Interplay between Size and Electronic Effects in Determining the Homogeneity Range of the A9Zn4+xPn9 and A9Cd4+xPn9 Phases (0 <=x<= 0.5), A = Ca, Sr, Yb, Eu; Pn = Sb, Bi
Sheng-qing Xia; Svilen Bobev; Journal of the American Chemical Society 129 (2007) 10011–10018; doi:10.1021/ja0728425

data_4109764
_publ_section_title
;
 Interplay between Size and Electronic Effects in Determining the
 Homogeneity Range of the A9Zn4+xPn9 and A9Cd4+xPn9 Phases (0 <=x<= 0.5),
 A = Ca, Sr, Yb, Eu; Pn = Sb, Bi
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10011
_journal_page_last               10018
_journal_paper_doi               10.1021/ja0728425
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'Bi9 Zn4.03,9(Yb)'
_chemical_formula_sum            'Bi9 Yb9 Zn4.03'
_chemical_formula_weight         3701.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           55
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2ab'
_symmetry_space_group_name_H-M   'P b a 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            2
_cell_length_a                   21.997(3)
_cell_length_b                   12.5243(14)
_cell_length_c                   4.6283(5)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      1.85
_cell_volume                     1275.1(3)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL 5.1 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart'
_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  0.0758
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            9832
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    98.139
_exptl_absorpt_correction_T_max  0.1106
_exptl_absorpt_correction_T_min  0.0668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    9.640
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2994
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.544
_refine_diff_density_min         -2.816
_refine_diff_density_rms         0.712
_refine_ls_extinction_coef       0.00061(4)
_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   1.091
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0413P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                1316
_reflns_number_total             1573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0728425si20070503_025634_6.cif
_cod_data_source_block           Yb9Zn4.03(2)Bi9_/_CSD-417977
_cod_original_cell_volume        1275.1(2)
_cod_database_code               4109764