#------------------------------------------------------------------------------ #$Date: 2013-12-29 11:49:26 +0000 (Sun, 29 Dec 2013) $ #$Revision: 91935 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/07/4000712.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000712 loop_ _publ_author_name 'Szklarz, Przemys\/law' 'Cha\'nski, Micha\/l' '\'Slepokura, Katarzyna' 'Lis, Tadeusz' _publ_section_title ; Discovery of Ferroelectric Properties in Diammonium Hypodiphosphate (NH4)2H2P2O6(ADhP) ; _journal_issue 5 _journal_name_full 'Chemistry of Materials' _journal_page_first 1082 _journal_volume 23 _journal_year 2011 _chemical_formula_sum 'H10 N2 O6 P2' _chemical_formula_weight 196.04 _chemical_name_systematic ; diammonium hypodiphosphate ; _space_group_IT_number 56 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ab 2ac' _symmetry_space_group_name_H-M 'P c c n' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.237(3) _cell_length_b 11.484(4) _cell_length_c 9.373(3) _cell_measurement_reflns_used 7496 _cell_measurement_temperature 210(2) _cell_measurement_theta_max 36.78 _cell_measurement_theta_min 3.33 _cell_volume 779.0(5) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 210(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.949 _diffrn_measurement_device_type 'Kuma KM-4 with CCD area detector' _diffrn_measurement_method omega _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 8393 _diffrn_reflns_theta_full 26.50 _diffrn_reflns_theta_max 36.78 _diffrn_reflns_theta_min 3.33 _exptl_absorpt_coefficient_mu 0.545 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_correction_T_min 0.903 _exptl_absorpt_correction_type analytical _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_description blocks _exptl_crystal_F_000 408 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.42 _refine_diff_density_min -0.27 _refine_diff_density_rms 0.074 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 66 _refine_ls_number_reflns 1848 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.172 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0352 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0836 _refine_ls_wR_factor_ref 0.0893 _reflns_number_gt 1468 _reflns_number_total 1848 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file cm102265e_si_001.cif _[local]_cod_data_source_block ; ; _cod_database_code 4000712 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' 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 P P 0.10097(4) 0.23824(2) 0.16782(3) 0.01677(9) Uani 1 1 d O1 O 0.02316(11) 0.30660(7) 0.29967(9) 0.02397(18) Uani 1 1 d H1 H 0.012(3) 0.2606(19) 0.380(2) 0.063(7) Uiso 1 1 d O2 O 0.06752(12) 0.10881(7) 0.17610(9) 0.02770(19) Uani 1 1 d O3 O 0.02772(11) 0.30048(7) 0.03706(9) 0.02505(18) Uani 1 1 d N1 N 0.26857(13) 0.51819(9) 0.41159(13) 0.0246(2) Uani 1 1 d H11 H 0.343(2) 0.5728(15) 0.4365(19) 0.035(4) Uiso 1 1 d H21 H 0.243(2) 0.4767(17) 0.495(2) 0.051(5) Uiso 1 1 d H31 H 0.310(3) 0.4785(17) 0.3481(17) 0.037(4) Uiso 1 1 d H41 H 0.160(2) 0.5433(15) 0.382(2) 0.041(4) Uiso 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 P 0.02054(13) 0.01359(12) 0.01618(14) -0.00002(8) -0.00183(9) 0.00107(8) O1 0.0314(4) 0.0239(4) 0.0167(4) 0.0012(3) 0.0047(3) 0.0043(3) O2 0.0262(4) 0.0151(3) 0.0418(5) 0.0014(3) -0.0087(3) -0.0026(3) O3 0.0333(4) 0.0258(4) 0.0161(4) -0.0005(3) -0.0028(3) 0.0106(3) N1 0.0237(4) 0.0182(4) 0.0319(6) -0.0004(4) -0.0053(4) -0.0001(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 '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' O O 0.0106 0.0060 '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' 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_3 O2 P O3 116.78(5) . O2 P O1 113.28(5) . O3 P O1 106.01(5) . O2 P P 106.36(4) 2 O3 P P 106.78(4) 2 O1 P P 107.10(4) 2 P O1 H1 112.6(14) . H11 N1 H21 105.7(15) . H11 N1 H31 112.5(17) . H21 N1 H31 113.8(17) . H11 N1 H41 114.0(15) . H21 N1 H41 104.5(14) . H31 N1 H41 106.3(17) . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 P O2 1.5079(10) . P O3 1.5146(9) . P O1 1.5686(9) . P P 2.1740(10) 2 O1 H1 0.92(2) . N1 H11 0.86(2) . N1 H21 0.93(2) . N1 H31 0.81(2) . N1 H41 0.88(2) . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O3 0.92(2) 1.64(2) 2.542(2) 167(2) 7_566 N1 H11 O3 0.86(2) 1.99(2) 2.844(2) 171(2) 4_565 N1 H21 O2 0.93(2) 2.34(2) 3.223(2) 159(2) 7_566 N1 H31 O2 0.81(2) 2.10(2) 2.899(2) 174(2) 2 N1 H41 O2 0.88(2) 1.89(2) 2.770(2) 176(2) 3 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O1 P P O1 68.97(7) 2 2 O1 P P O2 -52.44(5) 2 2 O1 P P O3 -177.83(4) 2 2 O2 P P O1 -52.44(5) 2 2 O2 P P O2 -173.86(7) 2 2 O2 P P O3 60.76(5) 2 2 O3 P P O1 -177.83(4) 2 2 O3 P P O2 60.76(5) 2 2 O3 P P O3 -64.62(7) 2 2 _journal_paper_doi 10.1021/cm102265e