#------------------------------------------------------------------------------ #$Date: 2014-07-11 19:31:04 +0200 (Fri, 11 Jul 2014) $ #$Revision: 120073 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/14/4001477.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4001477 loop_ _publ_author_name 'Ewald, Bastian' 'Prots, Yurii' 'Kudla, Christian' 'Gr\"uner, Daniel' 'Cardoso-Gil, Raul' 'Kniep, R\"udiger' _publ_section_title ; Crystal Structure and Thermochemical Properties of a First Scandium Borophosphate, Sc(H2O)2[BP2O8]·H2O ; _journal_issue 3 _journal_name_full 'Chemistry of Materials' _journal_page_first 673 _journal_volume 18 _journal_year 2006 _chemical_formula_sum 'B H6 O11 P2 Sc' _chemical_formula_weight 299.76 _chemical_name_systematic ; Diaqua-scandium catena-monoboro-bisphosphate monohydrate ; _space_group_IT_number 179 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall 'P 65 2 (0 0 1)' _symmetry_space_group_name_H-M 'P 65 2 2' _audit_creation_date 2005-05-24 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 6 _cell_length_a 9.5752(3) _cell_length_b 9.5752(3) _cell_length_c 15.8145(6) _cell_measurement_temperature 293(2) _cell_volume 1255.69(7) _computing_cell_refinement 'CSD (Akselrud, 1993)' _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 295.15 _diffrn_detector_area_resol_mean 14.6199 _diffrn_measured_fraction_theta_full 0.972 _diffrn_measured_fraction_theta_max 0.972 _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_measurement_device 'Rigaku AFC7' _diffrn_measurement_method oscillation _diffrn_radiation_detector 'Mercury CCD' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 13913 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_reflns_theta_full 33.5 _diffrn_reflns_theta_max 33.5 _diffrn_reflns_theta_min 2.77 _diffrn_source_current 40.0000 _diffrn_source_power 2.0000 _diffrn_source_voltage 50.0000 _exptl_absorpt_coefficient_mu 1.313 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8752 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular shape' _exptl_crystal_F_000 900 _exptl_crystal_size_max 0.125 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.075 _refine_diff_density_max 0.473 _refine_diff_density_min -0.515 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(5) _refine_ls_extinction_coef 0.0017(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_goodness_of_fit_ref 1.275 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 82 _refine_ls_number_reflns 1585 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.275 _refine_ls_R_factor_gt 0.033 _refine_ls_shift/su_max 0.001 _refine_ls_structure_factor_coef Fsqd _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_weighting_scheme calc _refine_ls_wR_factor_ref 0.080 _reflns_number_gt 1555 _reflns_number_total 1585 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file cm051577osi20050719_102835.cif _[local]_cod_data_source_block BE_H041b _[local]_cod_cif_authors_sg_H-M P6(5)22 _[local]_cod_chemical_formula_sum_orig 'H6 B O11 P2 Sc' _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 4001477 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' 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 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) 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_ _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 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_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 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_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) _journal_paper_doi 10.1021/cm051577o