Probing the Limits of the Zintl Concept: Structure and Bonding in Rare-Earth and Alkaline-Earth Zinc-Antimonides Yb9Zn4+xSb9 and Ca9Zn4.5Sb9
Svilen Bobev; Joe D. Thompson; John L. Sarrao; Marilyn M. Olmstead; Håkon Hope; Susan M. Kauzlarich; Inorganic Chemistry 43 (2004) 5044–5052; doi:10.1021/ic049836j

data_4311461
_publ_contact_author
;
Dr. Svilen Bobev
LANSCE-12   Mail Stop H805
Los Alamos National Laboratory
Los Alamos, NM 87545
Phone: (505) 665-7272
Fax: (505) 665-2676
e-mail: sbobev@lanl.gov
USA
;
_publ_section_title
;
 Probing the Limits of the Zintl Concept: Structure and Bonding in
 Rare-Earth and Alkaline-Earth Zinc-Antimonides Yb9Zn4+xSb9 and
 Ca9Zn4.5Sb9
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5044
_journal_page_last               5052
_journal_paper_doi               10.1021/ic049836j
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         Ca18Zn8.96Sb18
_chemical_formula_sum            'Ca18 Sb18 Zn8.96'
_chemical_formula_weight         3498.75
_chemical_melting_point          ?
_chemical_name_common            Ca18Zn8.96Sb18
_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_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            1
_cell_length_a                   21.830(1)
_cell_length_b                   12.4476(9)
_cell_length_c                   4.5414(3)
_cell_measurement_reflns_used    2224
_cell_measurement_temperature    90(3)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      1.9
_cell_volume                     1234.04(13)
_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      90(3)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker Smart 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            11188
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    15.791
_exptl_absorpt_correction_T_max  0.5712
_exptl_absorpt_correction_T_min  0.3653
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            dark-metallic
_exptl_crystal_density_diffrn    4.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1546.7
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.980
_refine_diff_density_min         -2.416
_refine_diff_density_rms         0.419
_refine_ls_extinction_coef       0.00024(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   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         2224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0216P)^2^+3.7788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                1644
_reflns_number_total             2224
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049836jsi20040209_113236_4.cif
_cod_data_source_block           Ca18Zn8.96(2)Sb18
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        1234.1(1)
_cod_database_code               4311461