# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Hill, Matthew' _publ_contact_author_email matthew.hill@csiro.au _publ_section_title ; A Simple Route to Full Structural Analysis of Biophosphates and their Application to Materials Discovery ; loop_ _publ_author_name M.Hill T.Bastow L.Bourgeois D.Turner A.Seeber K.McBean ; H.Whitfield ; # Attachment '- LTBa2Ca2P2O7amended.CIF' data_final _database_code_depnum_ccdc_archive 'CCDC 862497' #TrackingRef '- LTBa2Ca2P2O7amended.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'O7 P2, Ba, Ca' _chemical_formula_sum 'Ba Ca O7 P2' _chemical_formula_weight 351.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ba Ba -0.2820 2.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2290 0.3080 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.065(2) _cell_length_b 10.583(2) _cell_length_c 9.515(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.610(5) _cell_angle_gamma 90.00 _cell_volume 1211.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17063 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 27.08 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 7.919 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9250 _exptl_absorpt_correction_T_max 0.9250 _exptl_absorpt_process_details 'XDS (Kabsch, 1993)' _exptl_special_details ; High R(int) due to small, low quality sample and weak diffraction. Examination of absences and symmetry shows unambiguous space group selection. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71079 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Australian Synchrotron 3ID1' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 315r' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17063 _diffrn_reflns_av_R_equivalents 0.1747 _diffrn_reflns_av_sigmaI/netI 0.0922 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.08 _reflns_number_total 2613 _reflns_number_gt 2060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BluIce (McPhillips, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 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^)+(0.0939P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0136(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2613 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1486 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _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 Ba1 Ba 0.34356(5) 0.30840(6) 0.90789(6) 0.0098(2) Uani 1 1 d . . . Ba2 Ba 0.08429(5) 0.01314(6) 0.72517(6) 0.0091(2) Uani 1 1 d . . . Ca1 Ca 0.21673(15) 0.6539(2) 0.8270(2) 0.0081(4) Uani 1 1 d . . . Ca2 Ca 0.65182(16) 0.07652(19) 1.0107(2) 0.0081(4) Uani 1 1 d . . . P1 P 0.5022(2) 0.5928(3) 0.7568(3) 0.0076(5) Uani 1 1 d . . . P2 P 0.6568(2) 0.3955(3) 0.8834(3) 0.0078(5) Uani 1 1 d . . . P3 P 0.1588(2) 0.3610(3) 0.6128(3) 0.0077(5) Uani 1 1 d . . . P4 P -0.0604(2) 0.2713(3) 0.4705(3) 0.0077(5) Uani 1 1 d . . . O1 O 0.5487(6) 0.7089(7) 0.8278(8) 0.0126(16) Uani 1 1 d . . . O2 O 0.3768(6) 0.5743(7) 0.7437(7) 0.0102(15) Uani 1 1 d . . . O3 O 0.5466(6) 0.5767(7) 0.6105(8) 0.0104(15) Uani 1 1 d . . . O4 O 0.5412(6) 0.4697(7) 0.8513(8) 0.0104(15) Uani 1 1 d . . . O5 O 0.6201(6) 0.2866(7) 0.9684(8) 0.0121(16) Uani 1 1 d . . . O6 O 0.7038(6) 0.3639(7) 0.7439(8) 0.0113(15) Uani 1 1 d . . . O7 O 0.7360(6) 0.4822(7) 0.9697(8) 0.0109(15) Uani 1 1 d . . . O8 O 0.2245(6) 0.4020(7) 0.4909(8) 0.0120(15) Uani 1 1 d . . . O9 O 0.1904(6) 0.2306(7) 0.6617(8) 0.0114(15) Uani 1 1 d . . . O10 O 0.1604(6) 0.4553(7) 0.7332(8) 0.0112(15) Uani 1 1 d . . . O11 O 0.0305(6) 0.3646(7) 0.5482(8) 0.0103(15) Uani 1 1 d . . . O12 O -0.0525(6) 0.2827(7) 0.3129(8) 0.0107(15) Uani 1 1 d . . . O13 O -0.1684(6) 0.3228(8) 0.5196(8) 0.0121(16) Uani 1 1 d . . . O14 O -0.0418(6) 0.1375(7) 0.5218(8) 0.0130(16) Uani 1 1 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 Ba1 0.0069(3) 0.0105(4) 0.0121(4) -0.0008(2) -0.0001(2) 0.0003(2) Ba2 0.0051(3) 0.0101(4) 0.0120(4) 0.0000(2) -0.0003(2) 0.0002(2) Ca1 0.0024(9) 0.0095(10) 0.0124(10) -0.0005(8) 0.0005(7) -0.0002(7) Ca2 0.0045(9) 0.0088(10) 0.0109(10) -0.0006(8) 0.0000(7) -0.0012(8) P1 0.0038(11) 0.0099(12) 0.0091(12) -0.0005(11) 0.0001(9) -0.0003(10) P2 0.0034(11) 0.0084(12) 0.0116(13) 0.0003(11) 0.0007(9) -0.0006(9) P3 0.0053(11) 0.0088(13) 0.0087(12) 0.0007(10) -0.0012(9) -0.0012(9) P4 0.0036(11) 0.0097(13) 0.0100(13) -0.0005(11) 0.0014(9) -0.0014(9) O1 0.012(4) 0.011(4) 0.016(4) 0.004(3) 0.005(3) 0.001(3) O2 0.003(3) 0.017(4) 0.011(4) 0.000(3) 0.000(3) 0.000(3) O3 0.006(3) 0.017(4) 0.009(3) 0.003(3) 0.005(3) -0.003(3) O4 0.005(3) 0.010(4) 0.017(4) -0.001(3) 0.003(3) 0.000(3) O5 0.012(4) 0.009(4) 0.016(4) -0.003(3) 0.001(3) 0.004(3) O6 0.005(3) 0.012(4) 0.017(4) -0.007(3) 0.000(3) 0.000(3) O7 0.008(4) 0.011(4) 0.013(4) 0.001(3) -0.004(3) -0.004(3) O8 0.010(4) 0.011(4) 0.016(4) 0.005(3) 0.005(3) 0.002(3) O9 0.004(3) 0.012(4) 0.017(4) -0.001(3) -0.003(3) -0.002(3) O10 0.003(3) 0.015(4) 0.014(4) 0.001(3) -0.002(3) -0.003(3) O11 0.009(3) 0.010(4) 0.011(4) 0.001(3) -0.005(3) -0.001(3) O12 0.007(3) 0.017(4) 0.010(4) -0.006(3) 0.005(3) -0.004(3) O13 0.005(3) 0.020(4) 0.012(4) 0.003(3) 0.004(3) 0.004(3) O14 0.009(4) 0.010(4) 0.020(4) 0.001(3) 0.001(3) 0.004(3) _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 Ba1 O7 2.714(8) 3_667 ? Ba1 O1 2.743(8) 3_667 ? Ba1 O8 2.798(7) 4_566 ? Ba1 O3 2.799(7) 2_646 ? Ba1 O1 2.880(8) 2_646 ? Ba1 O9 2.980(7) . ? Ba1 O4 3.016(7) . ? Ba1 O10 3.078(7) . ? Ba1 O9 3.184(8) 4_566 ? Ba1 O2 3.259(8) . ? Ba2 O14 2.705(7) . ? Ba2 O9 2.725(8) . ? Ba2 O14 2.852(8) 3_556 ? Ba2 O12 2.883(7) 4_566 ? Ba2 O7 2.982(8) 2_646 ? Ba2 O6 3.000(7) 2_646 ? Ba2 O8 3.062(7) 4_566 ? Ba2 O10 3.071(7) 2_546 ? Ba2 O11 3.086(8) 2_546 ? Ba2 O12 3.171(8) 3_556 ? Ba2 O13 3.254(8) 2_546 ? Ca1 O2 2.305(7) . ? Ca1 O10 2.362(8) . ? Ca1 O12 2.393(8) 3_566 ? Ca1 O13 2.409(8) 2_556 ? Ca1 O7 2.442(8) 3_667 ? Ca1 O6 2.533(8) 2_656 ? Ca1 O14 2.654(8) 2_556 ? Ca1 O5 2.729(8) 3_667 ? Ca2 O5 2.287(8) . ? Ca2 O3 2.310(8) 4_566 ? Ca2 O6 2.344(8) 4_566 ? Ca2 O8 2.375(8) 2_646 ? Ca2 O13 2.412(7) 4_666 ? Ca2 O2 2.418(7) 2_646 ? Ca2 O3 2.573(7) 2_646 ? P1 O1 1.489(8) . ? P1 O2 1.521(7) . ? P1 O3 1.541(7) . ? P1 O4 1.631(8) . ? P2 O5 1.495(8) . ? P2 O7 1.518(7) . ? P2 O6 1.521(8) . ? P2 O4 1.609(7) . ? P3 O9 1.495(8) . ? P3 O10 1.518(8) . ? P3 O8 1.520(8) . ? P3 O11 1.619(7) . ? P4 O14 1.509(8) . ? P4 O12 1.515(8) . ? P4 O13 1.521(7) . ? P4 O11 1.610(7) . ? O1 Ba1 2.743(8) 3_667 ? O1 Ba1 2.880(8) 2_656 ? O2 Ca2 2.418(7) 2_656 ? O3 Ca2 2.310(8) 4_565 ? O3 Ca2 2.573(7) 2_656 ? O3 Ba1 2.799(7) 2_656 ? O5 Ca1 2.729(8) 3_667 ? O6 Ca2 2.344(8) 4_565 ? O6 Ca1 2.533(8) 2_646 ? O6 Ba2 3.000(7) 2_656 ? O7 Ca1 2.442(8) 3_667 ? O7 Ba1 2.714(8) 3_667 ? O7 Ba2 2.982(8) 2_656 ? O8 Ca2 2.375(8) 2_656 ? O8 Ba1 2.798(7) 4_565 ? O8 Ba2 3.062(7) 4_565 ? O9 Ba1 3.184(8) 4_565 ? O10 Ba2 3.071(7) 2_556 ? O11 Ba2 3.086(8) 2_556 ? O12 Ca1 2.393(8) 3_566 ? O12 Ba2 2.883(7) 4_565 ? O12 Ba2 3.171(8) 3_556 ? O13 Ca1 2.409(8) 2_546 ? O13 Ca2 2.412(7) 4_465 ? O13 Ba2 3.254(8) 2_556 ? O14 Ca1 2.654(8) 2_546 ? O14 Ba2 2.852(8) 3_556 ? 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 O7 Ba1 O1 79.6(2) 3_667 3_667 ? O7 Ba1 O8 108.7(2) 3_667 4_566 ? O1 Ba1 O8 84.5(2) 3_667 4_566 ? O7 Ba1 O3 158.0(2) 3_667 2_646 ? O1 Ba1 O3 78.9(2) 3_667 2_646 ? O8 Ba1 O3 65.0(2) 4_566 2_646 ? O7 Ba1 O1 146.1(2) 3_667 2_646 ? O1 Ba1 O1 118.6(2) 3_667 2_646 ? O8 Ba1 O1 101.7(2) 4_566 2_646 ? O3 Ba1 O1 52.1(2) 2_646 2_646 ? O7 Ba1 O9 110.1(2) 3_667 . ? O1 Ba1 O9 157.0(2) 3_667 . ? O8 Ba1 O9 72.7(2) 4_566 . ? O3 Ba1 O9 88.6(2) 2_646 . ? O1 Ba1 O9 65.0(2) 2_646 . ? O7 Ba1 O4 85.8(2) 3_667 . ? O1 Ba1 O4 83.0(2) 3_667 . ? O8 Ba1 O4 158.8(2) 4_566 . ? O3 Ba1 O4 95.7(2) 2_646 . ? O1 Ba1 O4 69.8(2) 2_646 . ? O9 Ba1 O4 117.7(2) . . ? O7 Ba1 O10 63.6(2) 3_667 . ? O1 Ba1 O10 142.7(2) 3_667 . ? O8 Ba1 O10 101.1(2) 4_566 . ? O3 Ba1 O10 137.0(2) 2_646 . ? O1 Ba1 O10 96.5(2) 2_646 . ? O9 Ba1 O10 48.9(2) . . ? O4 Ba1 O10 99.3(2) . . ? O7 Ba1 O9 62.2(2) 3_667 4_566 ? O1 Ba1 O9 63.7(2) 3_667 4_566 ? O8 Ba1 O9 48.7(2) 4_566 4_566 ? O3 Ba1 O9 103.9(2) 2_646 4_566 ? O1 Ba1 O9 150.3(2) 2_646 4_566 ? O9 Ba1 O9 101.50(19) . 4_566 ? O4 Ba1 O9 136.4(2) . 4_566 ? O10 Ba1 O9 92.29(19) . 4_566 ? O7 Ba1 O2 64.0(2) 3_667 . ? O1 Ba1 O2 115.4(2) 3_667 . ? O8 Ba1 O2 155.29(19) 4_566 . ? O3 Ba1 O2 130.5(2) 2_646 . ? O1 Ba1 O2 82.1(2) 2_646 . ? O9 Ba1 O2 87.38(19) . . ? O4 Ba1 O2 45.25(18) . . ? O10 Ba1 O2 54.26(18) . . ? O9 Ba1 O2 125.24(19) 4_566 . ? O14 Ba2 O9 71.2(2) . . ? O14 Ba2 O14 68.2(3) . 3_556 ? O9 Ba2 O14 110.3(2) . 3_556 ? O14 Ba2 O12 62.6(2) . 4_566 ? O9 Ba2 O12 73.8(2) . 4_566 ? O14 Ba2 O12 126.0(2) 3_556 4_566 ? O14 Ba2 O7 90.2(2) . 2_646 ? O9 Ba2 O7 65.0(2) . 2_646 ? O14 Ba2 O7 61.2(2) 3_556 2_646 ? O12 Ba2 O7 136.4(2) 4_566 2_646 ? O14 Ba2 O6 138.8(2) . 2_646 ? O9 Ba2 O6 93.1(2) . 2_646 ? O14 Ba2 O6 83.2(2) 3_556 2_646 ? O12 Ba2 O6 150.4(2) 4_566 2_646 ? O7 Ba2 O6 49.2(2) 2_646 2_646 ? O14 Ba2 O8 133.6(2) . 4_566 ? O9 Ba2 O8 72.4(2) . 4_566 ? O14 Ba2 O8 153.5(2) 3_556 4_566 ? O12 Ba2 O8 80.3(2) 4_566 4_566 ? O7 Ba2 O8 99.48(19) 2_646 4_566 ? O6 Ba2 O8 70.3(2) 2_646 4_566 ? O14 Ba2 O10 72.4(2) . 2_546 ? O9 Ba2 O10 132.1(2) . 2_546 ? O14 Ba2 O10 83.3(2) 3_556 2_546 ? O12 Ba2 O10 62.2(2) 4_566 2_546 ? O7 Ba2 O10 144.4(2) 2_646 2_546 ? O6 Ba2 O10 134.7(2) 2_646 2_546 ? O8 Ba2 O10 115.14(19) 4_566 2_546 ? O14 Ba2 O11 119.3(2) . 2_546 ? O9 Ba2 O11 146.1(2) . 2_546 ? O14 Ba2 O11 103.3(2) 3_556 2_546 ? O12 Ba2 O11 83.1(2) 4_566 2_546 ? O7 Ba2 O11 140.2(2) 2_646 2_546 ? O6 Ba2 O11 95.18(19) 2_646 2_546 ? O8 Ba2 O11 79.72(19) 4_566 2_546 ? O10 Ba2 O11 47.01(19) 2_546 2_546 ? O14 Ba2 O12 110.1(2) . 3_556 ? O9 Ba2 O12 149.7(2) . 3_556 ? O14 Ba2 O12 48.8(2) 3_556 3_556 ? O12 Ba2 O12 134.93(9) 4_566 3_556 ? O7 Ba2 O12 84.73(19) 2_646 3_556 ? O6 Ba2 O12 65.52(19) 2_646 3_556 ? O8 Ba2 O12 115.9(2) 4_566 3_556 ? O10 Ba2 O12 73.1(2) 2_546 3_556 ? O11 Ba2 O12 61.31(19) 2_546 3_556 ? O14 Ba2 O13 163.5(2) . 2_546 ? O9 Ba2 O13 124.4(2) . 2_546 ? O14 Ba2 O13 107.1(2) 3_556 2_546 ? O12 Ba2 O13 113.5(2) 4_566 2_546 ? O7 Ba2 O13 101.39(19) 2_646 2_546 ? O6 Ba2 O13 52.31(19) 2_646 2_546 ? O8 Ba2 O13 56.41(19) 4_566 2_546 ? O10 Ba2 O13 91.47(19) 2_546 2_546 ? O11 Ba2 O13 45.06(18) 2_546 2_546 ? O12 Ba2 O13 60.11(19) 3_556 2_546 ? O2 Ca1 O10 76.6(3) . . ? O2 Ca1 O12 126.2(3) . 3_566 ? O10 Ca1 O12 80.7(3) . 3_566 ? O2 Ca1 O13 136.9(3) . 2_556 ? O10 Ca1 O13 144.4(3) . 2_556 ? O12 Ca1 O13 84.2(3) 3_566 2_556 ? O2 Ca1 O7 84.7(3) . 3_667 ? O10 Ca1 O7 79.4(3) . 3_667 ? O12 Ca1 O7 137.4(3) 3_566 3_667 ? O13 Ca1 O7 90.6(3) 2_556 3_667 ? O2 Ca1 O6 83.3(3) . 2_656 ? O10 Ca1 O6 141.6(3) . 2_656 ? O12 Ca1 O6 85.4(2) 3_566 2_656 ? O13 Ca1 O6 68.0(3) 2_556 2_656 ? O7 Ca1 O6 131.2(2) 3_667 2_656 ? O2 Ca1 O14 152.6(3) . 2_556 ? O10 Ca1 O14 86.0(2) . 2_556 ? O12 Ca1 O14 70.2(2) 3_566 2_556 ? O13 Ca1 O14 58.5(2) 2_556 2_556 ? O7 Ca1 O14 71.2(2) 3_667 2_556 ? O6 Ca1 O14 122.4(2) 2_656 2_556 ? O2 Ca1 O5 75.7(2) . 3_667 ? O10 Ca1 O5 130.1(2) . 3_667 ? O12 Ca1 O5 148.2(3) 3_566 3_667 ? O13 Ca1 O5 66.0(2) 2_556 3_667 ? O7 Ca1 O5 57.4(2) 3_667 3_667 ? O6 Ca1 O5 73.8(2) 2_656 3_667 ? O14 Ca1 O5 100.8(2) 2_556 3_667 ? O5 Ca2 O3 131.7(3) . 4_566 ? O5 Ca2 O6 86.2(3) . 4_566 ? O3 Ca2 O6 85.0(3) 4_566 4_566 ? O5 Ca2 O8 148.4(3) . 2_646 ? O3 Ca2 O8 79.8(3) 4_566 2_646 ? O6 Ca2 O8 95.5(3) 4_566 2_646 ? O5 Ca2 O13 73.4(3) . 4_666 ? O3 Ca2 O13 144.9(3) 4_566 4_666 ? O6 Ca2 O13 71.1(3) 4_566 4_666 ? O8 Ca2 O13 77.3(3) 2_646 4_666 ? O5 Ca2 O2 79.9(3) . 2_646 ? O3 Ca2 O2 111.5(3) 4_566 2_646 ? O6 Ca2 O2 163.0(3) 4_566 2_646 ? O8 Ca2 O2 91.5(3) 2_646 2_646 ? O13 Ca2 O2 95.5(2) 4_666 2_646 ? O5 Ca2 O3 77.5(3) . 2_646 ? O3 Ca2 O3 70.3(3) 4_566 2_646 ? O6 Ca2 O3 126.4(3) 4_566 2_646 ? O8 Ca2 O3 124.1(3) 2_646 2_646 ? O13 Ca2 O3 144.8(3) 4_666 2_646 ? O2 Ca2 O3 59.9(2) 2_646 2_646 ? O1 P1 O2 118.6(5) . . ? O1 P1 O3 110.8(4) . . ? O2 P1 O3 109.1(4) . . ? O1 P1 O4 109.1(4) . . ? O2 P1 O4 100.6(4) . . ? O3 P1 O4 107.7(4) . . ? O5 P2 O7 112.0(4) . . ? O5 P2 O6 116.7(4) . . ? O7 P2 O6 110.1(4) . . ? O5 P2 O4 100.9(4) . . ? O7 P2 O4 107.8(4) . . ? O6 P2 O4 108.7(4) . . ? O9 P3 O10 112.6(4) . . ? O9 P3 O8 111.4(4) . . ? O10 P3 O8 114.3(4) . . ? O9 P3 O11 110.6(4) . . ? O10 P3 O11 103.0(4) . . ? O8 P3 O11 104.2(4) . . ? O14 P4 O12 112.0(4) . . ? O14 P4 O13 110.2(4) . . ? O12 P4 O13 113.5(4) . . ? O14 P4 O11 110.4(4) . . ? O12 P4 O11 108.1(4) . . ? O13 P4 O11 102.0(4) . . ? P1 O1 Ba1 119.6(4) . 3_667 ? P1 O1 Ba1 97.2(4) . 2_656 ? Ba1 O1 Ba1 121.9(3) 3_667 2_656 ? P1 O2 Ca1 141.3(5) . . ? P1 O2 Ca2 98.2(4) . 2_656 ? Ca1 O2 Ca2 106.5(3) . 2_656 ? P1 O2 Ba1 103.4(3) . . ? Ca1 O2 Ba1 90.7(2) . . ? Ca2 O2 Ba1 118.3(3) 2_656 . ? P1 O3 Ca2 133.8(4) . 4_565 ? P1 O3 Ca2 91.5(3) . 2_656 ? Ca2 O3 Ca2 109.7(3) 4_565 2_656 ? P1 O3 Ba1 99.2(4) . 2_656 ? Ca2 O3 Ba1 108.1(3) 4_565 2_656 ? Ca2 O3 Ba1 113.6(3) 2_656 2_656 ? P2 O4 P1 134.6(5) . . ? P2 O4 Ba1 112.1(4) . . ? P1 O4 Ba1 110.7(3) . . ? P2 O5 Ca2 142.3(5) . . ? P2 O5 Ca1 88.8(3) . 3_667 ? Ca2 O5 Ca1 89.9(2) . 3_667 ? P2 O6 Ca2 132.6(4) . 4_565 ? P2 O6 Ca1 126.9(4) . 2_646 ? Ca2 O6 Ca1 93.5(3) 4_565 2_646 ? P2 O6 Ba2 100.0(3) . 2_656 ? Ca2 O6 Ba2 96.4(3) 4_565 2_656 ? Ca1 O6 Ba2 98.6(2) 2_646 2_656 ? P2 O7 Ca1 99.7(4) . 3_667 ? P2 O7 Ba1 119.8(4) . 3_667 ? Ca1 O7 Ba1 102.1(3) 3_667 3_667 ? P2 O7 Ba2 100.8(4) . 2_656 ? Ca1 O7 Ba2 115.0(3) 3_667 2_656 ? Ba1 O7 Ba2 118.5(3) 3_667 2_656 ? P3 O8 Ca2 126.4(4) . 2_656 ? P3 O8 Ba1 107.4(4) . 4_565 ? Ca2 O8 Ba1 106.3(3) 2_656 4_565 ? P3 O8 Ba2 115.2(4) . 4_565 ? Ca2 O8 Ba2 94.1(2) 2_656 4_565 ? Ba1 O8 Ba2 105.2(2) 4_565 4_565 ? P3 O9 Ba2 137.4(4) . . ? P3 O9 Ba1 96.7(3) . . ? Ba2 O9 Ba1 109.4(3) . . ? P3 O9 Ba1 91.9(4) . 4_565 ? Ba2 O9 Ba1 111.7(2) . 4_565 ? Ba1 O9 Ba1 105.7(2) . 4_565 ? P3 O10 Ca1 148.9(5) . . ? P3 O10 Ba2 105.9(3) . 2_556 ? Ca1 O10 Ba2 91.4(2) . 2_556 ? P3 O10 Ba1 92.3(3) . . ? Ca1 O10 Ba1 94.2(2) . . ? Ba2 O10 Ba1 133.4(3) 2_556 . ? P4 O11 P3 139.0(5) . . ? P4 O11 Ba2 107.8(3) . 2_556 ? P3 O11 Ba2 102.5(3) . 2_556 ? P4 O12 Ca1 117.3(4) . 3_566 ? P4 O12 Ba2 115.4(4) . 4_565 ? Ca1 O12 Ba2 95.5(3) 3_566 4_565 ? P4 O12 Ba2 91.0(3) . 3_556 ? Ca1 O12 Ba2 97.3(2) 3_566 3_556 ? Ba2 O12 Ba2 140.7(3) 4_565 3_556 ? P4 O13 Ca1 100.1(4) . 2_546 ? P4 O13 Ca2 159.7(4) . 4_465 ? Ca1 O13 Ca2 95.1(3) 2_546 4_465 ? P4 O13 Ba2 103.1(4) . 2_556 ? Ca1 O13 Ba2 94.8(2) 2_546 2_556 ? Ca2 O13 Ba2 88.8(2) 4_465 2_556 ? P4 O14 Ca1 90.6(3) . 2_546 ? P4 O14 Ba2 138.5(4) . . ? Ca1 O14 Ba2 94.0(2) 2_546 . ? P4 O14 Ba2 104.2(4) . 3_556 ? Ca1 O14 Ba2 112.6(3) 2_546 3_556 ? Ba2 O14 Ba2 111.8(3) . 3_556 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.058 _refine_diff_density_min -2.532 _refine_diff_density_rms 0.563