# Supplementary Material (ESI) for Physical Chemistry Chemical Physics # This journal is (c) The Owner Societies 2010 data_global _journal_coden_Cambridge 1326 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Terra, Joice' 'Gonzalez, Gabriela' 'Rossi, Alexandre' 'Eon, Jean-Guillaume' 'Ellis, Donald E.' _publ_contact_author_name 'Terra, Joice' _publ_contact_author_email joice@cbpf.br, _publ_section_title ; Theoretical and Experimental Studies of Substitution of Cadmium into Hydroxyapatite ; # Attachment '- hapCd1C_A.cif' ############################################################################## ### FullProf-generated CIF output file (version: February 2008) ### ### Template of CIF submission form for structure report ### ############################################################################## # This file has been generated using FullProf.2k taking one example of # structure report provided by Acta Cryst. It is given as a 'template' with # filled structural items. Many other items are left unfilled and it is the # responsibility of the user to properly fill or suppress them. In principle # all question marks '?' should be replaced by the appropriate text or # numerical value depending on the kind of CIF item. # See the document: cif_core.dic (URL: http://www.iucr.org) for details. # Please notify any error or suggestion to: # Juan Rodriguez-Carvajal (jrc@ill.eu) # Improvements will be progressively added as needed. data_HACd _database_code_depnum_ccdc_archive 'CCDC 783220' #TrackingRef '- hapCd1C_A.cif' #============================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'Ca9.80 Cd0.20 O26 P6' _chemical_formula_structural 'Ca9.803 Cd0.197 (P O4)6 (O H)2' _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Ca9.80 Cd0.20 O26 P6' #_chemical_formula_sum 'Ca9.80 2+, Cd0.20 2+, O26 1-, P6' _chemical_formula_weight 1016.86 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products 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 O1- 4.19160 12.85730 1.63969 4.17236 1.52673 47.01790 -20.30700 -0.01404 21.94120 0.00300 0.00400 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 Ca2+ 15.63480 -0.00740 7.95180 0.60890 8.43720 10.31160 0.85370 25.99050 -14.87500 0.13700 0.19300 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 Cd2+ 19.15140 0.59792 17.25350 6.80639 4.47128 20.25210 0.00000 0.00000 5.11937 -1.63700 0.78300 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 0.05500 0.05800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 63/M' _symmetry_space_group_name_Hall '-P 6c' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z x-y,x,z+1/2 -y,x-y,z -x,-y,z+1/2 -x+y,-x,z y,-x+y,z+1/2 -x,-y,-z -x+y,-x,-z+1/2 y,-x+y,-z x,y,-z+1/2 x-y,x,-z -y,x-y,-z+1/2 _cell_length_a 9.432573(222) _cell_length_b 9.432573(222) _cell_length_c 6.883337(169) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 120.00000 _cell_volume 530.384(22) _cell_formula_units_Z 1 _cell_measurement_temperature 298 _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 ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode transmission _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ' white ' _exptl_crystal_density_diffrn 3.1837 # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # 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 ? #============================================================================= # 7. 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 ; ID15, ESRF ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 298 _diffrn_source Synchrotron _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.13846 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Goniometer in transmission geometry' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? # Not in version 2.0.1 _diffrn_detector ' area detector' _diffrn_detector_type ' MAR345 ' _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _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 1150 # Pattern 1 out of 3 _pd_meas_2theta_range_min 0.01155 _pd_meas_2theta_range_max 13.04671 _pd_meas_2theta_range_inc 0.011362 # Pattern 2 out of 3 #_pd_meas_2theta_range_min 0.009100 #_pd_meas_2theta_range_max 10.351180 #_pd_meas_2theta_range_inc 0.009018 # Pattern 3 out of 3 #_pd_meas_2theta_range_min 0.007510 #_pd_meas_2theta_range_max 8.571817 #_pd_meas_2theta_range_inc 0.007471 #============================================================================= # 8. 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 ? _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr ; ? ; # 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 1.7604 _pd_proc_ls_prof_wR_factor 2.2944 _pd_proc_ls_prof_wR_expected 1.8518 _refine_ls_goodness_of_fit_all 1.1198 _refine_ls_shift/su_max 0.01 # 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 4.1180 #_pd_proc_ls_prof_cwR_factor 4.5899 #_pd_proc_ls_prof_cwR_expected 3.7043 # The following items are not in the CIF standard, but are defined above #_pd_proc_ls_prof_chi2 1.5353 #_pd_proc_ls_prof_echi2 1.5353 # Items related to LS refinement _refine_ls_R_I_factor 1.9171 _refine_ls_number_reflns 902 _refine_ls_number_parameters 60 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment noref _refine_diff_density_max 3.4 _refine_diff_density_min 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 0.0025 _pd_proc_2theta_range_max 13.0377 _pd_proc_2theta_range_inc 0.011362 _pd_proc_wavelength 0.138457 _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 ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution ? _computing_structure_refinement FULLPROF _computing_molecular_graphics ? _computing_publication_material ? #============================================================================= # 9. 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 O3 0.3398(4) 0.2551(4) 0.0713(4) 0.0100(9) 1.00000 Uiso O-1 Ca1 0.33333 0.66667 0.0003(4) 0.0113(8) 0.979(3) Uiso Ca2+ Ca2 0.2461(2) -0.0077(3) 0.25000 0.0107(5) 0.981(2) Uiso Ca2+ Cd1 0.33333 0.66667 0.0003(4) 0.0113(8) 0.021(3) Uiso Cd2+ Cd2 0.2461(2) -0.0077(3) 0.25000 0.0107(5) 0.019(2) Uiso Cd2+ P 0.3987(3) 0.3696(3) 0.25000 0.0104(8) 1.00000 Uiso P O1 0.3286(6) 0.4831(6) 0.25000 0.0100(9) 1.00000 Uiso O-1 O2 0.5861(6) 0.4642(6) 0.25000 0.0100(9) 1.00000 Uiso O-1 O4 0.00000 0.00000 0.1967(14) 0.0100(9) 0.50000 Uiso O-1 # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # 10. 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_site_symmetry_2 _geom_bond_publ_flag O3 O3 2.460(4) 10_555 ? O3 Ca1 2.832(4) 7_665 ? O3 Ca2 2.500(4) . ? O3 Ca2 2.343(3) 2_554 ? O3 Cd1 2.832(4) 7_665 ? O3 Cd2 2.500(4) . ? O3 Cd2 2.343(3) 2_554 ? O3 P 1.545(3) . ? O3 O1 2.525(7) . ? O3 O1 2.984(6) 6_554 ? O3 O2 2.494(4) . ? O3 O2 2.972(8) 3_655 ? Ca1 O3 2.832(4) 7_665 ? Ca1 O3 2.832(4) 9_565 ? Ca1 O3 2.832(3) 11_555 ? Ca1 O1 2.424(5) . ? Ca1 O1 2.424(3) 3_665 ? Ca1 O1 2.424(5) 5_565 ? Ca1 O2 2.451(4) 2_554 ? Ca1 O2 2.451(5) 4_664 ? Ca1 O2 2.451(4) 6_564 ? Ca2 O3 2.500(4) . ? Ca2 O3 2.343(3) 6_555 ? Ca2 O3 2.343(3) 9_555 ? Ca2 O3 2.500(4) 10_555 ? Ca2 O1 2.701(6) 5_555 ? Ca2 O2 2.371(5) 3_655 ? Ca2 O4 2.387(3) . ? Ca2 O4 2.387(3) 8_555 ? Cd1 O3 2.832(4) 7_665 ? Cd1 O3 2.832(4) 9_565 ? Cd1 O3 2.832(3) 11_555 ? Cd1 O1 2.424(5) . ? Cd1 O1 2.424(3) 3_665 ? Cd1 O1 2.424(5) 5_565 ? Cd1 O2 2.451(4) 2_554 ? Cd1 O2 2.451(5) 4_664 ? Cd1 O2 2.451(4) 6_564 ? Cd2 O3 2.500(4) . ? Cd2 O3 2.343(3) 6_555 ? Cd2 O3 2.343(3) 9_555 ? Cd2 O3 2.500(4) 10_555 ? Cd2 O1 2.701(6) 5_555 ? Cd2 O2 2.371(5) 3_655 ? Cd2 O4 2.387(3) . ? Cd2 O4 2.387(3) 8_555 ? P O3 1.545(3) . ? P O3 1.545(3) 10_555 ? P O1 1.514(8) . ? P O2 1.531(5) . ? O1 O3 2.525(7) . ? O1 O3 2.984(4) 2_555 ? O1 O3 2.525(7) 10_555 ? O1 O3 2.984(4) 11_555 ? O1 Ca1 2.424(5) . ? O1 Ca1 2.424(5) 8_565 ? O1 Ca2 2.701(5) 3_555 ? O1 Cd1 2.424(5) . ? O1 Cd1 2.424(5) 8_565 ? O1 Cd2 2.701(5) 3_555 ? O1 P 1.514(8) . ? O1 O1 2.961(7) 3_665 ? O1 O1 2.961(10) 5_565 ? O1 O2 2.523(9) . ? O2 O3 2.494(4) . ? O2 O3 2.972(5) 5_665 ? O2 O3 2.972(5) 8_665 ? O2 O3 2.494(4) 10_555 ? O2 Ca1 2.451(5) 2_655 ? O2 Ca1 2.451(5) 7_665 ? O2 Ca2 2.371(5) 5_665 ? O2 Cd1 2.451(5) 2_655 ? O2 Cd1 2.451(5) 7_665 ? O2 Cd2 2.371(5) 5_665 ? O2 P 1.531(5) . ? O2 O1 2.523(9) . ? O4 Ca2 2.387(3) . ? O4 Ca2 2.387(3) 3_555 ? O4 Ca2 2.387(2) 5_555 ? O4 Cd2 2.387(3) . ? O4 Cd2 2.387(3) 3_555 ? O4 Cd2 2.387(2) 5_555 ? O4 O4 2.708(14) 7_555 ? O4 O4 0.734(14) 8_555 ? 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 O3 Ca1 100.02(18) 10_555 7_665 ? O3 O3 Ca2 60.52(16) 10_555 . ? O3 O3 Ca2 160.75(18) 10_555 2_554 ? O3 O3 Cd1 100.02(18) 10_555 9_555 ? O3 O3 Cd2 60.52(16) 10_555 10_555 ? O3 O3 Cd2 160.75(18) 10_555 11_555 ? O3 O3 P 37.25(17) 10_555 10_555 ? O3 O3 O1 60.8(2) 10_555 . ? O3 O3 O1 137.8(2) 10_555 6_554 ? O3 O3 O2 60.44(17) 10_555 . ? O3 O3 O2 65.6(2) 10_555 3_655 ? Ca1 O3 Ca2 98.23(14) 7_665 . ? Ca1 O3 Ca2 99.05(13) 7_665 2_554 ? Ca1 O3 Cd2 98.23(14) 7_665 10_555 ? Ca1 O3 Cd2 99.05(13) 7_665 11_555 ? Ca1 O3 P 89.56(20) 7_665 . ? Ca1 O3 O1 111.5(3) 7_665 . ? Ca1 O3 O1 49.19(15) 7_665 6_554 ? Ca1 O3 O2 54.36(17) 7_665 . ? Ca1 O3 O2 49.89(18) 7_665 3_655 ? Ca2 O3 Ca2 118.97(15) . . ? Ca2 O3 Cd1 98.23(14) . 9_555 ? Ca2 O3 Cd2 118.97(15) . 10_555 ? Ca2 O3 P 97.3(2) . . ? Ca2 O3 O1 117.4(3) . . ? Ca2 O3 O1 92.36(16) . 6_554 ? Ca2 O3 O2 105.6(2) . . ? Ca2 O3 O2 50.5(2) . 3_655 ? Ca2 O3 Cd1 99.05(13) 11_555 9_555 ? Ca2 O3 Cd2 118.97(15) 11_555 11_555 ? Ca2 O3 P 140.69(15) 11_555 . ? Ca2 O3 O1 109.2(2) 11_555 . ? Ca2 O3 O1 59.5(2) 11_555 6_554 ? Ca2 O3 O2 131.54(18) 11_555 . ? Ca2 O3 O2 130.8(3) 11_555 3_655 ? Cd1 O3 Cd2 98.23(14) 9_555 10_555 ? Cd1 O3 Cd2 99.05(13) 9_555 11_555 ? Cd1 O3 P 89.56(20) 9_555 . ? Cd1 O3 O1 111.5(3) 9_555 . ? Cd1 O3 O1 49.19(15) 9_555 6_554 ? Cd1 O3 O2 54.36(17) 9_555 . ? Cd1 O3 O2 49.89(18) 9_555 3_655 ? Cd2 O3 Cd2 118.97(15) 10_555 11_555 ? Cd2 O3 P 97.3(2) 10_555 . ? Cd2 O3 O1 117.4(3) 10_555 . ? Cd2 O3 O1 92.36(16) 10_555 6_554 ? Cd2 O3 O2 105.6(2) 10_555 . ? Cd2 O3 O2 50.5(2) 10_555 3_655 ? Cd2 O3 P 140.69(15) 2_554 10_555 ? Cd2 O3 O1 109.2(2) 2_554 . ? Cd2 O3 O1 59.5(2) 2_554 6_554 ? Cd2 O3 O2 131.54(18) 2_554 . ? Cd2 O3 O2 130.8(3) 2_554 3_655 ? P O3 O1 34.0(3) . . ? P O3 O1 138.6(3) . 6_554 ? P O3 O2 35.6(2) . . ? P O3 O2 83.3(4) . 3_655 ? O1 O3 O1 148.3(4) 10_555 6_554 ? O1 O3 O2 60.3(3) 10_555 . ? O1 O3 O2 117.3(4) 10_555 3_655 ? O1 O3 O2 103.1(2) 6_554 . ? O1 O3 O2 72.29(19) 6_554 12_655 ? O2 O3 O2 66.4(3) 10_555 3_655 ? O3 Ca1 O3 117.0(3) 7_665 7_665 ? O3 Ca1 O3 117.03(17) 7_665 9_565 ? O3 Ca1 O1 86.46(19) 7_665 . ? O3 Ca1 O1 68.67(19) 7_665 3_665 ? O3 Ca1 O1 142.7(3) 7_665 5_565 ? O3 Ca1 O2 124.7(3) 7_665 2_554 ? O3 Ca1 O2 55.77(17) 7_665 4_664 ? O3 Ca1 O2 68.0(2) 7_665 9_565 ? O3 Ca1 O3 117.0(2) 7_665 11_555 ? O3 Ca1 O1 142.7(3) 9_565 . ? O3 Ca1 O1 86.5(2) 9_565 3_665 ? O3 Ca1 O1 68.67(19) 9_565 5_565 ? O3 Ca1 O2 68.03(20) 9_565 2_554 ? O3 Ca1 O2 124.7(3) 9_565 4_664 ? O3 Ca1 O2 55.77(19) 9_565 6_564 ? O3 Ca1 O1 68.67(17) 11_555 . ? O3 Ca1 O1 142.7(2) 11_555 3_665 ? O3 Ca1 O1 86.5(2) 11_555 5_565 ? O3 Ca1 O2 55.77(17) 11_555 2_554 ? O3 Ca1 O2 68.03(19) 11_555 4_664 ? O3 Ca1 O2 124.7(2) 11_555 6_564 ? O1 Ca1 O1 75.3(2) 10_555 3_665 ? O1 Ca1 O1 75.3(3) 10_555 5_565 ? O1 Ca1 O2 123.7(3) 10_555 2_554 ? O1 Ca1 O2 92.19(17) 10_555 4_664 ? O1 Ca1 O2 154.3(3) 10_555 6_564 ? O1 Ca1 O1 75.3(2) 12_665 5_565 ? O1 Ca1 O2 154.4(2) 12_665 2_554 ? O1 Ca1 O2 123.7(2) 12_665 4_664 ? O1 Ca1 O2 92.19(14) 12_665 6_564 ? O1 Ca1 O2 92.20(16) 8_565 2_554 ? O1 Ca1 O2 154.3(4) 8_565 4_664 ? O1 Ca1 O2 123.7(2) 8_565 6_564 ? O2 Ca1 O2 76.0(3) 11_555 4_664 ? O2 Ca1 O2 76.0(2) 11_555 6_564 ? O2 Ca1 O2 76.0(3) 7_665 6_564 ? O3 Ca2 O3 136.3(2) . 6_555 ? O3 Ca2 O3 78.07(20) . 9_555 ? O3 Ca2 O3 58.96(16) . 10_555 ? O3 Ca2 O1 150.2(3) . 5_555 ? O3 Ca2 O2 75.2(3) . 3_655 ? O3 Ca2 O4 76.18(16) . . ? O3 Ca2 O4 85.0(2) . 8_555 ? O3 Ca2 O3 141.5(2) 6_555 9_555 ? O3 Ca2 O3 78.07(20) 6_555 10_555 ? O3 Ca2 O1 72.14(20) 6_555 5_555 ? O3 Ca2 O2 87.1(2) 6_555 3_655 ? O3 Ca2 O4 109.9(3) 6_555 . ? O3 Ca2 O4 92.9(3) 6_555 8_555 ? O3 Ca2 O3 136.3(2) 9_555 10_555 ? O3 Ca2 O1 72.14(20) 9_555 5_555 ? O3 Ca2 O2 87.1(2) 9_555 3_655 ? O3 Ca2 O4 92.9(3) 9_555 . ? O3 Ca2 O4 109.9(3) 9_555 8_555 ? O3 Ca2 O1 150.2(3) 10_555 5_555 ? O3 Ca2 O2 75.2(3) 10_555 3_655 ? O3 Ca2 O4 85.0(2) 10_555 . ? O3 Ca2 O4 76.18(16) 10_555 8_555 ? O1 Ca2 O2 102.6(3) 5_555 3_655 ? O1 Ca2 O4 105.3(3) 5_555 . ? O1 Ca2 O4 105.3(3) 5_555 8_555 ? O2 Ca2 O4 150.7(3) 12_655 . ? O2 Ca2 O4 150.7(3) 12_655 8_555 ? O4 Ca2 O4 17.68(14) 5_555 8_555 ? O3 Cd1 O3 117.0(3) 7_665 7_665 ? O3 Cd1 O3 117.03(17) 7_665 9_565 ? O3 Cd1 O1 86.46(19) 7_665 . ? O3 Cd1 O1 68.67(19) 7_665 3_665 ? O3 Cd1 O1 142.7(3) 7_665 5_565 ? O3 Cd1 O2 124.7(3) 7_665 2_554 ? O3 Cd1 O2 55.77(17) 7_665 4_664 ? O3 Cd1 O2 68.0(2) 7_665 6_564 ? O3 Cd1 O3 117.0(2) 9_565 11_555 ? O3 Cd1 O1 142.7(3) 9_565 . ? O3 Cd1 O1 86.5(2) 9_565 3_665 ? O3 Cd1 O1 68.67(19) 9_565 5_565 ? O3 Cd1 O2 68.03(20) 9_565 2_554 ? O3 Cd1 O2 124.7(3) 9_565 4_664 ? O3 Cd1 O2 55.77(19) 9_565 6_564 ? O3 Cd1 O1 68.67(17) 11_555 . ? O3 Cd1 O1 142.7(2) 11_555 3_665 ? O3 Cd1 O1 86.5(2) 11_555 5_565 ? O3 Cd1 O2 55.77(17) 11_555 2_554 ? O3 Cd1 O2 68.03(19) 11_555 4_664 ? O3 Cd1 O2 124.7(2) 11_555 6_564 ? O1 Cd1 O1 75.3(2) . 3_665 ? O1 Cd1 O1 75.3(3) . 5_565 ? O1 Cd1 O2 123.7(3) . 2_554 ? O1 Cd1 O2 92.19(17) . 4_664 ? O1 Cd1 O2 154.3(3) . 6_564 ? O1 Cd1 O1 75.3(2) 12_665 5_565 ? O1 Cd1 O2 154.4(2) 12_665 2_554 ? O1 Cd1 O2 123.7(2) 12_665 4_664 ? O1 Cd1 O2 92.19(14) 12_665 6_564 ? O1 Cd1 O2 92.20(16) 8_565 2_554 ? O1 Cd1 O2 154.3(4) 8_565 4_664 ? O1 Cd1 O2 123.7(2) 8_565 6_564 ? O2 Cd1 O2 76.0(3) 11_555 4_664 ? O2 Cd1 O2 76.0(2) 11_555 6_564 ? O2 Cd1 O2 76.0(3) 7_665 6_564 ? O3 Cd2 O3 136.3(2) . 6_555 ? O3 Cd2 O3 78.07(20) . 9_555 ? O3 Cd2 O3 58.96(16) . 10_555 ? O3 Cd2 O1 150.2(3) . 5_555 ? O3 Cd2 O2 75.2(3) . 3_655 ? O3 Cd2 O4 76.18(16) . . ? O3 Cd2 O4 85.0(2) . 8_555 ? O3 Cd2 O3 141.5(2) 6_555 9_555 ? O3 Cd2 O3 78.07(20) 6_555 10_555 ? O3 Cd2 O1 72.14(20) 6_555 5_555 ? O3 Cd2 O2 87.1(2) 6_555 3_655 ? O3 Cd2 O4 109.9(3) 6_555 . ? O3 Cd2 O4 92.9(3) 6_555 8_555 ? O3 Cd2 O3 136.3(2) 9_555 10_555 ? O3 Cd2 O1 72.14(20) 9_555 5_555 ? O3 Cd2 O2 87.1(2) 9_555 3_655 ? O3 Cd2 O4 92.9(3) 9_555 . ? O3 Cd2 O4 109.9(3) 9_555 8_555 ? O3 Cd2 O1 150.2(3) 10_555 5_555 ? O3 Cd2 O2 75.2(3) 10_555 3_655 ? O3 Cd2 O4 85.0(2) 10_555 . ? O3 Cd2 O4 76.18(16) 10_555 8_555 ? O1 Cd2 O2 102.6(3) 5_555 3_655 ? O1 Cd2 O4 105.3(3) 5_555 . ? O1 Cd2 O4 105.3(3) 5_555 8_555 ? O2 Cd2 O4 150.7(3) 12_655 . ? O2 Cd2 O4 150.7(3) 12_655 8_555 ? O4 Cd2 O4 17.68(14) 5_555 8_555 ? O3 P O3 105.5(3) . 10_555 ? O3 P O1 111.3(4) . . ? O3 P O2 108.3(4) . . ? O3 P O1 111.3(5) 10_555 . ? O3 P O2 108.3(4) 10_555 . ? O1 P O2 111.9(7) 10_555 . ? O3 O1 O3 109.0(2) . 2_555 ? O3 O1 O3 58.3(2) . 10_555 ? O3 O1 O3 66.7(2) . 11_555 ? O3 O1 Ca1 105.6(2) . . ? O3 O1 Ca1 163.7(3) . 8_565 ? O3 O1 Ca2 79.9(2) . 3_555 ? O3 O1 Cd1 105.6(2) . . ? O3 O1 Cd1 163.7(3) . 8_565 ? O3 O1 Cd2 79.9(2) . 3_555 ? O3 O1 P 34.8(3) . 10_555 ? O3 O1 O1 136.6(3) . 3_665 ? O3 O1 O1 141.5(4) . 5_565 ? O3 O1 O2 59.2(3) . . ? O3 O1 O3 66.7(2) 2_555 10_555 ? O3 O1 O3 95.68(16) 2_555 11_555 ? O3 O1 Ca1 125.72(20) 2_555 . ? O3 O1 Ca1 62.14(15) 2_555 10_555 ? O3 O1 Ca2 48.36(13) 2_555 12_555 ? O3 O1 Cd1 125.72(20) 2_555 . ? O3 O1 Cd1 62.14(15) 2_555 10_555 ? O3 O1 Cd2 48.36(13) 2_555 12_555 ? O3 O1 P 101.0(4) 2_555 . ? O3 O1 O1 113.9(2) 2_555 12_665 ? O3 O1 O1 74.8(2) 2_555 5_565 ? O3 O1 O2 121.3(3) 2_555 . ? O3 O1 O3 109.0(2) 10_555 11_555 ? O3 O1 Ca1 163.7(3) 10_555 . ? O3 O1 Ca1 105.6(2) 10_555 8_565 ? O3 O1 Ca2 79.9(2) 10_555 3_555 ? O3 O1 Cd1 163.7(3) 10_555 . ? O3 O1 Cd1 105.6(2) 10_555 8_565 ? O3 O1 Cd2 79.9(2) 10_555 3_555 ? O3 O1 P 34.8(3) 10_555 . ? O3 O1 O1 136.6(3) 10_555 3_665 ? O3 O1 O1 141.5(4) 10_555 5_565 ? O3 O1 O2 59.2(3) 10_555 . ? O3 O1 Ca1 62.14(15) 11_555 . ? O3 O1 Ca1 125.72(20) 11_555 10_555 ? O3 O1 Ca2 48.36(13) 11_555 12_555 ? O3 O1 Cd1 62.14(15) 11_555 . ? O3 O1 Cd1 125.72(20) 11_555 10_555 ? O3 O1 Cd2 48.36(13) 11_555 12_555 ? O3 O1 P 101.0(4) 11_555 . ? O3 O1 O1 113.9(2) 11_555 3_665 ? O3 O1 O1 74.8(2) 11_555 5_565 ? O3 O1 O2 121.3(3) 11_555 . ? Ca1 O1 Ca1 90.3(2) . 8_565 ? Ca1 O1 Ca2 100.66(17) . 3_555 ? Ca1 O1 Cd1 90.3(2) . 8_565 ? Ca1 O1 Cd2 100.66(17) . 3_555 ? Ca1 O1 P 130.3(4) . . ? Ca1 O1 O1 52.36(19) . 3_665 ? Ca1 O1 O1 52.4(2) . 5_565 ? Ca1 O1 O2 112.1(3) . . ? Ca1 O1 Ca2 100.66(17) 3_665 3_555 ? Ca1 O1 Cd1 90.3(2) 3_665 8_565 ? Ca1 O1 Cd2 100.66(17) 3_665 3_555 ? Ca1 O1 P 130.3(4) 3_665 . ? Ca1 O1 O1 52.36(19) 3_665 3_665 ? Ca1 O1 O1 52.4(2) 3_665 5_565 ? Ca1 O1 O2 112.1(3) 3_665 . ? Ca2 O1 Cd1 100.66(17) 3_555 . ? Ca2 O1 Cd1 100.66(17) 3_555 8_565 ? Ca2 O1 P 98.3(3) 3_555 . ? Ca2 O1 O1 135.2(2) 3_555 3_665 ? Ca2 O1 O1 75.2(3) 3_555 5_565 ? Ca2 O1 O2 132.6(3) 3_555 . ? Cd1 O1 Cd1 90.3(2) 5_565 8_565 ? Cd1 O1 Cd2 100.66(17) 5_565 3_555 ? Cd1 O1 P 130.3(4) 5_565 . ? Cd1 O1 O1 52.36(19) 5_565 3_665 ? Cd1 O1 O1 52.4(2) 5_565 5_565 ? Cd1 O1 O2 112.1(3) 5_565 . ? Cd1 O1 Cd2 100.66(17) 10_555 3_555 ? Cd1 O1 P 130.3(4) 10_555 . ? Cd1 O1 O1 52.36(19) 10_555 3_665 ? Cd1 O1 O1 52.4(2) 10_555 5_565 ? Cd1 O1 O2 112.1(3) 10_555 . ? Cd2 O1 P 98.3(3) 12_555 . ? Cd2 O1 O1 135.2(2) 12_555 3_665 ? Cd2 O1 O1 75.2(3) 12_555 5_565 ? Cd2 O1 O2 132.6(3) 12_555 . ? P O1 O1 126.5(5) 10_555 3_665 ? P O1 O1 173.5(6) 10_555 5_565 ? P O1 O2 34.3(4) 10_555 . ? O1 O1 O1 60.0(3) 3_665 5_565 ? O1 O1 O2 92.2(4) 3_665 . ? O1 O1 O2 152.2(5) 5_565 . ? O3 O2 O3 123.9(2) . 5_665 ? O3 O2 O3 165.2(2) . 8_665 ? O3 O2 O3 59.11(17) . 10_555 ? O3 O2 Ca1 110.4(2) . 2_655 ? O3 O2 Ca1 69.87(19) . 7_665 ? O3 O2 Ca2 135.7(2) . 5_665 ? O3 O2 Cd1 110.4(2) . 2_655 ? O3 O2 Cd1 69.87(19) . 7_665 ? O3 O2 Cd2 135.7(2) . 5_665 ? O3 O2 P 36.0(2) . . ? O3 O2 O1 60.4(3) . . ? O3 O2 O3 48.90(15) 5_665 8_665 ? O3 O2 O3 165.2(2) 5_665 10_555 ? O3 O2 Ca1 96.52(19) 5_665 2_655 ? O3 O2 Ca1 62.08(17) 5_665 7_665 ? O3 O2 Ca2 54.39(19) 5_665 5_665 ? O3 O2 Cd1 96.52(19) 5_665 2_655 ? O3 O2 Cd1 62.08(17) 5_665 7_665 ? O3 O2 Cd2 54.39(19) 5_665 5_665 ? O3 O2 P 154.9(3) 5_665 . ? O3 O2 O1 134.4(3) 5_665 . ? O3 O2 O3 123.9(2) 8_665 10_555 ? O3 O2 Ca1 62.08(17) 8_665 2_655 ? O3 O2 Ca1 96.52(19) 8_665 7_665 ? O3 O2 Ca2 54.39(19) 8_665 5_665 ? O3 O2 Cd1 62.08(17) 8_665 2_655 ? O3 O2 Cd1 96.52(19) 8_665 7_665 ? O3 O2 Cd2 54.39(19) 8_665 5_665 ? O3 O2 P 154.9(3) 8_665 . ? O3 O2 O1 134.4(3) 8_665 . ? O3 O2 Ca1 69.86(19) 10_555 2_655 ? O3 O2 Ca1 110.4(2) 10_555 7_665 ? O3 O2 Ca2 135.7(2) 10_555 5_665 ? O3 O2 Cd1 69.86(19) 10_555 2_655 ? O3 O2 Cd1 110.4(2) 10_555 7_665 ? O3 O2 Cd2 135.7(2) 10_555 5_665 ? O3 O2 P 36.0(2) 10_555 . ? O3 O2 O1 60.4(3) 10_555 . ? Ca1 O2 Ca1 89.3(2) 6_555 7_665 ? Ca1 O2 Ca2 113.7(2) 6_555 5_665 ? Ca1 O2 Cd1 89.3(2) 6_555 7_665 ? Ca1 O2 Cd2 113.7(2) 6_555 5_665 ? Ca1 O2 P 105.4(3) 6_555 . ? Ca1 O2 O1 126.0(4) 6_555 . ? Ca1 O2 Ca2 113.7(2) 4_665 5_665 ? Ca1 O2 Cd1 89.3(2) 4_665 7_665 ? Ca1 O2 Cd2 113.7(2) 4_665 5_665 ? Ca1 O2 P 105.4(3) 4_665 . ? Ca1 O2 O1 126.0(4) 4_665 . ? Ca2 O2 Cd1 113.7(2) 5_665 2_655 ? Ca2 O2 Cd1 113.7(2) 5_665 7_665 ? Ca2 O2 P 123.8(3) 5_665 . ? Ca2 O2 O1 90.0(3) 5_665 . ? Cd1 O2 Cd1 89.3(2) 2_655 7_665 ? Cd1 O2 Cd2 113.7(2) 2_655 5_665 ? Cd1 O2 P 105.4(3) 2_655 . ? Cd1 O2 O1 126.0(4) 2_655 . ? Cd1 O2 Cd2 113.7(2) 7_665 5_665 ? Cd1 O2 P 105.4(3) 7_665 . ? Cd1 O2 O1 126.0(4) 7_665 . ? Cd2 O2 P 123.8(3) 8_665 . ? Cd2 O2 O1 90.0(3) 8_665 . ? P O2 O1 33.8(3) 10_555 . ? Ca2 O4 Ca2 117.7(2) . 5_555 ? Ca2 O4 Ca2 117.68(13) . 3_555 ? Ca2 O4 Cd2 117.7(2) . 5_555 ? Ca2 O4 Cd2 117.68(13) . 3_555 ? Ca2 O4 O4 98.8(4) . 7_555 ? Ca2 O4 O4 81.2(11) . 8_556 ? Ca2 O4 Ca2 117.68(17) 12_555 3_555 ? Ca2 O4 Cd2 117.7(2) 12_555 3_555 ? Ca2 O4 Cd2 117.68(17) 12_555 5_555 ? Ca2 O4 O4 98.8(4) 12_555 7_555 ? Ca2 O4 O4 81.2(11) 12_555 3_555 ? Ca2 O4 Cd2 117.68(13) 3_555 5_555 ? Ca2 O4 Cd2 117.68(17) 3_555 5_555 ? Ca2 O4 O4 98.8(4) 3_555 7_555 ? Ca2 O4 O4 81.2(11) 3_555 8_556 ? Cd2 O4 Cd2 117.7(2) 10_555 3_555 ? Cd2 O4 Cd2 117.68(13) 10_555 5_555 ? Cd2 O4 O4 98.8(4) 10_555 7_555 ? Cd2 O4 O4 81.2(11) 10_555 8_556 ? Cd2 O4 Cd2 117.68(17) 5_555 5_555 ? Cd2 O4 O4 98.8(4) 5_555 7_555 ? Cd2 O4 O4 81.2(11) 5_555 8_556 ? Cd2 O4 O4 98.8(4) 8_555 7_555 ? Cd2 O4 O4 81.2(11) 8_555 8_556 ? O4 O4 O4 180.0(17) 7_555 8_556 ? # Attachment '- hapCd10C_A.cif' ############################################################################## ### FullProf-generated CIF output file (version: February 2008) ### ### Template of CIF submission form for structure report ### ############################################################################## # This file has been generated using FullProf.2k taking one example of # structure report provided by Acta Cryst. It is given as a 'template' with # filled structural items. Many other items are left unfilled and it is the # responsibility of the user to properly fill or suppress them. In principle # all question marks '?' should be replaced by the appropriate text or # numerical value depending on the kind of CIF item. # See the document: cif_core.dic (URL: http://www.iucr.org) for details. # Please notify any error or suggestion to: # Juan Rodriguez-Carvajal (jrc@ill.eu) # Improvements will be progressively added as needed. data_HACd _database_code_depnum_ccdc_archive 'CCDC 783221' #TrackingRef '- hapCd10C_A.cif' #============================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'Ca8.77 Cd1.23 O26 P6' _chemical_formula_structural 'Ca8.774 Cd0.1226 (P O4)6 (O H)2' _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Ca8.77 Cd1.23 O26 P6' #_chemical_formula_sum 'Ca8.77 2+, Cd1.23 2+, O26 1-, P6' _chemical_formula_weight 1091.29 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products 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 o-1 4.19160 12.85730 1.63969 4.17236 1.52673 47.01790 -20.30700 -0.01404 21.94120 0.00300 0.00400 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 ca+2 15.63480 -0.00740 7.95180 0.60890 8.43720 10.31160 0.85370 25.99050 -14.87500 0.13700 0.19300 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 cd+2 19.15140 0.59792 17.25350 6.80639 4.47128 20.25210 0.00000 0.00000 5.11937 -1.63700 0.78300 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 0.05500 0.05800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 63/M' _symmetry_space_group_name_Hall '-P 6c' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z x-y,x,z+1/2 -y,x-y,z -x,-y,z+1/2 -x+y,-x,z y,-x+y,z+1/2 -x,-y,-z -x+y,-x,-z+1/2 y,-x+y,-z x,y,-z+1/2 x-y,x,-z -y,x-y,-z+1/2 _cell_length_a 9.422709(213) _cell_length_b 9.422709(213) _cell_length_c 6.865845(162) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 120.00000 _cell_volume 527.93(2) _cell_formula_units_Z 1 _cell_measurement_temperature 298 _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 ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode transmission _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour white _exptl_crystal_density_diffrn 3.4326 # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # 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 ? #============================================================================= # 7. 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 ; ID15, ESRF ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 298 _diffrn_source Synchrotron _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.13846 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Goniometer in transmission geometry' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? # Not in version 2.0.1 _diffrn_detector ' area detector' _diffrn_detector_type MAR345 _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _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 1150 #Pattern 1 out of 3 _pd_meas_2theta_range_min 0.01154 _pd_meas_2theta_range_max 13.04485 _pd_meas_2theta_range_inc 0.011361 # Pattern 2 out of 3 #_pd_meas_2theta_range_min 0.009099 #_pd_meas_2theta_range_max 10.350001 #_pd_meas_2theta_range_inc 0.009017 # Pattern 3 out of 3 #_pd_meas_2theta_range_min 0.007509 #_pd_meas_2theta_range_max 8.571006 #_pd_meas_2theta_range_inc 0.007470 #============================================================================= # 8. 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 ? _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr ; ? ; # 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 1.5352 _pd_proc_ls_prof_wR_factor 2.0106 _pd_proc_ls_prof_wR_expected 1.7651 _refine_ls_goodness_of_fit_all 1.1167 _refine_ls_shift/su_max 0.01 # 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 3.9783 #_pd_proc_ls_prof_cwR_factor 4.3286 #_pd_proc_ls_prof_cwR_expected 3.8000 # The following items are not in the CIF standard, but are defined above #_pd_proc_ls_prof_chi2 1.2976 #_pd_proc_ls_prof_echi2 1.2976 # Items related to LS refinement _refine_ls_R_I_factor 1.6859 _refine_ls_number_reflns 899 _refine_ls_number_parameters 60 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment noref _refine_diff_density_max 3.4 _refine_diff_density_min 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 0.0026 _pd_proc_2theta_range_max 13.0359 _pd_proc_2theta_range_inc 0.011361 _pd_proc_wavelength 0.138457 _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 ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution ? _computing_structure_refinement FULLPROF _computing_molecular_graphics ? _computing_publication_material ? #============================================================================= # 9. 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 O3 0.3402(4) 0.2553(5) 0.0711(5) 0.0112(9) 1.00000 Uiso O-1 Ca1 0.33333 0.66667 0.0006(5) 0.0112(8) 0.915(4) Uiso CA+2 Ca2 0.2467(2) -0.0073(3) 0.25000 0.0113(5) 0.853(4) Uiso CA+2 Cd1 0.33333 0.66667 0.0006(5) 0.0112(8) 0.085(4) Uiso CD+2 Cd2 0.2467(2) -0.0073(3) 0.25000 0.0113(5) 0.147(4) Uiso CD+2 P 0.3981(3) 0.3696(3) 0.25000 0.0100(8) 1.00000 Uiso P O1 0.3284(6) 0.4834(7) 0.25000 0.0112(9) 1.00000 Uiso O-1 O2 0.5856(7) 0.4644(7) 0.25000 0.0112(9) 1.00000 Uiso O-1 O4 0.00000 0.00000 0.1991(14) 0.0112(9) 0.50000 Uiso O-1 # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # 10. 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_site_symmetry_2 _geom_bond_publ_flag O3 O3 2.457(5) 10_555 ? O3 Ca1 2.826(4) 7_665 ? O3 Ca2 2.496(5) . ? O3 Ca2 2.337(4) 2_554 ? O3 Cd1 2.826(4) 7_665 ? O3 Cd2 2.496(5) . ? O3 Cd2 2.337(4) 2_554 ? O3 P 1.542(4) . ? O3 O1 2.526(8) . ? O3 O1 2.975(7) 6_554 ? O3 O2 2.486(5) . ? O3 O2 2.970(9) 3_655 ? Ca1 O3 2.826(4) 7_665 ? Ca1 O3 2.826(5) 9_565 ? Ca1 O3 2.826(3) 11_555 ? Ca1 O1 2.416(6) . ? Ca1 O1 2.416(4) 3_665 ? Ca1 O1 2.416(5) 5_565 ? Ca1 O2 2.452(5) 2_554 ? Ca1 O2 2.452(6) 4_664 ? Ca1 O2 2.452(4) 6_564 ? Ca2 O3 2.496(5) . ? Ca2 O3 2.337(4) 6_555 ? Ca2 O3 2.337(4) 9_555 ? Ca2 O3 2.496(5) 10_555 ? Ca2 O1 2.699(7) 5_555 ? Ca2 O2 2.362(6) 3_655 ? Ca2 O4 2.385(3) . ? Ca2 O4 2.385(3) 8_555 ? Cd1 O3 2.826(4) 7_665 ? Cd1 O3 2.826(5) 9_565 ? Cd1 O3 2.826(3) 11_555 ? Cd1 O1 2.416(6) . ? Cd1 O1 2.416(4) 3_665 ? Cd1 O1 2.416(5) 5_565 ? Cd1 O2 2.452(5) 2_554 ? Cd1 O2 2.452(6) 4_664 ? Cd1 O2 2.452(4) 6_564 ? Cd2 O3 2.496(5) . ? Cd2 O3 2.337(4) 6_555 ? Cd2 O3 2.337(4) 9_555 ? Cd2 O3 2.496(5) 10_555 ? Cd2 O1 2.699(7) 5_555 ? Cd2 O2 2.362(6) 3_655 ? Cd2 O4 2.385(3) . ? Cd2 O4 2.385(3) 8_555 ? P O3 1.542(4) . ? P O3 1.542(4) 10_555 ? P O1 1.512(8) . ? P O2 1.530(6) . ? O1 O3 2.526(8) . ? O1 O3 2.975(5) 2_555 ? O1 O3 2.526(8) 10_555 ? O1 O3 2.975(5) 11_555 ? O1 Ca1 2.416(6) . ? O1 Ca1 2.416(6) 8_565 ? O1 Ca2 2.699(5) 3_555 ? O1 Cd1 2.416(6) . ? O1 Cd1 2.416(6) 8_565 ? O1 Cd2 2.699(5) 3_555 ? O1 P 1.512(8) . ? O1 O1 2.952(8) 3_665 ? O1 O1 2.952(11) 5_565 ? O1 O2 2.518(10) . ? O2 O3 2.486(5) . ? O2 O3 2.970(6) 5_665 ? O2 O3 2.970(6) 8_665 ? O2 O3 2.486(5) 10_555 ? O2 Ca1 2.452(6) 2_655 ? O2 Ca1 2.452(6) 7_665 ? O2 Ca2 2.362(6) 5_665 ? O2 Cd1 2.452(6) 2_655 ? O2 Cd1 2.452(6) 7_665 ? O2 Cd2 2.362(6) 5_665 ? O2 P 1.530(6) . ? O2 O1 2.518(10) . ? O4 Ca2 2.385(3) . ? O4 Ca2 2.385(3) 3_555 ? O4 Ca2 2.385(2) 5_555 ? O4 Cd2 2.385(3) . ? O4 Cd2 2.385(3) 3_555 ? O4 Cd2 2.385(2) 5_555 ? O4 O4 2.734(14) 7_555 ? O4 O4 0.699(14) 8_555 ? 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 O3 Ca1 100.0(2) 10_555 7_665 ? O3 O3 Ca2 60.51(19) 10_555 . ? O3 O3 Ca2 160.6(2) 10_555 2_554 ? O3 O3 Cd1 100.0(2) 10_555 9_555 ? O3 O3 Cd2 60.51(19) 10_555 10_555 ? O3 O3 Cd2 160.6(2) 10_555 11_555 ? O3 O3 P 37.2(2) 10_555 10_555 ? O3 O3 O1 60.9(3) 10_555 . ? O3 O3 O1 137.8(3) 10_555 6_554 ? O3 O3 O2 60.4(2) 10_555 . ? O3 O3 O2 65.6(3) 10_555 3_655 ? Ca1 O3 Ca2 98.19(15) 7_665 . ? Ca1 O3 Ca2 99.15(14) 7_665 2_554 ? Ca1 O3 Cd2 98.19(15) 7_665 10_555 ? Ca1 O3 Cd2 99.15(14) 7_665 11_555 ? Ca1 O3 P 89.9(2) 7_665 . ? Ca1 O3 O1 111.6(3) 7_665 . ? Ca1 O3 O1 49.14(16) 7_665 6_554 ? Ca1 O3 O2 54.53(19) 7_665 . ? Ca1 O3 O2 50.0(2) 7_665 3_655 ? Ca2 O3 Ca2 119.06(17) . . ? Ca2 O3 Cd1 98.19(15) . 9_555 ? Ca2 O3 Cd2 119.06(17) . 10_555 ? Ca2 O3 P 97.3(3) . . ? Ca2 O3 O1 117.4(4) . . ? Ca2 O3 O1 92.36(18) . 6_554 ? Ca2 O3 O2 105.7(3) . . ? Ca2 O3 O2 50.3(2) . 3_655 ? Ca2 O3 Cd1 99.15(14) 11_555 9_555 ? Ca2 O3 Cd2 119.06(17) 11_555 11_555 ? Ca2 O3 P 140.44(18) 11_555 . ? Ca2 O3 O1 109.0(2) 11_555 . ? Ca2 O3 O1 59.7(2) 11_555 6_554 ? Ca2 O3 O2 131.5(2) 11_555 . ? Ca2 O3 O2 130.8(3) 11_555 3_655 ? Cd1 O3 Cd2 98.19(15) 9_555 10_555 ? Cd1 O3 Cd2 99.15(14) 9_555 11_555 ? Cd1 O3 P 89.9(2) 9_555 . ? Cd1 O3 O1 111.6(3) 9_555 . ? Cd1 O3 O1 49.14(16) 9_555 6_554 ? Cd1 O3 O2 54.53(19) 9_555 . ? Cd1 O3 O2 50.0(2) 9_555 3_655 ? Cd2 O3 Cd2 119.06(17) 10_555 11_555 ? Cd2 O3 P 97.3(3) 10_555 . ? Cd2 O3 O1 117.4(4) 10_555 . ? Cd2 O3 O1 92.36(18) 10_555 6_554 ? Cd2 O3 O2 105.7(3) 10_555 . ? Cd2 O3 O2 50.3(2) 10_555 3_655 ? Cd2 O3 P 140.44(18) 2_554 10_555 ? Cd2 O3 O1 109.0(2) 2_554 . ? Cd2 O3 O1 59.7(2) 2_554 6_554 ? Cd2 O3 O2 131.5(2) 2_554 . ? Cd2 O3 O2 130.8(3) 2_554 3_655 ? P O3 O1 33.8(3) . . ? P O3 O1 138.9(3) . 6_554 ? P O3 O2 35.8(2) . . ? P O3 O2 83.7(4) . 3_655 ? O1 O3 O1 148.3(4) 10_555 6_554 ? O1 O3 O2 60.3(3) 10_555 . ? O1 O3 O2 117.5(5) 10_555 3_655 ? O1 O3 O2 103.2(2) 6_554 . ? O1 O3 O2 72.3(2) 6_554 12_655 ? O2 O3 O2 66.7(3) 10_555 3_655 ? O3 Ca1 O3 117.0(3) 7_665 7_665 ? O3 Ca1 O3 117.03(18) 7_665 9_565 ? O3 Ca1 O1 86.5(2) 7_665 . ? O3 Ca1 O1 68.6(2) 7_665 3_665 ? O3 Ca1 O1 142.7(3) 7_665 5_565 ? O3 Ca1 O2 124.8(3) 7_665 2_554 ? O3 Ca1 O2 55.67(20) 7_665 4_664 ? O3 Ca1 O2 68.1(3) 7_665 9_565 ? O3 Ca1 O3 117.0(3) 7_665 11_555 ? O3 Ca1 O1 142.7(4) 9_565 . ? O3 Ca1 O1 86.5(3) 9_565 3_665 ? O3 Ca1 O1 68.6(2) 9_565 5_565 ? O3 Ca1 O2 68.1(2) 9_565 2_554 ? O3 Ca1 O2 124.8(4) 9_565 4_664 ? O3 Ca1 O2 55.7(2) 9_565 6_564 ? O3 Ca1 O1 68.65(19) 11_555 . ? O3 Ca1 O1 142.7(2) 11_555 3_665 ? O3 Ca1 O1 86.5(3) 11_555 5_565 ? O3 Ca1 O2 55.7(2) 11_555 2_554 ? O3 Ca1 O2 68.1(2) 11_555 4_664 ? O3 Ca1 O2 124.8(3) 11_555 6_564 ? O1 Ca1 O1 75.3(3) 10_555 3_665 ? O1 Ca1 O1 75.3(4) 10_555 5_565 ? O1 Ca1 O2 123.6(3) 10_555 2_554 ? O1 Ca1 O2 92.1(2) 10_555 4_664 ? O1 Ca1 O2 154.4(3) 10_555 6_564 ? O1 Ca1 O1 75.3(3) 12_665 5_565 ? O1 Ca1 O2 154.4(3) 12_665 2_554 ? O1 Ca1 O2 123.6(3) 12_665 4_664 ? O1 Ca1 O2 92.11(16) 12_665 6_564 ? O1 Ca1 O2 92.11(18) 8_565 2_554 ? O1 Ca1 O2 154.4(4) 8_565 4_664 ? O1 Ca1 O2 123.6(2) 8_565 6_564 ? O2 Ca1 O2 76.2(4) 11_555 4_664 ? O2 Ca1 O2 76.2(2) 11_555 6_564 ? O2 Ca1 O2 76.2(3) 7_665 6_564 ? O3 Ca2 O3 136.4(3) . 6_555 ? O3 Ca2 O3 78.2(2) . 9_555 ? O3 Ca2 O3 58.97(19) . 10_555 ? O3 Ca2 O1 150.2(4) . 5_555 ? O3 Ca2 O2 75.3(3) . 3_655 ? O3 Ca2 O4 76.43(18) . . ? O3 Ca2 O4 84.8(2) . 8_555 ? O3 Ca2 O3 141.3(3) 6_555 9_555 ? O3 Ca2 O3 78.2(2) 6_555 10_555 ? O3 Ca2 O1 72.0(2) 6_555 5_555 ? O3 Ca2 O2 87.1(2) 6_555 3_655 ? O3 Ca2 O4 109.5(3) 6_555 . ? O3 Ca2 O4 93.3(3) 6_555 8_555 ? O3 Ca2 O3 136.4(3) 9_555 10_555 ? O3 Ca2 O1 72.0(2) 9_555 5_555 ? O3 Ca2 O2 87.1(2) 9_555 3_655 ? O3 Ca2 O4 93.3(3) 9_555 . ? O3 Ca2 O4 109.5(3) 9_555 8_555 ? O3 Ca2 O1 150.2(4) 10_555 5_555 ? O3 Ca2 O2 75.3(3) 10_555 3_655 ? O3 Ca2 O4 84.8(2) 10_555 . ? O3 Ca2 O4 76.43(18) 10_555 8_555 ? O1 Ca2 O2 102.4(3) 5_555 3_655 ? O1 Ca2 O4 105.2(3) 5_555 . ? O1 Ca2 O4 105.2(3) 5_555 8_555 ? O2 Ca2 O4 151.1(4) 12_655 . ? O2 Ca2 O4 151.1(4) 12_655 8_555 ? O4 Ca2 O4 16.85(13) 5_555 8_555 ? O3 Cd1 O3 117.0(3) 7_665 7_665 ? O3 Cd1 O3 117.03(18) 7_665 9_565 ? O3 Cd1 O1 86.5(2) 7_665 . ? O3 Cd1 O1 68.6(2) 7_665 3_665 ? O3 Cd1 O1 142.7(3) 7_665 5_565 ? O3 Cd1 O2 124.8(3) 7_665 2_554 ? O3 Cd1 O2 55.67(20) 7_665 4_664 ? O3 Cd1 O2 68.1(3) 7_665 6_564 ? O3 Cd1 O3 117.0(3) 9_565 11_555 ? O3 Cd1 O1 142.7(4) 9_565 . ? O3 Cd1 O1 86.5(3) 9_565 3_665 ? O3 Cd1 O1 68.6(2) 9_565 5_565 ? O3 Cd1 O2 68.1(2) 9_565 2_554 ? O3 Cd1 O2 124.8(4) 9_565 4_664 ? O3 Cd1 O2 55.7(2) 9_565 6_564 ? O3 Cd1 O1 68.65(19) 11_555 . ? O3 Cd1 O1 142.7(2) 11_555 3_665 ? O3 Cd1 O1 86.5(3) 11_555 5_565 ? O3 Cd1 O2 55.7(2) 11_555 2_554 ? O3 Cd1 O2 68.1(2) 11_555 4_664 ? O3 Cd1 O2 124.8(3) 11_555 6_564 ? O1 Cd1 O1 75.3(3) . 3_665 ? O1 Cd1 O1 75.3(4) . 5_565 ? O1 Cd1 O2 123.6(3) . 2_554 ? O1 Cd1 O2 92.1(2) . 4_664 ? O1 Cd1 O2 154.4(3) . 6_564 ? O1 Cd1 O1 75.3(3) 12_665 5_565 ? O1 Cd1 O2 154.4(3) 12_665 2_554 ? O1 Cd1 O2 123.6(3) 12_665 4_664 ? O1 Cd1 O2 92.11(16) 12_665 6_564 ? O1 Cd1 O2 92.11(18) 8_565 2_554 ? O1 Cd1 O2 154.4(4) 8_565 4_664 ? O1 Cd1 O2 123.6(2) 8_565 6_564 ? O2 Cd1 O2 76.2(4) 11_555 4_664 ? O2 Cd1 O2 76.2(2) 11_555 6_564 ? O2 Cd1 O2 76.2(3) 7_665 6_564 ? O3 Cd2 O3 136.4(3) . 6_555 ? O3 Cd2 O3 78.2(2) . 9_555 ? O3 Cd2 O3 58.97(19) . 10_555 ? O3 Cd2 O1 150.2(4) . 5_555 ? O3 Cd2 O2 75.3(3) . 3_655 ? O3 Cd2 O4 76.43(18) . . ? O3 Cd2 O4 84.8(2) . 8_555 ? O3 Cd2 O3 141.3(3) 6_555 9_555 ? O3 Cd2 O3 78.2(2) 6_555 10_555 ? O3 Cd2 O1 72.0(2) 6_555 5_555 ? O3 Cd2 O2 87.1(2) 6_555 3_655 ? O3 Cd2 O4 109.5(3) 6_555 . ? O3 Cd2 O4 93.3(3) 6_555 8_555 ? O3 Cd2 O3 136.4(3) 9_555 10_555 ? O3 Cd2 O1 72.0(2) 9_555 5_555 ? O3 Cd2 O2 87.1(2) 9_555 3_655 ? O3 Cd2 O4 93.3(3) 9_555 . ? O3 Cd2 O4 109.5(3) 9_555 8_555 ? O3 Cd2 O1 150.2(4) 10_555 5_555 ? O3 Cd2 O2 75.3(3) 10_555 3_655 ? O3 Cd2 O4 84.8(2) 10_555 . ? O3 Cd2 O4 76.43(18) 10_555 8_555 ? O1 Cd2 O2 102.4(3) 5_555 3_655 ? O1 Cd2 O4 105.2(3) 5_555 . ? O1 Cd2 O4 105.2(3) 5_555 8_555 ? O2 Cd2 O4 151.1(4) 12_655 . ? O2 Cd2 O4 151.1(4) 12_655 8_555 ? O4 Cd2 O4 16.85(13) 5_555 8_555 ? O3 P O3 105.6(4) . 10_555 ? O3 P O1 111.6(4) . . ? O3 P O2 108.0(4) . . ? O3 P O1 111.6(6) 10_555 . ? O3 P O2 108.0(4) 10_555 . ? O1 P O2 111.7(7) 10_555 . ? O3 O1 O3 109.1(3) . 2_555 ? O3 O1 O3 58.2(3) . 10_555 ? O3 O1 O3 66.8(3) . 11_555 ? O3 O1 Ca1 105.7(3) . . ? O3 O1 Ca1 163.7(3) . 8_565 ? O3 O1 Ca2 80.0(2) . 3_555 ? O3 O1 Cd1 105.7(3) . . ? O3 O1 Cd1 163.7(3) . 8_565 ? O3 O1 Cd2 80.0(2) . 3_555 ? O3 O1 P 34.6(4) . 10_555 ? O3 O1 O1 136.5(4) . 3_665 ? O3 O1 O1 141.7(5) . 5_565 ? O3 O1 O2 59.1(3) . . ? O3 O1 O3 66.8(3) 2_555 10_555 ? O3 O1 O3 95.65(19) 2_555 11_555 ? O3 O1 Ca1 125.8(2) 2_555 . ? O3 O1 Ca1 62.21(18) 2_555 10_555 ? O3 O1 Ca2 48.34(14) 2_555 12_555 ? O3 O1 Cd1 125.8(2) 2_555 . ? O3 O1 Cd1 62.21(18) 2_555 10_555 ? O3 O1 Cd2 48.34(14) 2_555 12_555 ? O3 O1 P 100.9(4) 2_555 . ? O3 O1 O1 113.9(2) 2_555 12_665 ? O3 O1 O1 74.9(3) 2_555 5_565 ? O3 O1 O2 121.3(4) 2_555 . ? O3 O1 O3 109.1(3) 10_555 11_555 ? O3 O1 Ca1 163.7(3) 10_555 . ? O3 O1 Ca1 105.7(3) 10_555 8_565 ? O3 O1 Ca2 80.0(2) 10_555 3_555 ? O3 O1 Cd1 163.7(3) 10_555 . ? O3 O1 Cd1 105.7(3) 10_555 8_565 ? O3 O1 Cd2 80.0(2) 10_555 3_555 ? O3 O1 P 34.6(4) 10_555 . ? O3 O1 O1 136.5(4) 10_555 3_665 ? O3 O1 O1 141.7(5) 10_555 5_565 ? O3 O1 O2 59.1(3) 10_555 . ? O3 O1 Ca1 62.21(18) 11_555 . ? O3 O1 Ca1 125.8(2) 11_555 10_555 ? O3 O1 Ca2 48.34(14) 11_555 12_555 ? O3 O1 Cd1 62.21(18) 11_555 . ? O3 O1 Cd1 125.8(2) 11_555 10_555 ? O3 O1 Cd2 48.34(14) 11_555 12_555 ? O3 O1 P 100.9(4) 11_555 . ? O3 O1 O1 113.9(2) 11_555 3_665 ? O3 O1 O1 74.9(3) 11_555 5_565 ? O3 O1 O2 121.3(4) 11_555 . ? Ca1 O1 Ca1 90.3(2) . 8_565 ? Ca1 O1 Ca2 100.70(18) . 3_555 ? Ca1 O1 Cd1 90.3(2) . 8_565 ? Ca1 O1 Cd2 100.70(18) . 3_555 ? Ca1 O1 P 130.3(4) . . ? Ca1 O1 O1 52.3(2) . 3_665 ? Ca1 O1 O1 52.3(3) . 5_565 ? Ca1 O1 O2 112.1(4) . . ? Ca1 O1 Ca2 100.70(18) 3_665 3_555 ? Ca1 O1 Cd1 90.3(2) 3_665 8_565 ? Ca1 O1 Cd2 100.70(18) 3_665 3_555 ? Ca1 O1 P 130.3(4) 3_665 . ? Ca1 O1 O1 52.3(2) 3_665 3_665 ? Ca1 O1 O1 52.3(3) 3_665 5_565 ? Ca1 O1 O2 112.1(4) 3_665 . ? Ca2 O1 Cd1 100.70(18) 3_555 . ? Ca2 O1 Cd1 100.70(18) 3_555 8_565 ? Ca2 O1 P 98.2(4) 3_555 . ? Ca2 O1 O1 135.3(3) 3_555 3_665 ? Ca2 O1 O1 75.3(3) 3_555 5_565 ? Ca2 O1 O2 132.6(4) 3_555 . ? Cd1 O1 Cd1 90.3(2) 5_565 8_565 ? Cd1 O1 Cd2 100.70(18) 5_565 3_555 ? Cd1 O1 P 130.3(4) 5_565 . ? Cd1 O1 O1 52.3(2) 5_565 3_665 ? Cd1 O1 O1 52.3(3) 5_565 5_565 ? Cd1 O1 O2 112.1(4) 5_565 . ? Cd1 O1 Cd2 100.70(18) 10_555 3_555 ? Cd1 O1 P 130.3(4) 10_555 . ? Cd1 O1 O1 52.3(2) 10_555 3_665 ? Cd1 O1 O1 52.3(3) 10_555 5_565 ? Cd1 O1 O2 112.1(4) 10_555 . ? Cd2 O1 P 98.2(4) 12_555 . ? Cd2 O1 O1 135.3(3) 12_555 3_665 ? Cd2 O1 O1 75.3(3) 12_555 5_565 ? Cd2 O1 O2 132.6(4) 12_555 . ? P O1 O1 126.5(5) 10_555 3_665 ? P O1 O1 173.5(6) 10_555 5_565 ? P O1 O2 34.4(4) 10_555 . ? O1 O1 O1 60.0(3) 3_665 5_565 ? O1 O1 O2 92.2(4) 3_665 . ? O1 O1 O2 152.2(5) 5_565 . ? O3 O2 O3 123.8(2) . 5_665 ? O3 O2 O3 164.9(2) . 8_665 ? O3 O2 O3 59.2(2) . 10_555 ? O3 O2 Ca1 110.4(3) . 2_655 ? O3 O2 Ca1 69.8(2) . 7_665 ? O3 O2 Ca2 136.0(3) . 5_665 ? O3 O2 Cd1 110.4(3) . 2_655 ? O3 O2 Cd1 69.8(2) . 7_665 ? O3 O2 Cd2 136.0(3) . 5_665 ? O3 O2 P 36.1(3) . . ? O3 O2 O1 60.6(3) . . ? O3 O2 O3 48.86(18) 5_665 8_665 ? O3 O2 O3 164.9(2) 5_665 10_555 ? O3 O2 Ca1 96.3(2) 5_665 2_655 ? O3 O2 Ca1 61.95(20) 5_665 7_665 ? O3 O2 Ca2 54.4(2) 5_665 5_665 ? O3 O2 Cd1 96.3(2) 5_665 2_655 ? O3 O2 Cd1 61.95(20) 5_665 7_665 ? O3 O2 Cd2 54.4(2) 5_665 5_665 ? O3 O2 P 154.9(3) 5_665 . ? O3 O2 O1 134.5(4) 5_665 . ? O3 O2 O3 123.8(2) 8_665 10_555 ? O3 O2 Ca1 61.95(20) 8_665 2_655 ? O3 O2 Ca1 96.3(2) 8_665 7_665 ? O3 O2 Ca2 54.4(2) 8_665 5_665 ? O3 O2 Cd1 61.95(20) 8_665 2_655 ? O3 O2 Cd1 96.3(2) 8_665 7_665 ? O3 O2 Cd2 54.4(2) 8_665 5_665 ? O3 O2 P 154.9(3) 8_665 . ? O3 O2 O1 134.5(4) 8_665 . ? O3 O2 Ca1 69.8(2) 10_555 2_655 ? O3 O2 Ca1 110.4(3) 10_555 7_665 ? O3 O2 Ca2 136.0(3) 10_555 5_665 ? O3 O2 Cd1 69.8(2) 10_555 2_655 ? O3 O2 Cd1 110.4(3) 10_555 7_665 ? O3 O2 Cd2 136.0(3) 10_555 5_665 ? O3 O2 P 36.1(3) 10_555 . ? O3 O2 O1 60.6(3) 10_555 . ? Ca1 O2 Ca1 89.1(3) 6_555 7_665 ? Ca1 O2 Ca2 113.5(2) 6_555 5_665 ? Ca1 O2 Cd1 89.1(3) 6_555 7_665 ? Ca1 O2 Cd2 113.5(2) 6_555 5_665 ? Ca1 O2 P 105.4(3) 6_555 . ? Ca1 O2 O1 126.1(4) 6_555 . ? Ca1 O2 Ca2 113.5(2) 4_665 5_665 ? Ca1 O2 Cd1 89.1(3) 4_665 7_665 ? Ca1 O2 Cd2 113.5(2) 4_665 5_665 ? Ca1 O2 P 105.4(3) 4_665 . ? Ca1 O2 O1 126.1(4) 4_665 . ? Ca2 O2 Cd1 113.5(2) 5_665 2_655 ? Ca2 O2 Cd1 113.5(2) 5_665 7_665 ? Ca2 O2 P 124.0(3) 5_665 . ? Ca2 O2 O1 90.1(3) 5_665 . ? Cd1 O2 Cd1 89.1(3) 2_655 7_665 ? Cd1 O2 Cd2 113.5(2) 2_655 5_665 ? Cd1 O2 P 105.4(3) 2_655 . ? Cd1 O2 O1 126.1(4) 2_655 . ? Cd1 O2 Cd2 113.5(2) 7_665 5_665 ? Cd1 O2 P 105.4(3) 7_665 . ? Cd1 O2 O1 126.1(4) 7_665 . ? Cd2 O2 P 124.0(3) 8_665 . ? Cd2 O2 O1 90.1(3) 8_665 . ? P O2 O1 33.9(4) 10_555 . ? Ca2 O4 Ca2 117.9(2) . 5_555 ? Ca2 O4 Ca2 117.89(13) . 3_555 ? Ca2 O4 Cd2 117.9(2) . 5_555 ? Ca2 O4 Cd2 117.89(13) . 3_555 ? Ca2 O4 O4 98.4(4) . 7_555 ? Ca2 O4 O4 81.6(11) . 8_556 ? Ca2 O4 Ca2 117.89(17) 12_555 3_555 ? Ca2 O4 Cd2 117.9(2) 12_555 3_555 ? Ca2 O4 Cd2 117.89(17) 12_555 5_555 ? Ca2 O4 O4 98.4(4) 12_555 7_555 ? Ca2 O4 O4 81.6(11) 12_555 3_555 ? Ca2 O4 Cd2 117.89(13) 3_555 5_555 ? Ca2 O4 Cd2 117.89(17) 3_555 5_555 ? Ca2 O4 O4 98.4(4) 3_555 7_555 ? Ca2 O4 O4 81.6(11) 3_555 8_556 ? Cd2 O4 Cd2 117.9(2) 10_555 3_555 ? Cd2 O4 Cd2 117.89(13) 10_555 5_555 ? Cd2 O4 O4 98.4(4) 10_555 7_555 ? Cd2 O4 O4 81.6(11) 10_555 8_556 ? Cd2 O4 Cd2 117.89(17) 5_555 5_555 ? Cd2 O4 O4 98.4(4) 5_555 7_555 ? Cd2 O4 O4 81.6(11) 5_555 8_556 ? Cd2 O4 O4 98.4(4) 8_555 7_555 ? Cd2 O4 O4 81.6(11) 8_555 8_556 ? O4 O4 O4 180.0(18) 7_555 8_556 ?