##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
#                                                                            #
##############################################################################
                                             
data_I
_audit_creation_method     SHELXL97
_chemical_name_systematic     'dysprosium ultraphosphate'
_chemical_name_common     'dysprosium ultraphosphate'
_chemical_formula_sum     'Dy O14 P5'
_chemical_formula_iupac     'Dy P5 O14'
_chemical_formula_weight     541.35
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'C 2/c'
_symmetry_space_group_name_Hall     '-C 2yc'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y, -z+1/2'
    'x+1/2, y+1/2, z'
    '-x+1/2, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y, z-1/2'
    '-x+1/2, -y+1/2, -z'
    'x+1/2, -y+1/2, z-1/2'
_cell_length_a     12.8934(6)
_cell_length_b     12.7756(5)
_cell_length_c     12.4415(5)
_cell_angle_alpha     90.00
_cell_angle_beta     91.313(3)
_cell_angle_gamma     90.00
_cell_volume     2048.84(15)
_cell_formula_units_Z     8
_cell_measurement_reflns_used     1946
_cell_measurement_theta_min     2.910
_cell_measurement_theta_max     26.878
_cell_measurement_temperature     298(2)
_exptl_crystal_description     Cubic
_exptl_crystal_colour     Colourless
_exptl_crystal_size_max     0.15
_exptl_crystal_size_mid     0.15
_exptl_crystal_size_min     0.15
_exptl_crystal_density_diffrn     3.510
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     2024
_exptl_absorpt_coefficient_mu     8.163
_exptl_absorpt_correction_type     refdelf
_exptl_absorpt_process_details     '(Parkin et al.,  1995)'
_exptl_absorpt_correction_T_min     0.2855
_exptl_absorpt_correction_T_max     0.3062
_exptl_special_details
;
;
_diffrn_ambient_temperature     298(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Nonius KappaCCD area-detector'
_diffrn_measurement_method     ω/2θ
_diffrn_detector_area_resol_mean     9
_diffrn_reflns_number     3807
_diffrn_reflns_av_R_equivalents     0.0000
_diffrn_reflns_av_sigmaI/netI     0.0670
_diffrn_reflns_theta_min     3.94
_diffrn_reflns_theta_max     26.83
_diffrn_reflns_theta_full     27.83
_diffrn_measured_fraction_theta_max     0.984
_diffrn_measured_fraction_theta_full     0.984
_diffrn_reflns_limit_h_min     -16
_diffrn_reflns_limit_h_max     16
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     16
_diffrn_reflns_limit_l_min     0
_diffrn_reflns_limit_l_max     16
_diffrn_standards_number     2
_diffrn_standards_interval_count     150
_diffrn_standards_interval_time     30
_diffrn_standards_decay_%     0
_refine_special_details
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_reflns_number_total     2290
_reflns_number_gt     1682
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0548
_refine_ls_R_factor_gt     0.0284
_refine_ls_wR_factor_gt     0.0551
_refine_ls_wR_factor_ref     0.0629
_refine_ls_goodness_of_fit_ref     0.980
_refine_ls_restrained_S_all     0.980
_refine_ls_number_reflns     2290
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     ?
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
                   'calc w = 1/[σ²(Fo²)+(0.0082P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     ?
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     1.645
_refine_diff_density_min     -1.266
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6'
_computing_data_collection     'COLLECT (Nonius, 1998)'
_computing_cell_refinement     'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction     'SCALEPACK and DENZO (Otwinowski & Minor, 1997)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'DIAMOND (Brandenburg, 1998)'
_computing_publication_material     'SHELXL97'
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_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Dy Dy1 1.0000 0.52187(2) 0.2500 0.00472(10) Uani d S 1 . .
    Dy Dy2 1.0000 -0.03118(2) 0.2500 0.00456(10) Uani d S 1 . .
    P P1 1.02500(9) 0.15233(9) 0.03255(11) 0.0054(3) Uani d . 1 . .
    P P2 1.18169(9) 0.13795(9) 0.39145(12) 0.0055(3) Uani d . 1 . .
    P P3 1.14714(9) 0.46602(9) 0.49867(12) 0.0064(3) Uani d . 1 . .
    P P4 1.14896(9) 0.33223(9) 0.10313(11) 0.0059(3) Uani d . 1 . .
    P P5 1.32072(9) 0.25021(9) 0.24096(11) 0.0055(3) Uani d . 1 . .
    O O1 1.0257(2) 0.1032(3) -0.0736(3) 0.0123(8) Uani d . 1 . .
    O O2 1.0607(2) 0.0973(3) 0.1306(3) 0.0105(8) Uani d . 1 . .
    O O3 1.0865(2) 0.2617(2) 0.0210(3) 0.0085(8) Uani d . 1 . .
    O O4 1.0914(2) 0.1981(2) 0.4457(3) 0.0095(8) Uani d . 1 . .
    O O5 1.1526(2) 0.0497(3) 0.3226(3) 0.0119(8) Uani d . 1 . .
    O O6 1.2398(3) 0.2283(2) 0.3355(3) 0.0118(8) Uani d . 1 . .
    O O7 1.2490(2) 0.1041(3) 0.4914(3) 0.0083(7) Uani d . 1 . .
    O O8 1.1159(3) 0.4636(2) 0.3857(3) 0.0104(8) Uani d . 1 . .
    O O9 1.0768(2) 0.4342(3) 0.5843(3) 0.0133(8) Uani d . 1 . .
    O O10 1.1946(2) 0.4182(2) 0.0282(3) 0.0078(7) Uani d . 1 . .
    O O11 1.0896(3) 0.3714(3) 0.1921(3) 0.0134(8) Uani d . 1 . .
    O O12 1.2437(2) 0.2633(2) 0.1365(3) 0.0090(8) Uani d . 1 . .
    O O13 1.3680(2) 0.3509(3) 0.2684(3) 0.0125(8) Uani d . 1 . .
    O O14 1.3833(3) 0.1578(3) 0.2183(3) 0.0154(9) Uani d . 1 . .
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
    Dy1 O14 4_755 2.326(3) ?
    Dy1 O14 3_455 2.326(3) ?
    Dy1 O8 2_755 2.350(3) ?
    Dy1 O8 . 2.350(3) ?
    Dy1 O11 2_755 2.364(3) ?
    Dy1 O11 . 2.364(3) ?
    Dy1 O9 5_766 2.375(4) ?
    Dy1 O9 6_565 2.375(4) ?
    Dy2 O13 3_445 2.288(3) ?
    Dy2 O13 4_745 2.288(3) ?
    Dy2 O2 2_755 2.359(3) ?
    Dy2 O2 . 2.359(3) ?
    Dy2 O5 . 2.382(3) ?
    Dy2 O5 2_755 2.382(3) ?
    Dy2 O1 6_556 2.396(4) ?
    Dy2 O1 5_755 2.396(4) ?
    P1 O1 . 1.462(4) ?
    P1 O2 . 1.473(4) ?
    P1 O3 . 1.615(3) ?
    P1 O4 2_755 1.638(3) ?
    P2 O5 . 1.459(4) ?
    P2 O6 . 1.550(4) ?
    P2 O7 . 1.561(4) ?
    P2 O4 . 1.562(3) ?
    P3 O8 . 1.454(4) ?
    P3 O9 . 1.472(4) ?
    P3 O7 7_756 1.614(3) ?
    P3 O10 6_566 1.640(3) ?
    P4 O11 . 1.450(4) ?
    P4 O12 . 1.554(3) ?
    P4 O10 . 1.564(3) ?
    P4 O3 . 1.570(4) ?
    P5 O13 . 1.460(3) ?
    P5 O14 . 1.461(4) ?
    P5 O6 . 1.615(4) ?
    P5 O12 . 1.626(4) ?
    O1 Dy2 5_755 2.396(4) ?
    O4 P1 2_755 1.638(3) ?
    O7 P3 7_756 1.614(3) ?
    O9 Dy1 5_766 2.375(4) ?
    O10 P3 6_565 1.640(3) ?
    O13 Dy2 3 2.288(3) ?
    O14 Dy1 3_545 2.326(3) ?
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
    O14 Dy1 O14 4_755 3_455 83.40(17) ?
    O14 Dy1 O8 4_755 2_755 139.20(13) ?
    O14 Dy1 O8 3_455 2_755 73.51(12) ?
    O14 Dy1 O8 4_755 . 73.51(12) ?
    O14 Dy1 O8 3_455 . 139.20(13) ?
    O8 Dy1 O8 2_755 . 143.05(15) ?
    O14 Dy1 O11 4_755 2_755 150.97(13) ?
    O14 Dy1 O11 3_455 2_755 109.89(12) ?
    O8 Dy1 O11 2_755 2_755 69.76(12) ?
    O8 Dy1 O11 . 2_755 80.24(12) ?
    O14 Dy1 O11 4_755 . 109.89(12) ?
    O14 Dy1 O11 3_455 . 150.97(13) ?
    O8 Dy1 O11 2_755 . 80.24(12) ?
    O8 Dy1 O11 . . 69.76(12) ?
    O11 Dy1 O11 2_755 . 71.14(17) ?
    O14 Dy1 O9 4_755 5_766 87.55(12) ?
    O14 Dy1 O9 3_455 5_766 71.94(13) ?
    O8 Dy1 O9 2_755 5_766 115.31(12) ?
    O8 Dy1 O9 . 5_766 73.87(12) ?
    O11 Dy1 O9 2_755 5_766 73.22(12) ?
    O11 Dy1 O9 . 5_766 132.30(12) ?
    O14 Dy1 O9 4_755 6_565 71.94(13) ?
    O14 Dy1 O9 3_455 6_565 87.55(12) ?
    O8 Dy1 O9 2_755 6_565 73.87(12) ?
    O8 Dy1 O9 . 6_565 115.31(12) ?
    O11 Dy1 O9 2_755 6_565 132.30(12) ?
    O11 Dy1 O9 . 6_565 73.22(12) ?
    O9 Dy1 O9 5_766 6_565 152.68(16) ?
    O13 Dy2 O13 3_445 4_745 97.64(17) ?
    O13 Dy2 O2 3_445 2_755 97.86(12) ?
    O13 Dy2 O2 4_745 2_755 141.19(12) ?
    O13 Dy2 O2 3_445 . 141.19(12) ?
    O13 Dy2 O2 4_745 . 97.86(12) ?
    O2 Dy2 O2 2_755 . 91.85(17) ?
    O13 Dy2 O5 3_445 . 149.04(13) ?
    O13 Dy2 O5 4_745 . 73.38(11) ?
    O2 Dy2 O5 2_755 . 75.08(11) ?
    O2 Dy2 O5 . . 69.75(12) ?
    O13 Dy2 O5 3_445 2_755 73.38(11) ?
    O13 Dy2 O5 4_745 2_755 149.04(13) ?
    O2 Dy2 O5 2_755 2_755 69.75(12) ?
    O2 Dy2 O5 . 2_755 75.08(11) ?
    O5 Dy2 O5 . 2_755 128.56(17) ?
    O13 Dy2 O1 3_445 6_556 75.10(12) ?
    O13 Dy2 O1 4_745 6_556 75.58(12) ?
    O2 Dy2 O1 2_755 6_556 74.42(12) ?
    O2 Dy2 O1 . 6_556 143.43(11) ?
    O5 Dy2 O1 . 6_556 73.96(12) ?
    O5 Dy2 O1 2_755 6_556 127.57(12) ?
    O13 Dy2 O1 3_445 5_755 75.58(12) ?
    O13 Dy2 O1 4_745 5_755 75.10(12) ?
    O2 Dy2 O1 2_755 5_755 143.43(11) ?
    O2 Dy2 O1 . 5_755 74.42(12) ?
    O5 Dy2 O1 . 5_755 127.57(12) ?
    O5 Dy2 O1 2_755 5_755 73.96(12) ?
    O1 Dy2 O1 6_556 5_755 134.80(16) ?
    O1 P1 O2 . . 122.3(2) ?
    O1 P1 O3 . . 106.1(2) ?
    O2 P1 O3 . . 110.0(2) ?
    O1 P1 O4 . 2_755 109.1(2) ?
    O2 P1 O4 . 2_755 107.7(2) ?
    O3 P1 O4 . 2_755 99.15(17) ?
    O5 P2 O6 . . 115.6(2) ?
    O5 P2 O7 . . 112.6(2) ?
    O6 P2 O7 . . 107.35(19) ?
    O5 P2 O4 . . 116.74(18) ?
    O6 P2 O4 . . 101.58(18) ?
    O7 P2 O4 . . 101.4(2) ?
    O8 P3 O9 . . 122.2(2) ?
    O8 P3 O7 . 7_756 105.87(19) ?
    O9 P3 O7 . 7_756 108.4(2) ?
    O8 P3 O10 . 6_566 109.2(2) ?
    O9 P3 O10 . 6_566 108.6(2) ?
    O7 P3 O10 7_756 6_566 100.33(17) ?
    O11 P4 O12 . . 114.7(2) ?
    O11 P4 O10 . . 115.18(19) ?
    O12 P4 O10 . . 104.65(18) ?
    O11 P4 O3 . . 115.0(2) ?
    O12 P4 O3 . . 103.71(18) ?
    O10 P4 O3 . . 102.1(2) ?
    O13 P5 O14 . . 121.8(2) ?
    O13 P5 O6 . . 104.8(2) ?
    O14 P5 O6 . . 111.7(2) ?
    O13 P5 O12 . . 109.89(19) ?
    O14 P5 O12 . . 105.0(2) ?
    O6 P5 O12 . . 101.96(18) ?
    P1 O1 Dy2 . 5_755 171.3(2) ?
    P1 O2 Dy2 . . 138.75(19) ?
    P4 O3 P1 . . 133.2(3) ?
    P2 O4 P1 . 2_755 126.2(2) ?
    P2 O5 Dy2 . . 139.2(2) ?
    P2 O6 P5 . . 141.6(2) ?
    P2 O7 P3 . 7_756 131.3(2) ?
    P3 O8 Dy1 . . 147.7(2) ?
    P3 O9 Dy1 . 5_766 147.1(2) ?
    P4 O10 P3 . 6_565 128.6(2) ?
    P4 O11 Dy1 . . 141.6(2) ?
    P4 O12 P5 . . 137.2(2) ?
    P5 O13 Dy2 . 3 149.8(2) ?
    P5 O14 Dy1 . 3_545 158.2(3) ?
data_global
_journal_date_recd_electronic     2007-01-30
_journal_date_accepted     2007-02-19
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2007
_journal_volume     63
_journal_issue      3
_journal_page_first     i89
_journal_page_last     i91
_journal_paper_category     EI
_journal_coeditor_code     BR2028
_publ_contact_author_name     "Professor Mokhtar, Ferid"
_publ_contact_author_address
;
Laboratoire des Materiaux
Institut National de Recherche Scientifique et Technique
BP 95
2050 Hammam-Lif
Tunisia
;
_publ_contact_author_email     mokhtar.ferid@inrst.rnrt.tn
_publ_contact_author_fax     '216 71 43 09 34'
_publ_contact_author_phone     '216 71 43 04 70'
_publ_section_title
;
DyP₅O₁₄
;
loop_
    _publ_author_name
    _publ_author_address
    'Chehimi-Moumen, Fathia'
;
Laboratoire d'Application de la Chimie aux Ressources et Substances Naturelles
et a l'Environnement
Faculté des Sciences de Bizerte
7021 Zarzouna
Tunisia
;
    "Mokhtar, Férid"
;
Laboratoire des Matériaux
Institut National de Recherche Scientifique et Technique
BP 95
2050 Hammam-Lif
Tunisia
;
