# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2078 data_global #================================= # TITLE AND AUTHOR LIST _publ_section_title ; A new Caesium Zinc Hydrogen Phosphate Hydrate, CsZn2.5(HPO4)3 2H2O; Synthesis and Crystal Structure ; loop_ _publ_author_name _publ_author_address 'Jensen, Torben R.' ; Condensed Matter Physics and Chemistry Department Risoe National Laboratory Frederiksborgvej 399 DK-4000 Roskilde Denmark ; 'Hazell, Rita G.' ; Department of Chemistry Aarhus University Langelandsgade 140 DK-8000 \%Arhus C Denmark ; _publ_contact_author ; Dr. Torben R. Jensen Condensed Matter Physics and Chemistry Department Risoe National Laboratory Frederiksborgvej 399 DK-4000 Roskilde Denmark ; _publ_contact_author_phone '+45 4677 4745' _publ_contact_author_fax '+45 4677 4790' _publ_contact_author_email torben.rene.jensen@risoe.dk data_csps #================================== # CHEMICAL DATA _chemical_name_systematic ; mono Caesium Zinc tris monoHydrogenPhosphate di hydrate ; _chemical_formula_sum 'Cs H7 O14 P3 Zn2.5' _chemical_formula_structural 'Cs~Zn~2.5~(HPO~4~)~3~2H~2~O' _chemical_formula_weight 620.34 #================================== # CRYSTAL DATA _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '-x,-y,-z' _cell_length_a 8.3918(6) _cell_length_b 9.8254(8) _cell_length_c 9.9090(7) _cell_angle_alpha 111.172(1) _cell_angle_beta 111.751(1) _cell_angle_gamma 97.560(1) _cell_volume 673.59 _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 3963 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.3 _exptl_crystal_description 'triangular fragment' _exptl_crystal_colour 'colourless'' _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 3.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 7.52 _exptl_absorpt_correction_type 'multi-scan, SADABS' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 1.00 #================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation scans with narrow frames' _diffrn_reflns_number 17148 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.3 _diffrn_reflns_theta_max 26.3 _diffrn_reflns_reduction_process 8574 _reflns_number_total 2340 _reflns_number_observed 2245 _reflns_observed_criterion I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Cascarano et al., 1996) KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ATOMS ver. 4.0 E. Dowty (1997), Program ATOMS 4.0, Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, USA ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^ ; _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method ; Type 1 Lorentzian isotropic Becker and Coppens (1974) ; _refine_ls_extinction_coef 18(3) _refine_ls_number_reflns 2245 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.032 _refine_ls_wR_factor_obs 0.061 _refine_ls_goodness_of_fit_obs 2.238 _refine_ls_shift/esd_max 0.071 _refine_ls_shift/esd_mean 0.006 _refine_diff_density_max 1.6(2) _refine_diff_density_min -0.8(2) #========================================== # ATOMIC COORDINATES AND THERMAL 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_thermal_displace_type CS -0.02262(5) -0.50150(4) 0.26230(5) 0.0298(4) Uij ZN1 0.44669(8) -0.16530(7) 0.27435(7) 0.0130(5) Uij ZN2 -0.07054(8) -0.16935(7) 0.07159(7) 0.0134(5) Uij ZN3 0.50000 -0.50000 0.50000 0.0174(7) Uij P1 0.2700(2) -0.0521(2) 0.0318(2) 0.0132(10) Uij P2 0.3716(2) -0.5157(1) 0.1356(2) 0.0126(10) Uij P3 0.1866(2) -0.0611(1) 0.4289(2) 0.0122(10) Uij O1 0.2319(5) 0.1017(4) 0.0695(5) 0.023(3) Uij O2 0.1217(5) -0.1777(4) 0.0082(5) 0.021(3) Uij O3 0.4517(5) -0.0307(4) 0.1678(4) 0.019(3) Uij O4 0.2800(6) -0.1141(5) -0.1331(5) 0.026(3) Uij O5 0.4197(5) -0.3686(4) 0.1183(4) 0.016(3) Uij O6 0.3762(5) -0.4827(5) 0.2952(5) 0.022(3) Uij O7 0.1912(5) -0.6194(4) -0.0075(5) 0.023(3) Uij O8 0.5226(5) -0.5952(5) 0.1275(5) 0.022(3) Uij O9 0.3178(5) 0.0968(4) 0.5397(4) 0.020(3) Uij O10 0.0201(5) -0.0485(4) 0.3048(4) 0.018(3) Uij O11 0.2653(5) -0.1766(4) 0.3498(5) 0.021(3) Uij O12 0.1270(5) -0.1311(4) 0.5304(5) 0.022(3) Uij O13 0.2758(6) -0.6998(5) 0.3985(5) 0.033(3) Uij O14 0.6484(6) -0.6435(6) 0.4022(5) 0.032(4) Uij H13a 0.288(7) -0.777(7) 0.422(7) 0.01(1) Uiso H13b 0.250(17) 0.192(14) 0.282(15) 0.12(5) Uiso H14a 0.590(12) -0.623(10) 0.308(11) 0.06(3) Uiso H14b 0.629(12) -0.707(10) 0.430(11) 0.05(3) Uiso H4 0.348(10) -0.083(9) -0.138(10) 0.03(3) Uiso H8 0.550(9) -0.607(7) 0.036(8) 0.02(2) Uiso H12 0.050(11) -0.062(9) 0.582(9) 0.05(2) Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 CS 0.0271(3) 0.0257(3) 0.0293(3) 0.0066(2) 0.0076(2) 0.0107(2) ZN1 0.0154(4) 0.0098(4) 0.0128(4) 0.0036(3) 0.0055(3) 0.0051(3) ZN2 0.0142(4) 0.0111(4) 0.0128(4) 0.0028(3) 0.0042(3) 0.0055(3) ZN3 0.0204(5) 0.0186(6) 0.0140(5) 0.0061(4) 0.0068(4) 0.0092(4) P1 0.0128(7) 0.0117(7) 0.0166(7) 0.0034(5) 0.0060(5) 0.0088(6) P2 0.0143(7) 0.0108(7) 0.0124(7) 0.0029(5) 0.0049(5) 0.0063(6) P3 0.0132(7) 0.0107(7) 0.0125(7) 0.0039(5) 0.0059(5) 0.0048(5) O1 0.024(2) 0.015(2) 0.022(2) 0.006(2) 0.003(2) 0.009(2) O2 0.022(2) 0.013(2) 0.027(2) 0.001(2) 0.014(2) 0.005(2) O3 0.016(2) 0.017(2) 0.023(2) 0.006(2) 0.004(2) 0.013(2) O4 0.024(2) 0.029(3) 0.022(2) 0.001(2) 0.014(2) 0.008(2) O5 0.025(2) 0.008(2) 0.018(2) 0.004(2) 0.014(2) 0.005(2) O6 0.030(2) 0.026(2) 0.021(2) 0.016(2) 0.016(2) 0.014(2) O7 0.026(2) 0.015(2) 0.019(2) 0.001(2) 0.003(2) 0.010(2) O8 0.029(2) 0.024(2) 0.023(2) 0.012(2) 0.017(2) 0.013(2) O9 0.017(2) 0.010(2) 0.018(2) 0.003(2) -0.003(2) 0.004(2) O10 0.018(2) 0.015(2) 0.015(2) 0.003(2) 0.005(2) 0.005(2) O11 0.027(2) 0.014(2) 0.032(2) 0.013(2) 0.021(2) 0.010(2) O12 0.030(2) 0.022(2) 0.026(2) 0.009(2) 0.019(2) 0.016(2) O13 0.040(3) 0.022(2) 0.026(2) -0.002(2) 0.002(2) 0.016(2) O14 0.042(3) 0.033(3) 0.023(2) 0.023(2) 0.012(2) 0.013(2) #================================= # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag ZN1 O11 1.936(4) . . ? ZN1 O9 1.952(4) . 2_656 ? ZN1 O5 1.956(4) . . ? ZN1 O3 1.973(4) . . ? ZN2 O7 1.938(4) . 2_545 ? ZN2 O10 1.951(4) . . ? ZN2 O1 1.933(4) . 2_555 ? ZN2 O2 1.937(4) . . ? ZN3 O6 1.990(4) . . ? ZN3 O13 2.146(5) . . ? ZN3 O14 2.202(4) . . ? P1 O2 1.516(4) . . ? P1 O1 1.528(4) . . ? P1 O3 1.540(4) . . ? P1 O4 1.563(5) . . ? P2 O6 1.479(4) . . ? P2 O5 1.535(4) . . ? P2 O7 1.517(4) . . ? P2 O8 1.585(4) . . ? P3 O9 1.500(4) . . ? P3 O11 1.508(4) . . ? P3 O10 1.538(4) . . ? P3 O12 1.586(4) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag CS O2 3.060(4) . 2_545 ? CS O7 3.122(4) . 2_545 ? CS O6 3.213(4) . . ? CS O14 3.257(5) . 2_646 ? CS O11 3.346(4) . . ? CS O12 3.350(4) . . ? CS O8 3.407(4) . 1_455 ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 CS O7 91.0(1) 2_545 . 2_545 ? O2 CS O6 83.3(1) 2_545 . . ? O2 CS O14 121.8(1) 2_545 . 2_646 ? O2 CS O11 128.0(1) 2_545 . . ? O2 CS O12 170.26(9) 2_545 . . ? O2 CS O8 82.5(1) 2_545 . 1_455 ? O6 CS O7 104.4(1) . . 2_545 ? O7 CS O14 132.1(1) 2_545 . 2_646 ? O7 CS O11 69.5(1) 2_545 . . ? O7 CS O12 84.2(1) 2_545 . . ? O7 CS O8 70.4(1) 2_545 . 1_455 ? O6 CS O14 53.3(1) . . 2_646 ? O6 CS O11 58.0(1) . . . ? O6 CS O12 89.7(1) . . . ? O6 CS O8 164.8(1) . . 1_455 ? O11 CS O14 62.8(1) . . 2_646 ? O12 CS O14 57.6(1) . . 2_646 ? O8 CS O14 140.7(1) 1_455 . 2_646 ? O11 CS O12 42.34(9) . . . ? O8 CS O11 128.97(9) 1_455 . . ? O8 CS O12 103.6(1) 1_455 . . ? O8 CS O12 103.6(1) 1_455 . . ? O9 ZN1 O11 107.9(2) 2_656 . . ? O5 ZN1 O11 110.5(2) . . . ? O3 ZN1 O11 117.1(2) . . . ? O5 ZN1 O9 106.9(2) . . 2_656 ? O3 ZN1 O9 108.1(2) . . 2_656 ? O3 ZN1 O5 105.9(2) . . . ? O7 ZN2 O10 109.9(2) 2_545 . . ? O1 ZN2 O7 107.7(2) 2_555 . 2_545 ? O2 ZN2 O7 105.1(2) . . 2_545 ? O1 ZN2 O10 117.3(2) 2_555 . . ? O2 ZN2 O10 112.3(2) . . . ? O1 ZN2 O2 103.7(2) 2_555 . . ? O6 ZN3 O13 86.6(2) . . . ? O6 ZN3 O14 92.6(2) . . . ? O13 ZN3 O14 90.5(2) . . . ? O1 P1 O2 113.4(2) . . . ? O2 P1 O3 110.5(2) . . . ? O2 P1 O4 104.2(2) . . . ? O1 P1 O3 109.2(2) . . . ? O1 P1 O4 110.4(2) . . . ? O3 P1 O4 108.9(2) . . . ? O5 P2 O6 112.0(2) . . . ? O6 P2 O7 113.8(2) . . . ? O6 P2 O8 106.5(2) . . . ? O5 P2 O7 107.6(2) . . . ? O5 P2 O8 107.1(2) . . . ? O7 P2 O8 109.5(2) . . . ? O9 P3 O11 114.1(2) . . . ? O9 P3 O10 108.2(2) . . . ? O9 P3 O12 109.9(2) . . . ? O10 P3 O11 112.6(2) . . . ? O11 P3 O12 102.8(2) . . . ? O10 P3 O12 109.1(2) . . . ? O10 P3 O12 109.1(2) . . . ? ZN2 O1 P1 130.3(2) 2_555 . . ? ZN2 O2 P1 131.6(2) . . . ? ZN1 O3 P1 116.0(2) . . . ? P1 O3 O4 108.6(2) . . 2_655 ? ZN1 O3 O4 131.5(2) . . 2_655 ? P1 O4 O3 121.2(3) . . 2_655 ? ZN1 O5 P2 123.7(2) . . . ? P2 O5 O8 115.1(2) . . 2_645 ? ZN1 O5 O8 121.2(2) . . 2_645 ? ZN3 O6 P2 143.7(3) . . . ? P2 O6 O13 126.9(2) . . . ? P2 O6 O14 165.7(3) . . 2_646 ? ZN3 O6 O13 49.0(1) . . . ? ZN3 O6 O14 49.3(1) . . 2_646 ? O13 O6 O14 64.5(2) . . 2_646 ? ZN2 O7 P2 128.1(2) 2_545 . . ? P2 O8 O5 114.0(2) . . 2_645 ? P2 O8 O14 105.7(2) . . . ? O5 O8 O14 140.3(2) 2_645 . . ? ZN1 O9 P3 130.2(2) 2_656 . . ? P3 O9 O13 113.2(2) . . 1_565 ? ZN1 O9 O13 112.9(2) 2_656 . 1_565 ? ZN2 O10 P3 121.9(2) . . . ? P3 O10 O12 107.9(2) . . 2_556 ? ZN2 O10 O12 129.8(2) . . 2_556 ? ZN1 O11 P3 134.1(2) . . . ? P3 O12 O10 111.6(2) . . 2_556 ? ZN3 O13 O9 117.9(2) . . 1_545 ? O6 O14 O8 133.2(2) 2_646 . . ? P1 O1 H13b 111(4) . . . ? ZN2 O1 H13b 111(4) 2_555 . . ? P1 O3 H4 107.1(23) . . 2_655 ? ZN1 O3 H4 133.2(23) . . 2_655 ? O4 O3 H4 1.7(24) 2_655 . 2_655 ? P1 O4 H4 120(7) . . . ? O3 O4 H4 5(8) 2_655 . . ? P2 O5 H8 114.5(23) . . 2_645 ? ZN1 O5 H8 121.8(23) . . 2_645 ? O8 O5 H8 1.5(24) 2_645 . 2_645 ? P2 O8 H8 115(4) . . . ? P2 O8 H14a 101.5(28) . . . ? ZN3 O13 H13b 120(6) . . 1_545 ? ZN3 O14 H14a 83(5) . . . ? ZN3 O14 H14b 97(7) . . . ? loop_ _publ_manuscript_incl_extra_item '_geom_bond_atom_site_label_D' '_geom_bond_atom_site_label_H' '_geom_contact_atom_site_label_A' '_geom_bond_distance_DH' '_geom_contact_distance_HA' '_geom_contact_distance_DA' '_geom_angle_DHA' '_geom_contact_site_symmetry_A' loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A O4 H4 O3 0.64(8) 2.06(8) 2.701(6) 173(10) 2_655 O8 H8 O5 0.99(7) 1.58(7) 2.567(5) 176(6) 2_645 O12 H12 O10 1.11(8) 1.60(8) 2.700(5) 167(7) 2_556 O14 H14a O8 0.99(10) 1.80(10) 2.772(6) 168(8) . O13 H13b O1 1.17(12) 1.91(12) 2.983(6) 151(10) 1_545 O13 H13a O9 0.87(6) 1.97(7) 2.813(6) 161(5) 1_545