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_4501133
_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_moiety         'K Si6'
_chemical_formula_sum            'K7.46 Si46'
_chemical_formula_weight         1604.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           223
_symmetry_cell_setting           'P m -3 n'
_symmetry_space_group_name_Hall  '-P 4n 2 3'
_symmetry_space_group_name_H-M   'P m -3 n'
_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                   10.2639(3)
_cell_length_b                   10.2639(3)
_cell_length_c                   10.2639(3)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      32.2852
_cell_measurement_theta_min      2.8066
_cell_volume                     1081.28(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  '\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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0069
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14545
_diffrn_reflns_theta_full        32.29
_diffrn_reflns_theta_max         32.29
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    2.096
_exptl_crystal_colour            gray
_exptl_crystal_density_diffrn    2.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     16
_refine_ls_number_reflns         377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0131
_refine_ls_R_factor_gt           0.0129
_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^)+(0.0128P)^2^+0.6934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0337
_refine_ls_wR_factor_ref         0.0338
_reflns_number_gt                369
_reflns_number_total             377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200756r_si_002.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      '-P 4~n~ 2 3'
_cod_database_code               4501133