#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2007030.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_2007030
loop_
_publ_author_name
'Flot, D.'
'Vincent, L.'
'Tillard-Charbonnel, M.'
'Belin, C.'
_publ_section_title
;
 Na~13~K~4~Ga~47.45~: a New Sodium Potassium Gallide Phase Containing
 Trimeric Icosahedral Gallium Clusters
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              174
_journal_page_last               175
_journal_volume                  54
_journal_year                    1998
_chemical_formula_sum            'Ga47.45 K4 Na13'
_chemical_formula_weight         3763.48
_chemical_name_systematic
;
 Sodium potassium gallium intermetallic compound
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_audit_creation_method           'SHELXL 93'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   16.325(3)
_cell_length_b                   16.325(3)
_cell_length_c                   35.135(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.79
_cell_measurement_theta_min      13.08
_cell_volume                     8109(2)
_computing_cell_refinement       'CAD4 Software'
_computing_data_collection       'CAD4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'local program'
_computing_molecular_graphics    'ATOMS (Dowty, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       \w--2/3\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3335
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    23.593
_exptl_absorpt_correction_T_max  0.210
_exptl_absorpt_correction_T_min  0.083
_exptl_absorpt_correction_type   'numerical (SHELX76; Sheldrick, 1976)'
_exptl_crystal_colour            'metallic luster'
_exptl_crystal_density_diffrn    4.624
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       wedge-shaped
_exptl_crystal_F_000             10140
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         3.043
_refine_diff_density_min         -2.593
_refine_ls_extinction_coef       0.000015(12)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.071
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_obs          0.0536
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0760P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.1376
_refine_ls_wR_factor_obs         0.1355
_reflns_number_observed          1026
_reflns_number_total             1328
_reflns_observed_criterion       I>2sigma(I)
_[local]_cod_data_source_file    oh1104.cif
_[local]_cod_data_source_block   I
_[local]_cod_cif_authors_sg_H-M  'R -3m'
_[local]_cod_chemical_formula_sum_orig 'Na13 K4 Ga47.45'
_cod_original_cell_volume        8110.(2)
_cod_database_code               2007030
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'-x, -x+y, -z'
'x-y, -y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'x, x-y, z'
'-x+y, y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
loop_
_atom_site_aniso_label
_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
Ga1 0.028(2) 0.035(2) 0.0193(13) 0.0146(15) 0.0018(13) 0.0027(13)
Ga2 0.0156(14) 0.0204(15) 0.0043(10) 0.0119(12) 0.0002(10) 0.0020(10)
Ga3 0.0166(14) 0.0129(14) 0.0124(10) 0.0085(12) 0.0057(11) 0.0021(10)
Ga4 0.013(2) 0.033(2) 0.011(2) 0.011(2) -0.0016(14) -0.0097(15)
Ga5 0.0092(13) 0.0092 0.0044(13) 0.003(2) 0.0002 -0.0002(7)
Ga6 0.0139(14) 0.0139 0.0046(14) 0.004(2) 0.0010 -0.0010(7)
Ga7 0.0135(14) 0.0135 0.0059(14) 0.004(2) -0.0002 0.0002(7)
Ga8 0.0111(14) 0.0111 0.0035(13) 0.006(2) 0.0009 -0.0009(7)
Ga9 0.0147(14) 0.0147 0.0056(14) 0.008(2) 0.0002 -0.0002(7)
Ga10 0.021(2) 0.021 0.0044(14) 0.016(2) 0.0004 -0.0004(7)
Ga11 0.0121(14) 0.0121 0.020(2) 0.004(2) -0.0035 0.0035(8)
Ga12 0.023(3) 0.023 0.013(2) 0.012(3) 0.0001 -0.0001(11)
Ga13 0.021(10) 0.021 0.013(10) -0.004(11) 0.011 -0.011(5)
Ga14 0.018(2) 0.018 0.013(3) 0.009 0.000 0.000
K1 0.039(4) 0.039 0.021(3) 0.023(5) 0.003 -0.003(2)
K2 0.024(5) 0.024 0.012(5) 0.012 0.000 0.000
Na1 0.045(7) 0.037(7) 0.022(4) 0.031(6) 0.005(5) 0.003(5)
Na2 0.047(7) 0.047 0.006(5) 0.020(9) -0.005 0.005(3)
Na3 0.019(6) 0.019 0.028(7) -0.001(7) 0.003 -0.003(4)
Na4 0.034(10) 0.034 0.028(13) 0.017 0.000 0.000
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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Ga1 0.5061(2) -0.1597(2) 0.48931(7) 0.0277(8) Uani d . 1 Ga
Ga2 0.6427(2) 0.0109(2) 0.46327(5) 0.0122(6) Uani d . 1 Ga
Ga3 0.2088(2) -0.0420(2) 0.57667(6) 0.0134(6) Uani d . 1 Ga
Ga4 0.6977(2) 0.1188(3) 0.68096(8) 0.0196(12) Uani d P 0.769(9) Ga
Ga5 0.61187(12) -0.61187(12) 0.39123(8) 0.0082(8) Uani d S 1 Ga
Ga6 0.55499(13) -0.55499(13) 0.44954(8) 0.0119(8) Uani d S 1 Ga
Ga7 0.54023(13) -0.54023(13) 0.56573(8) 0.0123(8) Uani d S 1 Ga
Ga8 0.24484(12) -0.24484(12) 0.65285(8) 0.0084(8) Uani d S 1 Ga
Ga9 0.56951(13) -0.56951(13) 0.63631(8) 0.0113(8) Uani d S 1 Ga
Ga10 0.51045(13) -0.51045(13) 0.69493(8) 0.0135(9) Uani d S 1 Ga
Ga11 0.08594(14) -0.08594(14) 0.40519(9) 0.0154(8) Uani d S 1 Ga
Ga12 -0.0538(2) 0.0538(2) 0.66931(12) 0.020(2) Uani d SP 0.758(13) Ga
Ga13 0.0515(9) -0.0515(9) 0.5496(5) 0.025(8) Uani d SP 0.188(13) Ga
Ga14 0.0000 0.0000 0.6098(2) 0.0161(15) Uani d S 1 Ga
K1 0.1289(3) -0.1289(3) 0.2586(2) 0.031(2) Uani d S 1 K
K2 0.0000 0.0000 0.7602(3) 0.020(3) Uani d S 1 K
Na1 0.4126(8) 0.0362(8) 0.3783(2) 0.030(3) Uani d . 1 Na
Na2 0.1327(6) -0.1327(6) 0.4905(3) 0.035(4) Uani d S 1 Na
Na3 0.8872(5) -0.8872(5) 0.8977(4) 0.027(3) Uani d S 1 Na
Na4 0.0000 0.0000 0.8606(7) 0.032(7) Uani d S 1 Na
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
Ga1 Ga7 20_666 2.639(4) yes
Ga1 Ga6 20_666 2.661(4) yes
Ga1 Ga2 . 2.712(4) yes
Ga1 Ga1 24_655 2.807(6) yes
Ga1 Ga2 6_556 2.811(4) yes
Ga1 Ga1 23_545 2.848(6) yes
Ga2 Ga2 6_556 2.599(4) yes
Ga2 Ga3 19_656 2.621(3) yes
Ga2 Ga6 2_545 2.686(3) yes
Ga2 Ga7 20_666 2.780(3) yes
Ga3 Ga11 21_556 2.528(3) yes
Ga3 Ga13 . 2.67(2) yes
Ga3 Ga10 25_546 2.705(3) yes
Ga3 Ga3 22 2.723(5) yes
Ga3 Ga4 27_446 2.854(4) yes
Ga4 Ga12 25_556 2.531(6) yes
Ga4 Ga4 10_546 2.676(7) yes
Ga4 Ga10 2_545 2.694(4) yes
Ga4 Ga11 7 2.724(4) yes
Ga4 Ga9 2_545 2.765(4) yes
Ga4 Ga4 22_665 2.995(7) yes
Ga5 Ga6 . 2.605(5) yes
Ga5 Ga8 21_546 2.680(3) yes
Ga5 Ga5 3_755 2.684(6) yes
Ga5 Ga8 13_544 2.694(4) yes
Ga6 Ga7 19_646 2.745(5) yes
Ga7 Ga9 . 2.614(4) yes
Ga7 Ga2 21_546 2.780(3) yes
Ga8 Ga10 25_546 2.557(5) yes
Ga8 Ga5 20_666 2.680(3) yes
Ga8 Ga8 26_556 2.684(4) yes
Ga8 Ga5 7_455 2.694(4) yes
Ga9 Ga12 26_546 2.575(3) yes
Ga9 Ga10 . 2.652(5) yes
Ga11 Ga14 19_556 2.486(4) yes
Ga11 Ga13 20_556 2.647(10) yes
Ga11 Ga12 19_556 2.771(5) yes
Ga12 Ga14 . 2.586(7) yes
Ga12 Ga12 3 2.633(9) yes
Ga13 Ga13 3 2.52(4) yes
Ga13 Ga14 . 2.57(2) yes