1 Sc1 -82.19(15) . . . . ? O3 Sc1 O1 P1 65.85(14) 2_674 . . . ? F4 Sc1 O1 P1 152.49(13) . . . . ? F4 Sc1 O1 P1 -22.65(13) 4_466 . . . ? O2 Sc1 O1 P1 -100.4(4) 4_566 . . . ? O5 Sc1 O1 P1 -121.19(13) . . . . ? O3 P1 O2 Sc1 -135.90(12) . . . 4_466 ? O1 P1 O2 Sc1 -13.69(16) . . . 4_466 ? C1 P1 O2 Sc1 105.15(14) . . . 4_466 ? O1 P1 O3 Sc1 93.25(18) . . . 2_675 ? O2 P1 O3 Sc1 -144.06(16) . . . 2_675 ? C1 P1 O3 Sc1 -26.0(2) . . . 2_675 ? O3 Sc1 F4 Sc1 -66.74(9) 2_674 . . 4_566 ? F4 Sc1 F4 Sc1 -50.9(3) 4_466 . . 4_566 ? O1 Sc1 F4 Sc1 -160.90(9) . . . 4_566 ? O2 Sc1 F4 Sc1 27.59(9) 4_566 . . 4_566 ? O5 Sc1 F4 Sc1 113.18(9) . . . 4_566 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O2 0.9798(11) 1.920(3) 2.899(2) 177(2) 3_646 O5 H5B O1 0.9799(11) 2.285(7) 3.246(2) 167(2) 3_746 O5 H5B F4 0.9799(11) 2.40(3) 2.9658(18) 117(2) 3_746 _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.264 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.047 data_scphos1 _database_code_depnum_ccdc_archive 'CCDC 266029' #============================================================================= # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'Na Sc C2 H7 P2 O6.5' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Na Sc C2 H7 P2 O6.5' _chemical_formula_weight 264.93 loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source sc 9.18900 9.02130 7.36790 0.57290 1.64090 136.10800 1.46800 51.35310 1.33290 0.21900 0.29900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 p 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490 0.08400 0.07500 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 na 4.76260 3.28500 3.17360 8.84220 1.26740 0.31360 1.11280 129.42400 0.67600 0.03000 0.02500 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.02700 0.00800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.00200 0.00100 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 h 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 42/N' _symmetry_space_group_name_Hall '-P 4bc' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z -y,x+1/2,z+1/2 -x+1/2,-y+1/2,z y+1/2,-x,z+1/2 -x,-y,-z y,-x+1/2,-z+1/2 x+1/2,y+1/2,-z -y+1/2,x,-z+1/2 _cell_length_a 17.79734(8) _cell_length_b 17.79734(8) _cell_length_c 5.38859(3) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 1706.812(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293 _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 10 _pd_spec_size_equat 0.5 _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting ; capillary ; _pd_spec_mount_mode transmission _pd_spec_shape cylinder _pd_char_particle_morphology 'tetragonal prisms' # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================= # EXPERIMENTAL DATA _exptl_special_details ; ? ; # 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 ; 'European Synchrotron Radiation Facilities (ESRF); ID 31 Beamline' ; _pd_calibration_special_details 'wavelength was calibrated using NIST standard Si 640c' # description of the method used # to calibrate the instrument _diffrn_ambient_temperature 293 _diffrn_source 'Synchrotron - undulator beamline' _diffrn_radiation_type X-ray _diffrn_radiation_wavelength 0.6325 _diffrn_radiation_monochromator 'Si(111) double crystal' _diffrn_measurement_device_type '2-circles theta/2theta instrument' _diffrn_measurement_method capillary _diffrn_detector_area_resol_mean ? # Not in version 2.0.1 _diffrn_detector ? _diffrn_detector_type 'multi detectors' _pd_meas_scan_method step _pd_meas_special_details ; ? ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 12316 _pd_meas_2theta_range_min 1.02000 _pd_meas_2theta_range_max 37.96500 _pd_meas_2theta_range_inc 0.003000 #============================================================================= # REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function 'pseudo Voigt' _pd_proc_ls_background_function 'linear interpolation between 49 points' _pd_proc_ls_pref_orient_corr 'The usual Rietveld function is used' # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 6.1930 _pd_proc_ls_prof_wR_factor 8.2002 _pd_proc_ls_prof_wR_expected 3.8612 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 17.1644 _pd_proc_ls_prof_cwR_factor 16.5248 _pd_proc_ls_prof_cwR_expected 7.7809 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 4.5104 _pd_proc_ls_prof_echi2 4.7758 # Items related to LS refinement _refine_ls_R_I_factor 7.7395 _refine_ls_number_reflns 1018 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 1.0223 _pd_proc_2theta_range_max 37.9673 _pd_proc_2theta_range_inc 0.003000 _pd_proc_wavelength 0.632500 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions 'One excluded range: 1-2%(2theta)' _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution 'EXPO + SHELXL' _computing_structure_refinement FULLPROF _computing_molecular_graphics ? _computing_publication_material ? #============================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type # Not in version 2.0.1 _atom_site_type_symbol Sc1 0.57778(15) 0.09480(15) 0.7391(7) 0.00000 1.00000 Uiso Sc P1 0.7037(2) 0.0662(2) 0.2404(11) 0.00000 1.00000 Uiso P P2 0.45911(20) 0.0955(2) 0.2540(11) 0.00000 1.00000 Uiso P Na1 0.6114(3) 0.2140(2) 0.2566(15) 0.00000 1.00000 Uiso Na O1 0.6752(5) 0.0935(6) 0.9937(15) 0.00000 1.00000 Uiso O O2 0.6562(5) 0.0964(6) 0.4482(16) 0.00000 1.00000 Uiso O O3 0.5912(4) 0.2153(4) 0.7796(19) 0.00000 1.00000 Uiso O O4 0.4856(5) 0.0961(5) 0.5118(14) 0.00000 1.00000 Uiso O O5 0.5116(5) 0.1148(5) 1.0449(15) 0.00000 1.00000 Uiso O O6 0.5701(5) -0.0225(4) 0.7890(18) 0.00000 1.00000 Uiso O C1 0.7031(7) -0.0341(6) 0.288(3) 0.00000 1.00000 Uiso C H1A 0.75210 -0.04870 0.34280 0.00000 1.00000 Uiso H H1B 0.69170 -0.05790 0.13330 0.00000 1.00000 Uiso H H1C 0.66640 -0.04630 0.40930 0.00000 1.00000 Uiso H C2 0.3806(5) 0.1634(6) 0.236(3) 0.00000 1.00000 Uiso C H2A 0.34350 0.14590 0.12500 0.00000 1.00000 Uiso H H2B 0.40010 0.21090 0.18550 0.00000 1.00000 Uiso H H2C 0.35930 0.16830 0.40150 0.00000 1.00000 Uiso H OW1 0.75000 0.25000 0.227(6) 0.00000 0.50000 Uiso O # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Sc1 O1 2.211(9) . Sc1 O2 2.100(9) . Sc1 O3 2.169(8) . Sc1 O4 2.048(9) . Sc1 O5 2.057(9) . Sc1 O6 2.109(8) . P1 O1 1.50(1) 1_554 P1 O2 1.50(1) . P1 O3 1.522(9) 2_644 P1 C1 1.80(1) . P2 O4 1.47(1) . P2 O5 1.50(1) 1_554 P2 O6 1.417(9) 5_656 P2 C2 1.85(1) . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Sc1 O2 86.7(6) . . ? O1 Sc1 O3 82.0(5) . . ? O1 Sc1 O4 178.4(7) . . ? O1 Sc1 O5 87.4(6) . . ? O1 Sc1 O6 87.8(6) . . ? O2 Sc1 O3 89.3(6) . . ? O2 Sc1 O4 94.9(6) . . ? O2 Sc1 O5 167.6(7) . . ? O2 Sc1 O6 98.7(6) . . ? O3 Sc1 O4 97.9(6) . . ? O3 Sc1 O5 79.1(5) . . ? O3 Sc1 O6 166.6(6) . . ? O4 Sc1 O5 91.0(6) . . ? O4 Sc1 O6 92.0(6) . . ? O5 Sc1 O6 91.8(6) . . ? O1 P1 O2 110.7(9) 1_554 . ? O1 P1 O3 110.4(9) 1_554 2_644 ? O1 P1 C1 116(1) 1_554 . ? O2 P1 O3 108.9(9) . 2_644 ? O2 P1 C1 104(1) . . ? O3 P1 C1 105.9(9) 2_644 . ? O4 P2 O5 120.5(9) . 1_554 ? O4 P2 O6 106.3(9) . 5_656 ? O4 P2 C2 107(1) . . ? O5 P2 O6 108.3(9) 1_554 5_656 ? O5 P2 C2 106.3(9) 1_554 . ? O6 P2 C2 108.3(9) 5_656 . ?