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_4315496
_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
'Au109.66 Ge32.91, 0.16(Ge24), 0.09(Au16), 0.17(Au24), 24(Ca)'
_chemical_formula_sum            'Au14.39 Ca3 Ge4.61'
_chemical_formula_weight         3289.69
_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                   14.8223(12)
_cell_length_b                   14.8223(12)
_cell_length_c                   14.8223(12)
_cell_measurement_reflns_used    725
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      1.94
_cell_volume                     3256.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_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  0.0890
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10257
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    138.367
_exptl_absorpt_correction_T_max  0.142
_exptl_absorpt_correction_T_min  0.009
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            metallic
_exptl_crystal_density_diffrn    13.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             10756
_exptl_crystal_size_max          0.033
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.015
_refine_diff_density_max         4.085
_refine_diff_density_min         -4.254
_refine_diff_density_rms         0.778
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0686P)^2^+697.8741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                656
_reflns_number_total             725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100118q_si_003_7.cif
_cod_data_source_block           crystal_s2
_cod_database_code               4315496