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_1543252
_publ_section_title
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 Synthesis and Structural Characterization of the New Clathrates
 K8Cd4Ge42, Rb8Cd4Ge42, and Cs8Cd4Ge42
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_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            'Cd4 Cs8 Ge42'
_chemical_formula_weight         4561.66
_chemical_name_systematic
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 ? 
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_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                   10.9643(7)
_cell_length_b                   10.9643(7)
_cell_length_c                   10.9643(7)
_cell_measurement_reflns_used    1629
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.89
_cell_measurement_theta_min      6.45
_cell_volume                     1318.08(15)
_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  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0141
_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            16830
_diffrn_reflns_theta_full        28.45
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    30.538
_exptl_absorpt_correction_T_max  0.4323
_exptl_absorpt_correction_T_min  0.2944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.885
_refine_diff_density_min         -4.017
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       0.00029(8)
_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   1.176
_refine_ls_matrix_type           full
_refine_ls_number_parameters     16
_refine_ls_number_reflns         327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0205
_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^)+(0.0204P)^2^+13.1876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0539
_reflns_number_gt                284
_reflns_number_total             327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Cs8Cd4Ge42_fixed.cif
_cod_data_source_block           Cs8Cd4Ge42_fixed
_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_database_code               1543252