Crystal Growth through Field-Assisted Electrochemical Redox and Ion-Exchange Reactions: A Case Study of K4.2Na3.8Si46Clathrate-I
Dong, Yongkwan; Nolas, George S.; Crystal Growth & Design 15 (2015) 4731–; doi:10.1021/acs.cgd.5b00329

data_4513624
_publ_section_title
;
 Crystal Growth through Field-Assisted Electrochemical Redox and
 Ion-Exchange Reactions: A Case Study of K4.2Na3.8Si46Clathrate-I
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4731
_journal_paper_doi               10.1021/acs.cgd.5b00329
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'K6 Na2 Si46'
_chemical_formula_weight         1572.72
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           223
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      223
_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                   10.2311(5)
_cell_length_b                   10.2311(5)
_cell_length_c                   10.2311(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1070.94(9)
_computing_cell_refinement       'APEX II (Bruker, 2010)'
_computing_data_collection       'APEX II (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5330
_diffrn_reflns_theta_full        69.23
_diffrn_reflns_theta_max         69.23
_diffrn_reflns_theta_min         6.12
_exptl_absorpt_coefficient_mu    18.236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            bluish
_exptl_crystal_density_diffrn    2.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             780
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_matrix_type           full
_refine_ls_number_parameters     16
_refine_ls_number_reflns         205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0222
_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^)+(0.0331P)^2^+0.0965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0532
_reflns_number_gt                191
_reflns_number_total             205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5b00329_si_003.cif
_cod_data_source_block           K4Na4Si46
_cod_depositor_comments
'Adding full bibliography for 4513624--4513625.cif.'
_cod_original_sg_symbol_H-M      Pm-3n
_cod_database_code               4513624