Crystal structure refinements of stoichiometric Ni~3~Se~2~ and NiSe
Unoki, Kohei; Yoshiasa, Akira; Kitahara, Ginga; Nishiayama, Tadao; Tokuda, Makoto; Sugiyama, Kazumasa; Nakatsuka, Akihiko; Acta Crystallographica Section C 77 (2021) 169–175; doi:10.1107/S2053229621002187

data_2022342
_publ_section_title
;
 Crystal structure refinements of stoichiometric Ni~3~Se~2~ and NiSe
;
_journal_coeditor_code           EP3012
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              169
_journal_page_last               175
_journal_paper_doi               10.1107/S2053229621002187
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'Ni3 Se2'
_chemical_formula_moiety         'Ni3 Se2'
_chemical_formula_sum            'Ni3 Se2'
_chemical_formula_weight         334.05
_chemical_name_systematic
;
Trinickel diselenide
;
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   6.02813(13)
_cell_length_b                   6.02813(13)
_cell_length_c                   7.24883(16)
_cell_measurement_reflns_used    5172
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1360
_cell_measurement_theta_min      4.7840
_cell_volume                     228.120(9)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
<i>VESTA</i> (Momma & Izumi, 2011)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009) and
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Rigaku SuperNova Single Source diffractometer with a HyPix3000 detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0090
_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       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5554
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.978
_diffrn_reflns_theta_min         4.812
_exptl_absorpt_coefficient_mu    41.991
_exptl_absorpt_correction_T_max  0.135
_exptl_absorpt_correction_T_min  0.056
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2019)
;
_exptl_crystal_colour            silver
_exptl_crystal_density_diffrn    7.295
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.077
_refine_diff_density_max         1.148
_refine_diff_density_min         -1.588
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 42 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.049(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.370
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.370
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+1.1728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0517
_reflns_number_gt                117
_reflns_number_total             117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ep3012sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 2022342--2022343.cif.'
_cod_original_cell_volume        228.120(11)
_cod_database_code               2022342
_cod_database_fobs_code          2022342
_shelx_hkl_checksum              2604
_shelx_res_checksum              36408