#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$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, Przemysław'
'Chański, Michał'
'Ślepokura, 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_paper_doi               10.1021/cm102265e
_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/[σ²(Fo²)+(0.0475P)²+0.0000P] where P=(Fo²+2Fc²)/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)
_cod_data_source_file            cm102265e_si_001.cif
_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
