Multiple Nonstoichiometric Phases with Discrete Composition Ranges in the CaAu5-CaAu4Bi-BiAu2 System. A Case Study of the Chemistry of Spinodal Decomposition
Qisheng Lin; John D. Corbett; Journal of the American Chemical Society 132 (2010) 5662–5671; doi:10.1021/ja100250d

data_4102302
_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
;
 Multiple Nonstoichiometric Phases with Discrete Composition Ranges in the
 CaAu5-CaAu4Bi-BiAu2 System. A Case Study of the Chemistry of Spinodal
 Decomposition
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5662
_journal_page_last               5671
_journal_paper_doi               10.1021/ja100250d
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'Bi4.78, 16(Au), 77.18(Ca0.04)'
_chemical_formula_sum            'Au16 Bi4.78 Ca3.22'
_chemical_formula_weight         4280.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           216
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'F -4 2 3'
_symmetry_space_group_name_H-M   'F -4 3 m'
_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            1
_cell_length_a                   7.9046(2)
_cell_length_b                   7.9046(2)
_cell_length_c                   7.9046(2)
_cell_measurement_reflns_used    775
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      4.47
_cell_volume                     493.90(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SMART APEX CCD'
_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  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            775
_diffrn_reflns_theta_full        27.85
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         4.47
_exptl_absorpt_coefficient_mu    162.421
_exptl_absorpt_correction_T_max  0.094
_exptl_absorpt_correction_T_min  0.018
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            metallic
_exptl_crystal_density_diffrn    14.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.898
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.438
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(14)
_refine_ls_extinction_coef       0.00051(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         88
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0169
_refine_ls_R_factor_gt           0.0169
_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^)+(0.0130P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0383
_refine_ls_wR_factor_ref         0.0383
_reflns_number_gt                87
_reflns_number_total             88
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja100250d_si_002_4.cif
_cod_data_source_block           crystal_4
_cod_database_code               4102302