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_4109765
_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 Zn4.09, 9(Ca)'
_chemical_formula_sum            'Bi9 Ca9 Zn4.09'
_chemical_formula_weight         2508.90
_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                   22.0688(16)
_cell_length_b                   12.5898(6)
_cell_length_c                   4.6336(4)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      1.9
_cell_volume                     1287.41(16)
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_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            13717
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    66.766
_exptl_absorpt_correction_T_max  0.1754
_exptl_absorpt_correction_T_min  0.0756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    6.472
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2099
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.031
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.247
_refine_ls_extinction_coef       0.00028(2)
_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   1.218
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.218
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0174
_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^)+(0.0152P)^2^+5.8547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0397
_reflns_number_gt                1525
_reflns_number_total             1592
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0728425si20070503_025634_7.cif
_cod_data_source_block           Ca9Zn4.10(1)Bi9_/_CSD-417978
_cod_database_code               4109765