Copper and Zinc Substitutions in Clathrates of Tin: Synthesis, Structural Characterization, and Physical Properties of A8Cu2.67Sn43.33 and A8Zn4Sn42 (A= K, Rb, Cs) with the Type-I Structure
Schäfer, Marion C.; Bobev, Svilen; Chemistry of Materials 25 (2013) 3737–; doi:10.1021/cm402276n

data_4001824
_publ_section_title
;
 Copper and Zinc Substitutions in Clathrates of Tin: Synthesis, Structural
 Characterization, and Physical Properties
 of A8Cu2.67Sn43.33 and A8Zn4Sn42 (A= K, Rb, Cs) with the Type-I Structure
;
_journal_issue                   18
_journal_name_full               'Chemistry of Materials'
_journal_page_first              3737
_journal_paper_doi               10.1021/cm402276n
_journal_volume                  25
_journal_year                    2013
_chemical_formula_moiety         K8Cu2.77Sn43.23
_chemical_formula_sum            'Cu2.77 K8 Sn43.23'
_chemical_formula_weight         5619.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           223
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 4n 2 3'
_symmetry_space_group_name_H-M   'P m -3 n'
_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                   12.0769(3)
_cell_length_b                   12.0769(3)
_cell_length_c                   12.0769(3)
_cell_measurement_reflns_used    2939
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.20
_cell_measurement_theta_min      3.37
_cell_volume                     1761.43(8)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'XP in SHELXTL'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SMART-APEX II DUO'
_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  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0107
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18924
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    16.287
_exptl_absorpt_correction_T_max  0.5548
_exptl_absorpt_correction_T_min  0.4221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            silver
_exptl_crystal_density_diffrn    5.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2394
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.123
_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   1.157
_refine_ls_matrix_type           full
_refine_ls_number_parameters     21
_refine_ls_number_reflns         341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0155
_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^)+(0.0093P)^2^+10.7243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0319
_refine_ls_wR_factor_ref         0.0325
_reflns_number_gt                318
_reflns_number_total             341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm402276n_si_002.cif
_cod_data_source_block           K8Cu2.77Sn43.23
_cod_original_sg_symbol_H-M      Pm-3n
_cod_database_code               4001824