#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/50/7215002.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_7215002
loop_
_publ_author_name
'Matulková, Irena'
'Cihelka, Jaroslav'
'Pojarová, Michaela'
'Fejfarová, Karla'
'Dušek, Michal'
'Vaněk, Přemysl'
'Kroupa, Jan'
'Krupková, Radmila'
'Fábry, Jan'
'Němec, Ivan'
_publ_section_title
;
 A new series of 3,5-diamino-1,2,4-triazolium(1+) inorganic salts and
 their potential in crystal engineering of novel NLO materials
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              4625
_journal_paper_doi               10.1039/c2ce00024e
_journal_volume                  14
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C2 H6 N5, H2 O4 P '
_chemical_formula_sum            'C2 H8 N5 O4 P'
_chemical_formula_weight         197.1
_chemical_name_systematic        ' ?'
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   13.3492(4)
_cell_length_b                   37.1096(12)
_cell_length_c                   6.0702(2)
_cell_measurement_reflns_used    7644
_cell_measurement_temperature    120
_cell_measurement_theta_max      66.6468
_cell_measurement_theta_min      4.7671
_cell_volume                     3007.08(17)
_computing_cell_refinement       'Crysalis RED (Oxford diffraction, 2009)'
_computing_data_collection       'Crysalis CCD (Oxford diffraction, 2009)'
_computing_data_reduction        'Crysalis RED'
_computing_molecular_graphics    'Diamond (Brandenburg & Putz, 2005)'
_computing_publication_material  Jana2006
_computing_structure_refinement
'Jana2006 (Petříček, Dušek & Palatinus, 2006)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type
'Goniometer Xcalibur, detector: Atlas (Gemini ultra Cu)'
_diffrn_measurement_method
'Rotation method data acquisition using ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0055
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8122
_diffrn_reflns_reduction_process
;
Integration of the CCD images was done by program Crysalis RED
(Oxford diffraction, 2008). The same program was used for indexing of the
crystal shape and absorption correction.
;
_diffrn_reflns_theta_full        66.79
_diffrn_reflns_theta_max         66.79
_diffrn_reflns_theta_min         7.05
_exptl_absorpt_coefficient_mu    3.270
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.51 (release 27-10-2009 CrysAlis171 .NET)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.7408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.3851
_exptl_crystal_size_mid          0.2734
_exptl_crystal_size_min          0.1800
_refine_diff_density_max         0.09
_refine_diff_density_min         -0.11
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.034(16)
_refine_ls_extinction_coef       1900(200)
_refine_ls_extinction_method
'B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_gt    1.52
_refine_ls_goodness_of_fit_ref   1.52
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_constraints    9
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1295
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0189
_refine_ls_shift/su_max          0.0100
_refine_ls_shift/su_mean         0.0013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(σ²(I)+0.0016I²)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0617
_reflns_number_gt                1290
_reflns_number_total             1295
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            c2ce00024e.txt
_cod_data_source_block           III
_cod_original_formula_sum        'C2 H8 N5 O4 P1'
_cod_database_code               7215002
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,z
3 x+1/4,-y+1/4,z+1/4
4 -x+1/4,y+1/4,z+1/4
5 x,y+1/2,z+1/2
6 -x,-y+1/2,z+1/2
7 x+1/4,-y+3/4,z+3/4
8 -x+1/4,y+3/4,z+3/4
9 x+1/2,y,z+1/2
10 -x+1/2,-y,z+1/2
11 x+3/4,-y+1/4,z+3/4
12 -x+3/4,y+1/4,z+3/4
13 x+1/2,y+1/2,z
14 -x+1/2,-y+1/2,z
15 x+3/4,-y+3/4,z+1/4
16 -x+3/4,y+3/4,z+1/4
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
P1 P 0.10815(3) 0.229170(8) 0.33533 Uani 0.01068(13) 16 1 d
O1 O 0.10097(8) 0.23298(3) 0.0797(2) Uani 0.0170(4) 16 1 d
O2 O 0.12943(9) 0.26783(3) 0.4298(2) Uani 0.0167(3) 16 1 d
O3 O 0.01071(8) 0.21727(3) 0.43643(19) Uani 0.0149(3) 16 1 d
O4 O 0.19550(7) 0.20384(3) 0.37417(19) Uani 0.0130(3) 16 1 d
N4 N 0.21523(10) 0.14230(4) 1.1209(2) Uani 0.0137(4) 16 1 d
N2 N 0.22888(10) 0.12095(4) 0.7812(2) Uani 0.0158(4) 16 1 d
N1 N 0.22293(10) 0.09308(3) 0.9377(2) Uani 0.0147(4) 16 1 d
N7 N 0.23167(11) 0.18427(4) 0.8286(3) Uani 0.0200(4) 16 1 d
N6 N 0.20645(10) 0.08810(4) 1.3276(2) Uani 0.0185(4) 16 1 d
C3 C 0.22433(12) 0.15011(4) 0.8992(3) Uani 0.0149(4) 16 1 d
C5 C 0.21481(11) 0.10610(4) 1.1402(3) Uani 0.0132(4) 16 1 d
H4A H 0.2088(15) 0.1581(5) 1.224(3) Uiso 0.0164 16 1 d
H1A H 0.2356(15) 0.0709(3) 0.897(3) Uiso 0.0176 16 1 d
H7B H 0.2185(15) 0.1867(6) 0.6881(17) Uiso 0.024 16 1 d
H7A H 0.2035(15) 0.2015(4) 0.905(3) Uiso 0.024 16 1 d
H6B H 0.1976(14) 0.0649(3) 1.312(4) Uiso 0.0222 16 1 d
H6A H 0.2082(16) 0.1008(5) 1.450(2) Uiso 0.0222 16 1 d
H1 H 0.0651(13) 0.2496(4) 0.034(3) Uiso 0.0203 16 1 d
H2 H 0.1861(9) 0.2760(5) 0.411(3) Uiso 0.02 16 1 d
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.018 0.009 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.000 0.000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.031 0.018 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.049 0.032 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
P 0.296 0.433 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O1 P1 O2 106.92(7) yes
O1 P1 O3 112.27(6) yes
O1 P1 O4 104.95(6) yes
O2 P1 O3 105.99(6) yes
O2 P1 O4 111.74(6) yes
O3 P1 O4 114.81(6) yes
P1 O1 H1 115.8(13) yes
P1 O2 H2 116.9(13) yes
C3 N4 C5 107.12(14) yes
C3 N4 H4A 125.0(11) yes
C5 N4 H4A 127.9(11) yes
N1 N2 C3 103.74(13) yes
N2 N1 C5 111.28(12) yes
N2 N1 H1A 119.5(13) yes
C5 N1 H1A 128.2(13) yes
C3 N7 H7B 113.1(15) yes
C3 N7 H7A 119.3(12) yes
H7B N7 H7A 111.0(19) yes
C5 N6 H6B 114.5(16) yes
C5 N6 H6A 117.1(12) yes
H6B N6 H6A 128.4(19) yes
N4 C3 N2 111.48(14) yes
N4 C3 N7 121.07(15) yes
N2 C3 N7 127.38(16) yes
N4 C5 N1 106.38(14) yes
N4 C5 N6 125.31(15) yes
N1 C5 N6 128.30(14) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
P1 O1 1.5610(13) yes
P1 O2 1.5710(11) yes
P1 O3 1.5045(11) yes
P1 O4 1.5160(11) yes
O1 H1 0.827(17) yes
O2 H2 0.823(13) yes
N4 C3 1.382(2) yes
N4 C5 1.348(2) yes
N4 H4A 0.864(16) yes
N2 N1 1.4065(19) yes
N2 C3 1.299(2) yes
N1 C5 1.326(2) yes
N1 H1A 0.873(13) yes
N7 C3 1.342(2) yes
N7 H7B 0.875(11) yes
N7 H7A 0.877(18) yes
N6 C5 1.324(2) yes
N6 H6B 0.875(11) yes
N6 H6A 0.882(16) yes
