# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Jose Garcia' 'Belen F. Alfonso' 'Jesus A. Blanco' 'M. T. Fernandez-Diaz' 'Sergei A. Khainakov' 'Camino Trobajo' _publ_contact_author_name 'Jose Garcia' _publ_contact_author_email JRGM@UNIOVI.ES _publ_section_title ; On the crystal structure and thermal decomposition of ammonium-iron(III) bis(hydrogenphosphate) ; # Attachment 'ND4Fe_DPO4_2.cif' data_FEND450K _database_code_depnum_ccdc_archive 'CCDC 737439' _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2009-06-14T22:53 _refine_ls_shift/su_max 0.04 _refine_ls_shift/su_mean 0.00 _computing_structure_refinement GSAS _refine_ls_number_parameters 269 _refine_ls_goodness_of_fit_all 0.89 _refine_ls_number_restraints 0 _refine_ls_matrix_type full _chemical_name_systematic 'ammonium-iron(III) bis(hydrogenphosphate)' _chemical_name_common 'ammonium-iron(iii) bis(hydrogenphosphate)' _chemical_melting_point ? _chemical_formula_moiety 'D2 Fe1 O8 P2, (D4 N)' _chemical_formula_sum 'D6 Fe1 N1 O8 P2' _chemical_formula_weight 271.87 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_length_neutron _atom_type_scat_source Fe 6.0 0.9450 International_Tables_Vol_C P 12.0 0.5130 International_Tables_Vol_C O 48.0 0.5805 International_Tables_Vol_C N 6.0 0.9360 International_Tables_Vol_C D 36.0 0.6674 International_Tables_Vol_C _pd_proc_ls_prof_R_factor 0.0410 _pd_proc_ls_prof_wR_factor 0.0547 _pd_proc_ls_prof_wR_expected 0.0645 _refine_ls_R_Fsqd_factor 0.06213 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'I -1' _symmetry_space_group_name_Hall '-I 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z -1 -x,-y,-z 101 +x+1/2,+y+1/2,+z+1/2 -101 -x+1/2,-y+1/2,-z+1/2 _cell_length_a 9.79196(17) _cell_length_b 7.11846(11) _cell_length_c 14.17371(25) _cell_angle_alpha 93.4228(13) _cell_angle_beta 85.5686(14) _cell_angle_gamma 89.3939(14) _cell_volume 983.135(28) _cell_formula_units_Z 6 _cell_measurement_temperature 50(2) _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 148.0 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 68.4 _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type none _exptl_absorpt_factor_muR ? _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 50(2) _diffrn_radiation_probe neutron _diffrn_radiation_polarisn_ratio ? _diffrn_radiation_wavelength 1.593613 _diffrn_radiation_type neutron _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 10.969 _diffrn_reflns_theta_max 147.97 _reflns_d_resolution_high 0.829 _reflns_d_resolution_low 8.337 _reflns_number_total 1810 loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Fe Fe1 0.0 0.0 0.5 1.0 Uani 0.01635 2 Fe Fe2 0.6162(7) 0.0375(10) 0.3342(5) 1.0 Uani 0.01231 4 P P1 0.0633(13) 0.1304(16) 0.7188(8) 1.0 Uani 0.01412 4 P P2 0.6659(15) 0.1572(18) 0.1105(10) 1.0 Uani 0.02214 4 P P3 0.3234(12) 0.0298(16) 0.4443(8) 1.0 Uani 0.00943 4 O O1 0.4222(12) 0.1276(16) 0.3761(9) 1.0 Uani 0.02472 4 O O2 0.4713(11) 0.2020(13) 0.7150(8) 1.0 Uani 0.01382 4 O O3 0.8135(11) 0.2172(15) 0.1239(8) 1.0 Uani 0.01735 4 O O4 0.3634(11) 0.0720(16) 0.5453(8) 1.0 Uani 0.01777 4 O O5 0.5815(10) 0.1396(14) 0.2063(8) 1.0 Uani 0.01119 4 O O6 0.0312(10) 0.1705(14) 0.6156(7) 1.0 Uani 0.00915 4 O O7 0.1736(10) 0.0954(14) 0.4367(6) 1.0 Uani 0.00866 4 O O8 0.2062(10) 0.0568(15) 0.7206(8) 1.0 Uani 0.01506 4 O O9 0.9099(12) 0.2131(14) 0.4503(8) 1.0 Uani 0.01828 4 O O10 0.0412(10) 0.0266(16) 0.2429(8) 1.0 Uani 0.01449 4 O O11 0.3164(12) 0.0448(17) 0.9442(8) 1.0 Uani 0.01826 4 O O12 0.6670(13) 0.1877(17) 0.5822(8) 1.0 Uani 0.01907 4 N N1 0.0 0.0 0.0 1.0 Uani 0.05233 2 N N2 0.3158(9) 0.0289(12) 0.1513(6) 1.0 Uani 0.02015 4 D D1 0.0016(12) 0.1570(16) 0.2583(8) 1.0 Uani 0.02764 4 D D2 0.5965(11) 0.2059(16) 0.6352(8) 1.0 Uani 0.02665 4 D D3 0.2213(12) 0.0324(17) 0.1935(9) 1.0 Uani 0.03562 4 D D4 0.3949(14) 0.0416(17) 0.1945(9) 1.0 Uani 0.03932 4 D D5 0.6733(13) 0.0900(19) 0.8936(9) 1.0 Uani 0.0422 4 D D6 0.3708(11) 0.1427(17) 0.9216(8) 1.0 Uani 0.02542 4 D D7 0.3192(11) 0.1448(16) 0.1122(8) 1.0 Uani 0.02814 4 D D8 0.944(6) 0.065(4) 0.0540(33) 0.5 Uani 0.20491 4 D D9 -0.0325(27) -0.033(6) 0.9501(24) 0.5 Uani 0.05402 4 D D10 0.0806(27) 0.1092(32) -0.0403(22) 0.5 Uani 0.0471 4 D D11 0.9405(24) 0.103(4) 0.9830(24) 0.5 Uani 0.03265 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Fe1 0.021(6) -0.014(5) -0.004(4) 0.009(5) -0.001(4) 0.019(5) Fe2 0.0115(34) -0.0003(32) 0.0015(26) 0.022(4) 0.0013(28) 0.0032(34) P1 0.027(7) 0.014(6) 0.010(5) 0.007(6) 0.014(5) 0.008(7) P2 0.031(8) -0.006(6) -0.003(6) 0.017(7) 0.005(6) 0.018(7) P3 0.021(6) -0.020(5) -0.001(5) 0.004(6) 0.012(4) 0.005(6) O1 0.031(7) -0.006(6) -0.002(6) 0.022(7) 0.014(6) 0.023(7) O2 0.019(7) -0.008(5) -0.014(5) 0.001(5) 0.001(4) 0.025(6) O3 0.021(7) -0.006(5) 0.007(5) 0.007(6) 0.000(5) 0.022(7) O4 0.023(7) 0.001(5) -0.008(5) 0.012(6) 0.007(5) 0.020(7) O5 0.001(5) 0.020(4) -0.002(4) 0.007(5) 0.000(4) 0.025(7) O6 0.009(6) 0.004(4) -0.006(4) 0.011(5) 0.013(4) 0.010(5) O7 0.009(5) 0.006(4) -0.001(4) 0.003(5) -0.006(4) 0.014(5) O8 0.007(6) 0.003(5) -0.007(5) 0.014(6) 0.011(5) 0.026(7) O9 0.014(6) -0.004(5) -0.002(5) 0.019(7) -0.011(5) 0.021(7) O10 0.008(6) -0.007(5) 0.009(5) 0.027(7) -0.006(5) 0.006(5) O11 0.010(7) -0.004(6) -0.007(5) 0.035(9) -0.005(5) 0.011(6) O12 0.022(7) -0.007(5) -0.009(6) 0.025(7) 0.006(5) 0.012(7) N1 0.107(18) -0.024(11) -0.069(13) 0.036(9) 0.015(9) 0.026(10) N2 0.030(6) -0.006(4) -0.006(4) 0.015(4) 0.007(4) 0.017(5) D1 0.039(7) 0.001(6) 0.003(5) 0.021(6) -0.008(5) 0.021(6) D2 0.024(7) -0.010(5) -0.004(5) 0.025(6) 0.007(5) 0.032(7) D3 0.022(7) 0.001(6) 0.001(6) 0.037(8) -0.005(6) 0.046(8) D4 0.050(9) 0.008(7) 0.002(7) 0.035(8) 0.001(7) 0.032(7) D5 0.052(9) 0.000(6) -0.002(7) 0.037(8) -0.009(7) 0.036(8) D6 0.027(7) 0.006(5) 0.011(5) 0.021(6) -0.010(5) 0.025(7) D7 0.018(6) 0.009(5) 0.003(5) 0.033(7) 0.003(6) 0.032(7) D8 0.37(7) -0.088(26) 0.29(4) 0.045(18) -0.103(20) 0.140(28) D9 0.008(14) 0.042(16) 0.049(13) 0.123(35) 0.070(24) 0.030(20) D10 0.041(17) 0.015(13) -0.039(15) 0.014(13) 0.001(14) 0.091(24) D11 0.00602 0.0123 0.0143 0.03572 -0.0015 0.05285 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 Fe1 O6 2.024(10) . 1_555 N Fe1 O6 2.024(10) . -1_556 N Fe1 O7 2.005(10) . 1_555 N Fe1 O7 2.005(10) . -1_556 N Fe1 O9 1.942(11) . 1_455 N Fe1 O9 1.942(11) . -1_656 N Fe2 O1 2.031(13) . 1_555 N Fe2 O2 2.027(11) . -1_656 N Fe2 O3 1.960(12) . -101_544 N Fe2 O4 1.942(12) . -1_656 N Fe2 O5 2.043(13) . 1_555 N Fe2 O8 1.945(11) . -1_656 N P1 O2 1.493(14) . -101_445 N P1 O6 1.562(14) . 1_555 N P1 O8 1.491(14) . 1_555 N P1 O10 1.613(15) . -1_556 N P1 D1 2.184(16) . -1_556 N P2 O3 1.534(16) . 1_555 N P2 O5 1.547(16) . 1_555 N P2 O9 1.525(16) . -101_544 N P2 O11 1.593(16) . -1_656 N P2 D6 2.195(16) . -1_656 N P3 O1 1.519(14) . 1_555 N P3 O4 1.526(16) . 1_555 N P3 O7 1.548(14) . 1_555 N P3 O12 1.571(15) . -1_656 N P3 D2 2.076(16) . -1_656 N O1 Fe2 2.031(13) . 1_555 N O1 P3 1.519(14) . 1_555 N O2 Fe2 2.027(11) . -1_656 N O2 P1 1.493(14) . -101_445 N O2 D2 1.605(14) . 1_555 N O3 Fe2 1.960(12) . -101_544 N O3 P2 1.534(16) . 1_555 N O3 D8 1.854(34) . 1_555 N O4 Fe2 1.942(12) . -1_656 N O4 P3 1.526(16) . 1_555 N O5 Fe2 2.043(13) . 1_555 N O5 P2 1.547(16) . 1_555 N O5 D1 1.684(12) . -101_444 N O5 D4 1.978(17) . 1_555 N O6 Fe1 2.024(10) . 1_555 N O6 P1 1.562(14) . 1_555 N O6 D6 1.732(14) . -101_445 N O7 Fe1 2.005(10) . 1_555 N O7 P3 1.548(14) . 1_555 N O7 D7 2.014(15) . -101_444 N O8 Fe2 1.945(11) . -1_656 N O8 P1 1.491(14) . 1_555 N O9 Fe1 1.942(11) . 1_655 N O9 P2 1.525(16) . -101_544 N O10 P1 1.613(15) . -1_556 N O10 D1 1.007(14) . 1_555 N O10 D3 1.848(14) . 1_555 N O11 P2 1.593(16) . -1_656 N O11 D6 0.938(16) . 1_555 N O12 P3 1.571(15) . -1_656 N O12 D2 0.981(14) . 1_555 N N1 D8 0.993(18) . 1_455 N N1 D8 0.993(18) . -1_655 N N1 D9 0.82(4) . 1_554 N N1 D9 0.82(4) . -1_556 N N1 D10 1.245(28) . 1_555 N N1 D10 1.245(28) . -1_555 N N1 D11 0.984(25) . 1_454 N N1 D11 0.984(25) . -1_656 N N2 D3 1.063(13) . 1_555 N N2 D4 1.025(16) . 1_555 N N2 D5 1.027(14) . -1_656 N N2 D7 1.020(12) . 1_555 N D1 P1 2.184(16) . -1_556 N D1 O5 1.684(12) . -101_444 N D1 O10 1.007(14) . 1_555 N D2 P3 2.076(16) . -1_656 N D2 O2 1.605(14) . 1_555 N D2 O12 0.981(14) . 1_555 N D3 O10 1.848(14) . 1_555 N D3 N2 1.063(13) . 1_555 N D3 D4 1.703(16) . 1_555 N D3 D5 1.733(16) . -1_656 N D3 D7 1.686(16) . 1_555 N D4 O5 1.978(17) . 1_555 N D4 N2 1.025(16) . 1_555 N D4 D3 1.703(16) . 1_555 N D4 D5 1.697(17) . -1_656 N D4 D7 1.634(16) . 1_555 N D5 N2 1.027(14) . -1_656 N D5 D3 1.733(16) . -1_656 N D5 D4 1.697(17) . -1_656 N D5 D7 1.669(17) . -1_656 N D6 P2 2.195(16) . -1_656 N D6 O6 1.732(14) . -101_445 N D6 O11 0.938(16) . 1_555 N D7 O7 2.014(15) . -101_444 N D7 N2 1.020(12) . 1_555 N D7 D3 1.686(16) . 1_555 N D7 D4 1.634(16) . 1_555 N D7 D5 1.669(17) . -1_656 N D8 O3 1.854(34) . 1_555 N D8 N1 0.993(18) . 1_655 N D8 D9 1.59(4) . 1_654 N D8 D9 0.89(7) . -1_656 N D8 D10 1.86(4) . 1_655 N D8 D10 1.277(34) . -1_655 N D8 D11 1.06(6) . 1_554 N D8 D11 1.67(4) . -1_756 N D9 N1 0.82(4) . 1_556 N D9 D8 1.59(4) . 1_456 N D9 D8 0.89(7) . -1_656 N D9 D9 1.64(8) . -1_557 N D9 D10 1.52(4) . 1_556 N D9 D10 1.46(4) . -1_556 N D9 D11 1.07(4) . 1_455 N D9 D11 1.463(32) . -1_657 N D10 N1 1.245(28) . 1_555 N D10 D8 1.86(4) . 1_455 N D10 D8 1.277(34) . -1_655 N D10 D9 1.52(4) . 1_554 N D10 D9 1.46(4) . -1_556 N D10 D11 1.388(35) . 1_454 N D10 D11 1.764(32) . -1_656 N D11 N1 0.984(25) . 1_656 N D11 D8 1.06(6) . 1_556 N D11 D8 1.67(4) . -1_756 N D11 D9 1.07(4) . 1_655 N D11 D9 1.463(32) . -1_657 N D11 D10 1.388(35) . 1_656 N D11 D10 1.764(32) . -1_656 N 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 O6 Fe1 O6 180.0 1_555 . -1_556 N O6 Fe1 O7 88.7(4) 1_555 . 1_555 N O6 Fe1 O7 91.3(4) 1_555 . -1_556 N O6 Fe1 O9 87.3(4) 1_555 . 1_455 N O6 Fe1 O9 92.7(4) 1_555 . -1_656 N O6 Fe1 O7 91.3(4) -1_556 . 1_555 N O6 Fe1 O7 88.7(4) -1_556 . -1_556 N O6 Fe1 O9 92.7(4) -1_556 . 1_455 N O6 Fe1 O9 87.3(4) -1_556 . -1_656 N O7 Fe1 O7 180.0 1_555 . -1_556 N O7 Fe1 O9 86.1(4) 1_555 . 1_455 N O7 Fe1 O9 93.9(4) 1_555 . -1_656 N O7 Fe1 O9 93.9(4) -1_556 . 1_455 N O7 Fe1 O9 86.1(4) -1_556 . -1_656 N O9 Fe1 O9 180.0 1_455 . -1_656 N O1 Fe2 O2 85.8(5) 1_555 . -1_656 N O1 Fe2 O3 90.1(6) 1_555 . -101_655 N O1 Fe2 O4 91.9(5) 1_555 . -1_656 N O1 Fe2 O5 85.7(5) 1_555 . 1_555 N O1 Fe2 O8 173.2(6) 1_555 . -1_656 N O2 Fe2 O3 174.3(6) -1_656 . -101_655 N O2 Fe2 O4 90.2(5) -1_656 . -1_656 N O2 Fe2 O5 85.9(5) -1_656 . 1_555 N O2 Fe2 O8 89.7(5) -1_656 . -1_656 N O3 Fe2 O4 93.9(6) -101_655 . -1_656 N O3 Fe2 O5 89.9(5) -101_655 . 1_555 N O3 Fe2 O8 94.0(6) -101_655 . -1_656 N O4 Fe2 O5 175.5(6) -1_656 . 1_555 N O4 Fe2 O8 93.3(5) -1_656 . -1_656 N O5 Fe2 O8 88.8(5) 1_555 . -1_656 N O2 P1 O6 110.8(8) -101_556 . 1_555 N O2 P1 O8 114.6(11) -101_556 . 1_555 N O2 P1 O10 103.2(9) -101_556 . -1_556 N O6 P1 O8 110.8(9) 1_555 . 1_555 N O6 P1 O10 108.4(10) 1_555 . -1_556 N O8 P1 O10 108.6(9) 1_555 . -1_556 N O3 P2 O5 112.0(10) 1_555 . 1_555 N O3 P2 O9 113.4(10) 1_555 . -101_655 N O3 P2 O11 103.8(10) 1_555 . -1_656 N O5 P2 O9 109.4(11) 1_555 . -101_655 N O5 P2 O11 109.5(10) 1_555 . -1_656 N O9 P2 O11 108.6(10) -101_655 . -1_656 N O1 P3 O4 109.0(9) 1_555 . 1_555 N O1 P3 O7 111.5(10) 1_555 . 1_555 N O1 P3 O12 108.2(10) 1_555 . -1_656 N O4 P3 O7 109.7(10) 1_555 . 1_555 N O4 P3 O12 110.4(9) 1_555 . -1_656 N O7 P3 O12 108.1(9) 1_555 . -1_656 N Fe2 O1 P3 125.1(9) 1_555 . 1_555 N Fe2 O2 P1 139.5(10) -1_656 . -101_556 N Fe2 O2 D2 97.7(7) -1_656 . 1_555 N P1 O2 D2 120.9(9) -101_556 . 1_555 N Fe2 O3 P2 129.8(9) -101_655 . 1_555 N Fe2 O4 P3 143.9(9) -1_656 . 1_555 N Fe2 O5 P2 135.9(8) 1_555 . 1_555 N Fe1 O6 P1 132.8(7) 1_555 . 1_555 N Fe1 O7 P3 129.3(7) 1_555 . 1_555 N Fe2 O8 P1 155.6(9) -1_656 . 1_555 N Fe1 O9 P2 164.9(8) 1_655 . -101_655 N P1 O10 D1 110.8(11) -1_556 . 1_555 N P2 O11 D6 117.9(14) -1_656 . 1_555 N P3 O12 D2 106.6(13) -1_656 . 1_555 N D8 N1 D8 180.0 1_455 . -1_655 N D8 N1 D9 122(4) 1_455 . 1_554 N D8 N1 D9 58(4) 1_455 . -1_556 N D8 N1 D10 111.5(20) 1_455 . 1_555 N D8 N1 D10 68.5(20) 1_455 . -1_555 N D8 N1 D11 65(4) 1_455 . 1_454 N D8 N1 D11 115(4) 1_455 . -1_656 N D8 N1 D9 58(4) -1_655 . 1_554 N D8 N1 D9 122(4) -1_655 . -1_556 N D8 N1 D10 68.5(20) -1_655 . 1_555 N D8 N1 D10 111.5(20) -1_655 . -1_555 N D8 N1 D11 115(4) -1_655 . 1_454 N D8 N1 D11 65(4) -1_655 . -1_656 N D9 N1 D9 180.0 1_554 . -1_556 N D9 N1 D10 92.1(21) 1_554 . 1_555 N D9 N1 D10 87.9(21) 1_554 . -1_555 N D9 N1 D11 72.0(25) 1_554 . 1_454 N D9 N1 D11 108.0(25) 1_554 . -1_656 N D9 N1 D10 87.9(21) -1_556 . 1_555 N D9 N1 D10 92.1(21) -1_556 . -1_555 N D9 N1 D11 108.0(25) -1_556 . 1_454 N D9 N1 D11 72.0(25) -1_556 . -1_656 N D10 N1 D10 180.0 1_555 . -1_555 N D10 N1 D11 76.0(16) 1_555 . 1_454 N D10 N1 D11 104.0(16) 1_555 . -1_656 N D10 N1 D11 104.0(16) -1_555 . 1_454 N D10 N1 D11 76.0(16) -1_555 . -1_656 N D11 N1 D11 179.9802 1_454 . -1_656 N D3 N2 D4 109.3(13) 1_555 . 1_555 N D3 N2 D5 112.1(13) 1_555 . -1_656 N D3 N2 D7 108.1(12) 1_555 . 1_555 N D4 N2 D5 111.7(13) 1_555 . -1_656 N D4 N2 D7 106.1(13) 1_555 . 1_555 N D5 N2 D7 109.3(13) -1_656 . 1_555 N O2 D2 O12 170.1(15) 1_555 . 1_555 N N1 D8 D9 51.3(24) 1_655 . -1_656 N N1 D8 D10 65.1(18) 1_655 . -1_655 N N1 D8 D11 57.2(19) 1_655 . 1_554 N D9 D8 D10 87(4) -1_656 . -1_655 N D9 D8 D11 97.0(23) -1_656 . 1_554 N D10 D8 D11 98(4) -1_655 . 1_554 N N1 D9 D8 71(5) 1_556 . -1_656 N N1 D9 D10 55.1(24) 1_556 . 1_556 N N1 D9 D10 58.1(17) 1_556 . -1_556 N N1 D9 D11 61.1(35) 1_556 . 1_455 N N1 D9 D11 39.8(14) 1_556 . -1_657 N D8 D9 D10 57.2(31) -1_656 . 1_556 N D8 D9 D10 101(4) -1_656 . -1_556 N D8 D9 D11 117(6) -1_656 . 1_455 N D8 D9 D11 46(4) -1_656 . -1_657 N D10 D9 D10 113.3(31) 1_556 . -1_556 N D10 D9 D11 62.1(28) 1_556 . 1_455 N D10 D9 D11 72.6(20) 1_556 . -1_657 N D10 D9 D11 86.7(27) -1_556 . 1_455 N D10 D9 D11 56.6(16) -1_556 . -1_657 N D11 D9 D11 101(4) 1_455 . -1_657 N N1 D10 D8 46.4(14) 1_555 . -1_655 N N1 D10 D9 32.7(14) 1_555 . 1_554 N N1 D10 D9 34.0(19) 1_555 . -1_556 N N1 D10 D11 43.5(15) 1_555 . 1_454 N D8 D10 D9 35.8(29) -1_655 . 1_554 N D8 D10 D9 70.6(24) -1_655 . -1_556 N D8 D10 D11 77.5(30) -1_655 . 1_454 N D9 D10 D9 66.7(31) 1_554 . -1_556 N D9 D10 D11 42.9(17) 1_554 . 1_454 N D9 D10 D11 61.6(20) -1_556 . 1_454 N N1 D11 D8 58.0(30) 1_656 . 1_556 N N1 D11 D9 46.8(21) 1_656 . 1_655 N N1 D11 D9 32.2(20) 1_656 . -1_657 N N1 D11 D10 60.5(15) 1_656 . 1_656 N D8 D11 D9 96.7(35) 1_556 . 1_655 N D8 D11 D9 37.0(32) 1_556 . -1_657 N D8 D11 D10 98(4) 1_556 . 1_656 N D9 D11 D9 79(4) 1_655 . -1_657 N D9 D11 D10 74.9(23) 1_655 . 1_656 N D9 D11 D10 61.8(18) -1_657 . 1_656 N #END # Attachment 'NH4FeP2O7.cif' data_NH4FeP2O7 _database_code_depnum_ccdc_archive 'CCDC 737440' _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2008-07-13T18:15 _refine_ls_shift/su_max 0.06 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 58 _refine_ls_goodness_of_fit_all 1.82 _refine_ls_number_restraints 14 _refine_ls_matrix_type full _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Fe O7 P2, N' _chemical_formula_sum 'Fe N O7 P2' _chemical_formula_weight 243.79 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source N 4.0 0.000 0.000 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630 0.58260 -11.529 International_Tables_Vol_C P 8.0 0.000 0.000 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080 68.1645 1.11490 International_Tables_Vol_C O 28.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C Fe 4.0 0.000 0.000 11.7695 4.76110 7.35730 0.30720 3.52220 15.3535 2.30450 76.8805 1.03690 International_Tables_Vol_C _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y+1/2,-z+1/2 -1 -x,-y,-z -2 +x,-y+1/2,+z+1/2 _cell_length_a 7.5205(4) _cell_length_b 10.0028(4) _cell_length_c 8.2713(4) _cell_angle_alpha 90.0 _cell_angle_beta 105.926(4) _cell_angle_gamma 90.0 _cell_volume 598.33(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 90.0 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476.0 _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type none _exptl_absorpt_factor_muR ? _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio ? _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _reflns_d_resolution_high 1.529 _reflns_d_resolution_low 7.232 _reflns_number_total 349 #_pd_proc_ls_prof_R_factor 0.1412 #_pd_proc_ls_prof_wR_factor 0.1841 #pd_proc_ls_prof_wR_expected 0.0929 #refine_ls_R_Fsqd_factor 0.17691 loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity N N1 0.2048(27) 0.3055(14) 0.0212(24) 1.0 Uiso 0.005 4 P P1 0.4502(13) 0.6291(9) 0.1789(12) 1.0 Uiso 0.005 4 O O1 0.3446(18) 0.5456(13) 0.2870(22) 1.0 Uiso 0.005 4 O O3 0.6415(18) 0.5787(13) 0.2420(25) 1.0 Uiso 0.005 4 O O5 0.3286(22) 0.6102(17) -0.0024(16) 1.0 Uiso 0.005 4 O O6 0.0020(20) 0.5068(15) 0.2224(23) 1.0 Uiso 0.005 4 O O7 0.4606(20) 0.7746(14) 0.2027(21) 1.0 Uiso 0.005 4 Fe Fe1 -0.2415(7) 0.1010(5) -0.2631(7) 1.0 Uiso 0.005 4 O O4 -0.1659(27) 0.0663(12) -0.0157(15) 1.0 Uiso 0.005 4 P P2 0.1265(12) 0.6013(9) 0.3436(11) 1.0 Uiso 0.005 4 O O2 -0.0949(19) 0.2531(14) -0.3822(17) 1.0 Uiso 0.005 4 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 P1 O1 1.586(13) . 1_555 N P1 O3 1.478(11) . 1_555 N P1 O5 1.539(11) . 1_555 N P1 O7 1.468(12) . 1_555 N O1 P1 1.586(13) . 1_555 N O1 P2 1.909(12) . 1_555 N O3 P1 1.478(11) . 1_555 N O3 Fe1 2.007(12) . -2_655 N O5 P1 1.539(11) . 1_555 N O5 Fe1 1.871(12) . 2_554 N O6 Fe1 2.157(13) . -2_555 N O6 P2 1.503(13) . 1_555 N O7 P1 1.468(12) . 1_555 N O7 Fe1 2.228(13) . -1_565 N Fe1 O3 2.007(12) . -2_454 N Fe1 O5 1.871(12) . 2_544 N Fe1 O6 2.157(13) . -2_554 N Fe1 O7 2.228(13) . -1_565 N Fe1 O4 1.998(12) . 1_555 N Fe1 O2 2.258(12) . 1_555 N O4 Fe1 1.998(12) . 1_555 N O4 P2 1.416(11) . 2_545 N O4 O2 2.109(18) . -2_555 N P2 O1 1.909(12) . 1_555 N P2 O6 1.503(13) . 1_555 N P2 O4 1.416(11) . 2_555 N P2 O2 1.524(12) . -1_565 N O2 Fe1 2.258(12) . 1_555 N O2 O4 2.109(18) . -2_554 N O2 P2 1.524(12) . -1_565 N 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 O1 P1 O3 102.2(11) 1_555 . 1_555 N O1 P1 O5 103.2(11) 1_555 . 1_555 N O1 P1 O7 117.6(11) 1_555 . 1_555 N O3 P1 O5 124.2(14) 1_555 . 1_555 N O3 P1 O7 106.3(10) 1_555 . 1_555 N O5 P1 O7 104.4(12) 1_555 . 1_555 N P1 O1 P2 125.6(9) 1_555 . 1_555 N P1 O3 Fe1 133.5(10) 1_555 . -2_666 N P1 O5 Fe1 164.1(14) 1_555 . 2_554 N Fe1 O6 P2 131.3(11) -2_566 . 1_555 N O3 Fe1 O5 92.0(8) -2_465 . 2_544 N O3 Fe1 O6 86.4(6) -2_465 . -2_565 N O3 Fe1 O4 80.0(7) -2_465 . 1_555 N O5 Fe1 O6 91.6(7) 2_544 . -2_565 N O5 Fe1 O4 172.0(8) 2_544 . 1_555 N O6 Fe1 O4 87.9(8) -2_565 . 1_555 N Fe1 O4 P2 155.3(10) 1_555 . 2_545 N O1 P2 O6 94.2(9) 1_555 . 1_555 N O1 P2 O4 102.6(12) 1_555 . 2_555 N O1 P2 O2 121.6(8) 1_555 . -1_565 N O6 P2 O4 115.8(11) 1_555 . 2_555 N O6 P2 O2 129.5(10) 1_555 . -1_565 N O4 P2 O2 91.6(9) 2_555 . -1_565 N #END # Attachment 'ND4Fe_DPO4_2.cif' data_FEND450K _database_code_depnum_ccdc_archive 'CCDC 751864' _chemical_name_systematic 'ammonium-iron(III) bis(hydrogenphosphate)' _refine_ls_shift/su_max 0.05 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement FULLPROF _refine_ls_number_parameters 121 _refine_ls_goodness_of_fit_all 0.93 _refine_ls_number_restraints 0 _refine_ls_matrix_type full _chemical_formula_moiety 'D6 Fe3 O24 P6, D4 N, D8 N2' _chemical_formula_sum 'D18 Fe3 N3 O24 P6' _chemical_formula_weight 815.58 #_pd_proc_ls_prof_R_factor 0.03305 #_pd_proc_ls_prof_wR_factor 0.04284 #_pd_proc_ls_prof_wR_expected 0.02878 #_refine_ls_R_Fsqd_factor ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 7.11830(3) _cell_length_b 8.83828(4) _cell_length_c 9.46407(4) _cell_angle_alpha 64.5802(4) _cell_angle_beta 70.3127(4) _cell_angle_gamma 69.5733(4) _cell_volume 491.495(4) _cell_formula_units_Z 1 _cell_measurement_temperature 50(2) _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 160.0 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 0.0 _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type none _exptl_absorpt_factor_muR ? _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 50(2) _diffrn_radiation_probe neutron _diffrn_radiation_polarisn_ratio ? _diffrn_radiation_wavelength 1.593613 _diffrn_radiation_type neutron _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _reflns_number_total 1971 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 Fe1 -0.50000 0.50000 0.50000 0.0082(10) 1.00000 Uiso FE Fe2 -0.2975(5) -0.2831(4) 0.9499(3) 0.0042(7) 1.00000 Uiso FE P1 -0.5897(9) 0.6552(7) 0.7802(7) 0.0039(12) 1.00000 Uiso P P2 0.0469(9) -0.5564(7) 0.7780(7) 0.0036(11) 1.00000 Uiso P P3 -0.4152(9) 0.1224(7) 0.7677(7) 0.0049(12) 1.00000 Uiso P O1 -0.2457(7) -0.0446(6) 0.7957(6) 0.0068(12) 1.00000 Uiso O O2 -0.5127(8) 0.2425(7) 0.1872(6) 0.0063(11) 1.00000 Uiso O O3 0.0951(8) -0.6897(6) 0.9377(6) 0.0071(10) 1.00000 Uiso O O4 -0.4757(8) 0.1824(6) 0.9100(6) 0.0080(11) 1.00000 Uiso O O5 -0.0657(8) -0.3759(7) 0.7874(6) 0.0068(10) 1.00000 Uiso O O6 -0.4459(8) 0.5887(7) 0.6444(6) 0.0081(11) 1.00000 Uiso O O7 -0.3424(8) 0.2616(6) 0.6131(6) 0.0073(11) 1.00000 Uiso O O8 -0.6665(8) 0.5164(7) 0.9281(6) 0.0065(10) 1.00000 Uiso O O9 -0.2383(8) -0.4568(7) 0.3582(6) 0.0066(11) 1.00000 Uiso O O10 -0.2166(8) 0.2026(6) 0.2857(6) 0.0064(11) 1.00000 Uiso O O11 -0.9023(8) 0.6265(7) 0.2601(6) 0.0081(11) 1.00000 Uiso O O12 -0.3959(8) -0.0874(7) 0.2507(6) 0.0093(11) 1.00000 Uiso O N1 0.00000 0.00000 0.00000 0.0144(10) 1.00000 Uiso N N2 -0.1189(5) -0.1654(5) 0.4672(4) 0.0115(8) 1.00000 Uiso N D1 -0.1032(9) 0.2582(8) 0.2574(7) 0.0233(14) 1.00000 Uiso D D2 -0.4270(9) 0.0388(7) 0.2304(7) 0.0217(14) 1.00000 Uiso D D3 -0.1603(9) -0.0311(7) 0.4154(7) 0.0241(12) 1.00000 Uiso D D4 -0.1549(9) -0.2043(7) 0.5931(7) 0.0247(13) 1.00000 Uiso D D5 -0.7991(9) 0.2170(7) 0.5657(7) 0.0269(13) 1.00000 Uiso D D6 -0.7740(9) 0.5489(7) 0.2935(7) 0.0227(13) 1.00000 Uiso D D7 0.0390(9) -0.2102(7) 0.4293(7) 0.0244(13) 1.00000 Uiso D D8 0.0265(18) -0.8877(14) 0.9718(14) 0.025(3) 0.50000 Uiso D D9 -0.9916(18) 0.9662(15) 0.9004(13) 0.028(3) 0.50000 Uiso D D10 0.1421(17) -0.1142(14) 0.0436(14) 0.029(3) 0.50000 Uiso D D11 -0.8788(17) 0.0370(15) 0.9189(14) 0.027(3) 0.50000 Uiso D #END # Attachment 'NH4FeP2O7.cif' data_NH4FeP2O7 _database_code_depnum_ccdc_archive 'CCDC 751865' _chemical_name_systematic 'ammonium-iron(III) diphosphate' _refine_ls_shift/su_max 0.19 _refine_ls_shift/su_mean 0.03 _computing_structure_refinement FULLPROF _refine_ls_number_parameters 44 _refine_ls_goodness_of_fit_all 2.78 _refine_ls_number_restraints ? _refine_ls_matrix_type full _chemical_formula_moiety 'Fe O7 P2, N' _chemical_formula_sum 'Fe N O7 P2' _chemical_formula_weight 243.80 #_pd_proc_ls_prof_R_factor 0.0545 #_pd_proc_ls_prof_wR_factor 0.0407 #_pd_proc_ls_prof_wR_expected 0.0281 #_refine_ls_R_Fsqd_factor ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y+1/2,-z+1/2 -1 -x,-y,-z -2 +x,-y+1/2,+z+1/2 _cell_length_a 7.5219(2) _cell_length_b 10.0018(3) _cell_length_c 8.2729(2) _cell_angle_alpha 90.0 _cell_angle_beta 105.887(3) _cell_angle_gamma 90.0 _cell_volume 598.62(3) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 140.0 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476.0 _exptl_absorpt_coefficient_mu 25.432 _exptl_absorpt_correction_type none _exptl_absorpt_factor_muR ? _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_probe X-ray _diffrn_radiation_polarisn_ratio ? _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _reflns_number_total 2422 loop_ _atom_type_symbol _atom_type_number_in_cell Fe 4.0 P 8.0 O 28.0 N 4.0 loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Fe Fe1 0.2442(9) 0.5958(6) 0.7585(8) 1.0 Uiso 0.0087(12) 4 P P1 0.4541(14) 0.6323(10) 0.1871(11) 1.0 Uiso 0.014(3) 4 P P2 0.1335(14) 0.6113(10) 0.3384(10) 1.0 Uiso 0.014(3) 4 O O1 0.3121(22) 0.5651(15) 0.2787(28) 1.0 Uiso 0.019(3) 4 O O2 0.3623(16) 0.4253(12) 0.7268(24) 1.0 Uiso 0.019(3) 4 O O3 0.1230(21) 0.7403(11) 0.8597(20) 1.0 Uiso 0.019(3) 4 O O4 0.1712(30) 0.5619(14) 0.5136(11) 1.0 Uiso 0.019(3) 4 O O5 0.0144(21) 0.4932(19) 0.7498(24) 1.0 Uiso 0.019(3) 4 O O6 0.4473(16) 0.7166(12) 0.7252(20) 1.0 Uiso 0.019(3) 4 O O7 0.3345(25) 0.6192(18) 1.0040(11) 1.0 Uiso 0.019(3) 4 N N1 0.2000(19) 0.1960(21) 0.5210(24) 1.0 Uiso 0.038(5) 4 #END