#------------------------------------------------------------------------------
#$Date: 2021-03-10 07:54:43 +0200 (Wed, 10 Mar 2021) $
#$Revision: 262962 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022343.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2022343
loop_
_publ_author_name
'Unoki, Kohei'
'Yoshiasa, Akira'
'Kitahara, Ginga'
'Nishiayama, Tadao'
'Tokuda, Makoto'
'Sugiyama, Kazumasa'
'Nakatsuka, Akihiko'
_publ_section_title
;
Crystal structure refinements of stoichiometric Ni3Se2 and NiSe
;
_journal_coeditor_code EP3012
_journal_issue 4
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi 10.1107/S2053229621002187
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac 'Ni Se'
_chemical_formula_moiety 'Ni Se'
_chemical_formula_sum 'Ni Se'
_chemical_formula_weight 137.67
_chemical_name_systematic
;
Nickel selenide
;
_space_group_IT_number 194
_space_group_name_Hall '-P 6c 2c'
_space_group_name_H-M_alt 'P 63/m m c'
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall '-P 6c 2c'
_symmetry_space_group_name_H-M 'P 63/m m c'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 2
_cell_length_a 3.66147(10)
_cell_length_b 3.66147(10)
_cell_length_c 5.35766(16)
_cell_measurement_reflns_used 2443
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 39.7390
_cell_measurement_theta_min 3.7540
_cell_volume 62.204(3)
_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
;
VESTA (Momma & Izumi, 2011)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
OLEX2 (Dolomanov et al., 2009) and
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.968
_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 0.0538
_diffrn_reflns_av_sigmaI/netI 0.0406
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 2898
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 39.7390
_diffrn_reflns_theta_min 3.7540
_exptl_absorpt_coefficient_mu 43.984
_exptl_absorpt_correction_T_max 0.349
_exptl_absorpt_correction_T_min 0.040
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2019)
;
_exptl_crystal_colour silver
_exptl_crystal_density_diffrn 7.350
_exptl_crystal_description plate
_exptl_crystal_F_000 124
_exptl_crystal_size_max 0.125
_exptl_crystal_size_mid 0.112
_exptl_crystal_size_min 0.034
_refine_diff_density_max 1.228
_refine_diff_density_min -1.735
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.238
_refine_ls_hydrogen_treatment undef
_refine_ls_matrix_type full
_refine_ls_number_parameters 5
_refine_ls_number_reflns 91
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.238
_refine_ls_R_factor_all 0.0193
_refine_ls_R_factor_gt 0.0176
_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^)+(0.0278P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0429
_reflns_number_gt 85
_reflns_number_total 91
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ep3012sup1.cif
_cod_data_source_block II
_cod_original_cell_volume 62.204(4)
_cod_database_code 2022343
_shelx_hkl_file
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4 -6 0 40.6981 90.5318 12
-6 2 0 59.4415 106.314 6
-2 -4 0 44.6972 82.5744 11
4 2 0 105.799 93.8768 19
-4 6 0 56.1935 76.5875 2
-6 4 0 123.704 81.6921 3
6 -4 0 150.288 127.227 5
2 -6 0 115.410 145.621 16
4 -6 0 118.366 124.282 16
6 -4 0 146.376 115.769 16
6 -2 0 20.4038 124.047 8
-6 2 0 15.6872 77.1344 15
4 2 0 62.0691 109.772 8
6 -4 1 3824.61 254.482 4
6 -4 -1 3614.58 244.424 4
-6 4 -1 3916.38 255.902 13
-4 6 -1 3576.36 248.604 2
-6 4 1 3658.39 253.184 13
-4 6 1 3699.38 252.269 2
-6 2 -1 3607.69 268.500 6
2 -6 1 3928.85 258.989 12
-4 -2 1 4211.62 341.541 23
-4 -2 -1 3336.21 267.594 23
4 -6 1 3853.96 260.423 12
2 -6 -1 3690.90 250.712 12
-4 -2 -1 3639.99 349.711 6
-2 -4 1 3371.52 333.396 23
-2 -4 -1 3813.44 309.001 23
-6 4 -1 3921.53 259.113 3
-2 -4 -1 3515.48 253.085 11
-2 -4 1 3877.35 281.820 11
-4 -2 1 3440.31 250.078 11
-6 4 1 3917.19 257.375 3
4 2 1 3694.41 271.373 19
4 2 -1 3727.17 274.372 19
2 4 1 4052.10 262.561 19
6 -4 -1 3766.53 308.906 5
4 2 -1 3489.82 327.691 17
2 -6 -1 3319.36 352.802 16
2 -6 1 2797.47 347.689 16
4 -6 -1 2895.93 292.272 16
4 -6 1 3128.97 346.887 16
6 -2 1 3559.73 345.804 8
6 -4 -1 3836.99 302.479 16
6 -2 -1 3152.16 357.674 8
6 -4 1 3927.27 360.955 16
4 2 1 3564.09 278.037 8
4 2 -1 3707.24 324.395 8
-6 2 -1 4010.45 256.687 15
-6 2 1 3763.69 242.754 15
2 4 -1 3793.39 317.855 8
6 -4 2 5706.75 328.021 4
-4 6 -2 5117.83 309.635 2
6 -2 2 5667.64 307.891 4
-6 4 2 4844.21 309.774 13
-4 6 2 5871.05 329.963 2
-6 2 -2 5670.09 339.961 6
2 -6 2 5475.59 324.313 12
-4 -2 2 4984.16 411.539 23
4 -6 2 5828.42 338.441 12
-6 4 -2 5523.65 323.291 3
-2 -4 2 4087.45 389.620 23
-2 -4 -2 5533.88 364.396 23
-4 -2 -2 5443.67 428.298 6
-2 -4 2 5465.25 359.711 11
-4 -2 2 5615.54 349.974 11
-6 4 2 6013.84 329.502 3
4 2 2 5937.76 349.653 19
4 2 -2 5199.58 346.216 19
6 -4 -2 5338.29 368.360 5
6 -2 -2 5456.91 335.873 5
4 2 -2 4072.32 379.081 17
2 4 -2 5207.52 445.926 17
-4 6 -2 6080.78 363.345 9
2 -6 -2 4416.79 382.710 16
4 -6 -2 5259.03 370.602 16
6 -2 2 4968.65 399.651 8
6 -4 2 4725.92 417.257 16
4 2 -2 4745.41 387.529 8
-6 2 -2 5268.68 316.280 15
-6 2 2 5400.04 307.837 15
2 4 -2 5943.36 437.579 8
6 -4 3 2869.77 235.392 4
-6 4 3 2908.41 228.329 13
-4 6 3 2946.12 230.098 2
-6 4 -3 3184.33 237.896 3
2 -6 3 3046.50 244.421 12
-4 -2 3 1934.98 273.658 23
-4 -2 -3 2599.32 289.103 6
-2 -4 -3 2598.74 287.090 6
-2 -4 3 2920.13 269.870 11
-4 -2 3 2934.14 267.989 11
-6 4 3 3172.45 234.080 3
4 -6 -3 2412.22 264.435 5
6 -2 3 2035.64 263.772 19
4 2 3 3200.51 250.955 19
6 -4 -3 2673.12 254.389 5
6 -2 -3 2732.97 227.579 5
4 2 -3 2361.26 265.870 17
2 4 -3 2869.38 297.702 17
-2 6 -3 2825.24 301.723 9
-4 6 -3 2506.64 242.470 9
2 -6 -3 2223.27 251.692 16
4 -6 -3 2263.33 233.917 16
6 -2 3 2313.72 266.299 8
6 -4 3 2848.42 284.344 16
-6 2 -3 2641.20 222.419 15
4 2 -3 1937.88 240.575 8
-6 2 3 2876.02 217.320 15
2 4 -3 2516.63 284.914 8
-4 6 -3 2687.66 219.308 2
-6 5 0 53.8032 83.4929 13
-5 -1 0 207.468 118.212 23
-1 -5 0-16.8521 131.749 23
1 -6 0-20.2412 146.788 23
-6 1 0 23.4795 112.846 6
-5 -1 0 78.2755 143.363 6
-1 -5 0 41.8895 91.7552 11
5 1 0 129.136 105.022 19
-5 6 0 76.3979 84.6810 2
-6 5 0 144.626 88.4296 3
1 -6 0-26.2430 156.435 16
5 -6 0-63.7805 107.541 16
6 -5 0 74.5480 120.562 16
6 -1 0-35.1936 112.980 8
-6 1 0 31.6272 77.1702 15
5 1 0 27.6248 102.844 8
-5 6 -1 3341.40 237.043 2
-6 5 1 2995.91 221.308 13
-5 6 1 3249.66 240.018 2
-6 1 1 2748.24 272.022 6
-6 1 -1 3068.08 265.967 6
-6 1 1 2902.72 283.115 23
-5 -1 -1 3242.98 310.096 6
-5 -1 1 3182.43 301.909 23
-1 -5 1 2797.35 322.947 23
-1 -5 -1 3026.23 305.518 23
-6 5 -1 2773.85 221.659 3
-1 -5 -1 3081.24 247.046 11
-1 -5 1 3339.29 275.125 11
-6 5 1 3202.33 235.183 3
5 1 1 2909.62 252.627 19
6 -5 -1 2946.93 306.938 5
5 1 -1 2654.19 270.302 17
-1 6 -1 2625.90 365.490 17
5 -6 -1 3136.95 290.118 16
5 -6 1 2750.82 309.762 16
6 -5 -1 2379.32 250.820 16
6 -5 1 2361.12 287.756 16
6 -1 1 2682.48 289.308 8
6 -1 -1 2906.42 323.848 8
5 1 1 3168.02 272.373 8
5 1 -1 2702.38 293.049 8
-6 1 -1 3168.44 224.230 15
-6 1 1 2992.27 216.740 15
1 5 -1 3321.15 298.917 8
6 -5 2 4658.78 300.481 4
-6 5 2 4562.22 282.455 13
-6 1 -2 4770.70 332.160 6
-6 1 2 4087.83 374.225 23
1 -6 2 4485.87 280.253 12
-5 -1 2 4433.30 381.193 23
-5 -1 -2 4367.99 347.760 6
-6 5 -2 4347.48 284.503 3
-1 -5 -2 4691.01 350.993 23
-1 -5 2 4522.59 339.644 11
6 -1 2 3969.32 339.839 19
6 -5 -2 4210.32 357.198 5
5 1 -2 4296.61 360.418 17
1 5 -2 3829.68 400.512 17
-1 6 -2 4634.87 435.786 17
5 -6 -2 3650.90 300.773 16
5 -6 2 3458.27 338.897 16
6 -5 2 3597.29 350.757 16
6 -1 2 4586.34 357.450 8
5 1 2 4617.79 322.874 8
5 1 -2 3829.15 345.142 8
-6 1 -2 4443.76 277.177 15
1 5 -2 4402.80 377.668 8
0 0 0 0.00 0.00 0
TITL NiSe26 in P6(3)/mmc
REM P6(3)/mmc (#194 in standard setting)
CELL 0.71073 3.661475 3.661475 5.357661 90.0000 90.0000 120.0000
ZERR 2.00 0.000100 0.000100 0.000160 0.0000 0.0000 0.0000
LATT 1
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM -x,-y, z+1/2
SYMM y,-x+y, z+1/2
SYMM x-y, x, z+1/2
SYMM y, x,-z
SYMM x-y,-y,-z
SYMM -x,-x+y,-z
SYMM -y,-x,-z+1/2
SYMM -x+y, y,-z+1/2
SYMM x, x-y,-z+1/2
SFAC Ni Se
UNIT 2.00 2.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 82777
_shelx_res_file
;
TITL NiSe26 in P63/mmc #194
shelx.res
created by SHELXL-2018/3 at 17:15:07 on 14-Sep-2020
REM reset to P63/mmc #194
CELL 0.71073 3.661475 3.661475 5.357661 90 90 120
ZERR 2 0.0001 0.0001 0.00016 0 0 0
LATT 1
SYMM -Y+X,+X,0.5+Z
SYMM -Y,+X-Y,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y-X,-X,+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SYMM +Y,+X,-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC Ni Se
UNIT 2 2
L.S. 4
PLAN 5
fmap 2
acta
OMIT 0 0 2
OMIT -1 2 0
OMIT -1 2 2
REM
REM
REM
WGHT 0.027800
FVAR 4.85414
SE1 2 0.333333 0.666667 0.250000 10.08333 0.00730 0.00730 =
0.01331 0.00000 0.00000 0.00365
NI2 1 0.000000 0.000000 0.000000 10.08333 0.01180 0.01180 =
0.01241 0.00000 0.00000 0.00590
HKLF 4
REM NiSe26 in P63/mmc #194
REM wR2 = 0.0429, GooF = S = 1.238, Restrained GooF = 1.238 for all data
REM R1 = 0.0176 for 85 Fo > 4sig(Fo) and 0.0193 for all 91 data
REM 5 parameters refined using 0 restraints
END
WGHT 0.0278 0.0000
REM Highest difference peak 1.228, deepest hole -1.735, 1-sigma level 0.233
Q1 1 0.0000 0.0000 0.2500 10.08333 0.05 1.23
Q2 1 -0.2514 0.2514 0.0568 10.50000 0.05 0.67
Q3 1 -0.0703 -0.1405 0.1039 10.50000 0.05 0.42
Q4 1 0.1391 0.2782 0.1820 10.50000 0.05 0.40
Q5 1 0.1887 0.3774 0.0689 10.50000 0.05 0.32
;
_shelx_res_checksum 71509
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Se Se1 0.333333 0.666667 0.250000 0.00930(13) Uani d 1 . .
Ni Ni2 0.000000 0.000000 0.000000 0.01201(15) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Se1 0.00730(14) 0.00730(14) 0.01331(18) 0.00365(7) 0.000 0.000
Ni2 0.01180(17) 0.01180(17) 0.0124(2) 0.00590(9) 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Ni2 Se1 Ni2 2_565 1_565 64.717(2) ?
Ni2 Se1 Ni2 2_565 2_665 94.0320(10) ?
Ni2 Se1 Ni2 1_565 2_665 130.0330(10) ?
Ni2 Se1 Ni2 2_565 . 130.0330(10) ?
Ni2 Se1 Ni2 1_565 . 94.0320(10) ?
Ni2 Se1 Ni2 2_665 . 130.0330(10) ?
Ni2 Se1 Ni2 2_565 1_665 130.0330(10) ?
Ni2 Se1 Ni2 1_565 1_665 94.0320(10) ?
Ni2 Se1 Ni2 2_665 1_665 64.717(2) ?
Ni2 Se1 Ni2 . 1_665 94.0320(10) ?
Ni2 Se1 Ni2 2_565 2 94.0320(10) ?
Ni2 Se1 Ni2 1_565 2 130.0330(10) ?
Ni2 Se1 Ni2 2_665 2 94.0320(10) ?
Ni2 Se1 Ni2 . 2 64.717(2) ?
Ni2 Se1 Ni2 1_665 2 130.0330(10) ?
Se1 Ni2 Se1 13_565 1_545 180.0 ?
Se1 Ni2 Se1 13_565 . 85.9680(10) ?
Se1 Ni2 Se1 1_545 . 94.0320(10) ?
Se1 Ni2 Se1 13_565 13 94.0320(10) ?
Se1 Ni2 Se1 1_545 13 85.9680(10) ?
Se1 Ni2 Se1 . 13 180.0 ?
Se1 Ni2 Se1 13_565 13_665 94.0320(10) ?
Se1 Ni2 Se1 1_545 13_665 85.9680(10) ?
Se1 Ni2 Se1 . 13_665 85.9680(10) ?
Se1 Ni2 Se1 13 13_665 94.0320(10) ?
Se1 Ni2 Se1 13_565 1_445 85.9680(10) ?
Se1 Ni2 Se1 1_545 1_445 94.0320(10) ?
Se1 Ni2 Se1 . 1_445 94.0320(10) ?
Se1 Ni2 Se1 13 1_445 85.9680(10) ?
Se1 Ni2 Se1 13_665 1_445 180.0 ?
Se1 Ni2 Ni2 13_565 2 122.3590(10) ?
Se1 Ni2 Ni2 1_545 2 57.6410(10) ?
Se1 Ni2 Ni2 . 2 57.6410(10) ?
Se1 Ni2 Ni2 13 2 122.3590(10) ?
Se1 Ni2 Ni2 13_665 2 122.3590(10) ?
Se1 Ni2 Ni2 1_445 2 57.6410(10) ?
Se1 Ni2 Ni2 13_565 2_554 57.6410(10) ?
Se1 Ni2 Ni2 1_545 2_554 122.3590(10) ?
Se1 Ni2 Ni2 . 2_554 122.3590(10) ?
Se1 Ni2 Ni2 13 2_554 57.6410(10) ?
Se1 Ni2 Ni2 13_665 2_554 57.6410(10) ?
Se1 Ni2 Ni2 1_445 2_554 122.3590(10) ?
Ni2 Ni2 Ni2 2 2_554 180.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Se1 Ni2 2_565 2.50257(5) ?
Se1 Ni2 1_565 2.50257(5) ?
Se1 Ni2 2_665 2.50257(5) ?
Se1 Ni2 . 2.50257(5) ?
Se1 Ni2 1_665 2.50257(5) ?
Se1 Ni2 2 2.50257(5) ?
Ni2 Ni2 2 2.67883(8) ?
Ni2 Ni2 2_554 2.67883(8) ?
_cod_database_fobs_code 2022343