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data_Pb5Al3F19/2003/Abrahams_et_al/structure
_journal_date_recd_electronic     2002-07-16
_journal_date_accepted     2003-05-23
_journal_name_full     'Acta Crystallographica, Section B'
_journal_year     2003
_journal_volume     59
_journal_issue      5
_journal_page_first     557
_journal_page_last     574
_journal_paper_category     FA
_publ_contact_author_name     'Abrahams, S. C.'
_publ_contact_author_address
;
  Physics Department
  Southern Oregon University
  Ashland, OR 97520
  USA
;
_publ_contact_author_email     'sca@mind.net'
_publ_contact_author_fax     '541 552 6415'
_publ_contact_author_phone     '541 482 7942'
_publ_section_title
;
  Structure-property correlation in Pb₅Al₃F₁₉ and its
  four successive phase transitions
;
loop_
    _publ_author_name
    _publ_author_address
    'Abrahams, S.C.'
;
 Physics Department, Southern Oregon University,
 Ashland, OR 97520, USA
;
    'J. Ravez'
;
 Institut de Chimie de la Matiere Condensee de Bordeaux,
 Av. du Dr A. Schweitzer, F-33608 Pessac, France
;
    'H. Ritter'
;
  Institut fuer Kristallographie der Universitaet Tuebingen,
  Auf der Morgenstelle 10, D-72076 Tuebingen, Germany
;
    'J. Ihringer'
;
  Institut fuer Kristallographie der Universitaet Tuebingen,
  Auf der Morgenstelle 10, D-72076 Tuebingen, Germany
;
data_I
_journal_date_recd_electronic     2002-07-16
_journal_date_accepted     2003-05-23
_journal_name_full     'Acta Crystallographica, Section B'
_journal_year     2003
_journal_volume     59
_journal_issue      5
_journal_page_first     557
_journal_page_last     574
_journal_paper_category     FA
_chemical_name_systematic
;
  pentalead trialuminum nonadecafluoride
;
_chemical_name_common     'lead aluminum fluoride'
_chemical_formula_sum     'Al3 F19 Pb5'
_chemical_formula_structural     'Pb5 Al3 F19'
_chemical_formula_iupac     'Pb5 Al3 F19'
_chemical_formula_weight     1477.94
_symmetry_cell_setting     triclinic
_symmetry_space_group_name_H-M     'I -1'
_symmetry_space_group_name_Hall     '-I 1'
loop_
    _symmetry_equiv_pos_site_id
    _symmetry_equiv_pos_as_xyz
    1 x,y,z
    2 1/2-x,1/2-y,1/2-z
    3 1/2+x,1/2+y,1/2+z
    4 -x,-y,-z
_cell_length_a     14.2624(2)
_cell_length_b     14.2808(2)
_cell_length_c     7.23400(10)
_cell_angle_alpha     90.001(10)
_cell_angle_beta     90.5090(10)
_cell_angle_gamma     90.001(10)
_cell_volume     1473.39(4)
_cell_formula_units_Z     4
_cell_measurement_temperature     320(2)
_exptl_crystal_density_diffrn     6.6630(10)
_exptl_crystal_density_meas     6.66(5)
_exptl_crystal_density_method     'phase IV, by immersion in bromobenzene'
_exptl_crystal_F_000     2480
_exptl_special_details
;
  Pb5 Al3 F19 melts incongruently at 825(5) K, the thermal
  limit of crystalline stability.
;
_refine_special_details
;
  Simultaneous refinement of dataset 1, dataset 2 and
  dataset 3
;
_refine_ls_structure_factor_coef     Inet
_refine_ls_matrix_type     fullcycle
_refine_ls_goodness_of_fit_all     2.300
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_number_constraints     0
_refine_ls_weighting_scheme     sigma
_refine_ls_shift/su_max     0.05
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_thermal_displace_type
    _atom_site_occupancy
    _atom_site_type_symbol
    Pb1 0.2603(2) 0.4174(2) 0.5038(6) 0.0300(10)
                                               Uiso 1.0 Pb
    Pb2 0.4124(5) -0.2633(5) 0.4920(3) 0.027(2) Uiso 1.0 Pb
    Pb3 0.2222(3) -0.0623(3) 0.4967(7) 0.034(2) Uiso 1.0 Pb
    Pb4 0.0610(3) 0.2110(3) 0.5001(5) 0.025(5) Uiso 1.0 Pb
    Pb5 0.0023(5) 0.4772(2) 0.2557(14) 0.0520(10)
                                                Uiso 1.0 Pb
    Al1 0.1519(14) 0.3193(13) -0.010(3) 0.0070(10)
                                                 Uiso 1.0 Al
    Al2 0.6925(13) 0.1735(13) 0.021(3) 0.0070(10)
                                                Uiso 1.0 Al
    Al3 0.0044(17) 0.0128(13) 0.245(3) 0.0070(10)
                                                Uiso 1.0 Al
    F1 0.2878(13) 0.1155(13) 0.681(3) 0.0270(10)
                                               Uiso 1.0 F
    F2 0.6116(16) -0.2637(17) 0.339(3) 0.0270(10)
                                                Uiso 1.0 F
    F3 0.2606(14) 0.6116(14) 0.349(3) 0.0120(10)
                                               Uiso 1.0 F
    F4 -0.2519(14) 0.3867(15) 0.333(2) 0.0120(10)
                                                Uiso 1.0 F
    F5 0.5735(13) 0.2107(13) 0.149(2) 0.0120(10)
                                               Uiso 1.0 F
    F6 0.4092(12) 0.2165(15) 0.305(3) 0.0270(10)
                                               Uiso 1.0 F
    F7 0.1895(13) 0.4066(14) 0.175(3) 0.0270(10)
                                               Uiso 1.0 F
    F8 -0.0912(11) 0.2937(13) 0.687(3) 0.0120(10)
                                                Uiso 1.0 F
    F9 0.0391(13) 0.3871(14) -0.045(2) 0.0270(10)
                                                Uiso 1.0 F
    F10 0.6078(11) 0.0683(10) -0.007(3) 0.0120(10)
                                                 Uiso 1.0 F
    F11 0.2524(15) 0.2458(13) 0.055(2) 0.0270(10)
                                                Uiso 1.0 F
    F12 0.7357(10) 0.2641(11) 0.015(3) 0.0120(10)
                                                Uiso 1.0 F
    F13 0.00000 0.00000 0.50000 0.039(2) Uiso 1.0 F
    F14 0.00000 0.00000 0.00000 0.039(2) Uiso 1.0 F
    F15 0.1171(14) 0.0421(14) 0.254(3) 0.0250(10)
                                                Uiso 1.0 F
    F16 -0.1273(14) -0.0583(14) 0.270(3) 0.0250(10)
                                                  Uiso 1.0 F
    F17 -0.0565(15) 0.1069(16) 0.711(3) 0.0250(10)
                                                 Uiso 1.0 F
    F18 0.0588(14) -0.1055(15) 0.740(3) 0.0250(10)
                                                 Uiso 1.0 F
    F19 0.1284(15) 0.5927(14) 0.037(2) 0.0240(10)
                                                Uiso 1.0 F
    F20 0.5811(13) -0.1257(13) 0.005(3) 0.0240(10)
                                                 Uiso 1.0 F
_geom_special_details
;
 atomic displacements at the phase transition from phase III
 to phase II are < or = 0.33 Å by Pb, < or = 0.37 Å by Al
 and < or = 0.69 Å by F; at the phase transition to phase IV,
 the atomic displacements are < or = 0.53 Å by Pb, < or
 0.49 Å by Al and < or = 0.92 Å by F.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    Al1 F1 2 1.78(3)
    Al1 F2 3_454 1.71(4)
    Al1 F6 2 1.80(3)
    Al1 F7 . 1.90(3)
    Al1 F9 . 1.87(4)
    Al1 F11 . 1.83(4)
    Al2 F3 3_544 1.81(4)
    Al2 F4 2 1.60(4)
    Al2 F5 5 2.01(4)
    Al2 F8 2 2.12(4)
    Al2 F10 . 1.94(3)
    Al2 F12 . 1.43(3)
    Al3 F13 . 1.85(3)
    Al3 F14 . 1.78(3)
    Al3 F15 . 1.66(4)
    Al3 F16 . 2.14(4)
    Al3 F17 4_556 1.89(4)
    Al3 F18 4_556 1.61(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
    F1 Al1 F2 2 3_454 95.0(10)
                            no
    F1 Al1 F6 2 2 164(3) no
    F1 Al1 F7 2 . 91.0(10)
                        no
    F1 Al1 F9 2 . 94.0(10)
                        no
    F1 Al1 F11 2 . 95.0(10)
                         no
    F2 Al1 F6 3_454 2 99.0(10)
                            no
    F2 Al1 F7 3_454 . 175(4) no
    F2 Al1 F9 3_454 . 88.0(10)
                            no
    F2 Al1 F11 3_454 . 91(2) no
    F6 Al1 F7 2 . 75.0(10)
                        no
    F6 Al1 F9 2 . 80.0(10)
                        no
    F6 Al1 F11 2 . 91.0(10)
                         no
    F7 Al1 F9 . . 90.0(10)
                        no
    F7 Al1 F11 . . 89.0(10)
                         no
    F9 Al1 F11 . . 171(2) no
    F3 Al2 F4 3_544 2 85.0(10)
                            no
    F3 Al2 F5 3_544 . 155(2) no
    F3 Al2 F8 3_544 2 89.0(10)
                            no
    F3 Al2 F10 3_544 . 84.0(10)
                             no
    F3 Al2 F12 3_544 . 101.0(10)
                              no
    F4 Al2 F5 2_555 . 106(2) no
    F4 Al2 F8 2 2 165(9) no
    F4 Al2 F10 2_555 . 89.0(10)
                             no
    F4 Al2 F12 2_555 . 106.0(10)
                              no
    F5 Al2 F8 1_555 2_555 72.0(10)
                                no
    F5 Al2 F10 1_555 1_555 74.0(10)
                                 no
    F5 Al2 F12 1_555 1_555 98(2) no
    F8 Al2 F10 2_555 1_555 71.0(10)
                                 no
    F8 Al2 F12 2_555 1_555 94.0(10)
                                 no
    F10 Al2 F12 1_555 1_555 165(2) no
    F13 Al3 F14 1_555 1_555 168(2) no
    F13 Al3 F15 1_555 1_555 92.0(10)
                                  no
    F13 Al3 F16 1_555 1_555 81.0(10)
                                  no
    F13 Al3 F17 1_555 4_556 76.0(10)
                                  no
    F13 Al3 F18 1_555 4_556 89.0(10)
                                  no
    F14 Al3 F15 1_555 1_555 95.0(10)
                                  no
    F14 Al3 F16 1_555 1_555 91.0(10)
                                  no
    F14 Al3 F17 1_555 4_556 95.0(10)
                                  no
    F14 Al3 F18 1_555 4_556 98.0(10)
                                  no
    F15 Al3 F16 1_555 1_555 165(2) no
    F15 Al3 F17 1_555 4_556 81.0(10)
                                  no
    F15 Al3 F18 1_555 4_556 110.0(10)
                                   no
    F16 Al3 F17 1_555 4_556 84.0(10)
                                  no
    F16 Al3 F18 1_555 4_556 84.0(10)
                                  no
    F17 Al3 F18 4_556 4_556 163(2) no
