Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 _publ_requested_journal ' J. Mater. Chem.' loop_ _publ_author_name 'Le Fur, E.' 'Pena, O.' 'Pivan, J. Y.' _publ_contact_author_name 'Jean Yves Pivan' _publ_contact_author_address ; Jean Yves Pivan Laboratoire de Physicochimie Ecole Nationale Superieure de Chimie Campus de Beaulieu Avenue du General Leclerc 35000 Rennes France ; _publ_contact_author_email 'jean-yves.pivan@ensc-rennes.fr' _publ_section_title ; Magnetic susceptibility and crystal structure of the new oxovanadium phosphate (NH4)ZN(H2O)(VO)2(PO4)2(H2PO4). ; data_nazn _database_code_CSD 166367 _audit_creation_date 'Mon Jun 12 2001' _audit_creation_method JANA2000 ; ? _cell_length_a 10.7451(2) _cell_length_b 9.19410(10) _cell_length_c 13.2112(2) _cell_angle_alpha 90 _cell_angle_beta 103.6600(8) _cell_angle_gamma 90 _cell_volume 1268.24(3) _cell_measurement_reflns_used 10962 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 34.97 _cell_measurement_theta_min 1 _cell_formula_units_Z 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _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 O 0 0 0.011 0.006 International_Tables_Vol_C 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.867 32.908901 0.2508 P 0 0 0.102 0.094 International_Tables_Vol_C 6.4345 1.9067 4.1791 27.157 1.78 0.526 1.4908 68.164497 1.1149 V 0 0 0.301 0.529 International_Tables_Vol_C 10.2971 6.8657 7.3511 0.4385 2.0703 26.893801 2.0571 102.477997 1.2199 Zn 0 0 0.284 1.430 International_Tables_Vol_C 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.41 58.709702 1.3041 N 0 0 0.006 0.003 International_Tables_Vol_C 12.2126 0.0057 3.1322 9.8933 2.0125 28.997499 1.1663 0.5826 -11.529 H 0 0 0.000 0.000 International_Tables_Vol_C 0.493002 10.5109 0.322912 26.1257 0.140191 3.14236 0.04081 57.799702 0.003038 _chemical_formula_sum 'O60 P12 V8 Zn4 N4 H32' _chemical_formula_weight 2088.94 _exptl_crystal_colour 'blue' _exptl_crystal_description 'plates' _exptl_crystal_size_max 0.5 _exptl_crystal_size_min 0.09 _exptl_crystal_F_000 992 _exptl_absorpt_correction_type none _exptl_absorpt_coefficient_mu 3.79 _exptl_absorpt_correction_T_min 0. _exptl_absorpt_correction_T_max 0.603 _diffrn_measurement_device 'Kappa CCD' _diffrn_measurement_method 'omega-phi scans' _diffrn_radiation_probe 'X-ray' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _reflns_limit_h_min -17 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _diffrn_reflns_number 5572 _diffrn_reflns_theta_min 1 _diffrn_reflns_theta_max 34.97 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI 0.0314 _reflns_observed_criterion >2sigma(I) _reflns_number_total 5572 _reflns_number_observed 5330 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/\s^2^(I)' _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_gt 0.0472 _refine_ls_R_factor_all 0.0298 _refine_ls_wR_factor_ref 0.0472 _refine_ls_number_reflns 3793 _refine_ls_number_parameters 200 _refine_ls_goodness_of_fit_ref 1.36 _refine_ls_goodness_of_fit_obs 1.36 _refine_ls_shift/su_max 0.0250 _refine_ls_shift/su_mean 0.0020 _refine_diff_density_max 0.78 _refine_diff_density_min -0.54 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic' _refine_ls_extinction_coef 0.27(1) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO (Otwinowski, 1997)' _computing_data_reduction 'SCALEPACK (Otwinowski, 1997)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'JANA2000 (Jellinek, 2000)' _computing_molecular_graphics ? 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_symmetry_multiplicity _atom_site_occupancy Zn1 Zn 0.639330(16) 0.248878(13) 0.521105(12) 0.015323 4 1 V1 V 0.99286(2) 0.244883(18) 0.468622(15) 0.009858 4 1 V2 V 0.788802(19) 0.249112(17) 0.263548(15) 0.00884 4 1 P1 P 0.72639(2) 0.49010(2) 0.07391(2) 0.008419 4 1 P2 P 0.78601(2) 0.50709(2) 0.43271(2) 0.008122 4 1 P3 P 0.60177(3) 0.33248(3) 0.74242(2) 0.013326 4 1 O1 O 0.86141(7) 0.38943(8) 0.38501(6) 0.010677 4 1 O2 O 0.64559(7) 0.60501(8) 0.11678(6) 0.011144 4 1 O3 O 0.80430(8) 0.40178(8) 0.16457(6) 0.013683 4 1 O4 O 0.70748(8) 0.59671(8) 0.34230(6) 0.01409 4 1 O5 O 0.64255(9) 0.25476(8) 0.26977(8) 0.019886 4 1 O6 O 0.51042(8) 0.26060(8) 0.79882(6) 0.012518 4 1 O7 O 0.88137(8) 0.59743(8) 0.51118(6) 0.015862 4 1 O8 O 0.63406(9) 0.39853(9) -0.00707(6) 0.016808 4 1 O9 O 0.69392(8) 0.43573(8) 0.48907(6) 0.016796 4 1 O10 O 0.82046(9) 0.56133(8) 0.01920(7) 0.018939 4 1 O11 O 0.94255(11) 0.24051(9) 0.57304(7) 0.022122 4 1 O12 O 0.72512(9) 0.38763(11) 0.82236(7) 0.02443 4 1 O13 O 0.64769(12) 0.23322(10) 0.66922(8) 0.025377 4 1 O14 O 0.53950(9) 0.47304(11) 0.68451(8) 0.029433 4 1 O15 O 0.44841(12) 0.27908(14) 0.45423(13) 0.050759 4 1 N1 N 1.05769(12) 0.54308(12) 0.26643(10) 0.025406 4 1 loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_adp_type _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 Zn1 Zn Uani 0.02219 0.00981 0.01619 -0.00101 0.00897 -0.00098 V1 V Uani 0.01087 0.00832 0.00856 -0.00047 -0.00135 0.00021 V2 V Uani 0.00981 0.00743 0.00798 -0.00029 -0.0005 0.00012 P1 P Uani 0.01092 0.00607 0.00776 0.00023 0.00119 0.0003 P2 P Uani 0.00942 0.00602 0.00828 -0.00033 0.0008 -0.00003 P3 P Uani 0.01371 0.01371 0.01304 0.0003 0.00412 0.00108 O1 O Uani 0.01198 0.00842 0.01049 0.0021 0.00037 -0.0017 O2 O Uani 0.01239 0.00923 0.01035 0.00208 -0.00024 -0.00198 O3 O Uani 0.01604 0.0115 0.01221 0.00242 0.00074 0.0043 O4 O Uani 0.01535 0.01197 0.01324 0.00386 -0.00004 0.0046 O5 O Uani 0.01238 0.02136 0.02468 -0.00077 0.0019 -0.00053 O6 O Uani 0.01103 0.01411 0.01267 -0.00102 0.00331 0.0008 O7 O Uani 0.01645 0.01232 0.01598 -0.00244 -0.00184 -0.00513 O8 O Uani 0.01847 0.01379 0.01494 -0.00262 -0.0025 -0.00565 O9 O Uani 0.01946 0.01382 0.02031 -0.00231 0.0111 0.00249 O10 O Uani 0.02213 0.01381 0.02521 0.00041 0.01425 0.00586 O11 O Uani 0.02797 0.02539 0.01338 -0.00121 0.00563 -0.00096 O12 O Uani 0.016 0.03715 0.02031 -0.00623 0.00463 -0.00546 O13 O Uani 0.03788 0.02455 0.01808 0.00298 0.01536 -0.00044 O14 O Uani 0.02229 0.02266 0.04429 0.00439 0.00974 0.01758 O15 O Uani 0.02316 0.04248 0.07802 -0.00446 -0.00528 -0.0037 N1 N Uani 0.02391 0.01716 0.03721 -0.00101 0.01134 -0.00188 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 Zn1 P1 3.1883(3) . 2_645 Zn1 P2 3.2174(3) . . Zn1 P3 3.1401(4) . . Zn1 O9 1.8971(8) . . Zn1 O10 1.8912(9) . 2_645 Zn1 O11 3.1667(12) . . Zn1 O13 1.9367(11) . . Zn1 O15 2.0439(13) . . V1 V2 3.0569(3) . . V1 P1 3.2760(3) . 2_645 V1 P2 3.2367(3) . . V1 O1 2.0595(8) . . V1 O2 2.0850(8) . 2_645 V1 O6 2.3008(10) . 4_554 V1 O7 1.9524(9) . 3_766 V1 O8 1.9764(9) . 4_555 V1 O11 1.5979(12) . . V2 V1 3.0569(3) . . V2 P1 3.2943(3) . . V2 P1 3.2372(3) . 2_645 V2 P2 3.2638(3) . . V2 O1 2.0667(8) . . V2 O2 2.0584(8) . 2_645 V2 O3 1.9555(9) . . V2 O4 1.9882(8) . 2_645 V2 O5 1.5941(11) . . V2 O6 2.3244(9) . 4_554 P1 Zn1 3.1883(3) . 2_655 P1 V1 3.2760(3) . 2_655 P1 V2 3.2943(3) . . P1 V2 3.2372(3) . 2_655 P1 O2 1.5570(9) . . P1 O3 1.5213(8) . . P1 O5 3.2859(9) . 2_655 P1 O8 1.5269(9) . . P1 O10 1.5196(11) . . P1 O11 3.2675(9) . 2_655 P2 Zn1 3.2174(3) . . P2 V1 3.2367(3) . . P2 V2 3.2638(3) . . P2 O1 1.5684(9) . . P2 O4 1.5288(8) . . P2 O5 3.2941(9) . . P2 O7 1.5208(8) . . P2 O9 1.5193(10) . . P2 O11 3.2869(9) . . P3 Zn1 3.1401(4) . . P3 O6 1.5102(10) . . P3 O12 1.5674(9) . . P3 O13 1.5049(12) . . P3 O14 1.5685(10) . . 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 P1 Zn1 P2 95.839(10) 2_645 . . P1 Zn1 P3 135.916(10) 2_645 . . P1 Zn1 O9 113.33(3) 2_645 . . P1 Zn1 O10 18.55(3) 2_645 . 2_645 P1 Zn1 O11 61.88(2) 2_645 . . P1 Zn1 O13 114.82(3) 2_645 . . P1 Zn1 O15 115.44(4) 2_645 . . P2 Zn1 P3 109.811(10) . . . P2 Zn1 O9 17.50(3) . . . P2 Zn1 O10 114.22(3) . . 2_645 P2 Zn1 O11 61.97(2) . . . P2 Zn1 O13 120.60(3) . . . P2 Zn1 O15 105.41(4) . . . P3 Zn1 O9 95.78(3) . . . P3 Zn1 O10 124.98(3) . . 2_645 P3 Zn1 O11 98.98(2) . . . P3 Zn1 O13 21.11(3) . . . P3 Zn1 O15 92.10(5) . . . O9 Zn1 O10 131.66(4) . . 2_645 O9 Zn1 O11 73.44(3) . . . O9 Zn1 O13 110.44(4) . . . O9 Zn1 O15 96.20(5) . . . O10 Zn1 O11 75.32(3) 2_645 . . O10 Zn1 O13 104.63(4) 2_645 . . O10 Zn1 O15 105.92(5) 2_645 . . O11 Zn1 O13 88.57(4) . . . O11 Zn1 O15 165.45(5) . . . O13 Zn1 O15 104.85(6) . . . V2 V1 P1 61.368(10) . . 2_645 V2 V1 P2 62.398(10) . . . V2 V1 O1 42.29(2) . . . V2 V1 O2 42.12(2) . . 2_645 V2 V1 O6 48.96(2) . . 4_554 V2 V1 O7 116.25(2) . . 3_766 V2 V1 O8 121.06(3) . . 4_555 V2 V1 O11 116.51(4) . . . P1 V1 P2 93.774(10) 2_645 . . P1 V1 O1 89.79(2) 2_645 . . P1 V1 O2 22.12(2) 2_645 . 2_645 P1 V1 O6 92.35(2) 2_645 . 4_554 P1 V1 O7 177.48(2) 2_645 . 3_766 P1 V1 O8 92.47(3) 2_645 . 4_555 P1 V1 O11 75.57(4) 2_645 . . P2 V1 O1 23.16(2) . . . P2 V1 O2 90.24(2) . . 2_645 P2 V1 O6 94.97(2) . . 4_554 P2 V1 O7 84.20(3) . . 3_766 P2 V1 O8 173.76(3) . . 4_555 P2 V1 O11 77.57(4) . . . O1 V1 O2 78.45(3) . . 2_645 O1 V1 O6 72.34(3) . . 4_554 O1 V1 O7 87.76(3) . . 3_766 O1 V1 O8 157.06(4) . . 4_555 O1 V1 O11 98.62(4) . . . O2 V1 O6 70.89(3) 2_645 . 4_554 O2 V1 O7 156.03(4) 2_645 . 3_766 O2 V1 O8 95.55(3) 2_645 . 4_555 O2 V1 O11 96.08(4) 2_645 . . O6 V1 O7 86.35(3) 4_554 . 3_766 O6 V1 O8 84.75(3) 4_554 . 4_555 O6 V1 O11 165.17(5) 4_554 . . O7 V1 O8 89.56(4) 3_766 . 4_555 O7 V1 O11 105.38(4) 3_766 . . O8 V1 O11 104.05(5) 4_555 . . V1 V2 P1 131.093(10) . . . V1 V2 P1 62.652(10) . . 2_645 V1 V2 P2 61.502(10) . . . V1 V2 O1 42.10(2) . . . V1 V2 O2 42.79(2) . . 2_645 V1 V2 O3 116.52(2) . . . V1 V2 O4 119.10(2) . . 2_645 V1 V2 O5 117.79(4) . . . V1 V2 O6 48.30(2) . . 4_554 P1 V2 P1 165.219(10) . . 2_645 P1 V2 P2 89.960(10) . . . P1 V2 O1 98.20(2) . . . P1 V2 O2 171.87(3) . . 2_645 P1 V2 O3 16.36(3) . . . P1 V2 O4 88.39(2) . . 2_645 P1 V2 O5 89.50(3) . . . P1 V2 O6 101.05(2) . . 4_554 P1 V2 P1 165.219(10) 2_645 . . P1 V2 P2 93.996(10) 2_645 . . P1 V2 O1 90.74(2) 2_645 . . P1 V2 O2 22.73(2) 2_645 . 2_645 P1 V2 O3 177.70(3) 2_645 . . P1 V2 O4 87.84(2) 2_645 . 2_645 P1 V2 O5 77.56(3) 2_645 . . P1 V2 O6 92.90(2) 2_645 . 4_554 P2 V2 O1 22.50(2) . . . P2 V2 O2 89.96(2) . . 2_645 P2 V2 O3 87.30(3) . . . P2 V2 O4 178.10(3) . . 2_645 P2 V2 O5 76.99(3) . . . P2 V2 O6 93.80(2) . . 4_554 O1 V2 O2 78.89(3) . . 2_645 O1 V2 O3 89.74(3) . . . O1 V2 O4 157.18(4) . . 2_645 O1 V2 O5 97.99(4) . . . O1 V2 O6 71.72(3) . . 4_554 O2 V2 O3 155.57(4) 2_645 . . O2 V2 O4 91.54(3) 2_645 . 2_645 O2 V2 O5 98.40(4) 2_645 . . O2 V2 O6 70.84(3) 2_645 . 4_554 O3 V2 O4 90.85(4) . . 2_645 O3 V2 O5 104.60(4) . . . O3 V2 O6 85.12(3) . . 4_554 O4 V2 O5 103.92(4) 2_645 . . O4 V2 O6 85.60(3) 2_645 . 4_554 O5 V2 O6 166.07(5) . . 4_554 Zn1 P1 V1 76.906(10) 2_655 . 2_655 Zn1 P1 V2 140.501(10) 2_655 . . Zn1 P1 V2 79.092(10) 2_655 . 2_655 Zn1 P1 O2 89.00(3) 2_655 . . Zn1 P1 O3 119.43(4) 2_655 . . Zn1 P1 O5 61.92(2) 2_655 . 2_655 Zn1 P1 O8 114.73(4) 2_655 . . Zn1 P1 O10 23.32(3) 2_655 . . Zn1 P1 O11 58.73(2) 2_655 . 2_655 V1 P1 V2 128.303(10) 2_655 . . V1 P1 V2 55.980(10) 2_655 . 2_655 V1 P1 O2 30.29(3) 2_655 . . V1 P1 O3 139.03(4) 2_655 . . V1 P1 O5 76.30(2) 2_655 . 2_655 V1 P1 O8 87.17(4) 2_655 . . V1 P1 O10 98.47(3) 2_655 . . V1 P1 O11 28.27(2) 2_655 . 2_655 V2 P1 V2 91.298(10) . . 2_655 V2 P1 O2 102.04(3) . . . V2 P1 O3 21.23(3) . . . V2 P1 O5 92.20(2) . . 2_655 V2 P1 O8 98.13(3) . . . V2 P1 O10 127.59(4) . . . V2 P1 O11 155.46(2) . . 2_655 V2 P1 V2 91.298(10) 2_655 . . V2 P1 O2 30.71(3) 2_655 . . V2 P1 O3 88.55(3) 2_655 . . V2 P1 O5 28.28(2) 2_655 . 2_655 V2 P1 O8 137.84(4) 2_655 . . V2 P1 O10 98.44(4) 2_655 . . V2 P1 O11 76.62(2) 2_655 . 2_655 O2 P1 O3 108.98(5) . . . O2 P1 O5 57.59(3) . . 2_655 O2 P1 O8 107.33(5) . . . O2 P1 O10 112.23(5) . . . O2 P1 O11 57.32(4) . . 2_655 O3 P1 O5 79.92(3) . . 2_655 O3 P1 O8 113.62(5) . . . O3 P1 O10 107.30(5) . . . O3 P1 O11 165.16(4) . . 2_655 O5 P1 O8 163.47(4) 2_655 . . O5 P1 O10 75.56(4) 2_655 . . O5 P1 O11 87.07(2) 2_655 . 2_655 O8 P1 O10 107.47(5) . . . O8 P1 O11 78.17(4) . . 2_655 O10 P1 O11 75.92(4) . . 2_655 Zn1 P2 V1 77.062(10) . . . Zn1 P2 V2 78.282(10) . . . Zn1 P2 O1 88.99(3) . . . Zn1 P2 O4 116.97(4) . . . Zn1 P2 O5 61.54(2) . . . Zn1 P2 O7 117.93(4) . . . Zn1 P2 O9 22.05(3) . . . Zn1 P2 O11 58.26(2) . . . V1 P2 V2 56.100(10) . . . V1 P2 O1 31.09(3) . . . V1 P2 O4 138.50(4) . . . V1 P2 O5 76.72(2) . . . V1 P2 O7 88.98(3) . . . V1 P2 O9 96.47(3) . . . V1 P2 O11 28.34(2) . . . V2 P2 O1 30.28(3) . . . V2 P2 O4 87.16(3) . . . V2 P2 O5 28.13(2) . . . V2 P2 O7 138.71(4) . . . V2 P2 O9 97.74(3) . . . V2 P2 O11 75.98(2) . . . O1 P2 O4 107.53(5) . . . O1 P2 O5 57.30(3) . . . O1 P2 O7 108.77(5) . . . O1 P2 O9 111.04(5) . . . O1 P2 O11 57.88(3) . . . O4 P2 O5 77.48(3) . . . O4 P2 O7 113.00(4) . . . O4 P2 O9 108.07(5) . . . O4 P2 O11 163.05(4) . . . O5 P2 O7 165.51(4) . . . O5 P2 O9 75.99(4) . . . O5 P2 O11 86.61(2) . . . O7 P2 O9 108.45(5) . . . O7 P2 O11 81.72(4) . . . O9 P2 O11 73.06(4) . . . Zn1 P3 O6 126.11(3) . . . Zn1 P3 O12 115.53(4) . . . Zn1 P3 O13 27.62(4) . . . Zn1 P3 O14 83.27(4) . . . O6 P3 O12 110.65(5) . . . O6 P3 O13 113.73(6) . . . O6 P3 O14 110.47(6) . . . O12 P3 O13 105.86(6) . . . O12 P3 O14 104.79(5) . . . O13 P3 O14 110.88(6) . . .