Structure refinement of the δ~1<i>p~</i> phase in the Fe‒Zn system by single-crystal X-ray diffraction combined with scanning transmission electron microscopy
Okamoto, Norihiko L.; Tanaka, Katsushi; Yasuhara, Akira; Inui, Haruyuki; Acta Crystallographica Section B 70 (2014) 275–282; doi:10.1107/S2052520613034410

data_2105806
_publ_section_title
;
 Structure refinement of the \d~1<i>p~</i> phase in the Fe--Zn system by
 single-crystal X-ray diffraction combined with scanning transmission
 electron microscopy
;
_journal_coeditor_code           DK5020
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              275
_journal_page_last               282
_journal_paper_doi               10.1107/S2052520613034410
_journal_volume                  70
_journal_year                    2014
_chemical_formula_sum            'Fe13 Zn126'
_chemical_formula_weight         8963.89
_space_group_IT_number           194
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_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                120.00
_cell_formula_units_Z            4
_cell_length_a                   12.8297(2)
_cell_length_b                   12.8297(2)
_cell_length_c                   57.2860(10)
_cell_measurement_reflns_used    301081
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      23.215
_cell_measurement_theta_min      0.355
_cell_volume                     8166.1(2)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction
'CrystalClear (Rigaku/MSC Inc., 2006), SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'HUBER 4-circle diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  'Si(111) double crystal'
_diffrn_radiation_source         'SPring-8 BL02B1'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.35450
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0091
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       127
_diffrn_reflns_limit_l_min       -99
_diffrn_reflns_number            203263
_diffrn_reflns_theta_full        23.19
_diffrn_reflns_theta_max         23.19
_diffrn_reflns_theta_min         0.35
_exptl_absorpt_coefficient_mu    20.094
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            metallic_silver
_exptl_crystal_density_diffrn    7.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             16472
_exptl_crystal_size_max          0.034
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.025
_refine_diff_density_max         5.906
_refine_diff_density_min         -4.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         16996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                14411
_reflns_number_total             16996
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            dk5020sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        8166.0(3)
_cod_database_code               2105806