Ti4Fe2C0.82O0.18

Liu, H.; Fan, C.; Wen, B.; Zhang, L.

doi:10.1107/S2414314624008903

inorganic compounds

IUCrDATA

ISSN: 2414-3146

Volume 9| Part 9| September 2024| x240890

https://doi.org/10.1107/S2414314624008903

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Ti₄Fe₂C_0.82O_0.18

Huizi Liu,^a Changzeng Fan,^a,^b ^* Bin Wen ^a and Lifeng Zhang ^a,^c

^aState Key Laboratory of Metastable Materials Science and Technology, Yanshan University, Qinhuangdao 066004, People's Republic of China, ^bHebei Key Lab for Optimizing Metal Product Technology and Performance, Yanshan University, Qinhuangdao 066004, People's Republic of China, and ^cSchool of Mechanical and Materials Engineering, North China University of Technology, Beijing 100144, People's Republic of China
^*Correspondence e-mail: chzfan@ysu.edu.cn

Edited by M. Weil, Vienna University of Technology, Austria (Received 12 March 2024; accepted 11 September 2024; online 30 September 2024)

The phase with composition Ti₄Fe₂C_0.82O_0.18, tetratitanium diiron carbide oxide, was unexpectedly synthesized by high-pressure sintering (HPS) of a stoichiometric mixture with nominal composition Ti₂Fe. The Ti₄Fe₂C_0.82O_0.18 phase crystallizes in the Fd $[\overline{3}]$ m space group and can be considered as the Ti₂Fe structure filled with C and O atoms co-occupying the same octahedral void [occupancy ratio 0.82 (7):0.18 (7)]. The Ti₄Fe₂C_0.82O_0.18 phase is isotypic with Ti₄Ni₂C and Ti₄Fe₂O_0.407, and is the first example where C and O atoms co-occupy the same site in filled Ti₂Fe structures.

Keywords: crystal structure; high-pressure sintering; co-occupation; intermetallics.

CCDC reference: 2383278

Structure description

Intermetallic phases usually are classified by structural or chemical similarities. For example, Duwez & Taylor (1950 ) investigated the crystal structure of Ti₂Fe on the basis of X-ray powder data. They determined that the Ti₂Fe phase crystallizes in a face centered cubic (f.c.c.) unit cell, with cell parameter a = 11.305 Å and with 96 atoms per unit cell. The related crystal structure of cubic Ti₄Fe₂O_0.407 was refined on the basis of neutron powder diffraction, affording the cell parameter a = 11.3326 (5) Å in space group Fd $[\overline{3}]$ m with Ti on position 48 f and on 16 d, Fe on 32 e and O (with a site occupation factor of 0.407) on 16 c (Rupp & Fischer, 1988 ). Liu et al. (2024 ) reported the isotypic crystal structure of Ti₄Ni₂C [a = 11.3235 (8) Å] by using single-crystal X-ray diffraction (SXRD) measurements. The latter phase can be considered as a partially filled Ti₂Ni structure with the C atom occupying an octahedral void. Holleck & Thummler (1967 ) studied a series of carbides, nitrides and oxides in ternary systems including Nb₄Ni₂C (a = 11.64 Å) and Ta₄Ni₂C (a =11.61 Å) phases. Although the title Ti₄Fe₂C_0.82O_0.18 phase is isotypic with Ti₄Ni₂C and Ti₄Fe₂O_0.407, no detailed study has been performed so far with respect to a phase where C and O atoms co-occupy the same site. The carbon present in the crystal structure of Ti₄Fe₂C_0.82O_0.18 most likely originated from the graphite crucible used during high pressure sintering (HPS), whereas oxygen may be incorporated due to surface oxidation during sample storage and subsequent HPS.

Ti₄Fe₂C_0.82O_0.18 crystallizes isotypically with Ti₄Fe₂O_0.407 and Ti₄Ni₂C in a partially filled Ti₂Fe structure in space group type Fd $[\overline{3}]$ m. Fig. 1 shows the distribution of the atoms in the the unit cell of Ti₄Fe₂C_0.82O_0.18. The environments of the Ti1 and (C1/O1) sites are shown in Figs. 2 and 3, respectively. The Ti1 atom is situated at a position with site symmetry . $[\overline{3}]$ m (multiplicity 16, Wyckoff letter c). It is surrounded by six Ti2 atoms (2.mm, 48 f) and six Fe1 atoms (.3m, 32 e), defining the center of an icosahedron. The (C1/O1) atoms co-occupy a position with site symmetry . $[\overline{3}]$ m (16 d) and center an octahedron defined by six Ti2 atoms. The shortest Ti1 to Ti2 separation is 2.9084 (10) Å and the shortest Ti1 to Fe1 separation is 2.4650 (4) Å; the (C1/O1)—Ti2 bond length is 2.1273 (5) Å.

Figure 1
The crystal structure of Ti₄Fe₂C_0.82O_0.18, with displacement ellipsoids drawn at the 99.9% probability level.

Figure 2
(a) The icosahedron formed around the Ti1 atom at the 16 c site; (b) the environment of the Ti1 atom with displacement ellipsoids drawn at the 99.9% probability level. [Symmetry codes: (i) −x, y − $[{1\over 4}]$ , z − $[{1\over 4}]$ ; (ii) x, −y + $[{1\over 4}]$ , −z + $[{1\over 4}]$ ; (iii) −x + $[{1\over 4}]$ , −y + $[{1\over 4}]$ , z; (iv) −x + $[{1\over 4}]$ , y, −z + $[{1\over 4}]$ ; (v) x − $[{1\over 4}]$ , −y, z − $[{1\over 4}]$ ; (vi) x − $[{1\over 4}]$ , y − $[{1\over 4}]$ , −z; (vii) y − $[{1\over 4}]$ , −z, x − $[{1\over 4}]$ ; (viii) z, −x + $[{1\over 4}]$ , −y + $[{1\over 4}]$ ; (ix) −z, x − $[{1\over 4}]$ , y − $[{1\over 4}]$ ; (x) −y + $[{1\over 4}]$ , z, −x + $[{1\over 4}]$ .]

Figure 3
(a) The octahedron formed around the (C1/O1) atoms at the 16 d site; (b) the environment of the (C1/O1) atoms with displacement ellipsoids drawn at the 99.9% probability level. [Symmetry codes: (xvi) −z + $[{1\over 2}]$ , −x + 1, −y + $[{1\over 2}]$ ; (xvii) z + $[{1\over 2}]$ , x, y + $[{1\over 2}]$ ; (xviii) x, y + $[{1\over 2}]$ , z + $[{1\over 2}]$ ; (xix) −x + 1, −y + $[{1\over 2}]$ , −z + $[{1\over 2}]$ ; (xx) −y + $[{1\over 2}]$ , −z + $[{1\over 2}]$ , −x + 1; (xxi) y + $[{1\over 2}]$ , z + $[{1\over 2}]$ , x.]

Synthesis and crystallization

Pure titanium powder (indicated purity 99.5%, 0.6312 g) and iron powder (indicated purity 99.9%, 0.3693 g) were evenly mixed according to the stoichiometric ratio of 2:1 and thoroughly ground in an agate mortar. The mixed powder was put into a 5 mm cemented carbide grinding mould and pressed into a tablet at about 6 MPa for 2 min to obtain a cylindrical block without deformations or cracks. Details of the high-pressure sintering experiment using a six-anvil high-temperature and high-pressure apparatus can be found elsewhere (Liu & Fan, 2018 ). The sample was pressurized up to 6 GPa and heated to 1473 K for 20 minutes, cooled to 1173 K, held at the temperature for 1 h, and then the furnace power was turned off to rapidly cool to room temperature. Different phases were isolated from two samples from the same batch. Ti₄Fe₂C_0.82O_0.18 originated from sample 1, together with TiFe. The refined chemical formula of Ti₄Fe₂C_0.82O_0.18 from sample 1 is in accordance with the complementary EDX results (see Table S1 of the electronic supporting information, ESI). Another phase with very similar refined composition, Ti₄Fe₂C_0.87O_0.13, was isolated from sample 2, and its composition is also in accordance with the complementary EDX results (see Table S2 of the ESI). Different options for refinements for the two phases Ti₄Fe₂C_1-δO_δ (δ = 0.18; δ = 0.13) are listed in Table S3 of the ESI. The crystal structures of Ti₄Fe₂C_0.82O_0.18 and Ti₄Fe₂C_0.87O_0.13 are very similar, just different in atomic proportions at the 16 d site, so the Ti₄Fe₂C_0.82O_0.18 phase was selected for the current report. Structural data for Ti₄Fe₂C_0.87O_0.13 can be found in Table S4 of the ESI.

Refinement

Crystal data, data collection and structure refinement details of Ti₄Fe₂C_0.82O_0.18 are summarized in Table 1. The labeling scheme and atomic coordinates of Ti₄Fe₂C_0.82O_0.18 were adapted from Ti₄Ni₂C for better comparison (Liu et al., 2024). The 16 d site is co-occupied by C and O atoms, with site occupancies refined to 0.82 (7) for C1 and 0.18 (7) for O1, assuming full occupancy. Both atoms were refined with the same displacement parameters. The maximum and minimum residual electron densities in the final difference map are located 1.16 Å from site Fe1 and 1.67 Å from Fe1, respectively.

Table 1
Experimental details

Crystal data
Chemical formula	Ti₄Fe₂C_0.82O_0.18
M_r	316.02
Crystal system, space group	Cubic, Fd $[\overline{3}]$ m
Temperature (K)	296
a (Å)	11.323 (4)
V (Å³)	1451.6 (3)
Z	16
Radiation type	Mo Kα
μ (mm⁻¹)	15.91
Crystal size (mm)	0.10 × 0.06 × 0.06

Data collection
Diffractometer	Bruker D8 Venture Photon 100 CMOS
Absorption correction	Multi-scan (SADABS; Krause et al., 2015 )
T_min, T_max	0.429, 0.746
No. of measured, independent and observed [I > 2σ(I)] reflections	5363, 102, 82
R_int	0.155
(sin θ/λ)_max (Å⁻¹)	0.643

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.022, 0.040, 1.14
No. of reflections	102
No. of parameters	13
Δρ_max, Δρ_min (e Å⁻³)	0.58, −0.83
Computer programs: APEX3 and SAINT (Bruker, 2015 ), SHELXT (Sheldrick, 2015a ), SHELXL (Sheldrick, 2015b ), DIAMOND (Brandenburg & Putz, 2017 ) and publCIF (Westrip, 2010 ).

Structural data

CCDC reference: 2383278

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S2414314624008903/wm5714sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2414314624008903/wm5714Isup6.hkl

Supporting information file. DOI: https://doi.org/10.1107/S2414314624008903/wm5714sup7.docx

checkCIF report

Computing details top

Tetratitanium diiron carbide oxide top

Crystal data top

Ti₄Fe₂C_0.82O_0.18	Mo Kα radiation, λ = 0.71073 Å
M_r = 316.02	Cell parameters from 1378 reflections
Cubic, Fd3m	θ = 3.1–26.7°
a = 11.323 (4) Å	µ = 15.91 mm⁻¹
V = 1451.6 (3) Å³	T = 296 K
Z = 16	Lump, gray
F(000) = 2342	0.10 × 0.06 × 0.06 mm
D_x = 5.784 Mg m⁻³

Data collection top

Bruker D8 Venture Photon 100 CMOS diffractometer	82 reflections with I > 2σ(I)
phi and ω scans	R_int = 0.155
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	θ_max = 27.2°, θ_min = 3.1°
T_min = 0.429, T_max = 0.746	h = −14→14
5363 measured reflections	k = −13→14
102 independent reflections	l = −14→14

Refinement top

Refinement on F²	13 parameters
Least-squares matrix: full	0 restraints
R[F² > 2σ(F²)] = 0.022	w = 1/[σ²(F_o²) + (0.0069P)² + 29.2966P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.040	(Δ/σ)_max < 0.001
S = 1.14	Δρ_max = 0.58 e Å⁻³
102 reflections	Δρ_min = −0.83 e Å⁻³

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ti1	0.000000	0.000000	0.000000	0.0018 (5)
Fe1	0.21037 (6)	0.21037 (6)	0.21037 (6)	0.0028 (4)
Ti2	0.43636 (12)	0.125000	0.125000	0.0021 (4)
C1	0.500000	0.500000	0.500000	0.012 (4)	0.82 (7)
O1	0.500000	0.500000	0.500000	0.012 (4)	0.18 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ti1	0.0018 (5)	0.0018 (5)	0.0018 (5)	0.0004 (6)	0.0004 (6)	0.0004 (6)
Fe1	0.0028 (4)	0.0028 (4)	0.0028 (4)	−0.0007 (3)	−0.0007 (3)	−0.0007 (3)
Ti2	0.0033 (8)	0.0016 (5)	0.0016 (5)	0.000	0.000	−0.0010 (5)
C1	0.012 (4)	0.012 (4)	0.012 (4)	0.002 (4)	0.002 (4)	0.002 (4)
O1	0.012 (4)	0.012 (4)	0.012 (4)	0.002 (4)	0.002 (4)	0.002 (4)

Geometric parameters (Å, º) top

Ti1—Fe1ⁱ	2.4650 (4)	Fe1—Ti2^xiii	2.6501 (10)
Ti1—Fe1ⁱⁱ	2.4650 (4)	Fe1—Fe1ⁱⁱⁱ	2.734 (2)
Ti1—Fe1ⁱⁱⁱ	2.4650 (4)	Fe1—Fe1ⁱⁱ	2.734 (2)
Ti1—Fe1^iv	2.4650 (4)	Fe1—Fe1^iv	2.734 (2)
Ti1—Fe1^v	2.4650 (4)	Fe1—Ti2	2.9011 (12)
Ti1—Fe1^vi	2.4650 (4)	Fe1—Ti2^xiv	2.9011 (12)
Ti1—Ti2^vii	2.9084 (10)	Fe1—Ti2^xv	2.9011 (12)
Ti1—Ti2ⁱⁱⁱ	2.9084 (10)	Ti2—C1^xvi	2.1273 (5)
Ti1—Ti2^vi	2.9084 (10)	Ti2—C1^xvii	2.1273 (5)
Ti1—Ti2^viii	2.9084 (10)	Ti2—Ti2^xviii	2.9963 (6)
Ti1—Ti2^ix	2.9084 (10)	Ti2—Ti2^xix	2.9963 (6)
Ti1—Ti2^x	2.9084 (10)	Ti2—Ti2^xi	2.9963 (6)
Fe1—Ti2^xi	2.6501 (10)	Ti2—Ti2^xii	2.9963 (6)
Fe1—Ti2^xii	2.6501 (10)

Fe1ⁱ—Ti1—Fe1ⁱⁱ	180.0	Ti2^xi—Fe1—Ti2^xiv	65.152 (14)
Fe1ⁱ—Ti1—Fe1ⁱⁱⁱ	112.64 (4)	Ti2^xii—Fe1—Ti2^xiv	124.00 (6)
Fe1ⁱⁱ—Ti1—Fe1ⁱⁱⁱ	67.36 (4)	Ti2^xiii—Fe1—Ti2^xiv	65.152 (14)
Fe1ⁱ—Ti1—Fe1^iv	112.64 (4)	Fe1ⁱⁱⁱ—Fe1—Ti2^xiv	112.83 (2)
Fe1ⁱⁱ—Ti1—Fe1^iv	67.36 (4)	Fe1ⁱⁱ—Fe1—Ti2^xiv	112.83 (2)
Fe1ⁱⁱⁱ—Ti1—Fe1^iv	67.36 (4)	Fe1^iv—Fe1—Ti2^xiv	61.89 (3)
Fe1ⁱ—Ti1—Fe1^v	67.36 (4)	Ti2—Fe1—Ti2^xiv	118.474 (12)
Fe1ⁱⁱ—Ti1—Fe1^v	112.64 (4)	Ti1ⁱⁱ—Fe1—Ti2^xv	65.047 (6)
Fe1ⁱⁱⁱ—Ti1—Fe1^v	112.64 (4)	Ti1ⁱⁱⁱ—Fe1—Ti2^xv	166.80 (5)
Fe1^iv—Ti1—Fe1^v	180.0	Ti1^iv—Fe1—Ti2^xv	65.047 (6)
Fe1ⁱ—Ti1—Fe1^vi	67.36 (4)	Ti2^xi—Fe1—Ti2^xv	124.00 (6)
Fe1ⁱⁱ—Ti1—Fe1^vi	112.64 (4)	Ti2^xii—Fe1—Ti2^xv	65.152 (14)
Fe1ⁱⁱⁱ—Ti1—Fe1^vi	180.0	Ti2^xiii—Fe1—Ti2^xv	65.152 (14)
Fe1^iv—Ti1—Fe1^vi	112.64 (4)	Fe1ⁱⁱⁱ—Fe1—Ti2^xv	61.89 (3)
Fe1^v—Ti1—Fe1^vi	67.36 (4)	Fe1ⁱⁱ—Fe1—Ti2^xv	112.83 (2)
Fe1ⁱ—Ti1—Ti2^vii	64.739 (17)	Fe1^iv—Fe1—Ti2^xv	112.83 (2)
Fe1ⁱⁱ—Ti1—Ti2^vii	115.261 (17)	Ti2—Fe1—Ti2^xv	118.474 (12)
Fe1ⁱⁱⁱ—Ti1—Ti2^vii	58.40 (3)	Ti2^xiv—Fe1—Ti2^xv	118.474 (12)
Fe1^iv—Ti1—Ti2^vii	115.261 (17)	C1^xvi—Ti2—C1^xvii	140.40 (7)
Fe1^v—Ti1—Ti2^vii	64.739 (17)	C1^xvi—Ti2—Fe1^xx	88.009 (14)
Fe1^vi—Ti1—Ti2^vii	121.60 (3)	C1^xvii—Ti2—Fe1^xx	88.009 (14)
Fe1ⁱ—Ti1—Ti2ⁱⁱⁱ	58.40 (3)	C1^xvi—Ti2—Fe1^xxi	88.009 (14)
Fe1ⁱⁱ—Ti1—Ti2ⁱⁱⁱ	121.60 (3)	C1^xvii—Ti2—Fe1^xxi	88.009 (14)
Fe1ⁱⁱⁱ—Ti1—Ti2ⁱⁱⁱ	64.739 (17)	Fe1^xx—Ti2—Fe1^xxi	168.22 (7)
Fe1^iv—Ti1—Ti2ⁱⁱⁱ	64.739 (17)	C1^xvi—Ti2—Fe1ⁱⁱ	137.91 (5)
Fe1^v—Ti1—Ti2ⁱⁱⁱ	115.261 (17)	C1^xvii—Ti2—Fe1ⁱⁱ	81.68 (3)
Fe1^vi—Ti1—Ti2ⁱⁱⁱ	115.261 (17)	Fe1^xx—Ti2—Fe1ⁱⁱ	95.19 (3)
Ti2^vii—Ti1—Ti2ⁱⁱⁱ	62.010 (9)	Fe1^xxi—Ti2—Fe1ⁱⁱ	95.19 (3)
Fe1ⁱ—Ti1—Ti2^vi	121.60 (3)	C1^xvi—Ti2—Fe1	81.69 (3)
Fe1ⁱⁱ—Ti1—Ti2^vi	58.40 (3)	C1^xvii—Ti2—Fe1	137.91 (5)
Fe1ⁱⁱⁱ—Ti1—Ti2^vi	115.261 (17)	Fe1^xx—Ti2—Fe1	95.19 (3)
Fe1^iv—Ti1—Ti2^vi	115.261 (17)	Fe1^xxi—Ti2—Fe1	95.19 (3)
Fe1^v—Ti1—Ti2^vi	64.739 (17)	Fe1ⁱⁱ—Ti2—Fe1	56.23 (6)
Fe1^vi—Ti1—Ti2^vi	64.739 (17)	C1^xvi—Ti2—Ti1^iv	104.226 (19)
Ti2^vii—Ti1—Ti2^vi	117.990 (9)	C1^xvii—Ti2—Ti1^iv	104.226 (19)
Ti2ⁱⁱⁱ—Ti1—Ti2^vi	180.0	Fe1^xx—Ti2—Ti1^iv	52.40 (2)
Fe1ⁱ—Ti1—Ti2^viii	115.261 (17)	Fe1^xxi—Ti2—Ti1^iv	139.38 (5)
Fe1ⁱⁱ—Ti1—Ti2^viii	64.739 (17)	Fe1ⁱⁱ—Ti2—Ti1^iv	50.21 (2)
Fe1ⁱⁱⁱ—Ti1—Ti2^viii	64.739 (17)	Fe1—Ti2—Ti1^iv	50.21 (2)
Fe1^iv—Ti1—Ti2^viii	121.60 (3)	C1^xvi—Ti2—Ti1ⁱⁱⁱ	104.226 (19)
Fe1^v—Ti1—Ti2^viii	58.40 (3)	C1^xvii—Ti2—Ti1ⁱⁱⁱ	104.226 (19)
Fe1^vi—Ti1—Ti2^viii	115.261 (17)	Fe1^xx—Ti2—Ti1ⁱⁱⁱ	139.38 (5)
Ti2^vii—Ti1—Ti2^viii	62.010 (9)	Fe1^xxi—Ti2—Ti1ⁱⁱⁱ	52.40 (2)
Ti2ⁱⁱⁱ—Ti1—Ti2^viii	117.990 (9)	Fe1ⁱⁱ—Ti2—Ti1ⁱⁱⁱ	50.21 (2)
Ti2^vi—Ti1—Ti2^viii	62.010 (9)	Fe1—Ti2—Ti1ⁱⁱⁱ	50.21 (2)
Fe1ⁱ—Ti1—Ti2^ix	64.739 (17)	Ti1^iv—Ti2—Ti1ⁱⁱⁱ	86.98 (4)
Fe1ⁱⁱ—Ti1—Ti2^ix	115.261 (17)	C1^xvi—Ti2—Ti2^xviii	149.47 (3)
Fe1ⁱⁱⁱ—Ti1—Ti2^ix	115.261 (17)	C1^xvii—Ti2—Ti2^xviii	45.23 (2)
Fe1^iv—Ti1—Ti2^ix	58.40 (3)	Fe1^xx—Ti2—Ti2^xviii	121.68 (3)
Fe1^v—Ti1—Ti2^ix	121.60 (3)	Fe1^xxi—Ti2—Ti2^xviii	61.47 (2)
Fe1^vi—Ti1—Ti2^ix	64.739 (17)	Fe1ⁱⁱ—Ti2—Ti2^xviii	53.38 (3)
Ti2^vii—Ti1—Ti2^ix	117.990 (9)	Fe1—Ti2—Ti2^xviii	100.81 (3)
Ti2ⁱⁱⁱ—Ti1—Ti2^ix	62.010 (9)	Ti1^iv—Ti2—Ti2^xviii	100.29 (4)
Ti2^vi—Ti1—Ti2^ix	117.990 (9)	Ti1ⁱⁱⁱ—Ti2—Ti2^xviii	58.995 (4)
Ti2^viii—Ti1—Ti2^ix	180.0	C1^xvi—Ti2—Ti2^xix	149.47 (3)
Fe1ⁱ—Ti1—Ti2^x	115.261 (17)	C1^xvii—Ti2—Ti2^xix	45.23 (2)
Fe1ⁱⁱ—Ti1—Ti2^x	64.739 (17)	Fe1^xx—Ti2—Ti2^xix	61.47 (2)
Fe1ⁱⁱⁱ—Ti1—Ti2^x	121.60 (3)	Fe1^xxi—Ti2—Ti2^xix	121.68 (3)
Fe1^iv—Ti1—Ti2^x	64.739 (17)	Fe1ⁱⁱ—Ti2—Ti2^xix	53.38 (3)
Fe1^v—Ti1—Ti2^x	115.261 (17)	Fe1—Ti2—Ti2^xix	100.81 (3)
Fe1^vi—Ti1—Ti2^x	58.40 (3)	Ti1^iv—Ti2—Ti2^xix	58.995 (4)
Ti2^vii—Ti1—Ti2^x	180.0	Ti1ⁱⁱⁱ—Ti2—Ti2^xix	100.29 (4)
Ti2ⁱⁱⁱ—Ti1—Ti2^x	117.990 (9)	Ti2^xviii—Ti2—Ti2^xix	60.54 (6)
Ti2^vi—Ti1—Ti2^x	62.010 (9)	C1^xvi—Ti2—Ti2^xi	45.23 (2)
Ti2^viii—Ti1—Ti2^x	117.990 (9)	C1^xvii—Ti2—Ti2^xi	149.47 (3)
Ti2^ix—Ti1—Ti2^x	62.010 (9)	Fe1^xx—Ti2—Ti2^xi	121.68 (3)
Ti1ⁱⁱ—Fe1—Ti1ⁱⁱⁱ	108.58 (3)	Fe1^xxi—Ti2—Ti2^xi	61.47 (2)
Ti1ⁱⁱ—Fe1—Ti1^iv	108.58 (3)	Fe1ⁱⁱ—Ti2—Ti2^xi	100.81 (3)
Ti1ⁱⁱⁱ—Fe1—Ti1^iv	108.58 (3)	Fe1—Ti2—Ti2^xi	53.38 (3)
Ti1ⁱⁱ—Fe1—Ti2^xi	124.77 (2)	Ti1^iv—Ti2—Ti2^xi	100.29 (4)
Ti1ⁱⁱⁱ—Fe1—Ti2^xi	69.20 (3)	Ti1ⁱⁱⁱ—Ti2—Ti2^xi	58.995 (4)
Ti1^iv—Fe1—Ti2^xi	124.77 (2)	Ti2^xviii—Ti2—Ti2^xi	112.60 (3)
Ti1ⁱⁱ—Fe1—Ti2^xii	124.77 (2)	Ti2^xix—Ti2—Ti2^xi	153.19 (5)
Ti1ⁱⁱⁱ—Fe1—Ti2^xii	124.77 (2)	C1^xvi—Ti2—Ti2^xii	45.23 (2)
Ti1^iv—Fe1—Ti2^xii	69.20 (3)	C1^xvii—Ti2—Ti2^xii	149.47 (3)
Ti2^xi—Fe1—Ti2^xii	69.49 (5)	Fe1^xx—Ti2—Ti2^xii	61.47 (2)
Ti1ⁱⁱ—Fe1—Ti2^xiii	69.20 (3)	Fe1^xxi—Ti2—Ti2^xii	121.68 (3)
Ti1ⁱⁱⁱ—Fe1—Ti2^xiii	124.77 (2)	Fe1ⁱⁱ—Ti2—Ti2^xii	100.81 (3)
Ti1^iv—Fe1—Ti2^xiii	124.77 (2)	Fe1—Ti2—Ti2^xii	53.38 (3)
Ti2^xi—Fe1—Ti2^xiii	69.49 (5)	Ti1^iv—Ti2—Ti2^xii	58.995 (4)
Ti2^xii—Fe1—Ti2^xiii	69.49 (5)	Ti1ⁱⁱⁱ—Ti2—Ti2^xii	100.29 (4)
Ti1ⁱⁱ—Fe1—Fe1ⁱⁱⁱ	56.32 (2)	Ti2^xviii—Ti2—Ti2^xii	153.19 (5)
Ti1ⁱⁱⁱ—Fe1—Fe1ⁱⁱⁱ	104.92 (3)	Ti2^xix—Ti2—Ti2^xii	112.60 (3)
Ti1^iv—Fe1—Fe1ⁱⁱⁱ	56.32 (2)	Ti2^xi—Ti2—Ti2^xii	60.54 (6)
Ti2^xi—Fe1—Fe1ⁱⁱⁱ	174.11 (3)	Ti2^xxii—C1—Ti2^xxiii	180.0
Ti2^xii—Fe1—Fe1ⁱⁱⁱ	115.14 (3)	Ti2^xxii—C1—Ti2^xxiv	89.54 (5)
Ti2^xiii—Fe1—Fe1ⁱⁱⁱ	115.14 (3)	Ti2^xxiii—C1—Ti2^xxiv	90.46 (5)
Ti1ⁱⁱ—Fe1—Fe1ⁱⁱ	104.92 (3)	Ti2^xxii—C1—Ti2^xxv	90.46 (5)
Ti1ⁱⁱⁱ—Fe1—Fe1ⁱⁱ	56.32 (2)	Ti2^xxiii—C1—Ti2^xxv	89.54 (5)
Ti1^iv—Fe1—Fe1ⁱⁱ	56.32 (2)	Ti2^xxiv—C1—Ti2^xxv	180.0
Ti2^xi—Fe1—Fe1ⁱⁱ	115.14 (3)	Ti2^xxii—C1—Ti2^xxvi	90.46 (5)
Ti2^xii—Fe1—Fe1ⁱⁱ	115.14 (3)	Ti2^xxiii—C1—Ti2^xxvi	89.54 (5)
Ti2^xiii—Fe1—Fe1ⁱⁱ	174.11 (3)	Ti2^xxiv—C1—Ti2^xxvi	89.54 (5)
Fe1ⁱⁱⁱ—Fe1—Fe1ⁱⁱ	60.0	Ti2^xxv—C1—Ti2^xxvi	90.46 (5)
Ti1ⁱⁱ—Fe1—Fe1^iv	56.32 (2)	Ti2^xxii—C1—Ti2^xxvii	89.54 (5)
Ti1ⁱⁱⁱ—Fe1—Fe1^iv	56.32 (2)	Ti2^xxiii—C1—Ti2^xxvii	90.46 (5)
Ti1^iv—Fe1—Fe1^iv	104.92 (3)	Ti2^xxiv—C1—Ti2^xxvii	90.46 (5)
Ti2^xi—Fe1—Fe1^iv	115.14 (3)	Ti2^xxv—C1—Ti2^xxvii	89.54 (5)
Ti2^xii—Fe1—Fe1^iv	174.11 (3)	Ti2^xxvi—C1—Ti2^xxvii	180.0
Ti2^xiii—Fe1—Fe1^iv	115.14 (3)	Ti2^xxii—O1—Ti2^xxiii	180.0
Fe1ⁱⁱⁱ—Fe1—Fe1^iv	60.0	Ti2^xxii—O1—Ti2^xxiv	89.54 (5)
Fe1ⁱⁱ—Fe1—Fe1^iv	60.0	Ti2^xxiii—O1—Ti2^xxiv	90.46 (5)
Ti1ⁱⁱ—Fe1—Ti2	166.80 (5)	Ti2^xxii—O1—Ti2^xxv	90.46 (5)
Ti1ⁱⁱⁱ—Fe1—Ti2	65.047 (6)	Ti2^xxiii—O1—Ti2^xxv	89.54 (5)
Ti1^iv—Fe1—Ti2	65.047 (6)	Ti2^xxiv—O1—Ti2^xxv	180.0
Ti2^xi—Fe1—Ti2	65.152 (14)	Ti2^xxii—O1—Ti2^xxvi	90.46 (5)
Ti2^xii—Fe1—Ti2	65.152 (14)	Ti2^xxiii—O1—Ti2^xxvi	89.54 (5)
Ti2^xiii—Fe1—Ti2	124.00 (6)	Ti2^xxiv—O1—Ti2^xxvi	89.54 (5)
Fe1ⁱⁱⁱ—Fe1—Ti2	112.83 (2)	Ti2^xxv—O1—Ti2^xxvi	90.46 (5)
Fe1ⁱⁱ—Fe1—Ti2	61.89 (3)	Ti2^xxii—O1—Ti2^xxvii	89.54 (5)
Fe1^iv—Fe1—Ti2	112.83 (2)	Ti2^xxiii—O1—Ti2^xxvii	90.46 (5)
Ti1ⁱⁱ—Fe1—Ti2^xiv	65.047 (6)	Ti2^xxiv—O1—Ti2^xxvii	90.46 (5)
Ti1ⁱⁱⁱ—Fe1—Ti2^xiv	65.047 (6)	Ti2^xxv—O1—Ti2^xxvii	89.54 (5)
Ti1^iv—Fe1—Ti2^xiv	166.80 (5)	Ti2^xxvi—O1—Ti2^xxvii	180.0

Symmetry codes: (i) −x, y−1/4, z−1/4; (ii) x, −y+1/4, −z+1/4; (iii) −x+1/4, −y+1/4, z; (iv) −x+1/4, y, −z+1/4; (v) x−1/4, −y, z−1/4; (vi) x−1/4, y−1/4, −z; (vii) y−1/4, −z, x−1/4; (viii) z, −x+1/4, −y+1/4; (ix) −z, x−1/4, y−1/4; (x) −y+1/4, z, −x+1/4; (xi) y+1/4, −z+1/2, x−1/4; (xii) −z+1/2, x−1/4, y+1/4; (xiii) x−1/4, y+1/4, −z+1/2; (xiv) z, x, y; (xv) y, z, x; (xvi) x, −y+3/4, −z+3/4; (xvii) x, y−1/2, z−1/2; (xviii) −z+1/2, −x+1/2, −y; (xix) −y+1/2, −z, −x+1/2; (xx) x+1/4, y−1/4, −z+1/2; (xxi) x+1/4, −y+1/2, z−1/4; (xxii) −z+1/2, −x+1, −y+1/2; (xxiii) z+1/2, x, y+1/2; (xxiv) x, y+1/2, z+1/2; (xxv) −x+1, −y+1/2, −z+1/2; (xxvi) −y+1/2, −z+1/2, −x+1; (xxvii) y+1/2, z+1/2, x.

Acknowledgements

The authors are indebted to Dr Bing Zhang from State Key Laboratory of Metastable Materials Science and Technology, Yanshan University for assistance in performing the SEM/EDX measurements.

Funding information

Funding for this research was provided by: The National Natural Science Foundation of China (grant Nos. 52173231 and 51925105); Hebei Natural Science Foundation (grant No. E2022203182); The Innovation Ability Promotion Project of Hebei supported by Hebei Key Lab for Optimizing Metal Product Technology and Performance (grant No. 22567609H).

References

Brandenburg, K. & Putz, H. (2017). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Bruker (2015). APEX3 and SAINT. Bruker AXS Inc. Madison, Wisconsin, USA, 2008. Google Scholar
Duwez, P. & Taylor, J. L. (1950). Trans AIME. Journal of Metals, 188, 1173–1176. CAS Google Scholar
Holleck, H. & Thummler, F. (1967). Monatshefte f?r Chemie, 98, 133–134. Google Scholar
Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015). J. Appl. Cryst. 48, 3–10. Web of Science CSD CrossRef ICSD CAS IUCr Journals Google Scholar
Liu, C. & Fan, C. (2018). IUCrData, 3, x180363. Google Scholar
Liu, H., Liang, X., Liu, Y., Fan, C., Wen, B. & Zhang, L. (2024). IUCrData, 9, x240043. Google Scholar
Rupp, B. & Fischer, P. (1988). J. Less-Common Met. 144, 275–281. CrossRef CAS Google Scholar
Sheldrick, G. M. (2015a). Acta Cryst. A71, 3–8. Web of Science CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (2015b). Acta Cryst. C71, 3–8. Web of Science CrossRef IUCr Journals Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar