#------------------------------------------------------------------------------
#$Date: 2018-08-23 01:04:45 +0300 (Thu, 23 Aug 2018) $
#$Revision: 210061 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/33/86/4338655.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4338655
loop_
_publ_author_name
'Lin, Qisheng'
'Corbett, John D.'
_publ_section_title
;
 Centric and Non-centric Ca3Au∼ 7.5Ge∼: Electron-Poor Derivatives
 of La3Al11. Syntheses, Structures, and Bonding Analyses
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5403
_journal_page_last               5411
_journal_paper_doi               10.1021/ic900383d
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'Au14.32 Ge7.68, 6(Ca)'
_chemical_formula_sum            'Au7.16 Ca3 Ge3.84'
_chemical_formula_weight         1809.27
_space_group_IT_number           44
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2'
_symmetry_space_group_name_H-M   'I m m 2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.3987(8)
_cell_length_b                   13.0600(10)
_cell_length_c                   9.6032(9)
_cell_measurement_reflns_used    973
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.64
_cell_volume                     551.68(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1139
_diffrn_reflns_theta_full        28.14
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    106.421
_exptl_absorpt_correction_T_max  0.096
_exptl_absorpt_correction_T_min  0.041
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'slivery metallic'
_exptl_crystal_density_diffrn    10.892
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1497
_exptl_crystal_size_max          0.048
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.022
_refine_diff_density_max         3.931
_refine_diff_density_min         -3.520
_refine_diff_density_rms         0.875
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         537
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0877P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1370
_reflns_number_gt                510
_reflns_number_total             537
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900383d_si_002.cif
_cod_data_source_block           crystal1
_cod_database_code               4338655
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_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
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Au1 Au 0.0000 0.0000 0.5048(3) 0.0231(6) Uani 1 4 d S
Au2 Au 0.0000 0.5000 0.2030(3) 0.0217(8) Uani 1 4 d S
Au3 Au 0.0000 0.5000 0.8156(3) 0.0252(8) Uani 1 4 d S
Au4 Au 0.0000 0.34145(17) 0.6229(2) 0.0227(6) Uani 1 2 d S
Ge5 Ge 0.0000 0.3210(4) 0.3617(5) 0.0181(13) Uani 1 2 d S
Au6 Au 0.0000 0.86666(15) 0.7441(2) 0.0192(5) Uani 1 2 d S
Au7 Au 0.0000 0.8681(4) 0.2797(4) 0.019(2) Uani 0.08(3) 2 d SP
Ge7 Ge 0.0000 0.8681(4) 0.2797(4) 0.019(2) Uani 0.92(3) 2 d SP
Ca1 Ca 0.0000 0.0000 0.000(2) 0.025(3) Uani 1 4 d S
Ca2 Ca 0.0000 0.3090(8) 0.0070(12) 0.022(2) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 '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_distance
_geom_bond_site_symmetry_2
Au1 Ge7 2.764(5) 1_545
Au1 Au7 2.764(5) 1_545
Au1 Ge7 2.764(5) 2_565
Au1 Au7 2.764(5) 2_565
Au1 Au3 2.853(3) 5_444
Au1 Au3 2.853(3) 5_544
Au1 Au6 2.883(3) 2_565
Au1 Au6 2.883(3) 1_545
Au1 Au2 2.908(3) 5_545
Au1 Au2 2.908(3) 5_445
Au1 Ca2 3.325(8) 6
Au1 Ca2 3.325(8) 5_445
Au2 Ge5 2.791(6) 2_565
Au2 Ge5 2.791(5) .
Au2 Au6 2.8330(14) 6_564
Au2 Au6 2.8330(14) 5_444
Au2 Au6 2.8330(14) 5_544
Au2 Au6 2.8330(14) 6_464
Au2 Au1 2.908(3) 5_454
Au2 Au1 2.908(3) 5_554
Au2 Ca2 3.124(12) .
Au2 Ca2 3.124(12) 2_565
Au2 Ca1 3.602(15) 5
Au2 Ca1 3.602(15) 5_455
Au3 Au4 2.777(3) .
Au3 Au4 2.777(3) 2_565
Au3 Ge7 2.815(4) 5_445
Au3 Au7 2.815(4) 5_445
Au3 Ge7 2.815(4) 6_565
Au3 Au7 2.815(4) 6_565
Au3 Ge7 2.815(4) 6_465
Au3 Au7 2.815(4) 6_465
Au3 Au7 2.815(4) 5_545
Au3 Ge7 2.815(4) 5_545
Au3 Au1 2.853(3) 5
Au3 Au1 2.853(3) 5_455
Au4 Ge5 2.522(5) .
Au4 Ge7 2.688(3) 5_545
Au4 Au7 2.688(3) 5_545
Au4 Ge7 2.688(3) 5_445
Au4 Au7 2.688(3) 5_445
Au4 Au6 2.957(3) 2_565
Au4 Ca2 3.152(7) 6_455
Au4 Ca2 3.152(7) 6
Au4 Ca1 3.243(7) 5
Au4 Ca1 3.243(7) 5_455
Au4 Ca2 3.713(12) 1_556
Ge5 Au6 2.543(3) 5_444
Ge5 Au6 2.543(3) 5_544
Ge5 Ge7 2.592(8) 2_565
Ge5 Au7 2.592(8) 2_565
Ge5 Ca2 3.109(9) 6_455
Ge5 Ca2 3.109(9) 6
Ge5 Ca2 3.410(13) .
Ge5 Ca1 3.474(9) 5
Ge5 Ca1 3.474(9) 5_455
Au6 Ge5 2.543(3) 5
Au6 Ge5 2.543(3) 5_455
Au6 Au2 2.8330(14) 5
Au6 Au2 2.8330(14) 5_455
Au6 Au1 2.883(3) 1_565
Au6 Au4 2.957(3) 2_565
Au6 Ca1 3.012(16) 1_566
Au6 Ca2 3.254(9) 5_455
Au6 Ca2 3.254(9) 5
Au6 Ca2 3.412(13) 2_566
Au7 Ge5 2.592(8) 2_565
Au7 Au4 2.688(3) 5_454
Au7 Au4 2.688(3) 5_554
Au7 Au1 2.764(5) 1_565
Au7 Au3 2.815(4) 5_554
Au7 Au3 2.815(4) 5_454
Au7 Ca1 3.191(17) 1_565
Au7 Ca2 3.193(9) 5
Au7 Ca2 3.193(9) 5_455
Au7 Ca2 3.494(12) 2_565
Ca1 Au6 3.012(16) 1_544
Ca1 Au6 3.012(16) 2_564
Ca1 Ge7 3.191(17) 2_565
Ca1 Au7 3.191(17) 2_565
Ca1 Ge7 3.191(17) 1_545
Ca1 Au7 3.191(17) 1_545
Ca1 Au4 3.243(7) 6_554
Ca1 Au4 3.243(7) 5_444
Ca1 Au4 3.243(7) 5_544
Ca1 Au4 3.243(7) 6_454
Ca1 Ge5 3.474(9) 5_444
Ca1 Ge5 3.474(9) 6_554
Ca2 Au3 3.098(10) 1_554
Ca2 Ge5 3.109(9) 6_454
Ca2 Ge5 3.109(9) 6_554
Ca2 Au4 3.152(7) 6_454
Ca2 Au4 3.152(7) 6_554
Ca2 Ge7 3.193(9) 5_444
Ca2 Au7 3.193(9) 5_444
Ca2 Ge7 3.193(9) 5_544
Ca2 Au7 3.193(9) 5_544
Ca2 Au6 3.254(9) 5_544
Ca2 Au6 3.254(9) 5_444
