# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FI _publ_contact_author_name 'Dr Hoffmann, Stefan' _publ_contact_author_email Ruediger.Kniep@cpfs.mpg.de loop_ _publ_author_name Y.Zhou S.Hoffmann P.Menezes C.-C.Wilder Y.-X.Huang ; L.Vasylechko ; M.Schmidt Yu.Prots J.-F.Deng J.Mi R.Kniep data_H3O{Ti2[B-PO4-4}H2O _database_code_depnum_ccdc_archive 'CCDC 833370' #TrackingRef 'H3O{Ti2[B-PO4-4}H2O.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2011-08-25 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_analytical ? _chemical_formula_sum 'H5 B O18 P4 Ti2' _chemical_formula_weight 523.53 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_space_group_name_H-M I41/amd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'y+1/4, x+3/4, -z+1/4' 'y+1/4, -x+1/4, z+3/4' '-y+1/4, x+3/4, z+1/4' '-y+1/4, -x+1/4, -z+3/4' 'x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1, -y+1/2, z+1' '-x+1, y+1/2, -z+1' 'y+3/4, x+5/4, -z+3/4' 'y+3/4, -x+3/4, z+5/4' '-y+3/4, x+5/4, z+3/4' '-y+3/4, -x+3/4, -z+5/4' '-x, -y, -z' '-x, y, z' 'x-1/2, y, -z-1/2' 'x-1/2, -y, z-1/2' '-y-1/4, -x-3/4, z-1/4' '-y-1/4, x-1/4, -z-3/4' 'y-1/4, -x-3/4, -z-1/4' 'y-1/4, x-1/4, z-3/4' '-x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x, y+1/2, -z' 'x, -y+1/2, z' '-y+1/4, -x-1/4, z+1/4' '-y+1/4, x+1/4, -z-1/4' 'y+1/4, -x-1/4, -z+1/4' 'y+1/4, x+1/4, z-1/4' _cell_length_a 6.3213(4) _cell_length_b 6.3213(4) _cell_length_c 16.461(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 657.76(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2960 _cell_measurement_theta_min 2.3599 _cell_measurement_theta_max 31.505 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.045 _exptl_crystal_size_min 0.045 _exptl_crystal_density_diffrn 2.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.811 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6449 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 14.6306 _diffrn_orient_matrix_type d*Trek _diffrn_orient_matrix_ub_11 -0.0422 _diffrn_orient_matrix_ub_12 -0.0976 _diffrn_orient_matrix_ub_13 -0.0346 _diffrn_orient_matrix_ub_21 0.0116 _diffrn_orient_matrix_ub_22 0.0327 _diffrn_orient_matrix_ub_23 -0.1063 _diffrn_orient_matrix_ub_31 0.028 _diffrn_orient_matrix_ub_32 -0.0119 _diffrn_orient_matrix_ub_33 -0.0006 _diffrn_measurement_device ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_unetI/netI 0.0346 _diffrn_reflns_number 2356 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 29.98 _diffrn_reflns_theta_full 29.98 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _reflns_number_total 280 _reflns_number_gt 268 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process 'Lp corrections applied' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution ; ???? ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens no #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0278P)^2^+2.2513P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_number_reflns 280 _refine_ls_number_parameters 32 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.028 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.289 _refine_ls_restrained_S_all 1.289 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.64 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.107 #----------------------------------------------------------------------------# # 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 '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' 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 Ti1 Ti 0 0.25 0.375 0.0064(3) Uani 1 8 d S . . P1 P 0 0.1729(2) 0.17227(8) 0.0059(3) Uani 0.5 2 d SP . . B1 B 0 0.75 0.125 0.005(2) Uiso 0.5 8 d SP . . O1 O 0 0.25 0.25839(19) 0.0115(6) Uani 1 4 d S . . O2 O 0 0.5563(3) 0.37551(12) 0.0107(5) Uani 1 2 d S . . O3 O 0 0.5695(7) 0.1802(2) 0.0131(9) Uani 0.5 2 d SP . . O4 O 0 0 0 0.069(6) Uani 0.25 4 d SP . . O5 O 0 0.634(6) 0.048(2) 0.069(6) Uani 0.125 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 Ti1 0.0065(4) 0.0065(4) 0.0061(5) 0 0 0 P1 0.0058(6) 0.0063(5) 0.0057(7) -0.0006(5) 0 0 O1 0.0143(14) 0.0138(14) 0.0065(14) 0 0 0 O2 0.0165(11) 0.0063(9) 0.0093(10) -0.0017(7) 0 0 O3 0.021(2) 0.0080(19) 0.010(2) 0.0013(15) 0 0 O4 0.087(15) 0.066(14) 0.053(13) -0.037(11) 0 0 O5 0.087(15) 0.066(14) 0.053(13) -0.037(11) 0 0 #----------------------------------------------------------------------------# # 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 Ti1 O1 1.919(3) 13_445 ? Ti1 O1 1.919(3) . ? Ti1 O2 1.936(2) . ? Ti1 O2 1.936(2) 30_556 ? Ti1 O2 1.936(2) 11_454 ? Ti1 O2 1.936(2) 13_445 ? P1 O1 1.499(3) . ? P1 O2 1.526(2) 6_454 ? P1 O2 1.526(2) 21_665 ? P1 O3 1.538(5) 11_454 ? B1 O3 1.459(4) 5_455 ? B1 O3 1.459(4) 11_464 ? B1 O3 1.459(4) . ? B1 O3 1.459(4) 22_666 ? 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 Ti1 O1 180 13_445 . ? O1 Ti1 O2 89.75(6) 13_445 . ? O1 Ti1 O2 90.25(6) . . ? O1 Ti1 O2 90.25(6) 13_445 30_556 ? O1 Ti1 O2 89.75(6) . 30_556 ? O2 Ti1 O2 90.0010(10) . 30_556 ? O1 Ti1 O2 89.75(6) 13_445 11_454 ? O1 Ti1 O2 90.25(6) . 11_454 ? O2 Ti1 O2 179.50(12) . 11_454 ? O2 Ti1 O2 90.0010(10) 30_556 11_454 ? O1 Ti1 O2 90.25(6) 13_445 13_445 ? O1 Ti1 O2 89.75(6) . 13_445 ? O2 Ti1 O2 90.0010(10) . 13_445 ? O2 Ti1 O2 179.50(12) 30_556 13_445 ? O2 Ti1 O2 90.0010(10) 11_454 13_445 ? O1 P1 O2 111.90(10) . 6_454 ? O1 P1 O2 111.90(10) . 21_665 ? O2 P1 O2 106.70(17) 6_454 21_665 ? O1 P1 O3 104.11(18) . 11_454 ? O2 P1 O3 111.16(10) 6_454 11_454 ? O2 P1 O3 111.16(10) 21_665 11_454 ? O3 B1 O3 112.84(18) 5_455 11_464 ? O3 B1 O3 112.84(18) 5_455 . ? O3 B1 O3 102.9(3) 11_464 . ? O3 B1 O3 102.9(3) 5_455 22_666 ? O3 B1 O3 112.84(18) 11_464 22_666 ? O3 B1 O3 112.84(18) . 22_666 ? # END of CIF # Attachment 'K{Ti2[B-PO4-4]}H2O.cif' #\#CIF_1.1 data_K{Ti2[B(PO4)4]}*H2O _database_code_depnum_ccdc_archive 'CCDC 833371' #TrackingRef 'K{Ti2[B-PO4-4]}H2O.cif' _audit_creation_date 2011-08-25T11:11:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_analytical ? _chemical_formula_sum 'H2 B K O17 P4 Ti2' _chemical_formula_weight 543.61 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_space_group_name_H-M I41/amd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' 'x, -y, -z' '-x, y+1/2, -z' '-y+1/4, -x+1/4, -z+3/4' 'y+1/4, x+3/4, -z+1/4' 'y+1/4, -x+1/4, z+3/4' '-y+1/4, x+3/4, z+1/4' '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' '-y+3/4, -x+3/4, -z+5/4' 'y+3/4, x+5/4, -z+3/4' 'y+3/4, -x+3/4, z+5/4' '-y+3/4, x+5/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' '-x, y, z' 'x, -y-1/2, z' 'y-1/4, x-1/4, z-3/4' '-y-1/4, -x-3/4, z-1/4' '-y-1/4, x-1/4, -z-3/4' 'y-1/4, -x-3/4, -z-1/4' '-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' 'y+1/4, x+1/4, z-1/4' '-y+1/4, -x-1/4, z+1/4' '-y+1/4, x+1/4, -z-1/4' 'y+1/4, -x-1/4, -z+1/4' _cell_length_a 6.3150(5) _cell_length_b 6.3150(5) _cell_length_c 16.375(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 653.02(13) _cell_formula_units_Z 2 _cell_measurement_temperature 295.15 _cell_measurement_reflns_used 8419 _cell_measurement_theta_min 2.3636 _cell_measurement_theta_max 32.2921 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Prism _exptl_crystal_colour 'light Bluish white' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.765 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.135 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5763 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 28.5714 _diffrn_orient_matrix_type d*Trek _diffrn_orient_matrix_ub_11 0.0309 _diffrn_orient_matrix_ub_12 -0.0758 _diffrn_orient_matrix_ub_13 0.0764 _diffrn_orient_matrix_ub_21 0.0618 _diffrn_orient_matrix_ub_22 -0.0526 _diffrn_orient_matrix_ub_23 -0.0771 _diffrn_orient_matrix_ub_31 0.024 _diffrn_orient_matrix_ub_32 0.0173 _diffrn_orient_matrix_ub_33 0.0075 _diffrn_measurement_device ; Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_unetI/netI 0.016 _diffrn_reflns_number 2596 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 29.98 _diffrn_reflns_theta_full 29.98 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 278 _reflns_number_gt 273 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process 'Lp corrections applied' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; ???? ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens no #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0226P)^2^+1.6206P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_number_reflns 278 _refine_ls_number_parameters 37 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0214 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.381 _refine_ls_restrained_S_all 1.381 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.254 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.071 #----------------------------------------------------------------------------# # 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ti1 Ti 0 0.25 0.375 0.0068(2) Uani 1 8 d S . . P1 P 0 0.1730(2) 0.17158(7) 0.0070(3) Uani 0.5 2 d SP . . B1 B 0 0.75 0.125 0.009(2) Uani 0.5 8 d SP . . O1 O 0 0.25 0.25781(16) 0.0140(5) Uani 1 4 d S . . O2 O 0 0.5563(3) 0.37452(10) 0.0114(4) Uani 1 2 d S . . O3 O 0 0.5688(6) 0.1802(2) 0.0136(7) Uani 0.5 2 d SP . . K1 K 0 0 0 0.085(3) Uani 0.25 4 d SP . . O4 O 0 0.673(5) 0.090(2) 0.081(14) Uani 0.125 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 Ti1 0.0068(3) 0.0068(3) 0.0068(4) 0 0 0 P1 0.0066(5) 0.0079(4) 0.0064(5) -0.0006(4) 0 0 B1 0.011(4) 0.011(4) 0.006(5) 0 0 0 O1 0.0151(12) 0.0200(13) 0.0070(11) 0 0 0 O2 0.0168(9) 0.0073(8) 0.0100(8) -0.0010(6) 0 0 O3 0.0187(18) 0.0093(15) 0.0130(15) 0.0014(12) 0 0 K1 0.095(6) 0.106(6) 0.055(4) -0.063(4) 0 0 O4 0.040(15) 0.05(2) 0.16(5) 0.04(2) 0 0 #----------------------------------------------------------------------------# # 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 Ti1 O1 1.919(3) . ? Ti1 O1 1.919(3) 5 ? Ti1 O2 1.9344(17) . ? Ti1 O2 1.9344(17) 14_445 ? Ti1 O2 1.9344(17) 2 ? Ti1 O2 1.9344(17) 5 ? P1 O1 1.493(3) . ? P1 O2 1.5253(17) 29_455 ? P1 O2 1.5253(17) 22_665 ? P1 O3 1.534(4) 2 ? B1 O3 1.458(4) 2_565 ? B1 O3 1.458(4) 6_455 ? B1 O3 1.458(4) 13_554 ? B1 O3 1.458(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 _geom_angle_publ_flag O1 Ti1 O1 180 . 5 ? O1 Ti1 O2 89.76(5) . . ? O1 Ti1 O2 90.24(5) 5 . ? O1 Ti1 O2 90.24(5) . 14_445 ? O1 Ti1 O2 89.76(5) 5 14_445 ? O2 Ti1 O2 90.0010(10) . 14_445 ? O1 Ti1 O2 89.76(5) . 2 ? O1 Ti1 O2 90.24(5) 5 2 ? O2 Ti1 O2 179.53(10) . 2 ? O2 Ti1 O2 90 14_445 2 ? O1 Ti1 O2 90.24(5) . 5 ? O1 Ti1 O2 89.76(5) 5 5 ? O2 Ti1 O2 90.0010(10) . 5 ? O2 Ti1 O2 179.53(10) 14_445 5 ? O2 Ti1 O2 90.0010(10) 2 5 ? O1 P1 O2 111.95(8) . 29_455 ? O1 P1 O2 111.95(8) . 22_665 ? O2 P1 O2 106.62(14) 29_455 22_665 ? O1 P1 O3 103.73(15) . 2 ? O2 P1 O3 111.35(9) 29_455 2 ? O2 P1 O3 111.35(9) 22_665 2 ? O3 B1 O3 112.60(15) 2_565 13_554 ? O3 B1 O3 103.4(3) 6_455 13_554 ? O3 B1 O3 103.4(3) 2_565 . ? O3 B1 O3 112.60(15) 6_455 . ? O3 B1 O3 112.60(15) 13_554 . ? # END of CIF