Four Polyanionic Compounds in the K-Au-Ga System: A Case Study in Exploratory Synthesis and of the Art of Structural Analysis
Volodymyr Smetana; John D. Corbett; Gordon J. Miller; Inorganic Chemistry 51 (2012) 1695–1702; doi:10.1021/ic201999u

data_4328188
_publ_section_title
;
 Four Polyanionic Compounds in the K-Au-Ga System: A Case Study in
 Exploratory Synthesis and of the Art of Structural Analysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1695
_journal_page_last               1702
_journal_paper_doi               10.1021/ic201999u
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'Au0.34 Ga2.66 K'
_chemical_formula_weight         290.89
_space_group_IT_number           119
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 -2'
_symmetry_space_group_name_H-M   'I -4 m 2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2011-07-06 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   6.0900(9)
_cell_length_b                   6.0900(9)
_cell_length_c                   15.450(3)
_cell_measurement_temperature    293(2)
_cell_volume                     573.01(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            1827
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    32.320
_exptl_absorpt_correction_T_max  0
_exptl_absorpt_correction_T_min  0
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    5.058
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(5)
_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   1.022
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          2.235
_refine_ls_shift/su_mean         0.090
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0178P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                390
_reflns_number_total             417
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201999u_si_001_4.cif
_cod_data_source_block           KAuxGa3-x
_cod_original_cell_volume        573.01(17)
_cod_database_code               4328188