Tetrahedral Framework Structures: Polymorphic Phase Transition with Reorientation of Hexagonal Helical Channels in the Zintl Compound Na~2~ZnSn~5~ and its Relation to Na~5~Zn~2+<i>x</i>~Sn~10-<i>x</i>~
Saskia Stegmaier; Sung-Jin Kim; Alexander Henze; Thomas F. Fässler; Journal of the American Chemical Society 135 (2013) 10654–10663; doi:10.1021/ja401043b

data_4120135
_publ_contact_author_address
;Department Chemie
Technische Universit\"at M\"unchen
Lichtenbergstr. 4
85747 Garching
Germany
;
_publ_contact_author_email       thomas.faessler@lrz.tu-muenchen.de
_publ_contact_author_fax         '+49 89 28913186'
_publ_contact_author_name        'Prof. Dr. Thomas F. F\"assler'
_publ_contact_author_phone       '+49 89 28913134'
_publ_section_title
;
 Tetrahedral Framework Structures: Polymorphic Phase Transition with
 Reorientation of Hexagonal Helical Channels in the Zintl Compound
 Na~2~ZnSn~5~ and its Relation to Na~5~Zn~2+<i>x</i>~Sn~10-<i>x</i>~
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10654
_journal_page_last               10663
_journal_paper_doi               10.1021/ja401043b
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'Na2 Sn5 Zn'
_chemical_formula_weight         704.80
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      122
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL-97 cif-file'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.3360(10)
_cell_length_b                   6.3360(10)
_cell_length_c                   22.3820(10)
_cell_measurement_temperature    298
_cell_volume                     898.5(2)
_computing_cell_refinement
;
WinXPOW (Version 2.08), STOE & Cie GmbH, Darmstadt, 2003.
FullProf Suite, Rodriguez-Carvajal, J.
FullProf.2k (Version 4.80), Rodriguez-Carvajal, J., 2010.
WinPLOTR, T. Roisnel; Rodriguez-Carvajal, J., 2010.
;
_computing_data_collection
;CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       '\w and \j scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            2919
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    16.312
_exptl_absorpt_correction_T_max  0.1463
_exptl_absorpt_correction_T_min  0.1069
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'STOE X-RED (crystal shape optimized with STOE X-SHAPE)'
_exptl_crystal_colour            silvery
_exptl_crystal_density_diffrn    5.210
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1208
_refine_diff_density_max         1.963
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.440
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         449
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                379
_reflns_number_total             449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja401043b_si_003.cif
_cod_data_source_block           tI-Na2ZnSn5
_cod_database_code               4120135