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_4302372
_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         'Au14.86 Ge7.14, 6(Ca)'
_chemical_formula_sum            'Au7.43 Ca3 Ge3.57'
_chemical_formula_weight         1842.85
_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                   4.4154(6)
_cell_length_b                   13.100(2)
_cell_length_c                   9.5770(10)
_cell_measurement_reflns_used    731
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      2.64
_cell_volume                     553.95(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1738
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    108.823
_exptl_absorpt_correction_T_max  0.0658
_exptl_absorpt_correction_T_min  0.0104
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'silvery metallic'
_exptl_crystal_density_diffrn    11.048
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1522
_exptl_crystal_size_max          0.042
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.816
_refine_diff_density_min         -2.627
_refine_diff_density_rms         0.603
_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_coef       0.00045(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   1.074
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         641
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                604
_reflns_number_total             641
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4338656
_cod_data_source_file            ic900383d_si_002_2.cif
_cod_data_source_block           crystal2
_cod_database_code               4302372