#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/39/2213985.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_2213985
loop_
_publ_author_name
'Boujelben, Mohamed'
'Toumi, Mohamed'
'Mhiri, Tahar'
_publ_section_title
;
 NH₄Ce(SO₄)₂·4H₂O
;
_journal_coeditor_code           WM2108
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i144
_journal_page_last               i145
_journal_paper_doi               10.1107/S1600536807024555
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'N H4 Ce (S O4)2 , 4H2 O'
_chemical_formula_structural     '(N H4) Ce (S O4)2 , 4H2 O'
_chemical_formula_sum            'Ce H12 N O12 S2'
_chemical_formula_weight         422.35
_chemical_name_systematic
;
ammonium cerium(III) bis(sulfate) tetrahydrate
;
_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                 97.29(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.673(2)
_cell_length_b                   18.9920(5)
_cell_length_c                   8.808(2)
_cell_measurement_reflns_used    6883
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.82
_cell_measurement_theta_min      1.77
_cell_volume                     1107.2(4)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction        DENZO
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge et al.,  2003)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius Kappa CCD area-detector'
_diffrn_measurement_method       'φ rotation scans with 2° steps'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6836
_diffrn_reflns_theta_full        29.961
_diffrn_reflns_theta_max         29.961
_diffrn_reflns_theta_min         2.145
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.545
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS in PLATON; Spek, 1998)'
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    2.533
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.00
_refine_diff_density_min         -2.62
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0490
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1489
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.000650
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, 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: 0.119E+04 -0.128E+04 956.
Prince, E. (1982). Mathematical Techniques in Crystallography and Materials
Science. New York: Springer-Verlag.
Watkin, D. J. (1994). Acta Cryst. A50, 411--437.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0713
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0684
_reflns_number_gt                1489
_reflns_number_total             3225
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            wm2108.cif
_cod_data_source_block           I
_cod_original_cell_volume        1107.3(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2213985
_cod_database_fobs_code          2213985
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
Ce Ce1 0.64763(5) 0.37838(2) 0.78484(4) 0.0152 Uani 1.0000
S S1 0.6215(3) 0.22283(10) 0.9125(2) 0.0227 Uani 1.0000
S S2 0.1859(2) 0.42436(10) 0.7628(3) 0.0268 Uani 1.0000
O O1 0.5880(11) 0.1595(3) 0.8189(7) 0.0339 Uani 1.0000
O O2 0.4532(9) 0.2738(3) 0.8726(8) 0.0299 Uani 1.0000
O O3 0.6324(14) 0.2963(4) 0.5734(8) 0.0477 Uani 1.0000
O O4 0.8046(9) 0.2604(3) 0.8841(8) 0.0317 Uani 1.0000
O O5 0.2958(9) 0.3919(4) 0.6427(7) 0.0421 Uani 1.0000
O O6 0.1221(12) 0.4953(4) 0.7296(18) 0.0859 Uani 1.0000
O O7 0.3358(10) 0.4220(5) 0.9017(9) 0.0481 Uani 1.0000
O O8 0.0153(8) 0.3808(4) 0.7888(9) 0.0384 Uani 1.0000
O O9 0.7475(12) 0.3922(4) 1.0692(7) 0.0424 Uani 1.0000
O O10 0.6715(11) 0.4456(4) 0.5367(8) 0.0374 Uani 1.0000
O O11 0.6946(14) 0.5064(4) 0.8336(8) 0.0433 Uani 1.0000
N N1 1.1550(14) 0.2781(5) 1.1103(10) 0.0465 Uani 1.0000
O O12 1.1383(12) 0.3893(5) 1.3333(11) 0.0566 Uani 1.0000
H H1 1.1104 0.3072 1.1611 0.0500 Uiso 1.0000
H H2 1.1757 0.2387 1.1504 0.0500 Uiso 1.0000
H H3 1.0699 0.2738 1.0347 0.0500 Uiso 1.0000
H H4 1.2787 0.2884 1.0602 0.0500 Uiso 1.0000
H H7 0.7780 0.4503 0.4859 0.0500 Uiso 1.0000
H H5 0.6188 0.3895 0.9994 0.0500 Uiso 1.0000
H H6 0.7483 0.3625 1.1406 0.0500 Uiso 1.0000
H H8 0.5980 0.4851 0.5266 0.0500 Uiso 1.0000
H H9 0.7458 0.5349 0.7810 0.0500 Uiso 1.0000
H H10 0.6884 0.5296 0.9120 0.0500 Uiso 1.0000
H H11 1.2719 0.3790 1.3297 0.0500 Uiso 1.0000
H H12 1.0854 0.3554 1.3679 0.0500 Uiso 1.0000
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Ce -0.2486 2.6331 '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'
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
O8 Ce1 S1 1_655 . 96.44(18) no
O8 Ce1 O2 1_655 . 123.9(2) no
S1 Ce1 O2 . . 27.51(14) no
O8 Ce1 O3 1_655 . 88.1(3) no
S1 Ce1 O3 . . 70.99(17) no
O2 Ce1 O3 . . 76.0(2) no
O8 Ce1 O4 1_655 . 69.4(2) no
S1 Ce1 O4 . . 27.05(13) no
O2 Ce1 O4 . . 54.6(2) no
O3 Ce1 O4 . . 71.1(2) no
O8 Ce1 O5 1_655 . 150.5(2) no
S1 Ce1 O5 . . 100.40(19) no
O2 Ce1 O5 . . 75.7(2) no
O3 Ce1 O5 . . 74.9(3) no
O4 Ce1 O5 . . 124.6(2) no
O8 Ce1 O7 1_655 . 148.0(2) no
S1 Ce1 O7 . . 94.3(2) no
O2 Ce1 O7 . . 70.2(3) no
O3 Ce1 O7 . . 123.9(3) no
O4 Ce1 O7 . . 117.3(3) no
O8 Ce1 O9 1_655 . 81.1(3) no
S1 Ce1 O9 . . 76.39(17) no
O2 Ce1 O9 . . 82.0(2) no
O3 Ce1 O9 . . 144.2(2) no
O4 Ce1 O9 . . 73.1(2) no
O8 Ce1 O10 1_655 . 80.3(2) no
S1 Ce1 O10 . . 141.35(17) no
O2 Ce1 O10 . . 137.7(2) no
O3 Ce1 O10 . . 70.4(2) no
O4 Ce1 O10 . . 131.1(2) no
O8 Ce1 O11 1_655 . 82.8(3) no
S1 Ce1 O11 . . 149.54(17) no
O2 Ce1 O11 . . 140.3(2) no
O3 Ce1 O11 . . 139.1(2) no
O4 Ce1 O11 . . 139.1(3) no
O8 Ce1 H5 1_655 . 101.977 no
S1 Ce1 H5 . . 74.861 no
O2 Ce1 H5 . . 70.786 no
O3 Ce1 H5 . . 145.265 no
O4 Ce1 H5 . . 81.389 no
O5 Ce1 O7 . . 54.4(2) no
O5 Ce1 O9 . . 126.3(2) no
O7 Ce1 O9 . . 72.2(3) no
O5 Ce1 O10 . . 71.4(2) no
O7 Ce1 O10 . . 108.8(3) no
O9 Ce1 O10 . . 139.5(2) no
O5 Ce1 O11 . . 94.3(3) no
O7 Ce1 O11 . . 72.9(3) no
O9 Ce1 O11 . . 73.4(2) no
O10 Ce1 O11 . . 68.8(2) no
O5 Ce1 H5 . . 105.736 no
O7 Ce1 H5 . . 52.304 no
O9 Ce1 H5 . . 20.850 no
O10 Ce1 H5 . . 143.699 no
O11 Ce1 H5 . . 75.529 no
Ce1 S1 O3 . 4_555 125.4(3) no
Ce1 S1 O1 . . 125.3(3) no
O3 S1 O1 4_555 . 109.2(4) no
Ce1 S1 O2 . . 52.1(2) no
O3 S1 O2 4_555 . 109.6(4) no
O1 S1 O2 . . 110.2(4) no
Ce1 S1 O4 . . 53.2(2) no
O3 S1 O4 4_555 . 110.4(5) no
O1 S1 O4 . . 112.1(4) no
O2 S1 O4 . . 105.2(3) no
O5 S2 O6 . . 113.8(7) no
O5 S2 O7 . . 103.4(3) no
O6 S2 O7 . . 110.5(7) no
O5 S2 O8 . . 110.0(5) no
O6 S2 O8 . . 110.5(5) no
O7 S2 O8 . . 108.3(5) no
Ce1 O2 S1 . . 100.4(3) no
Ce1 O3 S1 . 4_554 154.4(5) no
Ce1 O4 S1 . . 99.8(3) no
Ce1 O5 S2 . . 101.5(3) no
Ce1 O7 S2 . . 100.1(3) no
Ce1 O8 S2 1_455 . 144.5(5) no
H5 O9 H6 . . 110.455 no
Ce1 O10 H7 . . 128.308 no
Ce1 O10 H8 . . 114.254 no
H7 O10 H8 . . 109.248 no
H9 O11 H10 . . 101.042 no
H1 N1 H2 . . 116.347 no
H1 N1 H3 . . 104.775 no
H2 N1 H3 . . 108.423 no
H1 N1 H4 . . 119.964 no
H2 N1 H4 . . 105.124 no
H3 N1 H4 . . 100.646 no
H11 O12 H12 . . 108.302 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
Ce1 O8 1_655 2.450(5) yes
Ce1 S1 . 3.1736(18) no
Ce1 O2 . 2.545(6) yes
Ce1 O3 . 2.420(7) yes
Ce1 O4 . 2.578(6) yes
Ce1 O5 . 2.530(6) yes
Ce1 O7 . 2.573(6) yes
Ce1 O9 . 2.523(6) yes
Ce1 O10 . 2.554(6) yes
Ce1 O11 . 2.482(7) yes
Ce1 H5 . 1.935 no
S1 O3 4_555 1.456(7) yes
S1 O1 . 1.459(6) yes
S1 O2 . 1.491(6) yes
S1 O4 . 1.464(6) yes
S2 O5 . 1.495(6) yes
S2 O6 . 1.432(8) yes
S2 O7 . 1.479(8) yes
S2 O8 . 1.449(6) yes
O9 H5 . 0.992 no
O9 H6 . 0.845 no
O10 H7 . 0.891 no
O10 H8 . 0.893 no
O11 H9 . 0.815 no
O11 H10 . 0.824 no
N1 H1 . 0.793 no
N1 H2 . 0.831 no
N1 H3 . 0.823 no
N1 H4 . 1.003 no
O12 H11 . 0.917 no
O12 H12 . 0.812 no
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
N1 H1 O12 . 0.793(9) 2.167(10) 2.918(14) 153.1(7) yes
N1 H3 O4 . 0.823(9) 2.088(6) 2.882(12) 165.6(7) yes
N1 H4 O2 1_655 1.003(10) 2.157(6) 3.067(11) 150.0(6) yes
O9 H5 O7 . 0.992(7) 2.068(7) 2.998(10) 156.2(5) yes
O9 H6 O1 4_555 0.845(7) 2.052(6) 2.738(9) 138.7(6) yes
O11 H9 O12 2_767 0.815(7) 1.969(9) 2.776(11) 174.6(6) yes
O11 H10 O7 2_667 0.824(6) 1.906(7) 2.705(9) 176.1(6) yes
