M3(Au,Ge)19 and M3.25(Au,Ge)18 (M = Ca, Yb): Distinctive Phase Separations Driven by Configurational Disorder in Cubic YCd6-Type Derivatives
Qisheng Lin; John D. Corbett; Inorganic Chemistry 49 (2010) 4570–4577; doi:10.1021/ic100118q

data_4315492
_publ_contact_author_address
;359 Spedding Hall
Iowa State University
Ames, IA, 50010
;
_publ_contact_author_email       jdc@ameslab.gov
_publ_contact_author_name        'John D Corbett'
_publ_section_title
;
 M3(Au,Ge)19 and M3.25(Au,Ge)18 (M = Ca, Yb): Distinctive Phase
 Separations Driven by Configurational Disorder in Cubic YCd6-Type
 Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4570
_journal_page_last               4577
_journal_paper_doi               10.1021/ic100118q
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
'Au108.23 Ge35.77, 0.28(Ge24), 0.05(Au24), 24(Ca), 10.56(Ca0.0)'
_chemical_formula_sum            'Au13.69 Ca3.05 Ge5.31'
_chemical_formula_weight         3204.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           204
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 2 2 3'
_symmetry_space_group_name_H-M   'I m -3'
_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            8
_cell_length_a                   14.764(5)
_cell_length_b                   14.764(5)
_cell_length_c                   14.764(5)
_cell_measurement_reflns_used    743
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      1.95
_cell_volume                     3218.2(19)
_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_measurement_device_type  'Smart CCD APEX II'
_diffrn_measurement_method       w/
_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  0.1930
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14192
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    134.977
_exptl_absorpt_correction_T_max  0.075
_exptl_absorpt_correction_T_min  0.035
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            metallic
_exptl_crystal_density_diffrn    13.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             10501
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.019
_refine_diff_density_max         5.322
_refine_diff_density_min         -4.309
_refine_diff_density_rms         0.853
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0575
_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/[\s^2^(Fo^2^)+(0.0171P)^2^+772.3358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                535
_reflns_number_total             743
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100118q_si_003_3.cif
_cod_data_source_block           CRYSTAL_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'CUBIC' changed to 'cubic' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29.

'_exptl_absorpt_correction_type'
value 'Empirical' changed to 'empirical' according to the built-in
table from CIF Core dictionary named 'cif_core.dic' version 2.4.1
from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3217.9(17)
_cod_database_code               4315492