Electron-Precise/Deficient La5-xCaxGe4 (3.4 <= x <= 3.8) and Ce5-xCaxGe4 (3.0 <= x <= 3.3): Probing Low-Valence Electron Concentrations in Metal-Rich Gd5Si4- type Germanides
Li-Ming Wu; Sang-Hwan Kim; Dong-Kyun Seo; Journal of the American Chemical Society 127 (2005) 15682–15683; doi:10.1021/ja055568s

data_4112072
_publ_section_title
;
 Electron-Precise/Deficient La5-xCaxGe4 (3.4 <= x <= 3.8) and Ce5-xCaxGe4
 (3.0 <= x <= 3.3): Probing Low-Valence Electron Concentrations in
 Metal-Rich Gd5Si4- type Germanides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15682
_journal_page_last               15683
_journal_paper_doi               10.1021/ja055568s
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'Ca1.74 Ce3.26 Ge4'
_chemical_formula_weight         816.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_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            4
_cell_length_a                   7.6358(6)
_cell_length_b                   15.4222(11)
_cell_length_c                   8.0475(6)
_cell_measurement_temperature    293(2)
_cell_volume                     947.68(12)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5559
_diffrn_reflns_theta_full        22.52
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    28.676
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Silver
_exptl_crystal_density_diffrn    5.725
_exptl_crystal_description       Block
_exptl_crystal_F_000             1407
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.341
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         651
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.339
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0207
_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^)+(0.0000P)^2^+3.6812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0425
_reflns_number_gt                638
_reflns_number_total             651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja055568ssi20050811_094635.cif
_cod_data_source_block           sad
_cod_database_code               4112072