#------------------------------------------------------------------------------
#$Date: 2019-08-01 06:03:29 +0200 (jue 01 de ago de 2019) $
#$Revision: 217346 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/84/2108457.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_2108457
loop_
_publ_author_name
'Lanza, Arianna E.'
'Gemmi, Mauro'
'Bindi, Luca'
'Mugnaioli, Enrico'
'Paar, Werner H.'
_publ_section_title
;
 Daliranite, PbHgAs₂S₅: determination of the incommensurately
 modulated structure and revision of the chemical formula
;
_journal_coeditor_code           DK5082SUP1
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520619007340
_journal_volume                  75
_journal_year                    2019
_chemical_formula_moiety         'As2 Hg Pb S5'
_chemical_formula_sum            'As2 Hg Pb S5'
_chemical_formula_weight         717.9
_chemical_name_common            daliranite
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.246(5)
_cell_length_b                   4.2897(9)
_cell_length_c                   9.5257(12)
_cell_measurement_reflns_used    2033
_cell_measurement_temperature    298
_cell_measurement_theta_max      1.2
_cell_measurement_theta_min      0.05
_cell_volume                     868.2(3)
_computing_data_reduction        'PETS 2.0 (Palatinus et al., 2011)'
_computing_molecular_graphics    'Vesta (Momma & Izumi, 2011)'
_computing_structure_refinement  'Jana2006 (Petricek et al., 2014)'
_computing_structure_solution    'SIR2014 (Burla et al., 2015)'
_diffrn_ambient_temperature      298
_diffrn_detector                 Timepix2
_diffrn_measured_fraction_theta_full 0.79
_diffrn_measured_fraction_theta_max 0.57
_diffrn_measurement_device       'ZEISS Libra 120'
_diffrn_measurement_device_type  TEM
_diffrn_radiation_probe          electron
_diffrn_radiation_source         LaB6
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0335
_diffrn_reflns_av_R_equivalents  0.3349
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10451
_diffrn_reflns_theta_full        0.95
_diffrn_reflns_theta_max         1.2
_diffrn_reflns_theta_min         0.05
_diffrn_source_voltage           '120 kV'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    5.4927
_exptl_crystal_description       needle
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.0002
_exptl_crystal_size_mid          0.0001
_exptl_crystal_size_min          0.0001
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.40
_refine_ls_goodness_of_fit_gt    16.27
_refine_ls_goodness_of_fit_ref   13.93
_refine_ls_number_constraints    0
_refine_ls_number_parameters     34
_refine_ls_number_reflns         562
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.3222
_refine_ls_R_factor_gt           0.2435
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(σ²(F)+0.0001F²)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.2946
_refine_ls_wR_factor_ref         0.3025
_reflns_number_gt                401
_reflns_number_total             562
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            dk5082sup1.cif
_cod_data_source_block           average
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               2108457
_diffrn_measurement_             'phi scan'
_refine_ls_extinction_           none
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 'x, y, z'
2 '-x, -y, -z'
3 '-x+1/2, -y, z+1/2'
4 'x+1/2, y, -z+1/2'
5 'x+1/2, -y+1/2, -z+1/2'
6 '-x+1/2, y+1/2, z+1/2'
7 '-x, y+1/2, -z'
8 'x, -y+1/2, z'
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_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
Pb1 Pb 0.2886(7) 0.25 1.3368(8) Uani 0.083(6) 4 1 d
Hg1 Hg 0.4150(6) 0.25 0.9831(7) Uani 0.065(5) 4 1 d
As1 As 0.1286(13) 0.356(3) 1.1428(18) Uiso 0.030(6) 8 0.5 d
As2 As 0.0526(12) 0.356(3) 0.8089(16) Uiso 0.019(6) 8 0.5 d
S1 S 0.2233(15) 0.25 1.060(2) Uiso 0.034(7) 4 1 d
S2 S 0.1437(15) 0.25 0.690(2) Uiso 0.036(7) 4 1 d
S3 S 0.3337(16) 0.25 0.805(2) Uiso 0.042(7) 4 1 d
S4 S 0.4132(13) 0.25 1.4762(19) Uiso 0.019(6) 4 1 d
S5 S 0.4954(15) 0.25 1.160(2) Uiso 0.040(7) 4 1 d
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pb1 Pb 0.137(16) 0.101(8) 0.011(5) 0 -0.002332 0
Hg1 Hg 0.118(14) 0.069(6) 0.009(5) 0 0.001652 0
loop_
_atom_type_symbol
_atom_type_scat_source
As International_Tables_Vol_C
Hg International_Tables_Vol_C
Pb International_Tables_Vol_C
S International_Tables_Vol_C
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
Pb1 S1 S2 177.9
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pb1 S1 2.982(17)

_cod_database_fobs_code 2108457
