Centric and Non-centric Ca3Au∼7.5Ge\σim: Electron-Poor Derivatives of La3Al11. Syntheses, Structures, and Bonding Analyses
Lin, Qisheng; Corbett, John D.; Inorganic Chemistry 48 (2009) 5403–5411; doi:10.1021/ic900383d

data_4338655
_publ_section_title
;
 Centric and Non-centric Ca3Au\\sim 7.5Ge\\sim: 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/[\s^2^(Fo^2^)+(0.0877P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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