Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_contact_author_name 'Dr. Isaac Abrahams' _publ_contact_author_address ; Department of Chemistry Queen Mary, University of London Mile End Road London E1 4NS UK ; _publ_contact_author_email i.abrahams@qmul.ac.uk _publ_contact_author_fax '44(0)207 882 7794' _publ_contact_author_phone '44(0)207 882 3235' _publ_requested_journal 'J. Chem. Soc Dalton Trans' _publ_section_title ; Structure of calcium terasodium bis-cyclotriphosphate CaNa4(P3O9)2 by X-ray diffraction and solid state NMR ; loop_ _publ_author_name _publ_author_address 'Isaac Abrahams' ; Structural Chemistry Group Department of Chemistry Queen Mary, University of London Mile End Road London E1 4NS UK ; 'Geoffery E. Hawkes' ; Structural Chemistry Group Department of Chemistry Queen Mary, University of London Mile End Road London E1 4NS UK ; 'Aliya Ahmed' ; Structural Chemistry Group Department of Chemistry Queen Mary, University of London Mile End Road London E1 4NS UK ; 'Katrin Franks' ; Department of Biomaterials Eastman Dental Institute, University of London Gray's Inn Road London WC1X 8LD UK ; 'Philippe Bodart' ; ICTPOL/IST Departamento de Engenharia de Materiais Av. Rovisco Pais 1096 Lisboa Codex Portugal ; 'Teresa Nunes' ; ICTPOL/IST Departamento de Engenharia de Materiais Av. Rovisco Pais 1096 Lisboa Codex Portugal ; _publ_section_exptl_refinement ; Single crystal X-ray diffraction data were collected on the title compound. Intensity data were collected on an Enraf-Nonius CAD-4 diffractometer using MoK-alpha radiation (lambda = 0.71073 angstroms) with theta-2theta scans at 293(2) K. Systematic absences in the data were consistent with the monoclinic space groups, Cc and C2/c. Solution and refinement proceeded in the centrosymmetric space group as suggested by the solid state NMR results. The structure was solved by direct methods using SHELXS-976 and developed by difference Fourier techniques with subsequent refinement on F-squared by full matrix least squares using SHELXL-97.6 In the final stages of refinement, data were corrected for absorption against a refined isotropic model with the program DIFABS. Anisotropic thermal parameters were refined for all atoms. ; # CIF produced by WinGX routine CIF_UPDATE # Created on 2001-09-07 at 18:34:31 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1beta5 # Request file : c:\wingx\files\archive.dat # CIF files read : aakzn dreduc struct difabs data_aakzn _database_code_CSD 172172 _audit_creation_date 2001-09-07T18:34:31-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FI #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'Ca1 Na4 O18 P6' _chemical_formula_structural 'NA4 O18 P6 CA1' _chemical_formula_sum 'Ca Na4 O18 P6' _chemical_formula_weight 605.86 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.069(2) _cell_length_b 8.054(2) _cell_length_c 14.164(3) _cell_angle_alpha 90 _cell_angle_beta 94.60(2) _cell_angle_gamma 90 _cell_volume 1486.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.6845 _cell_measurement_theta_max 12.2505 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 2.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.292 _exptl_absorpt_factor_muR 0.155 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166 ; _exptl_absorpt_correction_T_min 0.2149 _exptl_absorpt_correction_T_max 0.8564 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.74475E-1 _diffrn_orient_matrix_ub_12 -0.13406E-1 _diffrn_orient_matrix_ub_13 -0.20953E-1 _diffrn_orient_matrix_ub_21 -0.18394E-1 _diffrn_orient_matrix_ub_22 0.34152E-1 _diffrn_orient_matrix_ub_23 0.64373E-1 _diffrn_orient_matrix_ub_31 -0.2868E-2 _diffrn_orient_matrix_ub_32 0.118618 _diffrn_orient_matrix_ub_33 -0.20826E-1 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2 _diffrn_standards_decay_corr_max 1.182 _diffrn_standards_decay_corr_min 0.957 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 -2 -5 0 0 6 _diffrn_reflns_number 1466 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 24.96 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 1300 _reflns_number_gt 1018 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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^)+(0.0790P)^2^+7.1813P] 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 none _refine_ls_number_reflns 1300 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.134 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.527 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.133 #----------------------------------------------------------------------------# # 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 Na Na 0.0362 0.0249 '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' Ca Ca 0.2262 0.3064 '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 Ca1 Ca 0.5 0.12189(17) 0.75 0.0164(4) Uani 1 2 d S . . P1 P 0.59259(8) 0.44869(16) 0.61506(8) 0.0151(3) Uani 1 1 d . . . P2 P 0.72812(8) 0.63760(16) 0.74811(8) 0.0159(3) Uani 1 1 d . . . P3 P 0.58656(8) 0.80764(16) 0.61116(8) 0.0155(4) Uani 1 1 d . . . Na1 Na 0.66300(16) 0.1221(3) 0.4555(2) 0.0424(7) Uani 1 1 d . . . Na2 Na 0.66603(13) 0.6251(3) 0.41597(13) 0.0227(5) Uani 1 1 d . . . O1 O 0.5123(2) 0.3252(4) 0.6333(2) 0.0216(8) Uani 1 1 d . . . O2 O 0.6597(2) 0.4199(5) 0.5380(2) 0.0216(8) Uani 1 1 d . . . O3 O 0.5355(2) 0.6265(4) 0.6001(2) 0.0174(7) Uani 1 1 d . . . O4 O 0.6596(2) 0.4799(4) 0.7131(2) 0.0192(8) Uani 1 1 d . . . O5 O 0.8232(2) 0.6411(4) 0.6969(2) 0.0208(8) Uani 1 1 d . . . O6 O 0.7345(3) 0.6387(4) 0.8516(2) 0.0237(8) Uani 1 1 d . . . O7 O 0.6554(2) 0.7884(4) 0.7097(2) 0.0192(8) Uani 1 1 d . . . O8 O 0.5026(2) 0.9246(4) 0.6276(2) 0.0204(8) Uani 1 1 d . . . O9 O 0.6537(2) 0.8396(4) 0.5345(2) 0.0208(8) 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 Ca1 0.0064(6) 0.0211(8) 0.0225(7) 0 0.0054(5) 0 P1 0.0059(6) 0.0182(7) 0.0218(7) 0.0010(5) 0.0050(5) -0.0016(5) P2 0.0061(6) 0.0210(7) 0.0215(6) 0.0005(5) 0.0057(4) -0.0020(5) P3 0.0050(6) 0.0198(7) 0.0225(7) -0.0008(5) 0.0052(5) 0.0012(5) Na1 0.0125(10) 0.0455(16) 0.0694(17) 0.0092(12) 0.0041(10) 0.0006(11) Na2 0.0123(10) 0.0288(12) 0.0279(10) 0.0015(8) 0.0069(8) -0.0007(9) O1 0.0090(16) 0.029(2) 0.0263(18) 0.0047(15) 0.0022(13) -0.0049(15) O2 0.0130(16) 0.027(2) 0.0257(17) -0.0011(15) 0.0085(13) 0.0001(15) O3 0.0061(15) 0.0164(18) 0.0301(18) 0.0009(14) 0.0029(13) -0.0010(13) O4 0.0106(15) 0.0239(19) 0.0231(18) 0.0023(14) 0.0006(13) -0.0011(14) O5 0.0067(15) 0.0250(19) 0.0321(19) 0.0036(15) 0.0099(13) -0.0034(14) O6 0.0191(17) 0.0257(19) 0.0265(18) 0.0011(15) 0.0030(14) -0.0018(16) O7 0.0100(15) 0.0231(19) 0.0244(18) -0.0022(14) 0.0006(13) 0.0012(15) O8 0.0100(16) 0.0230(18) 0.0287(18) -0.0033(15) 0.0052(13) 0.0070(15) O9 0.0118(16) 0.027(2) 0.0250(18) 0.0012(14) 0.0092(13) -0.0020(15) #----------------------------------------------------------------------------# # 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 Ca1 O1 2.341(3) 2_656 ? Ca1 O1 2.341(3) . y Ca1 O8 2.354(3) 1_545 y Ca1 O8 2.354(3) 2_646 ? Ca1 O5 2.377(3) 4_646 y Ca1 O5 2.377(3) 3_445 ? Ca1 P3 3.4510(17) 2_646 ? Ca1 P3 3.4510(17) 1_545 ? Ca1 P1 3.5236(17) 2_656 ? Ca1 P1 3.5236(17) . ? Ca1 P2 3.5534(12) 3_445 ? Ca1 P2 3.5534(12) 4_646 ? P1 O2 1.472(3) . y P1 O1 1.484(3) . y P1 O4 1.602(3) . y P1 O3 1.621(3) . y P1 Na2 3.366(2) . ? P1 Na2 3.425(2) 5_666 ? P2 O6 1.462(4) . y P2 O5 1.488(3) . y P2 O4 1.609(4) . y P2 O7 1.609(3) . y P2 Na2 3.331(2) 6_566 ? P2 Na2 3.389(2) 7_666 ? P2 Ca1 3.5534(12) 3 ? P3 O9 1.473(3) . y P3 O8 1.478(3) . y P3 O7 1.606(3) . y P3 O3 1.606(3) . y P3 Na2 3.331(2) 7_666 ? P3 Na2 3.368(2) . ? P3 Na1 3.370(2) 5_666 ? P3 Ca1 3.4510(17) 1_565 ? Na1 O2 2.336(4) 7_656 y Na1 O8 2.409(4) 5_666 y Na1 O9 2.543(4) 1_545 y Na1 O6 2.640(5) 6_565 y Na1 O2 2.670(4) . y Na1 O6 2.948(4) 4_646 y Na1 Na1 3.248(5) 7_656 ? Na1 P3 3.370(2) 5_666 ? Na1 Na2 3.409(3) 7_656 ? Na1 Ca1 3.984(3) 5_656 ? Na1 Na2 4.042(4) 1_545 ? Na1 Na2 4.090(4) . ? Na2 O2 2.398(4) . y Na2 O1 2.412(4) 5_666 y Na2 O9 2.420(4) 7_666 y Na2 O9 2.423(4) . y Na2 O5 2.482(4) 7_666 y Na2 O6 2.505(4) 6_565 y Na2 O4 2.989(4) 6_565 y Na2 P3 3.331(2) 7_666 ? Na2 P2 3.331(2) 6_565 ? Na2 P2 3.389(2) 7_666 ? O1 Na2 2.412(4) 5_666 ? O2 Na1 2.336(4) 7_656 ? O4 Na2 2.989(4) 6_566 ? O5 Ca1 2.377(3) 3 ? O5 Na2 2.482(4) 7_666 ? O6 Na2 2.505(4) 6_566 ? O6 Na1 2.640(5) 6_566 ? O6 Na1 2.948(4) 4_656 ? O8 Ca1 2.354(3) 1_565 ? O8 Na1 2.409(4) 5_666 ? O9 Na2 2.420(4) 7_666 ? O9 Na1 2.543(4) 1_565 ? 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 Ca1 O1 91.26(18) 2_656 . y O1 Ca1 O8 176.30(11) 2_656 1_545 y O1 Ca1 O8 86.90(12) . 1_545 y O1 Ca1 O8 86.90(12) 2_656 2_646 ? O1 Ca1 O8 176.30(11) . 2_646 ? O8 Ca1 O8 95.12(18) 1_545 2_646 y O1 Ca1 O5 81.44(11) 2_656 4_646 y O1 Ca1 O5 93.33(12) . 4_646 y O8 Ca1 O5 101.86(11) 1_545 4_646 y O8 Ca1 O5 83.23(11) 2_646 4_646 y O1 Ca1 O5 93.33(12) 2_656 3_445 ? O1 Ca1 O5 81.44(11) . 3_445 ? O8 Ca1 O5 83.23(11) 1_545 3_445 ? O8 Ca1 O5 101.86(11) 2_646 3_445 ? O5 Ca1 O5 172.55(18) 4_646 3_445 y O1 Ca1 P3 93.80(9) 2_656 2_646 ? O1 Ca1 P3 163.61(8) . 2_646 ? O8 Ca1 P3 87.12(10) 1_545 2_646 ? O8 Ca1 P3 20.03(8) 2_646 2_646 ? O5 Ca1 P3 102.83(9) 4_646 2_646 ? O5 Ca1 P3 82.71(9) 3_445 2_646 ? O1 Ca1 P3 163.61(8) 2_656 1_545 ? O1 Ca1 P3 93.80(9) . 1_545 ? O8 Ca1 P3 20.03(8) 1_545 1_545 ? O8 Ca1 P3 87.12(10) 2_646 1_545 ? O5 Ca1 P3 82.71(9) 4_646 1_545 ? O5 Ca1 P3 102.83(9) 3_445 1_545 ? P3 Ca1 P3 85.66(6) 2_646 1_545 ? O1 Ca1 P1 17.96(8) 2_656 2_656 ? O1 Ca1 P1 84.64(10) . 2_656 ? O8 Ca1 P1 158.38(8) 1_545 2_656 ? O8 Ca1 P1 94.51(9) 2_646 2_656 ? O5 Ca1 P1 98.47(9) 4_646 2_656 ? O5 Ca1 P1 75.86(9) 3_445 2_656 ? P3 Ca1 P1 95.52(3) 2_646 2_656 ? P3 Ca1 P1 178.09(3) 1_545 2_656 ? O1 Ca1 P1 84.64(10) 2_656 . ? O1 Ca1 P1 17.96(8) . . ? O8 Ca1 P1 94.51(9) 1_545 . ? O8 Ca1 P1 158.38(8) 2_646 . ? O5 Ca1 P1 75.86(9) 4_646 . ? O5 Ca1 P1 98.47(9) 3_445 . ? P3 Ca1 P1 178.09(3) 2_646 . ? P3 Ca1 P1 95.52(3) 1_545 . ? P1 Ca1 P1 83.34(5) 2_656 . ? O1 Ca1 P2 81.68(8) 2_656 3_445 ? O1 Ca1 P2 95.44(8) . 3_445 ? O8 Ca1 P2 95.29(8) 1_545 3_445 ? O8 Ca1 P2 87.47(8) 2_646 3_445 ? O5 Ca1 P2 161.12(8) 4_646 3_445 ? O5 Ca1 P2 18.04(8) 3_445 3_445 ? P3 Ca1 P2 69.95(3) 2_646 3_445 ? P3 Ca1 P2 113.27(4) 1_545 3_445 ? P1 Ca1 P2 65.85(3) 2_656 3_445 ? P1 Ca1 P2 110.85(4) . 3_445 ? O1 Ca1 P2 95.44(8) 2_656 4_646 ? O1 Ca1 P2 81.68(8) . 4_646 ? O8 Ca1 P2 87.47(8) 1_545 4_646 ? O8 Ca1 P2 95.29(8) 2_646 4_646 ? O5 Ca1 P2 18.04(8) 4_646 4_646 ? O5 Ca1 P2 161.12(8) 3_445 4_646 ? P3 Ca1 P2 113.27(4) 2_646 4_646 ? P3 Ca1 P2 69.95(3) 1_545 4_646 ? P1 Ca1 P2 110.85(4) 2_656 4_646 ? P1 Ca1 P2 65.85(3) . 4_646 ? P2 Ca1 P2 175.92(6) 3_445 4_646 ? O2 P1 O1 119.7(2) . . y O2 P1 O4 110.52(19) . . y O1 P1 O4 107.44(19) . . y O2 P1 O3 109.73(19) . . y O1 P1 O3 106.91(18) . . y O4 P1 O3 100.89(18) . . y O2 P1 Na2 38.62(15) . . ? O1 P1 Na2 133.01(15) . . ? O4 P1 Na2 119.18(14) . . ? O3 P1 Na2 71.12(12) . . ? O2 P1 Na2 121.19(15) . 5_666 ? O1 P1 Na2 37.01(14) . 5_666 ? O4 P1 Na2 127.16(14) . 5_666 ? O3 P1 Na2 72.41(12) . 5_666 ? Na2 P1 Na2 108.09(5) . 5_666 ? O2 P1 Ca1 122.35(16) . . ? O1 P1 Ca1 29.11(13) . . ? O4 P1 Ca1 80.47(13) . . ? O3 P1 Ca1 123.83(12) . . ? Na2 P1 Ca1 154.59(5) . . ? Na2 P1 Ca1 64.00(4) 5_666 . ? O6 P2 O5 120.4(2) . . y O6 P2 O4 107.4(2) . . y O5 P2 O4 109.3(2) . . y O6 P2 O7 108.61(19) . . y O5 P2 O7 108.3(2) . . y O4 P2 O7 101.12(17) . . y O6 P2 Na2 44.39(15) . 6_566 ? O5 P2 Na2 128.34(15) . 6_566 ? O4 P2 Na2 63.70(13) . 6_566 ? O7 P2 Na2 123.34(13) . 6_566 ? O6 P2 Na2 133.72(16) . 7_666 ? O5 P2 Na2 41.63(14) . 7_666 ? O4 P2 Na2 118.80(13) . 7_666 ? O7 P2 Na2 66.73(13) . 7_666 ? Na2 P2 Na2 169.70(5) 6_566 7_666 ? O6 P2 Ca1 90.94(14) . 3 ? O5 P2 Ca1 29.66(13) . 3 ? O4 P2 Ca1 120.36(13) . 3 ? O7 P2 Ca1 126.31(13) . 3 ? Na2 P2 Ca1 105.82(5) 6_566 3 ? Na2 P2 Ca1 64.04(4) 7_666 3 ? O9 P3 O8 119.9(2) . . y O9 P3 O7 109.38(18) . . y O8 P3 O7 107.23(19) . . y O9 P3 O3 110.73(19) . . y O8 P3 O3 106.67(18) . . y O7 P3 O3 101.32(18) . . y O9 P3 Na2 40.97(13) . 7_666 ? O8 P3 Na2 130.82(15) . 7_666 ? O7 P3 Na2 68.56(13) . 7_666 ? O3 P3 Na2 122.38(12) . 7_666 ? O9 P3 Na2 39.62(14) . . ? O8 P3 Na2 133.53(15) . . ? O7 P3 Na2 118.86(13) . . ? O3 P3 Na2 71.12(13) . . ? Na2 P3 Na2 67.06(6) 7_666 . ? O9 P3 Na1 112.65(15) . 5_666 ? O8 P3 Na1 39.05(14) . 5_666 ? O7 P3 Na1 136.21(14) . 5_666 ? O3 P3 Na1 74.95(12) . 5_666 ? Na2 P3 Na1 150.13(7) 7_666 5_666 ? Na2 P3 Na1 101.46(7) . 5_666 ? O9 P3 Ca1 122.28(15) . 1_565 ? O8 P3 Ca1 33.05(13) . 1_565 ? O7 P3 Ca1 76.25(13) . 1_565 ? O3 P3 Ca1 124.69(12) . 1_565 ? Na2 P3 Ca1 108.18(5) 7_666 1_565 ? Na2 P3 Ca1 157.61(5) . 1_565 ? Na1 P3 Ca1 71.47(5) 5_666 1_565 ? O2 Na1 O8 147.82(18) 7_656 5_666 y O2 Na1 O9 86.29(14) 7_656 1_545 y O8 Na1 O9 90.14(14) 5_666 1_545 y O2 Na1 O6 74.54(13) 7_656 6_565 y O8 Na1 O6 100.74(14) 5_666 6_565 y O9 Na1 O6 158.41(14) 1_545 6_565 y O2 Na1 O2 99.41(13) 7_656 . y O8 Na1 O2 107.98(14) 5_666 . y O9 Na1 O2 127.43(15) 1_545 . y O6 Na1 O2 66.88(12) 6_565 . y O2 Na1 O6 66.07(12) 7_656 4_646 y O8 Na1 O6 141.58(14) 5_666 4_646 y O9 Na1 O6 70.53(12) 1_545 4_646 y O6 Na1 O6 109.17(12) 6_565 4_646 y O2 Na1 O6 64.88(12) . 4_646 y O2 Na1 Na1 54.20(11) 7_656 7_656 ? O8 Na1 Na1 149.61(16) 5_666 7_656 ? O9 Na1 Na1 116.95(15) 1_545 7_656 ? O6 Na1 Na1 59.02(11) 6_565 7_656 ? O2 Na1 Na1 45.21(10) . 7_656 ? O6 Na1 Na1 50.14(10) 4_646 7_656 ? O2 Na1 P3 165.93(14) 7_656 5_666 ? O8 Na1 P3 22.74(8) 5_666 5_666 ? O9 Na1 P3 101.21(10) 1_545 5_666 ? O6 Na1 P3 95.69(11) 6_565 5_666 ? O2 Na1 P3 85.55(10) . 5_666 ? O6 Na1 P3 127.57(11) 4_646 5_666 ? Na1 Na1 P3 129.35(12) 7_656 5_666 ? O2 Na1 Na2 44.68(10) 7_656 7_656 ? O8 Na1 Na2 133.98(13) 5_666 7_656 ? O9 Na1 Na2 45.13(9) 1_545 7_656 ? O6 Na1 Na2 118.55(11) 6_565 7_656 ? O2 Na1 Na2 108.88(11) . 7_656 ? O6 Na1 Na2 45.70(8) 4_646 7_656 ? Na1 Na1 Na2 75.79(9) 7_656 7_656 ? P3 Na1 Na2 145.68(9) 5_666 7_656 ? O2 Na1 Ca1 115.34(13) 7_656 5_656 ? O8 Na1 Ca1 32.80(9) 5_666 5_656 ? O9 Na1 Ca1 80.72(10) 1_545 5_656 ? O6 Na1 Ca1 98.36(11) 6_565 5_656 ? O2 Na1 Ca1 137.43(11) . 5_656 ? O6 Na1 Ca1 151.16(10) 4_646 5_656 ? Na1 Na1 Ca1 155.97(13) 7_656 5_656 ? P3 Na1 Ca1 55.21(4) 5_666 5_656 ? Na2 Na1 Ca1 113.03(8) 7_656 5_656 ? O2 Na1 Na2 80.88(11) 7_656 1_545 ? O8 Na1 Na2 78.24(11) 5_666 1_545 ? O9 Na1 Na2 34.53(9) 1_545 1_545 ? O6 Na1 Na2 129.64(12) 6_565 1_545 ? O2 Na1 Na2 161.93(12) . 1_545 ? O6 Na1 Na2 99.46(9) 4_646 1_545 ? Na1 Na1 Na2 131.88(11) 7_656 1_545 ? P3 Na1 Na2 98.49(7) 5_666 1_545 ? Na2 Na1 Na2 58.82(6) 7_656 1_545 ? Ca1 Na1 Na2 54.63(5) 5_656 1_545 ? O2 Na1 Na2 97.36(12) 7_656 . ? O8 Na1 Na2 96.09(11) 5_666 . ? O9 Na1 Na2 161.40(13) 1_545 . ? O6 Na1 Na2 36.20(9) 6_565 . ? O2 Na1 Na2 34.00(8) . . ? O6 Na1 Na2 94.20(10) 4_646 . ? Na1 Na1 Na2 53.89(8) 7_656 . ? P3 Na1 Na2 79.35(6) 5_666 . ? Na2 Na1 Na2 129.67(7) 7_656 . ? Ca1 Na1 Na2 113.52(7) 5_656 . ? Na2 Na1 Na2 164.06(9) 1_545 . ? O2 Na2 O1 103.56(13) . 5_666 y O2 Na2 O9 87.77(12) . 7_666 y O1 Na2 O9 163.70(15) 5_666 7_666 y O2 Na2 O9 89.08(13) . . y O1 Na2 O9 88.04(13) 5_666 . y O9 Na2 O9 80.35(13) 7_666 . y O2 Na2 O5 174.00(15) . 7_666 y O1 Na2 O5 77.94(12) 5_666 7_666 y O9 Na2 O5 89.62(12) 7_666 7_666 y O9 Na2 O5 85.16(13) . 7_666 y O2 Na2 O6 73.24(13) . 6_565 y O1 Na2 O6 113.61(14) 5_666 6_565 y O9 Na2 O6 80.65(12) 7_666 6_565 y O9 Na2 O6 154.44(14) . 6_565 y O5 Na2 O6 111.65(13) 7_666 6_565 y O2 Na2 O4 119.86(13) . 6_565 y O1 Na2 O4 79.46(11) 5_666 6_565 y O9 Na2 O4 105.28(12) 7_666 6_565 y O9 Na2 O4 150.36(13) . 6_565 y O5 Na2 O4 66.06(11) 7_666 6_565 y O6 Na2 O4 52.68(11) 6_565 6_565 y O2 Na2 P3 106.58(10) . 7_666 ? O1 Na2 P3 149.77(11) 5_666 7_666 ? O9 Na2 P3 23.52(8) 7_666 7_666 ? O9 Na2 P3 94.75(10) . 7_666 ? O5 Na2 P3 72.33(9) 7_666 7_666 ? O6 Na2 P3 73.61(9) 6_565 7_666 ? O4 Na2 P3 83.55(8) 6_565 7_666 ? O2 Na2 P2 95.81(11) . 6_565 ? O1 Na2 P2 100.60(10) 5_666 6_565 ? O9 Na2 P2 89.68(10) 7_666 6_565 ? O9 Na2 P2 168.74(11) . 6_565 ? O5 Na2 P2 89.57(10) 7_666 6_565 ? O6 Na2 P2 24.10(9) 6_565 6_565 ? O4 Na2 P2 28.85(7) 6_565 6_565 ? P3 Na2 P2 74.14(5) 7_666 6_565 ? O2 Na2 P1 22.52(8) . . ? O1 Na2 P1 88.77(10) 5_666 . ? O9 Na2 P1 98.22(10) 7_666 . ? O9 Na2 P1 71.42(9) . . ? O5 Na2 P1 153.50(11) 7_666 . ? O6 Na2 P1 94.63(10) 6_565 . ? O4 Na2 P1 134.26(10) 6_565 . ? P3 Na2 P1 120.67(6) 7_666 . ? P2 Na2 P1 115.59(7) 6_565 . ? O2 Na2 P3 71.23(10) . . ? O1 Na2 P3 79.08(10) 5_666 . ? O9 Na2 P3 93.88(10) 7_666 . ? O9 Na2 P3 22.81(8) . . ? O5 Na2 P3 103.58(10) 7_666 . ? O6 Na2 P3 144.23(11) 6_565 . ? O4 Na2 P3 157.76(9) 6_565 . ? P3 Na2 P3 112.94(6) 7_666 . ? P2 Na2 P3 166.38(7) 6_565 . ? P1 Na2 P3 50.88(4) . . ? O2 Na2 P2 157.34(10) . 7_666 ? O1 Na2 P2 98.40(10) 5_666 7_666 ? O9 Na2 P2 72.02(9) 7_666 7_666 ? O9 Na2 P2 97.26(10) . 7_666 ? O5 Na2 P2 23.47(8) 7_666 7_666 ? O6 Na2 P2 92.96(10) 6_565 7_666 ? O4 Na2 P2 58.80(8) 6_565 7_666 ? P3 Na2 P2 51.37(4) 7_666 7_666 ? P2 Na2 P2 74.49(4) 6_565 7_666 ? P1 Na2 P2 166.49(7) . 7_666 ? P3 Na2 P2 119.11(7) . 7_666 ? P1 O1 Ca1 132.94(19) . . ? P1 O1 Na2 121.3(2) . 5_666 ? Ca1 O1 Na2 101.60(13) . 5_666 ? P1 O2 Na1 129.9(2) . 7_656 ? P1 O2 Na2 118.9(2) . . ? Na1 O2 Na2 92.09(14) 7_656 . ? P1 O2 Na1 119.9(2) . . ? Na1 O2 Na1 80.59(13) 7_656 . ? Na2 O2 Na1 107.49(14) . . ? P3 O3 P1 127.35(19) . . y P1 O4 P2 130.0(2) . . y P1 O4 Na2 139.49(18) . 6_566 ? P2 O4 Na2 87.46(14) . 6_566 ? P2 O5 Ca1 132.3(2) . 3 ? P2 O5 Na2 114.89(19) . 7_666 ? Ca1 O5 Na2 98.57(12) 3 7_666 ? P2 O6 Na2 111.5(2) . 6_566 ? P2 O6 Na1 124.7(2) . 6_566 ? Na2 O6 Na1 105.31(15) 6_566 6_566 ? P2 O6 Na1 156.1(2) . 4_656 ? Na2 O6 Na1 76.91(11) 6_566 4_656 ? Na1 O6 Na1 70.83(12) 6_566 4_656 ? P3 O7 P2 129.9(2) . . y P3 O8 Ca1 126.93(19) . 1_565 ? P3 O8 Na1 118.2(2) . 5_666 ? Ca1 O8 Na1 113.54(14) 1_565 5_666 ? P3 O9 Na2 115.50(19) . 7_666 ? P3 O9 Na2 117.57(19) . . ? Na2 O9 Na2 99.65(13) 7_666 . ? P3 O9 Na1 122.2(2) . 1_565 ? Na2 O9 Na1 86.73(13) 7_666 1_565 ? Na2 O9 Na1 108.96(15) . 1_565 ? #===END