#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/78/2217841.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_2217841
loop_
_publ_author_name
'Ktari, Lilia'
'Abdelhedi, Mohamed'
'Dammak, Mohamed'
'Cousson, Alain'
'Kolsi, Abdelwaheb'
_publ_section_title
;
 The solid solution Na~0.39~(NH₄)~1.61~SO₄·Te(OH)₆
;
_journal_coeditor_code           WM2171
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i18
_journal_page_last               i19
_journal_paper_doi               10.1107/S1600536808003425
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'Na0.39 (N H4)1.61 S O4, Te (O H)6'
_chemical_formula_structural     '((N H4)1.61 Na0.39) (S O4) Te (O H)6'
_chemical_formula_sum            'H6 N1.61 Na0.39 O10 S Te'
_chemical_formula_weight         357.22
_chemical_name_systematic
;
sodium ammonium sulfate--telluric acid (1/1)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           CRYSTALS_ver_12.51
_cell_angle_alpha                90
_cell_angle_beta                 106.580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6900(10)
_cell_length_b                   6.5920(10)
_cell_length_c                   11.3450(10)
_cell_measurement_reflns_used    919
_cell_measurement_temperature    298
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      2.7
_cell_volume                     981.26(19)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'CRYSTALS (Betteridge et al.,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al.,  2003)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      297
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            919
_diffrn_reflns_theta_full        29.571
_diffrn_reflns_theta_max         30.174
_diffrn_reflns_theta_min         1.596
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.301
_exptl_absorpt_correction_T_max  0.719
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS in PLATON; Spek, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.418
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             678.224
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.51
_refine_diff_density_min         -1.15
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9335
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         638
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.000105
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982);
 W = [weight] * [1-(deltaF/6*sigmaF)²]²
 Ai are: 0.527 0.367 0.302
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0535
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0433
_reflns_number_gt                638
_reflns_number_total             849
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            wm2171.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'H6 N1.61 Na0.39 O10 S1 Te1'
_cod_database_code               2217841
_cod_database_fobs_code          2217841
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2
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
Te Te1 0.5000 0.5000 0.0000 0.0099 Uani 1.0000
Te Te2 0.0000 1.0000 0.0000 0.0106 Uani 1.0000
S S1 -0.24900(9) -0.49139(17) -0.2352(2) 0.0124 Uani 1.0000
Na Na1 -0.1448(2) 0.0149(2) -0.3454(2) 0.0181 Uani 0.2590
N N1 -0.1448(2) 0.0149(2) -0.3454(2) 0.0181 Uani 0.7410
Na Na2 -0.3539(2) 0.0047(2) -0.0920(2) 0.0229 Uani 0.1300
N N2 -0.3539(2) 0.0047(2) -0.0920(2) 0.0229 Uani 0.8700
O O1 0.5309(3) 0.5871(6) -0.1453(6) 0.0241 Uani 1.0000
O O2 0.4606(3) 0.2370(5) -0.0661(5) 0.0232 Uani 1.0000
O O3 0.3647(2) 0.6044(5) -0.0656(5) 0.0174 Uani 1.0000
O O4 -0.1350(2) 1.0859(5) -0.0867(5) 0.0188 Uani 1.0000
O O5 0.0167(2) 1.2375(5) 0.1011(5) 0.0150 Uani 1.0000
O O6 0.0519(2) 1.1390(5) -0.1165(6) 0.0174 Uani 1.0000
O O7 -0.1698(3) -0.5105(5) -0.1149(6) 0.0221 Uani 1.0000
O O8 -0.3350(2) -0.6287(5) -0.2355(5) 0.0160 Uani 1.0000
O O9 -0.2843(2) -0.2792(5) -0.2508(5) 0.0202 Uani 1.0000
O O10 -0.2079(3) -0.5499(6) -0.3357(6) 0.0213 Uani 1.0000
H H1 0.5496 0.4942 -0.1631 0.0500 Uiso 1.0000
H H2 0.4006 0.2489 -0.1288 0.0500 Uiso 1.0000
H H3 0.3748 0.7041 -0.1257 0.0500 Uiso 1.0000
H H4 -0.1328 1.2273 -0.0942 0.0500 Uiso 1.0000
H H5 -0.0379 1.3302 0.0591 0.0500 Uiso 1.0000
H H6 0.1037 1.0563 -0.1347 0.0500 Uiso 1.0000
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Te -0.5308 1.6751 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 'International Tables Vol C 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Te1 O2 2_665 2_665 92.32(15) no
O3 Te1 O1 2_665 2_665 89.1(2) no
O2 Te1 O1 2_665 2_665 92.4(2) no
O3 Te1 O1 2_665 . 90.9(2) no
O2 Te1 O1 2_665 . 87.6(2) no
O1 Te1 O1 2_665 . 179.994 no
H1 Te1 O2 2_665 . 103.413 no
O3 Te1 O2 2_665 . 87.68(15) no
O2 Te1 O2 2_665 . 179.994 no
O1 Te1 O2 2_665 . 87.6(2) no
O1 Te1 O2 . . 92.4(2) no
H1 Te1 O3 2_665 . 79.615 no
O3 Te1 O3 2_665 . 179.994 no
O2 Te1 O3 2_665 . 87.68(15) no
O1 Te1 O3 2_665 . 90.9(2) no
O1 Te1 O3 . . 89.1(2) no
O2 Te1 O3 . . 92.32(15) no
O5 Te2 O4 2_575 2_575 89.93(16) no
O5 Te2 O6 2_575 2_575 91.02(19) no
O4 Te2 O6 2_575 2_575 89.85(18) no
O5 Te2 O4 2_575 . 90.07(16) no
O4 Te2 O4 2_575 . 179.994 no
O6 Te2 O4 2_575 . 90.15(18) no
O5 Te2 O5 2_575 . 179.994 no
O4 Te2 O5 2_575 . 90.07(16) no
O6 Te2 O5 2_575 . 88.98(19) no
O4 Te2 O5 . . 89.93(16) no
O5 Te2 O6 2_575 . 88.98(19) no
O4 Te2 O6 2_575 . 90.15(18) no
O6 Te2 O6 2_575 . 179.994 no
O4 Te2 O6 . . 89.85(18) no
O5 Te2 O6 . . 91.02(19) no
O7 S1 O8 . . 108.7(3) no
O7 S1 O9 . . 108.6(3) no
O8 S1 O9 . . 110.21(19) no
O7 S1 O10 . . 110.6(3) no
O8 S1 O10 . . 108.6(3) no
O9 S1 O10 . . 110.1(3) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Te1 H1 2_665 2.146 no
Te1 O3 2_665 1.916(3) no
Te1 O2 2_665 1.905(4) no
Te1 O1 2_665 1.903(6) no
Te1 O1 . 1.903(6) yes
Te1 O2 . 1.905(4) yes
Te1 O3 . 1.916(3) yes
Te1 H1 . 2.146 no
Te2 O5 2_575 1.915(4) no
Te2 O4 2_575 1.914(3) no
Te2 O6 2_575 1.904(5) no
Te2 O4 . 1.914(3) yes
Te2 O5 . 1.915(4) yes
Te2 O6 . 1.904(5) yes
S1 O7 . 1.486(6) yes
S1 O8 . 1.485(3) yes
S1 O9 . 1.474(3) yes
S1 O10 . 1.460(6) yes
O1 H1 . 0.715 no
O2 H2 . 0.924 no
O3 H3 . 0.985 no
O4 H4 . 0.937 no
O5 H5 . 0.978 no
O6 H6 . 0.963 no
Na1 O6 3_534 2.873(4) yes
Na1 O4 1_545 2.937(6) yes
Na1 O5 4_564 2.947(4) yes
Na1 O3 3_544 2.950(4) yes
Na1 O7 4_544 2.978(7) yes
Na1 O10 1_565 3.008(4) yes
Na1 O9 . 3.120(4) yes
Na1 O6 1_545 3.267(6) yes
Na1 O5 2_565 3.278(5) yes
Na2 O9 . 2.938(5) yes
Na2 O8 1_565 2.966(4) yes
Na2 O4 1_545 3.029(4) yes
Na2 O10 4_545 3.037(7) yes
Na2 O2 1_455 3.050(4) yes
Na2 O2 2_555 3.063(5) yes
Na2 O1 1_445 3.144(5) yes
Na2 O3 2_565 3.164(5) yes
Na2 O1 3_544 3.305(6) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O2 H2 O9 3_554 0.924(4) 1.787(4) 2.700(6) 169.2(2) yes
O3 H3 O8 3_564 0.985(5) 1.871(5) 2.799(7) 155.7(2) yes
O4 H4 O7 1_575 0.937(3) 1.798(3) 2.706(7) 162.4(2) yes
O6 H6 O10 3_564 0.963(4) 1.706(4) 2.658(6) 169.5(3) yes
N1 . O6 3_534 . . 2.873(4) . yes
N1 . O4 1_545 . . 2.937(6) . yes
N1 . O5 4_564 . . 2.947(4) . yes
N1 . O3 3_544 . . 2.950(4) . yes
N1 . O7 4_544 . . 2.978(7) . yes
N1 . O10 1_565 . . 3.008(4) . yes
N2 . O9 . . . 2.938(5) . yes
N2 . O8 1_565 . . 2.966(4) . yes
N2 . O4 1_545 . . 3.029(4) . yes
N2 . O10 4_545 . . 3.037(7) . yes
N2 . O2 1_455 . . 3.050(4) . yes
N2 . O2 2_555 . . 3.063(5) . yes
