Synthesis and Structural Characterization of Single-Crystal K7.5Si46and K17.8Si136Clathrates
Stefanoski, Stevce; Nolas, George S.; Crystal Growth & Design 11 (2011) 4533–; doi:10.1021/cg200756r

data_4501132
_publ_section_title
;
 Synthesis and Structural Characterization of Single-Crystal K7.5Si46and
 K17.8Si136Clathrates
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4533
_journal_paper_doi               10.1021/cg200756r
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'K17.7 Si136'
_chemical_formula_weight         4758.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           227
_symmetry_cell_setting           'F d -3 m'
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_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                   14.7264(6)
_cell_length_b                   14.7264(6)
_cell_length_c                   14.7264(6)
_cell_measurement_reflns_used    729
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      31.5186
_cell_measurement_theta_min      2.3954
_cell_volume                     3193.7(2)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Saint-plus
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker, X8 Apex II'
_diffrn_measurement_method       '\w scann'
_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  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            3257
_diffrn_reflns_theta_full        32.36
_diffrn_reflns_theta_max         32.36
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    2.109
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS, Sheldrick, 2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pyramidal
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.00039(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   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     17
_refine_ls_number_reflns         309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0220
_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^)+(0.0293P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0563
_reflns_number_gt                255
_reflns_number_total             309
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200756r_si_001.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      '-F 4~vw~ 2~vw~ 3'
_cod_database_code               4501132