Time-of-flight neutron powder diffraction with milligram samples: the crystal structures of NaCoF~3~ and NaNiF~3~ post-perovskites
Lindsay-Scott, Alex; Dobson, David; Nestola, Fabrizio; Alvaro, Matteo; Casati, Nicola; Liebske, Christian; Knight, Kevin S.; Smith, Ronald I.; Wood, Ian G.; Journal of Applied Crystallography 47 (2014) 1939–1947; doi:10.1107/S1600576714021803

data_2300484
_publ_section_title
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 Time-of-flight neutron powder diffraction with milligram samples: the
 crystal structures of NaCoF~3~ and NaNiF~3~ post-perovskites
;
_journal_coeditor_code           ks5440
_journal_issue                   6
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              1939
_journal_page_last               1947
_journal_paper_doi               10.1107/S1600576714021803
_journal_volume                  47
_journal_year                    2014
_chemical_formula_sum            'F3 Na Ni'
_chemical_formula_weight         138.70
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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            4
_cell_length_a                   3.0294(4)
_cell_length_b                   10.0534(12)
_cell_length_c                   7.3938(7)
_cell_measurement_temperature    293(2)
_cell_volume                     225.18(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.788
_diffrn_measured_fraction_theta_max 0.788
_diffrn_radiation_monochromator  'double-bounce silicon (1 1 1) plus mirrors'
_diffrn_radiation_source         'ID15 Diamond synchrotron'
_diffrn_radiation_type           X-ray
_diffrn_radiation_wavelength     0.20675
_diffrn_reflns_av_R_equivalents  0.1107
_diffrn_reflns_av_sigmaI/netI    0.0780
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3527
_diffrn_reflns_theta_full        13.95
_diffrn_reflns_theta_max         13.95
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    4.481
_exptl_crystal_density_diffrn    4.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             264
_refine_diff_density_max         2.338
_refine_diff_density_min         -2.934
_refine_diff_density_rms         0.487
_refine_ls_extinction_coef       0.00(7)
_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   1.057
_refine_ls_matrix_type           full
_refine_ls_number_parameters     20
_refine_ls_number_reflns         680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          1.014
_refine_ls_shift/su_mean         0.051
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0915P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1900
_reflns_number_gt                438
_reflns_number_total             680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ks5440sup6.cif
_cod_data_source_block           nanif3_anisotropic_synchrotron_Diamond
_cod_depositor_comments
;Adding full bibliography for 2300484.cif.

 Adding Fobs data.

 Adding a comment to the HKL file concerning the change of
 _cod_data_source_block value.
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_cod_database_code               2300484
_cod_database_fobs_code          2300484