#------------------------------------------------------------------------------
#$Date: 2023-12-15 19:00:07 +0100 (Fri 15 de Dec de 2023) $
#$Revision: 288351 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/06/2100627.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2100627
loop_
_publ_author_name
'Oh, I.H.'
'Merz, M.'
'Mattauch, S.'
'Heger, G.'
_publ_section_title
;
Structural phase transition and hydrogen ordering of
TlH₂PO₄ at low temperature
;
_journal_coeditor_code           LC5039
_journal_issue                   4
_journal_name_full               'Acta Crystallographica, Section B'
_journal_page_first              719
_journal_page_last               728
_journal_paper_doi               10.1107/S0108768106018222
_journal_volume                  62
_journal_year                    2006
_chemical_formula_sum            'H8 O16 P4 Tl4'
_chemical_formula_weight         1206.4
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1 (1/2*x+1/2*y,1/2*x-1/2*y,-z)'
_space_group_name_H-M_alt        'C -1'
_atom_type_scat_source           International_Tables_Vol_C
_audit_creation_method           enCIFer
_cell_angle_alpha                90.09(5)
_cell_angle_beta                 92.21(3)
_cell_angle_gamma                90.49(3)
_cell_formula_units_Z            16
_cell_length_a                   28.483(12)
_cell_length_b                   9.016(5)
_cell_length_c                   6.502(3)
_cell_measurement_reflns_used    12
_cell_measurement_temperature    210
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      17.5
_cell_volume                     1668.4(14)
_computing_cell_refinement       pron
_computing_data_collection       pron
_computing_data_reduction        pron
_computing_molecular_graphics    'drawxtal(Finger and Kroeker, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      210
_diffrn_measured_fraction_theta_max 0.7025
_diffrn_measurement_device_type  'four circle diffractometer'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  'Cu (220)'
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.8724
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3170
_diffrn_reflns_theta_max         37.80
_diffrn_reflns_theta_min         3.51
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_time  540
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.04
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.820
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             474.3
_exptl_crystal_size_max          5
_exptl_crystal_size_mid          3
_exptl_crystal_size_min          3
_refine_diff_density_max         3.03
_refine_diff_density_min         -2.28
_refine_ls_extinction_coef       0.00300(15)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.933
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2982
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/σ²(Fo²)
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0544
_reflns_number_gt                1428
_reflns_number_total             2982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            lc5039.cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_ambient_temperature' value '210K ' was changed to '210' -
the value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        ' H8 O16 P4 Tl4'
_cod_database_code               2100627
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_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
Tl Tl1 0.0644(3) 0.4990(10) 0.2650(10) 0.027(2) Uiso 1
Tl Tl2 0.1883(2) 0.2490(10) 0.7270(10) 0.029(2) Uiso 1
Tl Tl3 0.0639(3) 0.9950(10) 0.2530(10) 0.027(2) Uiso 1
Tl Tl4 0.1838(2) 0.7440(10) 0.749(2) 0.029(2) Uiso 1
P P1 0.0620(4) 0.261(2) 0.762(2) 0.016(2) Uiso 1
P P2 0.1881(4) 0.013(2) 0.231(2) 0.020(3) Uiso 1
P P3 0.0625(3) 0.761(2) 0.756(2) 0.013(2) Uiso 1
P P4 0.1876(4) 0.512(2) 0.231(2) 0.015(2) Uiso 1
O O1 0.0410(3) 0.2160(10) 0.9730(10) 0.019(2) Uiso 1
O O2 0.2148(4) 0.438(2) 0.064(2) 0.025(2) Uiso 1
O O3 0.0348(3) 0.686(2) 0.934(2) 0.020(2) Uiso 1
O O4 0.2092(3) 0.961(2) 0.032(2) 0.018(2) Uiso 1
O O5 0.0290(4) 0.323(2) 0.594(2) 0.022(2) Uiso 1
O O6 0.2263(4) 0.085(2) 0.374(2) 0.021(2) Uiso 1
O O7 0.0266(4) 0.828(2) 0.603(2) 0.023(3) Uiso 1
O O8 0.2266(4) 0.589(2) 0.375(2) 0.017(2) Uiso 1
O O9 0.0999(3) 0.388(2) 0.812(2) 0.021(2) Uiso 1
O O10 0.1509(4) 0.138(2) 0.181(2) 0.014(2) Uiso 1
O O11 0.0936(4) 0.886(2) 0.845(2) 0.024(2) Uiso 1
O O12 0.1571(3) 0.6360(10) 0.1540(10) 0.014(2) Uiso 1
O O13 0.0890(4) 0.138(2) 0.658(2) 0.014(2) Uiso 1
O O14 0.1591(4) 0.389(2) 0.332(2) 0.022(3) Uiso 1
O O15 0.0878(4) 0.640(2) 0.657(2) 0.019(2) Uiso 1
O O16 0.1559(3) 0.888(2) 0.317(2) 0.025(2) Uiso 1
H H1 0.9920(6) 0.267(3) 0.018(3) 0.048(4) Uiso 1
H H2 0.2509(9) 1.001(4) -0.010(3) 0.010(3) Uiso 1
H H3 0.9992(6) 0.254(3) 0.516(3) 0.023(2) Uiso 1
H H4 0.2567(5) -0.018(2) 0.538(2) 0.037(4) Uiso 1
H H5 0.1585(6) 0.775(2) 0.258(2) 0.030(4) Uiso 1
H H6 0.4065(7) 0.507(3) 0.223(3) 0.038(5) Uiso 1
H H7 0.3413(8) 0.243(4) 0.755(3) 0.038(4) Uiso 1
H H8 0.4066(6) 0.012(3) 0.243(3) 0.029(4) Uiso 1
loop_
_atom_type_symbol
H
Tl
P
O
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
0 0 2
12 0 -1
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 P1 O9 . . 105.7(9)
O1 P1 O5 . . 118.3(9)
O1 P1 O13 . . 114.7(9)
O5 P1 O9 . . 106.5(9)
O5 P1 O13 . . 105.1(9)
O4 P2 O6 11 . 104.4(9)
O4 P2 O10 11 . 111.70(10)
O4 P2 O16 11 11 106.60(10)
O3 P3 O7 . . 107.8(9)
O3 P3 O11 . . 109.4(9)
O3 P3 O15 . . 106.0(9)
O7 P3 O11 . . 107.9(9)
O7 P3 O15 . . 109.9(9)
O11 P3 O15 . . 115.2(9)
O2 P4 O8 . . 104.5(9)
O2 P4 O12 . . 113.8(9)
O2 P4 O14 . . 106.3(9)
O8 P4 O12 . . 105.9(9)
O8 P4 O14 . . 115.2(9)
O12 P4 O14 . . 111.8(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
P1 O1 . . 1.57(2)
P1 O5 . . 1.53(2)
P1 O9 . . 1.59(2)
P1 O13 . . 1.52(2)
P2 O4 . 11 1.53(2)
P2 O6 . . 1.54(2)
P2 O10 . . 1.58(2)
P2 O16 . 11 1.57(2)
P3 O3 . . 1.58(2)
P3 O7 . . 1.53(2)
P3 O11 . . 1.53(2)
P3 O15 . . 1.47(2)
P4 O2 . . 1.52(2)
P4 O8 . . 1.58(2)
P4 O12 . . 1.50(2)
P4 O14 . . 1.53(2)
Tl1 O3 . 9 2.850(10)
Tl1 O5 . . 2.870(10)
Tl1 O14 . . 2.90(2)
Tl1 O15 . . 2.90(2)
Tl1 O12 . . 3.020(10)
Tl1 O1 . 9 3.23(2)
Tl2 O2 9 . 2.85(2)
Tl2 O9 . . 2.900(10)
Tl2 O6 . 7 2.94(2)
Tl2 O14 . . 2.96(2)
Tl2 O6 . . 2.97(2)
Tl2 O13 . . 3.010(10)
Tl3 O1 . 10 2.76(3)
Tl3 O16 . . 2.820(10)
Tl3 O10 . 17 2.840(10)
Tl3 O7 . . 2.96(2)
Tl3 O11 . 9 2.99(2)
Tl3 O13 . 17 2.99(2)
Tl3 O7 . 14 3.21(2)
Tl4 O4 9 . 2.75(2)
Tl4 O15 . . 2.930(10)
Tl4 O12 9 . 2.940(10)
Tl4 O11 . . 2.97(2)
Tl4 O8 . 8 3.090(10)
Tl4 O8 . . 3.100(10)
Tl4 O16 . . 3.170(10)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O3 H1 O1 5 15 0.94(2) 1.51(2) 2.44(3) 167.5(2)
O2 H2 O4 6 . 1.18(3) 1.28(3) 2.450(10) 167.4(9)
O5 H3 O7 5 5 1.12(2) 1.30(3) 2.410(10) 169.3(9)
O8 H4 O6 7 . 0.97(2) 1.64(2) 2.606(9) 173.1(9)
O16 H5 O12 . . 1.09(3) 1.42(3) 2.50(2) 170.9(9)
O11 H6 O13 8 7 1.06(3) 1.52(3) 2.58(2) 172.6(3)
O10 H7 O14 7 7 1.17(3) 1.32(2) 2.48(2) 168.8(6)
O9 H8 O15 8 8 0.99(3) 1.53(3) 2.51(2) 173.9(2)
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2023-12-15T18:00:00+02:00
;
 Changed the y coordinate of atom site 'O6' from '374(2)' to '0.374(2)' after
 consulting the original publication.
;
