#------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_BE_H041b #------------------ SUBMISSION DETAILS --------------------------------------# # Name and address of author for correspondence _publ_contact_author_name 'Kniep, R\"udiger' _publ_contact_author_address ; Max-Planck Institut f\"ur Chemische Physik fester Stoffe N\"othnitzer Str. 40 D-01187 Dresden Germany ; _publ_contact_author_email kniep@cpfs.mpg.de _publ_contact_author_fax '49(351)46463002' _publ_contact_author_phone '49(351)46463000' _publ_requested_journal 'Chemistry of Materials' #------------------ TITLE AND AUTHOR LIST------------------------------------# _publ_section_title ; Crystal Structure and Properties of a First Scandium Borophosphate, Sc(H20)2[BP2O8]·H20 ; loop_ _publ_author_name _publ_author_address 'Ewald, Bastian' ; Max-Planck Institut f\"ur Chemische Physik fester Stoffe N\"othnitzer Str. 40 01187 Dresden Germany ; 'Prots, Yurii' ; Max-Planck Institut f\"ur Chemische Physik fester Stoffe N\"othnitzer Str. 40 01187 Dresden Germany ; 'Menezes, Prashanth' ; Max-Planck Institut f\"ur Chemische Physik fester Stoffe N\"othnitzer Str. 40 01187 Dresden Germany ; 'Srinivisan, Natarajan' ; Framework Solids Laboratory, Solid State and Structural Chemistry Unit, Indian Institute of Science Bangalore 560012 India ; 'Kniep, R\"udiger' ; Max-Planck Institut f\"ur Chemische Physik fester Stoffe N\"othnitzer Str. 40 01187 Dresden Germany ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# _audit_creation_date 2005-05-24 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_name_systematic ; Diaqua-scandium catena-monoboro-bisphosphate monohydrate ; _chemical_formula_sum 'H6 B O11 P2 Sc' _chemical_formula_weight 299.76 #------------------ UNIT CELL INFORMATION -----------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' 'y, x, -z+2/3' 'x-y, -y, -z' '-x, -x+y, -z+1/3' '-y, -x, -z+1/6' '-x+y, y, -z+1/2' 'x, x-y, -z+5/6' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P6(5)22' _cell_length_a 9.5752(3) _cell_length_b 9.5752(3) _cell_length_c 15.8145(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1255.69(7) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description 'irregular shape' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.125 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.075 _exptl_crystal_density_diffrn 2.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 1.313 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8752 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 295.15 _diffrn_source_power 2.0000 _diffrn_source_voltage 50.0000 _diffrn_source_current 40.0000 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector 'Mercury CCD' _diffrn_measurement_device 'Rigaku AFC7' _diffrn_detector_area_resol_mean 14.6199 _diffrn_measurement_method 'oscillation' _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_details ; scan: Number of images: 400 Slice: -70.0000 - 170.0000 Image width: 0.6000 Exp time: 40.0000 Rotation axis: Phi Omega: 0.0000 Chi: 0.0000 Phi: 0.0000 XTD: 41.9000 2theta: -25.0000 scan: Number of images: 95 Slice: -38.0000 - 19.0000 Image width: 0.6000 Exp time: 40.0000 Rotation axis: Omega Omega: 0.0000 Chi: -90.0000 Phi: 55.0000 XTD: 41.9000 2theta: -25.0000 ; _diffrn_reflns_number 13913 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 33.5 _diffrn_reflns_theta_full 33.5 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measured_fraction_theta_full 0.972 #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CSD (Akselrud, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #------------------ REFINEMENT INFORMATION ----------------------------------# _reflns_number_total 1585 _reflns_number_gt 1555 _reflns_threshold_expression >2sigma(I) _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^)+(0.0113P)^2^+6.1759P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0017(10) _refine_ls_number_reflns 1585 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.033 _refine_ls_wR_factor_ref 0.080 _refine_ls_goodness_of_fit_ref 1.275 _refine_ls_restrained_S_all 1.275 _refine_ls_shift/su_max 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(5) _refine_diff_density_max 0.473 _refine_diff_density_min -0.515 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_symmetry_multiplicity _atom_site_Wyckoff_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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Sc1 Sc 6 b 0.55524(3) 0.11049(6) 0.75 0.01195(11) Uani 1 d S . . P1 P 12 c 0.37645(5) 0.16872(6) 0.58420(3) 0.01103(11) Uani 1 d . . . O1 O 12 c 0.40424(17) 0.17114(17) 0.48673(8) 0.0137(3) Uani 1 d . . . O2 O 12 c 0.20629(17) 0.02422(17) 0.60287(9) 0.0138(3) Uani 1 d . . . O3 O 12 c 0.50368(19) 0.1436(2) 0.62635(9) 0.0180(3) Uani 1 d . . . O4 O 12 c 0.3777(2) 0.32059(19) 0.61117(10) 0.0185(3) Uani 1 d . . . O5 O 12 c 0.4949(3) 0.2919(3) 0.78373(15) 0.0333(5) Uani 1 d . . . H51 H 12 c 0.414(6) 0.269(5) 0.797(3) 0.04 Uiso 1 d . . . H52 H 12 c 0.561(5) 0.376(5) 0.792(2) 0.04 Uiso 1 d . . . O6 O 12 c 0.1795(10) 0.1592(11) 0.8528(12) 0.091(5) Uani 0.5 d P . . B1 B 6 b 0.2919(3) 0.14595(17) 0.4167 0.0128(5) Uani 1 d S . . 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 0.01212(16) 0.0120(2) 0.01170(19) 0 -0.00248(14) 0.00600(10) P1 0.01166(19) 0.01095(19) 0.00970(18) 0.00087(15) -0.00083(15) 0.00506(15) O1 0.0127(6) 0.0163(6) 0.0102(5) 0.0018(4) -0.0007(4) 0.0059(5) O2 0.0137(6) 0.0104(5) 0.0154(6) 0.0004(5) 0.0022(5) 0.0045(5) O3 0.0176(7) 0.0247(8) 0.0143(6) 0.0024(5) -0.0034(5) 0.0125(6) O4 0.0238(7) 0.0127(6) 0.0181(6) -0.0007(5) 0.0006(6) 0.0086(6) O5 0.0389(11) 0.0284(9) 0.0431(11) -0.0166(9) -0.0182(10) 0.0247(9) O6 0.073(5) 0.093(6) 0.144(16) -0.010(6) 0.002(6) 0.070(4) B1 0.0132(10) 0.0139(9) 0.0111(10) 0.0010(8) 0 0.0066(5) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 O4 2.0523(16) 5 ? Sc1 O4 2.0523(16) 9_656 ? Sc1 O3 2.0795(14) 11_656 ? Sc1 O3 2.0795(14) . ? Sc1 O5 2.154(2) 11_656 ? Sc1 O5 2.154(2) . ? P1 O4 1.5097(16) . ? P1 O3 1.5098(15) . ? P1 O2 1.5498(15) . ? P1 O1 1.5624(14) . ? O1 B1 1.478(2) . ? O2 B1 1.464(2) 5 ? O4 Sc1 2.0523(16) 6_554 ? O5 H51 0.72(5) . ? O5 H52 0.75(4) . ? O6 O6 0.70(3) 7_556 ? B1 O2 1.464(2) 6_554 ? B1 O2 1.464(2) 8_556 ? B1 O1 1.478(2) 12 ? 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 O4 Sc1 O4 94.75(10) 5 9_656 ? O4 Sc1 O3 96.22(6) 5 11_656 ? O4 Sc1 O3 94.04(6) 9_656 11_656 ? O4 Sc1 O3 94.04(6) 5 . ? O4 Sc1 O3 96.22(6) 9_656 . ? O3 Sc1 O3 164.83(10) 11_656 . ? O4 Sc1 O5 177.08(8) 5 11_656 ? O4 Sc1 O5 86.98(9) 9_656 11_656 ? O3 Sc1 O5 85.99(8) 11_656 11_656 ? O3 Sc1 O5 83.43(7) . 11_656 ? O4 Sc1 O5 86.98(9) 5 . ? O4 Sc1 O5 177.08(8) 9_656 . ? O3 Sc1 O5 83.43(7) 11_656 . ? O3 Sc1 O5 85.99(8) . . ? O5 Sc1 O5 91.40(15) 11_656 . ? O4 P1 O3 114.23(10) . . ? O4 P1 O2 107.73(9) . . ? O3 P1 O2 110.21(9) . . ? O4 P1 O1 110.19(8) . . ? O3 P1 O1 107.03(8) . . ? O2 P1 O1 107.24(8) . . ? B1 O1 P1 129.25(13) . . ? B1 O2 P1 127.38(12) 5 . ? P1 O3 Sc1 135.35(10) . . ? P1 O4 Sc1 147.29(10) . 6_554 ? Sc1 O5 H51 120(4) . . ? Sc1 O5 H52 120(3) . . ? H51 O5 H52 119(5) . . ? O2 B1 O2 103.0(2) 6_554 8_556 ? O2 B1 O1 112.66(8) 6_554 . ? O2 B1 O1 113.53(8) 8_556 . ? O2 B1 O1 113.53(8) 6_554 12 ? O2 B1 O1 112.66(8) 8_556 12 ? O1 B1 O1 101.8(2) . 12 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O5 H51 O6 . 0.72(5) 2.14(5) 2.844(13) 167(5) O5 H51 O6 7_556 0.72(5) 2.16(5) 2.874(12) 170(5) O5 H52 O1 3_665 0.75(4) 2.09(4) 2.828(3) 171(4)