# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_sad1 _database_code_CSD 166478 _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Choudhury, Amitava' 'Jayaraman, K.' 'Rao, C. N. R.' 'Vaidhyanathan, R.' _publ_contact_author_name 'Prof C N R Rao' _publ_contact_author_address ; Chemistry & Physics of Materials Unit Jawaharlal Nehru Centre for Advanced Scientific Research Jaakur P.O. Bangalore 560 064 INDIA ; _publ_contact_author_email 'CNRRAO@JNCASR.AC.IN' _publ_section_title ; A Layered Chlorophosphate, Na3[Cd4C13(HPO4)2(H2PO4)4] Containing Na+ Ions in the Interlamellar Space ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'H2.50 Cd Cl0.75 Na0.75 O6 P1.50' _chemical_formula_weight 301.20 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fmm2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, z' '-x, y, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x, -y+1/2, z+1/2' '-x, y+1/2, z+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' _cell_length_a 14.5678(4) _cell_length_b 21.26020(10) _cell_length_c 7.8893(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2443.43(9) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description chunky _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.275 _exptl_crystal_density_method ? _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 4.313 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2566 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 23.24 _reflns_number_total 919 _reflns_number_observed 882 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00094(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(4) _refine_ls_number_reflns 919 _refine_ls_number_parameters 106 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0216 _refine_ls_R_factor_obs 0.0199 _refine_ls_wR_factor_all 0.0450 _refine_ls_wR_factor_obs 0.0444 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.037 _refine_ls_restrained_S_all 1.026 _refine_ls_restrained_S_obs 1.036 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd -0.35758(2) -0.91334(2) 0.31867(9) 0.0154(2) Uani 1 d . . Cl1 Cl -0.5000 -0.84203(9) 0.2634(2) 0.0196(5) Uani 1 d S . Cl2 Cl -0.5000 -1.0000 0.3809(4) 0.0185(7) Uani 1 d S . P1 P -0.1737(2) -1.0000 0.4468(3) 0.0123(5) Uani 1 d S . P2 P -0.16685(12) -0.83316(7) 0.2049(2) 0.0146(4) Uani 1 d . . O1 O -0.1359(3) -0.8853(2) 0.0911(6) 0.0247(10) Uani 1 d . . O2 O -0.3492(2) -0.9402(2) 0.0427(5) 0.0194(10) Uani 1 d . . O3 O -0.2694(3) -0.8299(2) 0.2405(5) 0.0213(11) Uani 1 d . . O4 O -0.2730(3) -1.0000 0.3850(7) 0.0164(13) Uani 1 d S . O5 O -0.1101(4) -1.0000 0.2845(8) 0.025(2) Uani 1 d S . H1 H -0.1201(4) -1.0317 0.2283(8) 0.037 Uiso 0.50 calc PR . O6 O -0.1339(3) -0.7687(2) 0.1303(6) 0.0214(10) Uani 1 d . . H2 H -0.1507(3) -0.7400(2) 0.1925(6) 0.032 Uiso 1 calc R . O7 O -0.1114(3) -0.8380(2) 0.3758(5) 0.0214(11) Uani 1 d . . H3 H -0.1215(3) -0.8721(2) 0.4205(5) 0.032 Uiso 1 calc R . Na1 Na 0.0000 -0.76465(14) 0.4724(4) 0.0238(8) Uani 1 d S . Na2 Na 0.0000 -0.9335(3) 0.1963(9) 0.023(2) Uani 0.50 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 Cd1 0.0142(2) 0.0132(2) 0.0188(2) 0.0012(2) -0.0001(3) 0.0004(2) Cl1 0.0122(10) 0.0167(9) 0.0298(13) 0.0040(8) 0.000 0.000 Cl2 0.0134(15) 0.0148(14) 0.027(2) 0.000 0.000 0.000 P1 0.0118(11) 0.0124(11) 0.0129(12) 0.000 -0.0004(9) 0.000 P2 0.0126(8) 0.0119(8) 0.0195(8) 0.0001(7) -0.0009(7) -0.0013(6) O1 0.026(3) 0.024(3) 0.024(2) -0.012(2) -0.008(2) 0.006(2) O2 0.023(2) 0.017(2) 0.018(2) 0.002(2) 0.005(2) 0.004(2) O3 0.016(3) 0.014(2) 0.034(3) 0.005(2) 0.004(2) -0.004(2) O4 0.009(3) 0.019(3) 0.021(3) 0.000 -0.003(2) 0.000 O5 0.021(3) 0.036(3) 0.017(5) 0.000 0.004(3) 0.000 O6 0.025(2) 0.012(2) 0.027(2) 0.000(2) 0.007(2) -0.002(2) O7 0.025(3) 0.016(2) 0.023(3) 0.003(2) -0.003(2) -0.007(2) Na1 0.019(2) 0.023(2) 0.029(2) -0.002(2) 0.000 0.000 Na2 0.015(4) 0.025(4) 0.029(4) 0.001(3) 0.000 0.000 _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 Cd1 O1 2.232(5) 12_455 ? Cd1 O2 2.255(4) . ? Cd1 O3 2.275(3) . ? Cd1 O4 2.277(3) . ? Cd1 Cl1 2.6064(12) . ? Cd1 Cl2 2.8178(6) . ? Cl1 Cd1 2.6064(12) 4_455 ? Cl2 Cd1 2.8178(6) 2_435 ? Cl2 Cd1 2.8178(6) 4_455 ? Cl2 Cd1 2.8178(6) 3_535 ? P1 O2 1.516(5) 12_455 ? P1 O2 1.516(5) 10_435 ? P1 O4 1.527(5) . ? P1 O5 1.580(6) . ? P2 O1 1.496(4) . ? P2 O3 1.521(4) . ? P2 O6 1.567(4) . ? P2 O7 1.575(4) . ? O1 Cd1 2.232(5) 12_454 ? O2 P1 1.516(5) 10_434 ? O4 Cd1 2.277(3) 3_535 ? O5 H1 0.82 . ? O6 H2 0.82 . ? O7 H3 0.82 . ? 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 Cd1 O2 179.0(2) 12_455 . ? O1 Cd1 O3 94.4(2) 12_455 . ? O2 Cd1 O3 84.6(2) . . ? O1 Cd1 O4 91.0(2) 12_455 . ? O2 Cd1 O4 89.3(2) . . ? O3 Cd1 O4 112.79(14) . . ? O1 Cd1 Cl1 88.39(12) 12_455 . ? O2 Cd1 Cl1 91.66(11) . . ? O3 Cd1 Cl1 87.20(10) . . ? O4 Cd1 Cl1 159.99(11) . . ? O1 Cd1 Cl2 88.61(12) 12_455 . ? O2 Cd1 Cl2 92.43(11) . . ? O3 Cd1 Cl2 166.59(10) . . ? O4 Cd1 Cl2 80.16(11) . . ? Cl1 Cd1 Cl2 79.82(4) . . ? Cd1 Cl1 Cd1 105.51(7) 4_455 . ? Cd1 Cl2 Cd1 159.95(12) . 2_435 ? Cd1 Cl2 Cd1 94.84(3) . 4_455 ? Cd1 Cl2 Cd1 81.67(2) 2_435 4_455 ? Cd1 Cl2 Cd1 81.66(2) . 3_535 ? Cd1 Cl2 Cd1 94.84(3) 2_435 3_535 ? Cd1 Cl2 Cd1 159.95(12) 4_455 3_535 ? O2 P1 O2 113.9(3) 12_455 10_435 ? O2 P1 O4 111.6(2) 12_455 . ? O2 P1 O4 111.6(2) 10_435 . ? O2 P1 O5 106.0(2) 12_455 . ? O2 P1 O5 106.0(2) 10_435 . ? O4 P1 O5 107.3(3) . . ? O1 P2 O3 116.1(2) . . ? O1 P2 O6 109.3(3) . . ? O3 P2 O6 109.4(2) . . ? O1 P2 O7 108.1(2) . . ? O3 P2 O7 110.3(2) . . ? O6 P2 O7 102.8(2) . . ? P2 O1 Cd1 139.7(3) . 12_454 ? P1 O2 Cd1 134.9(3) 10_434 . ? P2 O3 Cd1 124.7(2) . . ? P1 O4 Cd1 125.87(10) . . ? P1 O4 Cd1 125.87(10) . 3_535 ? Cd1 O4 Cd1 108.0(2) . 3_535 ? P1 O5 H1 109.47(12) . . ? P2 O6 H2 109.5(2) . . ? P2 O7 H3 109.47(15) . . ? _refine_diff_density_max 0.360 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.110