Synthesis and Structural Characterization of the New Clathrates K8Cd4Ge42, Rb8Cd4Ge42, and Cs8Cd4Ge42
Schäfer, Marion; Bobev, Svilen; Materials 9 (2016) 236–; doi:10.3390/ma9040236

data_1543250
_publ_section_title
;
 Synthesis and Structural Characterization of the New Clathrates
 K8Cd4Ge42, Rb8Cd4Ge42, and Cs8Cd4Ge42
;
_journal_issue                   4
_journal_name_full               Materials
_journal_page_first              236
_journal_paper_doi               10.3390/ma9040236
_journal_volume                  9
_journal_year                    2016
_chemical_formula_sum            'Cd3.8 Ge42.2 K8'
_chemical_formula_weight         3803.22
_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                   10.8710(4)
_cell_length_b                   10.8710(4)
_cell_length_c                   10.8710(4)
_cell_measurement_reflns_used    943
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      19.67
_cell_measurement_theta_min      4.19
_cell_volume                     1284.72(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1020
_diffrn_reflns_av_sigmaI/netI    0.0178
_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            15158
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    26.428
_exptl_absorpt_correction_T_max  0.2784
_exptl_absorpt_correction_T_min  0.2293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.916
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1685
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.00058(10)
_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   1.156
_refine_ls_matrix_type           full
_refine_ls_number_parameters     17
_refine_ls_number_reflns         291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0182
_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^)+(0.0127P)^2^+3.3180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0359
_refine_ls_wR_factor_ref         0.0378
_reflns_number_gt                254
_reflns_number_total             291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            K8Cd4Ge42.cif
_cod_data_source_block           K8Cd4Ge42
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to
/usr/data/users/saulius/crontab/automatic-downloads/current/MDPI/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      Pm-3n
_cod_original_formula_sum        'Cd3.80 Ge42.20 K8'
_cod_database_code               1543250