Ab initio constrained crystal-chemical Rietveld refinement of Ca10(VxP1 − xO4)6F2 apatites

Mercier, P.H.J.; Dong, Z.; Baikie, T.; Le Page, Y.; White, T.J.; Whitfield, P.S.; Mitchel, L.D.

doi:10.1107/S0108768106045538

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Ab initio constrained crystal-chemical Rietveld refinement of Ca₁₀(V_xP_1 − xO₄)₆F₂ apatites

P. H. J. Mercier, Z. Dong, T. Baikie, Y. Le Page, T. J. White, P. S. Whitfield and L. D. Mitchel

Extraction of reliable bond distances and angles for Ca₁₀(V_xP_1 − xO₄)₆F₂ apatites using standard Rietveld refinement with Cu Kα X-ray powder data was significantly impaired by large imprecision for the O-atom coordinates. An initial attempt to apply crystal-chemical Rietveld refinements to the same compounds was partly successful, and exposed the problematic determination of two oxygen–metal–oxygen angles. Ab initio modeling with VASP in space groups P6₃/m, P2₁/m and Pm showed that both these angular parameters exhibited a linear dependence with the vanadium content. Stable crystal-chemical Rietveld refinements in agreement with quantum results were obtained by fixing these angles at the values from ab initio simulations. Residuals were comparable with the less precise standard refinements. The larger vanadium ion is accommodated primarily by uniform expansion and rotation of BO₄ tetrahedra combined with a rotation of the Ca–Ca–Ca triangular units. It is proposed that the reduction of symmetry for the vanadium end-member is necessary to avoid considerable departures from formal valences at the A^II and B sites in P6₃/m. The complementarity of quantum methods and structural analysis by powder diffraction in cases with problematic least-squares extraction of the crystal chemistry is discussed.

Keywords: apatite; crystal chemistry; ab initio calculations; X-ray powder diffraction; Rietveld refinement; crystal-chemical constraints.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768106045538/kd5006sup1.cif Contains datablocks Vx=0p0_C-CH, Vx=0p0_unrestrained, Vx=0p0_restrained, Vx=0p1_C-CH, Vx=0p1_unrestrained, Vx=0p1_restrained, Vx=0p2_C-CH, Vx=0p2_unrestrained, Vx=0p2_restrained, Vx=0p3_C-CH, Vx=0p3_unrestrained, Vx=0p3_restrained, Vx=0p4_C-CH, Vx=0p4_unrestrained, Vx=0p4_restrained, Vx=0p5_C-CH, Vx=0p5_unrestrained, Vx=0p5_restrained, Vx=0p6_C-CH, Vx=0p6_unrestrained, Vx=0p6_restrained, Vx=0p7_C-CH, Vx=0p7_unrestrained, Vx=0p7_restrained, Vx=0p8_C-CH, Vx=0p8_unrestrained, Vx=0p8_restrained, Vx=0p9_C-CH, Vx=0p9_unrestrained, Vx=0p9_restrained
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768106045538/kd5006Vx=0p0sup2.rtv Contains datablock Vx=0p0
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768106045538/kd5006Vx=0p1sup3.rtv Contains datablock Vx=0p1
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768106045538/kd5006Vx=0p2sup4.rtv Contains datablock Vx=0p2
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768106045538/kd5006Vx=0p3sup5.rtv Contains datablock Vx=0p3
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768106045538/kd5006Vx=0p4sup6.rtv Contains datablock Vx=0p4
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768106045538/kd5006Vx=0p5sup7.rtv Contains datablock Vx=0p5
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768106045538/kd5006Vx=0p6sup8.rtv Contains datablock Vx=0p6
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768106045538/kd5006Vx=0p7sup9.rtv Contains datablock Vx=0p7
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768106045538/kd5006Vx=0p8sup10.rtv Contains datablock Vx=0p8
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768106045538/kd5006Vx=0p9sup11.rtv Contains datablock Vx=0p9
	Portable Document Format (PDF) file https://doi.org/10.1107/S0108768106045538/kd5006sup12.pdf Structural data

Computing details top

Figures top

(Vx=0p0_C-CH) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 524.5 (10) Å³
a = 9.377 (11) Å	Z = ?
b = 9.377318 Å	? radiation, λ = ? Å
c = 6.888 (4) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 524.5 (10) Å³
a = 9.377 (11) Å	Z = ?
b = 9.377318 Å	? radiation, λ = ? Å
c = 6.888 (4) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq
Ca1	0.333333	0.666667	0	0.75 (2)
Ca2	0.00854 (13)	0.2498 (4)	0.25	0.599 (15)
O1	0.32597 (14)	0.4853 (3)	0.25	1.20 (3)
O2	0.58953 (18)	0.4655 (2)	0.25	1.20 (3)
P	0.3979 (4)	0.3674 (2)	0.25	0.70 (2)
O3	0.3413 (4)	0.2543 (3)	0.06768 (16)	1.20 (3)
F	0	0	0.25	1.97 (9)

(Vx=0p0_unrestrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 524.72 (1) Å³
a = 9.37834 (7) Å	Z = ?
b = 9.37834 (7) Å	? radiation, λ = ? Å
c = 6.88877 (7) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 524.72 (1) Å³
a = 9.37834 (7) Å	Z = ?
b = 9.37834 (7) Å	? radiation, λ = ? Å
c = 6.88877 (7) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq
Ca1	0.333333	0.666667	0.0022 (2)	0.809663
Ca2	0.24146 (12)	−0.00825 (14)	0.25	0.665979
P1	0.39863 (17)	0.36890 (16)	0.25	0.728429
O1	0.3267 (3)	0.4870 (3)	0.25	1.295546
O2	0.5906 (4)	0.4667 (4)	0.25	1.295546
O3	0.3410 (3)	0.2563 (3)	0.0688 (2)	1.295546
F1	0	0	0.25	2.251558

(Vx=0p0_restrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 524.72 (1) Å³
a = 9.37834 (7) Å	Z = ?
b = 9.37834 (7) Å	? radiation, λ = ? Å
c = 6.88877 (7) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 524.72 (1) Å³
a = 9.37834 (7) Å	Z = ?
b = 9.37834 (7) Å	? radiation, λ = ? Å
c = 6.88877 (7) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq
Ca1	0.333333	0.666667	0.0021 (2)	0.809663
Ca2	0.24151 (12)	−0.00825 (14)	0.25	0.665979
P1	0.39854 (12)	0.36890 (11)	0.25	0.728429
O1	0.3274 (2)	0.48644 (19)	0.25	1.295546
O2	0.5892 (2)	0.4658 (3)	0.25	1.295546
O3	0.3413 (3)	0.2566 (2)	0.06919 (18)	1.295546
F1	0	0	0.25	2.251558

(Vx=0p1_C-CH) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 525 (2) Å³
a = 9.38 (3) Å	Z = ?
b = 9.378214 Å	? radiation, λ = ? Å
c = 6.888 (7) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 525 (2) Å³
a = 9.38 (3) Å	Z = ?
b = 9.378214 Å	? radiation, λ = ? Å
c = 6.888 (7) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0	0.50 (4)
Ca2	0.0084 (2)	0.2502 (9)	0.25	0.27 (3)
O1	0.3265 (3)	0.4855 (6)	0.25	0.77 (5)
O2	0.5904 (4)	0.4660 (5)	0.25	0.77 (5)
P	0.3988 (8)	0.3679 (5)	0.25	0	0.9
P	0.3988 (8)	0.3679 (5)	0.25	2	0.1
O3	0.3424 (8)	0.2546 (8)	0.0677 (3)	0.77 (5)
F	0	0	0.25	1.11 (15)

(Vx=0p1_unrestrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 524.92 (3) Å³
a = 9.3801 (3) Å	Z = ?
b = 9.3801 (3) Å	? radiation, λ = ? Å
c = 6.8889 (2) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 524.92 (3) Å³
a = 9.3801 (3) Å	Z = ?
b = 9.3801 (3) Å	? radiation, λ = ? Å
c = 6.8889 (2) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0031 (5)	0.774898
Ca2	0.2425 (3)	−0.0075 (3)	0.25	0.440883
P1/V1	0.3993 (4)	0.3682 (4)	0.25	0.869392	0.9
P1/V1	0.3993 (4)	0.3682 (4)	0.25	0.869392	0.1
O1	0.3279 (8)	0.4899 (7)	0.25	1.122925
O2	0.5941 (8)	0.4678 (8)	0.25	1.122925
O3	0.3448 (6)	0.2613 (6)	0.0648 (5)	1.122925
F1	0	0	0.25	2.280982

(Vx=0p1_restrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 524.92 (3) Å³
a = 9.3801 (3) Å	Z = ?
b = 9.3801 (3) Å	? radiation, λ = ? Å
c = 6.8889 (2) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 524.92 (3) Å³
a = 9.3801 (3) Å	Z = ?
b = 9.3801 (3) Å	? radiation, λ = ? Å
c = 6.8889 (2) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0030 (5)	0.774898
Ca2	0.2428 (3)	−0.0074 (3)	0.25	0.440883
P1/V1	0.3992 (3)	0.3685 (3)	0.25	0.869392	0.9
P1/V1	0.3992 (3)	0.3685 (3)	0.25	0.869392	0.1
O1	0.3286 (5)	0.4889 (4)	0.25	1.122925
O2	0.5923 (5)	0.4662 (7)	0.25	1.122925
O3	0.3442 (5)	0.2604 (4)	0.0640 (4)	1.122925
F1	0	0	0.25	2.280982

(Vx=0p2_C-CH) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 532.8 (13) Å³
a = 9.437 (15) Å	Z = ?
b = 9.436671 Å	? radiation, λ = ? Å
c = 6.909 (4) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 532.8 (13) Å³
a = 9.437 (15) Å	Z = ?
b = 9.436671 Å	? radiation, λ = ? Å
c = 6.909 (4) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0	0.64 (3)
Ca2	0.00753 (16)	0.2488 (6)	0.25	0.411 (19)
O1	0.3267 (2)	0.4873 (3)	0.25	0.90 (4)
O2	0.5899 (3)	0.4652 (3)	0.25	0.90 (4)
P	0.3978 (5)	0.3683 (3)	0.25	0	0.8
P	0.3978 (5)	0.3683 (3)	0.25	2.35 (13)	0.2
O3	0.3407 (5)	0.2546 (5)	0.06682 (15)	0.90 (4)
F	0	0	0.25	1.27 (11)

(Vx=0p2_unrestrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 533.02 (3) Å³
a = 9.4379 (2) Å	Z = ?
b = 9.4379 (2) Å	? radiation, λ = ? Å
c = 6.90967 (17) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 533.02 (3) Å³
a = 9.4379 (2) Å	Z = ?
b = 9.4379 (2) Å	? radiation, λ = ? Å
c = 6.90967 (17) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0015 (4)	0.711874
Ca2	0.24176 (19)	−0.0067 (2)	0.25	0.573324
P1/V1	0.3982 (2)	0.3696 (2)	0.25	0.481970	0.8
P1/V1	0.3982 (2)	0.3696 (2)	0.25	0.481970	0.2
O1	0.3247 (5)	0.4869 (5)	0.25	1.310567
O2	0.5922 (5)	0.4697 (5)	0.25	1.310567
O3	0.3421 (4)	0.2556 (4)	0.0688 (4)	1.310567
F1	0	0	0.25	1.991941

(Vx=0p2_restrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 533.02 (3) Å³
a = 9.4379 (2) Å	Z = ?
b = 9.4379 (2) Å	? radiation, λ = ? Å
c = 6.90968 (17) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 533.02 (3) Å³
a = 9.4379 (2) Å	Z = ?
b = 9.4379 (2) Å	? radiation, λ = ? Å
c = 6.90968 (17) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0014 (4)	0.711874
Ca2	0.24188 (19)	−0.0067 (2)	0.25	0.573324
P1/V1	0.39819 (17)	0.36969 (16)	0.25	0.481970	0.8
P1/V1	0.39819 (17)	0.36969 (16)	0.25	0.481970	0.2
O1	0.3245 (3)	0.4870 (3)	0.25	1.310567
O2	0.5916 (3)	0.4691 (5)	0.25	1.310567
O3	0.3416 (4)	0.2547 (3)	0.0678 (3)	1.310567
F1	0	0	0.25	1.991941

(Vx=0p3_C-CH) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 537.9 (14) Å³
a = 9.472 (16) Å	Z = ?
b = 9.472342 Å	? radiation, λ = ? Å
c = 6.922 (5) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 537.9 (14) Å³
a = 9.472 (16) Å	Z = ?
b = 9.472342 Å	? radiation, λ = ? Å
c = 6.922 (5) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0	0.81 (3)
Ca2	0.00666 (16)	0.2478 (6)	0.25	0.566 (19)
O1	0.32522 (19)	0.4877 (4)	0.25	1.12 (4)
O2	0.5908 (2)	0.4663 (3)	0.25	1.12 (4)
P	0.3974 (5)	0.3684 (3)	0.25	0	0.7
P	0.3974 (5)	0.3684 (3)	0.25	1.62 (7)	0.3
O3	0.3404 (5)	0.2539 (5)	0.0653 (2)	1.12 (4)
F	0	0	0.25	1.28 (11)

(Vx=0p3_unrestrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 538.04 (3) Å³
a = 9.4733 (2) Å	Z = ?
b = 9.4733 (2) Å	? radiation, λ = ? Å
c = 6.92272 (17) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 538.04 (3) Å³
a = 9.4733 (2) Å	Z = ?
b = 9.4733 (2) Å	? radiation, λ = ? Å
c = 6.92272 (17) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0015 (4)	0.880670
Ca2	0.24145 (18)	−0.0059 (2)	0.25	0.748749
P1/V1	0.3980 (2)	0.3696 (2)	0.25	0.521135	0.7
P1/V1	0.3980 (2)	0.3696 (2)	0.25	0.521135	0.3
O1	0.3236 (5)	0.4866 (5)	0.25	1.533673
O2	0.5929 (5)	0.4707 (5)	0.25	1.533673
O3	0.3417 (4)	0.2552 (4)	0.0687 (4)	1.533673
F1	0	0	0.25	2.166388

(Vx=0p3_restrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 538.04 (3) Å³
a = 9.4733 (2) Å	Z = ?
b = 9.4733 (2) Å	? radiation, λ = ? Å
c = 6.92276 (17) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 538.04 (3) Å³
a = 9.4733 (2) Å	Z = ?
b = 9.4733 (2) Å	? radiation, λ = ? Å
c = 6.92276 (17) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0013 (3)	0.880670
Ca2	0.24161 (18)	−0.0058 (2)	0.25	0.748749
P1/V1	0.39803 (16)	0.36968 (15)	0.25	0.521135	0.7
P1/V1	0.39803 (16)	0.36968 (15)	0.25	0.521135	0.3
O1	0.3231 (3)	0.4870 (3)	0.25	1.533673
O2	0.5926 (3)	0.4703 (5)	0.25	1.533673
O3	0.3408 (4)	0.2538 (3)	0.0668 (3)	1.533673
F1	0	0	0.25	2.166388

(Vx=0p4_C-CH) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 543.3 (18) Å³
a = 9.51 (2) Å	Z = ?
b = 9.509835 Å	? radiation, λ = ? Å
c = 6.937 (6) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 543.3 (18) Å³
a = 9.51 (2) Å	Z = ?
b = 9.509835 Å	? radiation, λ = ? Å
c = 6.937 (6) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0	0.84 (4)
Ca2	0.00593 (19)	0.2471 (7)	0.25	0.53 (2)
O1	0.3246 (2)	0.4886 (4)	0.25	1.12 (4)
O2	0.5922 (3)	0.4663 (4)	0.25	1.12 (4)
P	0.3971 (7)	0.3680 (4)	0.25	0	0.6
P	0.3971 (7)	0.3680 (4)	0.25	1.15 (6)	0.4
O3	0.3395 (6)	0.2524 (6)	0.0635 (3)	1.12 (4)
F	0	0	0.25	1.31 (13)

(Vx=0p4_unrestrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 543.35 (3) Å³
a = 9.5103 (2) Å	Z = ?
b = 9.5103 (2) Å	? radiation, λ = ? Å
c = 6.93674 (18) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 543.35 (3) Å³
a = 9.5103 (2) Å	Z = ?
b = 9.5103 (2) Å	? radiation, λ = ? Å
c = 6.93674 (18) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0018 (4)	0.834320
Ca2	0.24134 (18)	−0.0053 (2)	0.25	0.771284
P1/V1	0.3980 (2)	0.36981 (19)	0.25	0.502578	0.6
P1/V1	0.3980 (2)	0.36981 (19)	0.25	0.502578	0.4
O1	0.3215 (5)	0.4856 (5)	0.25	1.539692
O2	0.5938 (5)	0.4709 (5)	0.25	1.539692
O3	0.3410 (4)	0.2545 (4)	0.0687 (4)	1.539692
F1	0	0	0.25	2.421492

(Vx=0p4_restrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 543.35 (3) Å³
a = 9.5103 (2) Å	Z = ?
b = 9.5103 (2) Å	? radiation, λ = ? Å
c = 6.93677 (18) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 543.35 (3) Å³
a = 9.5103 (2) Å	Z = ?
b = 9.5103 (2) Å	? radiation, λ = ? Å
c = 6.93677 (18) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0016 (3)	0.834320
Ca2	0.24156 (18)	−0.0051 (2)	0.25	0.771284
P1/V1	0.39809 (15)	0.36992 (14)	0.25	0.502578	0.6
P1/V1	0.39809 (15)	0.36992 (14)	0.25	0.502578	0.4
O1	0.3207 (3)	0.4861 (3)	0.25	1.539692
O2	0.5940 (3)	0.4706 (4)	0.25	1.539692
O3	0.3397 (4)	0.2525 (3)	0.0661 (3)	1.539692
F1	0	0	0.25	2.421492

(Vx=0p5_C-CH) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 550.5 (18) Å³
a = 9.57 (2) Å	Z = ?
b = 9.565158 Å	? radiation, λ = ? Å
c = 6.947 (6) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 550.5 (18) Å³
a = 9.57 (2) Å	Z = ?
b = 9.565158 Å	? radiation, λ = ? Å
c = 6.947 (6) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0	0.70 (3)
Ca2	0.00465 (19)	0.2482 (7)	0.25	0.61 (2)
O1	0.3240 (2)	0.4896 (4)	0.25	1.07 (5)
O2	0.5933 (3)	0.4681 (4)	0.25	1.07 (5)
P	0.3974 (6)	0.3691 (4)	0.25	0	0.5
P	0.3974 (6)	0.3691 (4)	0.25	0.77 (4)	0.5
O3	0.3401 (6)	0.2529 (6)	0.0620 (3)	1.07 (5)
F	0	0	0.25	2.81 (16)

(Vx=0p5_unrestrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 550.47 (3) Å³
a = 9.56534 (19) Å	Z = ?
b = 9.56534 (19) Å	? radiation, λ = ? Å
c = 6.94712 (16) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 550.47 (3) Å³
a = 9.56534 (19) Å	Z = ?
b = 9.56534 (19) Å	? radiation, λ = ? Å
c = 6.94712 (16) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0023 (3)	0.803017
Ca2	0.24346 (18)	−0.0043 (2)	0.25	0.858005
P1/V1	0.39809 (19)	0.37025 (17)	0.25	0.381452	0.5
P1/V1	0.39809 (19)	0.37025 (17)	0.25	0.381452	0.5
O1	0.3218 (5)	0.4863 (5)	0.25	1.561057
O2	0.5942 (5)	0.4709 (5)	0.25	1.561057
O3	0.3407 (4)	0.2542 (4)	0.0660 (4)	1.561057
F1	0	0	0.25	4.196881

(Vx=0p5_restrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 550.48 (3) Å³
a = 9.5654 (2) Å	Z = ?
b = 9.5654 (2) Å	? radiation, λ = ? Å
c = 6.94713 (16) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 550.48 (3) Å³
a = 9.5654 (2) Å	Z = ?
b = 9.5654 (2) Å	? radiation, λ = ? Å
c = 6.94713 (16) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0021 (3)	0.803017
Ca2	0.24359 (17)	−0.0041 (2)	0.25	0.858005
P1/V1	0.39818 (14)	0.37023 (13)	0.25	0.381452	0.5
P1/V1	0.39818 (14)	0.37023 (13)	0.25	0.381452	0.5
O1	0.3208 (3)	0.4874 (3)	0.25	1.561057
O2	0.5950 (3)	0.4712 (4)	0.25	1.561057
O3	0.3395 (4)	0.2525 (2)	0.0634 (2)	1.561057
F1	0	0	0.25	4.196881

(Vx=0p6_C-CH) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 554 (2) Å³
a = 9.58 (3) Å	Z = ?
b = 9.581942 Å	? radiation, λ = ? Å
c = 6.963 (8) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 554 (2) Å³
a = 9.58 (3) Å	Z = ?
b = 9.581942 Å	? radiation, λ = ? Å
c = 6.963 (8) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0	0.93 (5)
Ca2	0.0038 (2)	0.2453 (9)	0.25	0.61 (3)
O1	0.3245 (3)	0.4906 (5)	0.25	1.24 (6)
O2	0.5939 (4)	0.4666 (5)	0.25	1.24 (6)
P	0.3971 (8)	0.3684 (5)	0.25	0	0.4
P	0.3971 (8)	0.3684 (5)	0.25	0.76 (4)	0.6
O3	0.3389 (8)	0.2515 (7)	0.0612 (3)	1.24 (6)
F	0	0	0.25	1.31 (17)

(Vx=0p6_unrestrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 553.64 (4) Å³
a = 9.5820 (3) Å	Z = ?
b = 9.5820 (3) Å	? radiation, λ = ? Å
c = 6.9628 (2) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 553.64 (4) Å³
a = 9.5820 (3) Å	Z = ?
b = 9.5820 (3) Å	? radiation, λ = ? Å
c = 6.9628 (2) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0018 (4)	0.928721
Ca2	0.24135 (19)	−0.0035 (2)	0.25	1.023342
P1/V1	0.3978 (2)	0.37031 (18)	0.25	0.546907	0.4
P1/V1	0.3978 (2)	0.37031 (18)	0.25	0.546907	0.6
O1	0.3201 (5)	0.4857 (5)	0.25	1.815361
O2	0.5949 (5)	0.4720 (5)	0.25	1.815361
O3	0.3397 (4)	0.2533 (4)	0.0687 (4)	1.815361
F1	0	0	0.25	2.781671

(Vx=0p6_restrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 553.65 (4) Å³
a = 9.5821 (3) Å	Z = ?
b = 9.5821 (3) Å	? radiation, λ = ? Å
c = 6.9628 (2) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 553.65 (4) Å³
a = 9.5821 (3) Å	Z = ?
b = 9.5821 (3) Å	? radiation, λ = ? Å
c = 6.9628 (2) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0014 (4)	0.928721
Ca2	0.24160 (18)	−0.0032 (2)	0.25	1.023342
P1/V1	0.39772 (15)	0.37030 (14)	0.25	0.546907	0.4
P1/V1	0.39772 (15)	0.37030 (14)	0.25	0.546907	0.6
O1	0.3184 (3)	0.4870 (3)	0.25	1.815361
O2	0.5959 (3)	0.4724 (5)	0.25	1.815361
O3	0.3384 (4)	0.2506 (3)	0.0648 (3)	1.815361
F1	0	0	0.25	2.781671

(Vx=0p7_C-CH) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 556 (3) Å³
a = 9.60 (3) Å	Z = ?
b = 9.598996 Å	? radiation, λ = ? Å
c = 6.969 (10) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 556 (3) Å³
a = 9.60 (3) Å	Z = ?
b = 9.598996 Å	? radiation, λ = ? Å
c = 6.969 (10) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0	1.00 (7)
Ca2	0.0045 (3)	0.2442 (12)	0.25	0.35 (4)
O1	0.3248 (4)	0.4912 (7)	0.25	1.14 (8)
O2	0.5953 (5)	0.4667 (6)	0.25	1.14 (8)
P	0.3976 (11)	0.3684 (6)	0.25	0	0.3
P	0.3976 (11)	0.3684 (6)	0.25	0.29 (4)	0.7
O3	0.3392 (11)	0.2509 (10)	0.0603 (4)	1.14 (8)
F	0	0	0.25	2

(Vx=0p7_unrestrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 556.73 (6) Å³
a = 9.6029 (5) Å	Z = ?
b = 9.6029 (5) Å	? radiation, λ = ? Å
c = 6.9712 (4) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 556.73 (6) Å³
a = 9.6029 (5) Å	Z = ?
b = 9.6029 (5) Å	? radiation, λ = ? Å
c = 6.9712 (4) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0014 (5)	0.86846
Ca2	0.2402 (3)	−0.0034 (3)	0.25	1.054825
P1/V1	0.3980 (3)	0.3711 (2)	0.25	0.559052	0.3
P1/V1	0.3980 (3)	0.3711 (2)	0.25	0.559052	0.7
O1	0.3189 (7)	0.4850 (6)	0.25	1.74186
O2	0.5943 (7)	0.4697 (7)	0.25	1.74186
O3	0.3397 (6)	0.2530 (5)	0.0687 (5)	1.74186
F1	0	0	0.25	3.41911

(Vx=0p7_restrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 556.74 (7) Å³
a = 9.6029 (5) Å	Z = ?
b = 9.6029 (5) Å	? radiation, λ = ? Å
c = 6.9713 (4) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 556.74 (7) Å³
a = 9.6029 (5) Å	Z = ?
b = 9.6029 (5) Å	? radiation, λ = ? Å
c = 6.9713 (4) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0012 (5)	0.86846
Ca2	0.2407 (2)	−0.0029 (3)	0.25	1.054825
P1/V1	0.3980 (2)	0.37133 (19)	0.25	0.559052	0.3
P1/V1	0.3980 (2)	0.37133 (19)	0.25	0.559052	0.7
O1	0.3168 (4)	0.4870 (4)	0.25	1.74186
O2	0.5971 (4)	0.4705 (6)	0.25	1.74186
O3	0.3385 (5)	0.2499 (3)	0.0638 (3)	1.74186
F1	0	0	0.25	3.41911

(Vx=0p8_C-CH) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 563 (4) Å³
a = 9.65 (5) Å	Z = ?
b = 9.646212 Å	? radiation, λ = ? Å
c = 6.981 (14) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 563 (4) Å³
a = 9.65 (5) Å	Z = ?
b = 9.646212 Å	? radiation, λ = ? Å
c = 6.981 (14) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0	1.06 (10)
Ca2	0.0037 (5)	0.2433 (17)	0.25	0.25 (5)
O1	0.3246 (5)	0.4923 (10)	0.25	1.20 (11)
O2	0.5957 (6)	0.4660 (8)	0.25	1.20 (11)
P	0.3969 (15)	0.3681 (9)	0.25	0	0.2
P	0.3969 (15)	0.3681 (9)	0.25	0.2	0.8
O3	0.3379 (14)	0.2499 (13)	0.0588 (6)	1.20 (11)
F	0	0	0.25	1.6

(Vx=0p8_unrestrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 562.81 (10) Å³
a = 9.6454 (7) Å	Z = ?
b = 9.6454 (7) Å	? radiation, λ = ? Å
c = 6.9855 (6) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 562.81 (10) Å³
a = 9.6454 (7) Å	Z = ?
b = 9.6454 (7) Å	? radiation, λ = ? Å
c = 6.9855 (6) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0019 (6)	0.987961
Ca2	0.2398 (3)	−0.0033 (4)	0.25	1.050758
P1/V1	0.3974 (3)	0.3700 (3)	0.25	0.371541	0.2
P1/V1	0.3974 (3)	0.3700 (3)	0.25	0.371541	0.8
O1	0.3166 (9)	0.4870 (8)	0.25	1.744234
O2	0.5928 (9)	0.4699 (9)	0.25	1.744234
O3	0.3394 (7)	0.2533 (7)	0.0673 (6)	1.744234
F1	0	0	0.25	3.25111

(Vx=0p8_restrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 562.80 (10) Å³
a = 9.6452 (7) Å	Z = ?
b = 9.6452 (7) Å	? radiation, λ = ? Å
c = 6.9855 (6) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 562.80 (10) Å³
a = 9.6452 (7) Å	Z = ?
b = 9.6452 (7) Å	? radiation, λ = ? Å
c = 6.9855 (6) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0014 (6)	0.987961
Ca2	0.2404 (3)	−0.0027 (4)	0.25	1.050758
P1/V1	0.3972 (2)	0.3706 (2)	0.25	0.371541	0.2
P1/V1	0.3972 (2)	0.3706 (2)	0.25	0.371541	0.8
O1	0.3152 (5)	0.4885 (4)	0.25	1.744234
O2	0.5969 (5)	0.4711 (7)	0.25	1.744234
O3	0.3392 (6)	0.2497 (4)	0.0616 (4)	1.744234
F1	0	0	0.25	3.25111

(Vx=0p9_C-CH) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 568 (4) Å³
a = 9.68 (4) Å	Z = ?
b = 9.680008 Å	? radiation, λ = ? Å
c = 6.999 (12) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 568 (4) Å³
a = 9.68 (4) Å	Z = ?
b = 9.680008 Å	? radiation, λ = ? Å
c = 6.999 (12) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0	1.18 (8)
Ca2	0.0031 (4)	0.2446 (14)	0.25	0.49 (4)
O1	0.3241 (4)	0.4931 (8)	0.25	1.21 (9)
O2	0.5963 (5)	0.4674 (7)	0.25	1.21 (9)
P	0.3971 (12)	0.3691 (7)	0.25	0	0.1
P	0.3971 (12)	0.3691 (7)	0.25	0.45 (4)	0.9
O3	0.3383 (12)	0.2504 (11)	0.0583 (5)	1.21 (9)
F	0	0	0.25	2

(Vx=0p9_unrestrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 568.39 (6) Å³
a = 9.6819 (5) Å	Z = ?
b = 9.6819 (5) Å	? radiation, λ = ? Å
c = 7.0015 (4) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 568.39 (6) Å³
a = 9.6819 (5) Å	Z = ?
b = 9.6819 (5) Å	? radiation, λ = ? Å
c = 7.0015 (4) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0011 (6)	1.207491
Ca2	0.2404 (3)	−0.0034 (4)	0.25	1.052215
P1/V1	0.3976 (3)	0.3690 (3)	0.25	0.454766	0.1
P1/V1	0.3976 (3)	0.3690 (3)	0.25	0.454766	0.9
O1	0.3188 (8)	0.4918 (8)	0.25	1.718776
O2	0.5946 (8)	0.4704 (8)	0.25	1.718776
O3	0.3434 (7)	0.2588 (6)	0.0672 (6)	1.718776
F1	0	0	0.25	4.420721

(Vx=0p9_restrained) top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 568.36 (7) Å³
a = 9.6817 (5) Å	Z = ?
b = 9.6817 (5) Å	? radiation, λ = ? Å
c = 7.0014 (4) Å	× × mm
α = 90°

Data collection top

h = ?→?	l = ?→?
k = ?→?

Refinement top

Crystal data top

?	β = 90°
M_r = ?	γ = 120°
?, ?	V = 568.36 (7) Å³
a = 9.6817 (5) Å	Z = ?
b = 9.6817 (5) Å	? radiation, λ = ? Å
c = 7.0014 (4) Å	× × mm
α = 90°

Data collection top

Refinement top

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

	x	y	z	B_iso*/B_eq	Occ. (<1)
Ca1	0.333333	0.666667	0.0008 (6)	1.207491
Ca2	0.2418 (3)	−0.0020 (4)	0.25	1.052215
P1/V1	0.3965 (2)	0.3698 (2)	0.25	0.454766	0.1
P1/V1	0.3965 (2)	0.3698 (2)	0.25	0.454766	0.9
O1	0.3191 (5)	0.4928 (4)	0.25	1.718776
O2	0.5971 (4)	0.4668 (7)	0.25	1.718776
O3	0.3412 (6)	0.2517 (4)	0.0583 (4)	1.718776
F1	0	0	0.25	4.420721

Experimental details

	(Vx=0p0_C-CH)	(Vx=0p0_unrestrained)	(Vx=0p0_restrained)	(Vx=0p1_C-CH)
Crystal data
Chemical formula	?	?	?	?
M_r	?	?	?	?
Crystal system, space group	?, ?	?, ?	?, ?	?, ?
Temperature (K)	?	?	?	?
a, b, c (Å)	9.377 (11), 9.377318, 6.888 (4)	9.37834 (7), 9.37834 (7), 6.88877 (7)	9.37834 (7), 9.37834 (7), 6.88877 (7)	9.38 (3), 9.378214, 6.888 (7)
α, β, γ (°)	90, 90, 120	90, 90, 120	90, 90, 120	90, 90, 120
V (Å³)	524.5 (10)	524.72 (1)	524.72 (1)	525 (2)
Z	?	?	?	?
Radiation type	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å
µ (mm⁻¹)	?	?	?	?
Crystal size (mm)	× ×	× ×	× ×	× ×

Data collection
Diffractometer	?	?	?	?
Absorption correction	?	?	?	?
No. of measured, independent and observed (?) reflections	?, ?, ?	?, ?, ?	?, ?, ?	?, ?, ?
R_int	?	?	?	?

Refinement
R[F² > 2σ(F²)], wR(F²), S	?, ?, ?	?, ?, ?	?, ?, ?	?, ?, ?
No. of reflections	?	?	?	?
No. of parameters	?	?	?	?
No. of restraints	?	?	?	?
Δρ_max, Δρ_min (e Å⁻³)	?, ?	?, ?	?, ?	?, ?

	(Vx=0p1_unrestrained)	(Vx=0p1_restrained)	(Vx=0p2_C-CH)	(Vx=0p2_unrestrained)
Crystal data
Chemical formula	?	?	?	?
M_r	?	?	?	?
Crystal system, space group	?, ?	?, ?	?, ?	?, ?
Temperature (K)	?	?	?	?
a, b, c (Å)	9.3801 (3), 9.3801 (3), 6.8889 (2)	9.3801 (3), 9.3801 (3), 6.8889 (2)	9.437 (15), 9.436671, 6.909 (4)	9.4379 (2), 9.4379 (2), 6.90967 (17)
α, β, γ (°)	90, 90, 120	90, 90, 120	90, 90, 120	90, 90, 120
V (Å³)	524.92 (3)	524.92 (3)	532.8 (13)	533.02 (3)
Z	?	?	?	?
Radiation type	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å
µ (mm⁻¹)	?	?	?	?
Crystal size (mm)	× ×	× ×	× ×	× ×

Data collection
Diffractometer	?	?	?	?
Absorption correction	?	?	?	?
No. of measured, independent and observed (?) reflections	?, ?, ?	?, ?, ?	?, ?, ?	?, ?, ?
R_int	?	?	?	?

Refinement
R[F² > 2σ(F²)], wR(F²), S	?, ?, ?	?, ?, ?	?, ?, ?	?, ?, ?
No. of reflections	?	?	?	?
No. of parameters	?	?	?	?
No. of restraints	?	?	?	?
Δρ_max, Δρ_min (e Å⁻³)	?, ?	?, ?	?, ?	?, ?

	(Vx=0p2_restrained)	(Vx=0p3_C-CH)	(Vx=0p3_unrestrained)	(Vx=0p3_restrained)
Crystal data
Chemical formula	?	?	?	?
M_r	?	?	?	?
Crystal system, space group	?, ?	?, ?	?, ?	?, ?
Temperature (K)	?	?	?	?
a, b, c (Å)	9.4379 (2), 9.4379 (2), 6.90968 (17)	9.472 (16), 9.472342, 6.922 (5)	9.4733 (2), 9.4733 (2), 6.92272 (17)	9.4733 (2), 9.4733 (2), 6.92276 (17)
α, β, γ (°)	90, 90, 120	90, 90, 120	90, 90, 120	90, 90, 120
V (Å³)	533.02 (3)	537.9 (14)	538.04 (3)	538.04 (3)
Z	?	?	?	?
Radiation type	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å
µ (mm⁻¹)	?	?	?	?
Crystal size (mm)	× ×	× ×	× ×	× ×

Data collection
Diffractometer	?	?	?	?
Absorption correction	?	?	?	?
No. of measured, independent and observed (?) reflections	?, ?, ?	?, ?, ?	?, ?, ?	?, ?, ?
R_int	?	?	?	?

Refinement
R[F² > 2σ(F²)], wR(F²), S	?, ?, ?	?, ?, ?	?, ?, ?	?, ?, ?
No. of reflections	?	?	?	?
No. of parameters	?	?	?	?
No. of restraints	?	?	?	?
Δρ_max, Δρ_min (e Å⁻³)	?, ?	?, ?	?, ?	?, ?

	(Vx=0p4_C-CH)	(Vx=0p4_unrestrained)	(Vx=0p4_restrained)	(Vx=0p5_C-CH)
Crystal data
Chemical formula	?	?	?	?
M_r	?	?	?	?
Crystal system, space group	?, ?	?, ?	?, ?	?, ?
Temperature (K)	?	?	?	?
a, b, c (Å)	9.51 (2), 9.509835, 6.937 (6)	9.5103 (2), 9.5103 (2), 6.93674 (18)	9.5103 (2), 9.5103 (2), 6.93677 (18)	9.57 (2), 9.565158, 6.947 (6)
α, β, γ (°)	90, 90, 120	90, 90, 120	90, 90, 120	90, 90, 120
V (Å³)	543.3 (18)	543.35 (3)	543.35 (3)	550.5 (18)
Z	?	?	?	?
Radiation type	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å
µ (mm⁻¹)	?	?	?	?
Crystal size (mm)	× ×	× ×	× ×	× ×

Data collection
Diffractometer	?	?	?	?
Absorption correction	?	?	?	?
No. of measured, independent and observed (?) reflections	?, ?, ?	?, ?, ?	?, ?, ?	?, ?, ?
R_int	?	?	?	?

Refinement
R[F² > 2σ(F²)], wR(F²), S	?, ?, ?	?, ?, ?	?, ?, ?	?, ?, ?
No. of reflections	?	?	?	?
No. of parameters	?	?	?	?
No. of restraints	?	?	?	?
Δρ_max, Δρ_min (e Å⁻³)	?, ?	?, ?	?, ?	?, ?

	(Vx=0p5_unrestrained)	(Vx=0p5_restrained)	(Vx=0p6_C-CH)	(Vx=0p6_unrestrained)
Crystal data
Chemical formula	?	?	?	?
M_r	?	?	?	?
Crystal system, space group	?, ?	?, ?	?, ?	?, ?
Temperature (K)	?	?	?	?
a, b, c (Å)	9.56534 (19), 9.56534 (19), 6.94712 (16)	9.5654 (2), 9.5654 (2), 6.94713 (16)	9.58 (3), 9.581942, 6.963 (8)	9.5820 (3), 9.5820 (3), 6.9628 (2)
α, β, γ (°)	90, 90, 120	90, 90, 120	90, 90, 120	90, 90, 120
V (Å³)	550.47 (3)	550.48 (3)	554 (2)	553.64 (4)
Z	?	?	?	?
Radiation type	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å
µ (mm⁻¹)	?	?	?	?
Crystal size (mm)	× ×	× ×	× ×	× ×

Data collection
Diffractometer	?	?	?	?
Absorption correction	?	?	?	?
No. of measured, independent and observed (?) reflections	?, ?, ?	?, ?, ?	?, ?, ?	?, ?, ?
R_int	?	?	?	?

Refinement
R[F² > 2σ(F²)], wR(F²), S	?, ?, ?	?, ?, ?	?, ?, ?	?, ?, ?
No. of reflections	?	?	?	?
No. of parameters	?	?	?	?
No. of restraints	?	?	?	?
Δρ_max, Δρ_min (e Å⁻³)	?, ?	?, ?	?, ?	?, ?

	(Vx=0p6_restrained)	(Vx=0p7_C-CH)	(Vx=0p7_unrestrained)	(Vx=0p7_restrained)
Crystal data
Chemical formula	?	?	?	?
M_r	?	?	?	?
Crystal system, space group	?, ?	?, ?	?, ?	?, ?
Temperature (K)	?	?	?	?
a, b, c (Å)	9.5821 (3), 9.5821 (3), 6.9628 (2)	9.60 (3), 9.598996, 6.969 (10)	9.6029 (5), 9.6029 (5), 6.9712 (4)	9.6029 (5), 9.6029 (5), 6.9713 (4)
α, β, γ (°)	90, 90, 120	90, 90, 120	90, 90, 120	90, 90, 120
V (Å³)	553.65 (4)	556 (3)	556.73 (6)	556.74 (7)
Z	?	?	?	?
Radiation type	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å
µ (mm⁻¹)	?	?	?	?
Crystal size (mm)	× ×	× ×	× ×	× ×

Data collection
Diffractometer	?	?	?	?
Absorption correction	?	?	?	?
No. of measured, independent and observed (?) reflections	?, ?, ?	?, ?, ?	?, ?, ?	?, ?, ?
R_int	?	?	?	?

Refinement
R[F² > 2σ(F²)], wR(F²), S	?, ?, ?	?, ?, ?	?, ?, ?	?, ?, ?
No. of reflections	?	?	?	?
No. of parameters	?	?	?	?
No. of restraints	?	?	?	?
Δρ_max, Δρ_min (e Å⁻³)	?, ?	?, ?	?, ?	?, ?

	(Vx=0p8_C-CH)	(Vx=0p8_unrestrained)	(Vx=0p8_restrained)	(Vx=0p9_C-CH)
Crystal data
Chemical formula	?	?	?	?
M_r	?	?	?	?
Crystal system, space group	?, ?	?, ?	?, ?	?, ?
Temperature (K)	?	?	?	?
a, b, c (Å)	9.65 (5), 9.646212, 6.981 (14)	9.6454 (7), 9.6454 (7), 6.9855 (6)	9.6452 (7), 9.6452 (7), 6.9855 (6)	9.68 (4), 9.680008, 6.999 (12)
α, β, γ (°)	90, 90, 120	90, 90, 120	90, 90, 120	90, 90, 120
V (Å³)	563 (4)	562.81 (10)	562.80 (10)	568 (4)
Z	?	?	?	?
Radiation type	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å
µ (mm⁻¹)	?	?	?	?
Crystal size (mm)	× ×	× ×	× ×	× ×

Data collection
Diffractometer	?	?	?	?
Absorption correction	?	?	?	?
No. of measured, independent and observed (?) reflections	?, ?, ?	?, ?, ?	?, ?, ?	?, ?, ?
R_int	?	?	?	?

Refinement
R[F² > 2σ(F²)], wR(F²), S	?, ?, ?	?, ?, ?	?, ?, ?	?, ?, ?
No. of reflections	?	?	?	?
No. of parameters	?	?	?	?
No. of restraints	?	?	?	?
Δρ_max, Δρ_min (e Å⁻³)	?, ?	?, ?	?, ?	?, ?

	(Vx=0p9_unrestrained)	(Vx=0p9_restrained)
Crystal data
Chemical formula	?	?
M_r	?	?
Crystal system, space group	?, ?	?, ?
Temperature (K)	?	?
a, b, c (Å)	9.6819 (5), 9.6819 (5), 7.0015 (4)	9.6817 (5), 9.6817 (5), 7.0014 (4)
α, β, γ (°)	90, 90, 120	90, 90, 120
V (Å³)	568.39 (6)	568.36 (7)
Z	?	?
Radiation type	?, λ = ? Å	?, λ = ? Å
µ (mm⁻¹)	?	?
Crystal size (mm)	× ×	× ×

Data collection
Diffractometer	?	?
Absorption correction	?	?
No. of measured, independent and observed (?) reflections	?, ?, ?	?, ?, ?
R_int	?	?

Refinement
R[F² > 2σ(F²)], wR(F²), S	?, ?, ?	?, ?, ?
No. of reflections	?	?
No. of parameters	?	?
No. of restraints	?	?
Δρ_max, Δρ_min (e Å⁻³)	?, ?	?, ?

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Format		BIBTeX
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Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text