Cluster configurations in modulated EuVxMo8±yO14 crystals

Leligny, H.; Grebille, D.; Roussel, P.; Labbé, Ph.; Hervieu, M.; Raveau, B.; Tortelier, J.; Gougeon, P.

doi:10.1107/S0108768199000452

Cluster configurations in modulated EuV_xMo_8±yO₁₄ crystals

H. Leligny, D. Grebille, P. Roussel, Ph. Labbé, M. Hervieu, B. Raveau, J. Tortelier and P. Gougeon

Three orthorhombic crystals of chemical formula Eu_xV_yMo_8±zO₁₄ were investigated by X-ray diffraction (Mo Kα radiation, λ = 0.71073 Å). They have nearly the same lattice parameters (a ≃ 11.3, b ≃ 10.0, c ≃ 9.2 Å), display one-dimensional incommensurate modulations of wavevector q* = γc* and are characterized by the same superspace group Cmca(00γ)s00. The crystals differ both in their compositions (namely Eu_0.976(6)V_1.13(5)Mo_7.10(5)O₁₄, Eu_0.986(4)V_1.10(3)Mo_7.30(1)O₁₄ and EuMo_7.96(1)O₁₄) and in their γ components [0.195 (2), 0.245 (2) and 0.286 (3), respectively]. The average structures of these crystals appear closely related to the structures of LaMo_7.7O₁₄ (not modulated) and LaMo₈O₁₄ (modulated); however, two main differences are outlined: first, the modulation direction is c in the Eu-containing crystals but b in the modulated La-containing crystal [q* = (1/3)b*], second, the Eu-containing crystals have centrosymmetric structures while the La-containing crystals have polar structures (space group C2ca). The Mo (or Mo and V) atoms are stacked to form (001) layers of metallic clusters. The density modulation of these structures implies the existence of the new types of clusters Mo₉, Mo₁₀, Mo₆V₄, Mo₇V₃ and Mo₈V₂ besides the clusters M₈ (Mo₈, Mo₆V₂ and Mo₇V) and M₇ (Mo₇ and Mo₆V) which are already known. Mo₈ units with cis and trans configurations and Mo₆V₂ units with a trans configuration appear as the main cluster types in these crystals. The nature of the metallic clusters changes along c, but inside one (001) layer it is likely that only one cluster type with a given configuration is present. The main structural result is the formation, in some unit cells, of strong intercluster Mo—Mo, Mo—V or V—V bonds with distances close to 2.6 Å within a layer as well as between two neighbouring layers.

Keywords: modulated stuctures; europium molybdenum oxide; europium molybdenum vanadium oxide.

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Supporting information

	Crystallographic Information File (CIF) Contains datablocks Crystal1, Crystal2, Crystal3
	Structure factor file (CIF format) Contains datablock Crystal1
	Structure factor file (CIF format) Contains datablock Crystal2
	Structure factor file (CIF format) Contains datablock Crystal3

Computing details top

Figures top

(Crystal1) top

Crystal data top

Eu_0.976(6)V_1.13(5)Mo_7.10(5)O₁₄	F(000) = 1992
M_r = ?	D_x = 7.02 Mg m⁻³
Orthorhombic, ?	Mo Kα radiation, λ = 0.71073 Å
q = 0.195(2)c*	Cell parameters from 25 reflections
a = 11.306 (1) Å	θ = 18–25°
b = 10.025 (1) Å	µ = 14.8 mm⁻¹
c = 9.254 (1) Å	T = 293 K
V = 1048.9 (2) Å³	× × mm
Z = 4

Data collection top

CAD4 diffractometer	θ_max = 45.0°, θ_min = 3.5°
θ/2/3θ scans	h = 0→22
Absorption correction: gaussian ?	k = 0→19
T_min = 0.26, T_max = 0.42	l = 0→18
13556 measured reflections	3 standard reflections every 3600 min
2711 reflections with I > 3σ(I)	intensity decay: 0.1%
R_int = 0.030

Refinement top

Refinement on F	Unit
R[F² > 2σ(F²)] = 0.041	(Δ/σ)_max = 0.002
wR(F²) = 0.0481	Δρ_max = 3.5 e Å⁻³
132 parameters	Δρ_min = −3.6 e Å⁻³

Crystal data top

Eu_0.976(6)V_1.13(5)Mo_7.10(5)O₁₄	V = 1048.9 (2) Å³
M_r = ?	Z = 4
Orthorhombic, ?	Mo Kα radiation
q = 0.195(2)c*	µ = 14.8 mm⁻¹
a = 11.306 (1) Å	T = 293 K
b = 10.025 (1) Å	× × mm
c = 9.254 (1) Å

Data collection top

CAD4 diffractometer	2711 reflections with I > 3σ(I)
Absorption correction: gaussian ?	R_int = 0.030
T_min = 0.26, T_max = 0.42	3 standard reflections every 3600 min
13556 measured reflections	intensity decay: 0.1%

Refinement top

R[F² > 2σ(F²)] = 0.041	Δρ_max = 3.5 e Å⁻³
wR(F²) = 0.0481	Δρ_min = −3.6 e Å⁻³
132 parameters

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Eu	0.0022 (8)	0	0	0.0200 (5)	0.488 (3)
Mo1	−0.12075 (4)	0.07793 (4)	0.37758 (4)	0.0054 (1)	0.93 (1)
V1	−0.12075 (4)	0.07793 (4)	0.37758 (4)	0.0054 (1)	0.07 (1)
Mo3	0	−0.16077 (4)	0.38118 (5)	0.0063 (1)	0.93 (1)
V3	0	−0.16077 (4)	0.38118 (5)	0.0063 (1)	0.07 (1)
Mo4	0.2331 (8)	−0.1609 (8)	0.371 (1)	0.0106 (1)	0.380 (4)
V4	0.2410 (6)	−0.1656 (5)	0.3783 (7)	0.0106 (1)	0.178 (2)
O1	0.2547 (5)	0	0.5	0.0100 (7)
O2	0	−0.1596 (4)	−0.2388 (4)	0.0082 (6)
O3	−0.1227 (3)	−0.0823 (3)	0.2444 (4)	0.0100 (5)
O5	−0.25	0.1694 (4)	0.25	0.0077 (7)
O6	0.1223 (3)	0.2516 (3)	0.4915 (4)	0.0111 (5)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Eu	0.023 (1)	0.029 (2)	0.0097 (5)	0	0	−0.009 (1)
Mo1	0.0043 (1)	0.0060 (1)	0.0059 (1)	0.0007 (1)	−0.0005 (1)	0.0015 (1)
V1	0.0043 (1)	0.0060 (1)	0.0059 (1)	0.0007 (1)	−0.0005 (1)	0.0015 (1)
Mo3	0.0088 (2)	0.0046 (2)	0.0055 (2)	0	0	0.0004 (1)
V3	0.0088 (2)	0.0046 (2)	0.0055 (2)	0	0	0.0004 (1)
Mo4	0.010 (2)	0.011 (2)	0.010 (2)	−0.004 (1)	−0.008 (1)	0.008 (1)
V4	0.010 (2)	0.011 (2)	0.010 (2)	−0.004 (1)	−0.008 (1)	0.008 (1)

Bond lengths (Å) top

Eu—Eu	0.631 (3)	Mo4—O3	1.885 (6)
Eu—Mo4	3.366 (5)	Mo4—O3	2.101 (6)
Eu—Mo4	3.366 (5)	Mo4—O5	2.044 (7)
Eu—V4	3.294 (2)	Mo4—O5	3.514 (5)
Eu—V4	3.294 (2)	Mo4—O5	3.501 (7)
Eu—O1	3.089 (6)	Mo4—O6	2.164 (6)
Eu—O1	2.457 (6)	Mo4—O6	2.004 (6)
Eu—O2	2.746 (4)	V4—V4	2.824
Eu—O2	2.746 (4)	V4—V4	2.3837
Eu—O3	2.949 (4)	V4—O1	2.0121 (4)
Eu—O3	2.635 (4)	V4—O3	2.006 (3)
Eu—O3	2.635 (4)	V4—O3	2.088 (3)
Eu—O3	2.949 (4)	V4—O5	2.038 (4)
Eu—O6	2.711 (4)	V4—O6	2.043 (3)
Eu—O6	3.016 (4)	V4—O6	1.998 (3)
Eu—O6	3.016 (4)	O1—O3	2.916 (4)
Eu—O6	2.711 (4)	O1—O3	2.916 (4)
Mo1—Mo1	2.7304 (6)	O1—O3	2.777 (4)
Mo1—Mo1	2.7522 (5)	O1—O3	2.777 (4)
Mo1—Mo3	2.7553 (6)	O1—O5	2.871 (2)
Mo1—Mo3	2.7453 (6)	O1—O5	2.871 (2)
Mo1—Mo4	3.096 (5)	O1—O6	2.934 (4)
Mo1—Mo4	2.780 (5)	O1—O6	2.853 (4)
Mo1—Mo4	2.712 (5)	O1—O6	2.853 (4)
Mo1—V4	3.0087 (4)	O1—O6	2.934 (4)
Mo1—V4	2.7792 (4)	O2—O3	2.794 (5)
Mo1—V4	2.7946 (4)	O2—O3	2.794 (5)
Mo1—O1	2.046 (4)	O2—O3	2.941 (5)
Mo1—O2	2.045 (3)	O2—O3	2.941 (5)
Mo1—O3	2.025 (3)	O2—O5	2.8301 (3)
Mo1—O5	2.091 (2)	O2—O5	2.8301 (3)
Mo1—O6	2.035 (3)	O2—O6	2.870 (5)
Mo3—Mo4	2.638 (5)	O2—O6	2.870 (5)
Mo3—Mo4	2.638 (5)	O2—O6	2.818 (5)
Mo3—V4	2.7255	O2—O6	2.818 (5)
Mo3—V4	2.7255	O3—O3	2.775 (4)
Mo3—O2	2.116 (4)	O3—O3	2.880 (4)
Mo3—O3	2.036 (3)	O3—O5	2.905 (5)
Mo3—O3	2.036 (3)	O3—O5	2.875 (5)
Mo3—O6	2.032 (3)	O3—O6	2.976 (5)
Mo3—O6	2.032 (3)	O3—O6	2.746 (5)
Mo4—Mo4	3.007 (8)	O5—O6	2.785 (4)
Mo4—Mo4	2.270 (7)	O5—O6	2.904 (4)
Mo4—V4	0.122 (5)	O5—O6	2.904 (4)
Mo4—V4	2.914 (5)	O5—O6	2.785 (4)
Mo4—V4	2.325 (5)	O6—O6	2.891 (5)
Mo4—O1	2.023 (5)	O6—O6	2.766 (5)
Mo4—O2	3.349 (6)

(Crystal2) top

Crystal data top

Eu_0.986(4)V_1.10(3)Mo_7.30(1)O₁₄	F(000) = 2024
M_r = ?	D_x = 7.15 Mg m⁻³
Orthorhombic, ?	Mo Kα radiation, λ = 0.71073 Å
q = 0.245(2)c*	Cell parameters from 25 reflections
a = 11.325 (1) Å	θ = 18–25°
b = 10.024 (1) Å	µ = 15.2 mm⁻¹
c = 9.240 (1) Å	T = 293 K
V = 1048.9 (2) Å³	× × mm
Z = 4

Data collection top

CAD4 diffractometer	θ_max = 45.0°, θ_min = 3.5°
θ/θ scans	h = 0→22
Absorption correction: gaussian ?	k = 0→19
T_min = 0.23, T_max = 0.49	l = 0→18
13556 measured reflections	3 standard reflections every 3600 min
2423 reflections with I > 3σ(I)	intensity decay: 0.1%
R_int = 0.031

Refinement top

Refinement on F	Unit
R[F² > 2σ(F²)] = 0.041	(Δ/σ)_max = 0.002
wR(F²) = 0.0449	Δρ_max = 3.0 e Å⁻³
134 parameters	Δρ_min = −3.7 e Å⁻³

Crystal data top

Eu_0.986(4)V_1.10(3)Mo_7.30(1)O₁₄	V = 1048.9 (2) Å³
M_r = ?	Z = 4
Orthorhombic, ?	Mo Kα radiation
q = 0.245(2)c*	µ = 15.2 mm⁻¹
a = 11.325 (1) Å	T = 293 K
b = 10.024 (1) Å	× × mm
c = 9.240 (1) Å

Data collection top

CAD4 diffractometer	2423 reflections with I > 3σ(I)
Absorption correction: gaussian ?	R_int = 0.031
T_min = 0.23, T_max = 0.49	3 standard reflections every 3600 min
13556 measured reflections	intensity decay: 0.1%

Refinement top

R[F² > 2σ(F²)] = 0.041	Δρ_max = 3.0 e Å⁻³
wR(F²) = 0.0449	Δρ_min = −3.7 e Å⁻³
134 parameters

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Eu	0.0021 (6)	0	0	0.0180 (5)	0.493 (2)
Mo1	−0.12057 (4)	0.07766 (4)	0.37728 (4)	0.00516 (6)
Mo3	0	−0.16060 (5)	0.38162 (5)	0.00603 (8)
Mo4	0.238 (1)	−0.159 (1)	0.371 (3)	0.016 (5)	0.325 (3)
V4	0.2424 (5)	−0.1676 (4)	0.377 (3)	0.016 (5)	0.274 (6)
O1	0.2531 (4)	0	0.5	0.008 (1)
O2	0	−0.1589 (4)	−0.2385 (5)	0.0071 (6)
O3	−0.1224 (3)	−0.0835 (3)	0.2449 (4)	0.0094 (5)
O5	−0.25	0.1684 (5)	0.25	0.0071 (8)
O6	0.1221 (3)	0.2508 (3)	0.4910 (4)	0.0090 (5)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Eu	0.020 (1)	0.024 (2)	0.0087 (5)	0	0	−0.006 (1)
Mo1	0.0047 (1)	0.0068 (1)	0.0039 (1)	0.0004 (1)	−0.0003 (1)	0.0013 (1)
Mo3	0.0092 (2)	0.0051 (2)	0.0038 (2)	0	0	0.0006 (1)
Mo4	0.023 (2)	0.017 (2)	0.009 (1)	−0.008 (1)	−0.011 (1)	0.004 (1)
V4	0.023 (2)	0.017 (2)	0.009 (1)	−0.008 (1)	−0.011 (1)	0.004 (1)

Bond lengths (Å) top

Eu—Eu	0.664 (3)	Mo3—O2	2.122 (4)
Eu—Mo4	3.31 (1)	Mo3—O3	2.029 (3)
Eu—Mo4	3.31 (1)	Mo3—O3	2.029 (3)
Eu—V4	3.285 (2)	Mo3—O6	2.029 (3)
Eu—V4	3.285 (2)	Mo3—O6	2.029 (3)
Eu—O1	3.128 (6)	Mo4—Eu	3.31 (1)
Eu—O1	2.464 (6)	Mo4—Mo1	3.09 (1)
Eu—O2	2.739 (4)	Mo4—Mo1	2.81 (1)
Eu—O2	2.739 (4)	Mo4—Mo1	2.72 (1)
Eu—O3	2.962 (4)	Mo4—Mo3	2.70 (1)
Eu—O3	2.633 (4)	Mo4—Mo4	3.02 (2)
Eu—O3	2.633 (4)	Mo4—Mo4	2.24 (2)
Eu—O3	2.962 (4)	Mo4—V4	0.12 (1)
Eu—O6	2.711 (4)	Mo4—V4	2.91 (1)
Eu—O6	3.031 (4)	Mo4—V4	2.30 (1)
Eu—O6	3.031 (4)	Mo4—O1	2.00 (1)
Eu—O6	2.711 (4)	Mo4—O2	3.41 (1)
Mo1—Mo1	2.7309 (6)	Mo4—O3	1.91 (1)
Mo1—Mo1	2.7509 (5)	Mo4—O3	2.05 (1)
Mo1—Mo3	2.7513 (6)	Mo4—O5	2.06 (1)
Mo1—Mo3	2.7420 (6)	Mo4—O5	3.51 (1)
Mo1—Mo4	3.09 (1)	Mo4—O5	3.47 (1)
Mo1—Mo4	2.81 (1)	Mo4—O6	2.14 (1)
Mo1—Mo4	2.72 (1)	Mo4—O6	2.05 (1)
Mo1—V4	2.9867 (4)	V4—Eu	3.285 (2)
Mo1—V4	2.8007 (4)	V4—Mo1	2.9867 (4)
Mo1—V4	2.8205 (4)	V4—Mo1	2.8007 (4)
Mo1—O1	2.036 (4)	V4—Mo1	2.8205 (4)
Mo1—O2	2.043 (3)	V4—Mo3	2.7463
Mo1—O3	2.027 (3)	V4—Mo4	0.12 (1)
Mo1—O5	2.088 (2)	V4—Mo4	2.91 (1)
Mo1—O6	2.029 (4)	V4—Mo4	2.30 (1)
Mo3—Mo1	2.7513 (6)	V4—V4	2.8026
Mo3—Mo1	2.7420 (6)	V4—V4	2.3663
Mo3—Mo1	2.7513 (6)	V4—O1	2.0295 (3)
Mo3—Mo1	2.7420 (6)	V4—O3	2.016 (3)
Mo3—Mo4	2.70 (1)	V4—O3	2.083 (3)
Mo3—Mo4	2.70 (1)	V4—O5	2.024 (4)
Mo3—V4	2.7463	V4—O6	2.029 (3)
Mo3—V4	2.7463	V4—O6	2.005 (3)

(Crystal3) top

Crystal data top

EuMo_7.96(1)O₁₄	F(000) = 2038
M_r = ?	D_x = 7.20 Mg m⁻³
Orthorhombic, ?	Mo Kα radiation, λ = 0.71073 Å
q = 0.286(3)c*	Cell parameters from 25 reflections
a = 11.315 (1) Å	θ = 18–25°
b = 10.035 (1 Å	µ = 14.9 mm⁻¹
c = 9.265 (1) Å	T = 293 K
V = 1052 (2) Å³	× × mm
Z = 4

Data collection top

CAD4 diffractometer	θ_max = 45.0°, θ_min = 3.5°
θ/θ scans	h = 0→22
Absorption correction: gaussian ?	k = 0→19
T_min = 0.21, T_max = 0.52	l = 0→18
13556 measured reflections	3 standard reflections every 3600 min
2695 reflections with I > 3σ(I)	intensity decay: 0.2%
R_int = 0.029

Refinement top

Refinement on F	Unit
R[F² > 2σ(F²)] = 0.048	(Δ/σ)_max = 0.010
wR(F²) = 0.0553	Δρ_max = 4.0 e Å⁻³
120 parameters	Δρ_min = −4.4 e Å⁻³

Crystal data top

EuMo_7.96(1)O₁₄	V = 1052 (2) Å³
M_r = ?	Z = 4
Orthorhombic, ?	Mo Kα radiation
q = 0.286(3)c*	µ = 14.9 mm⁻¹
a = 11.315 (1) Å	T = 293 K
b = 10.035 (1 Å	× × mm
c = 9.265 (1) Å

Data collection top

CAD4 diffractometer	2695 reflections with I > 3σ(I)
Absorption correction: gaussian ?	R_int = 0.029
T_min = 0.21, T_max = 0.52	3 standard reflections every 3600 min
13556 measured reflections	intensity decay: 0.2%

Refinement top

R[F² > 2σ(F²)] = 0.048	Δρ_max = 4.0 e Å⁻³
wR(F²) = 0.0553	Δρ_min = −4.4 e Å⁻³
120 parameters

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Eu	0.006 (3)	0	0	0.0149 (5)	0.500 (2)
Mo1	−0.12065 (2)	0.07781 (2)	0.37760 (2)	0.00452 (3)
Mo3	0	−0.16072 (2)	0.38119 (3)	0.00622 (4)
Mo4	0.2378 (2)	−0.1623 (2)	0.3726 (7)	0.0120 (3)	0.489 (2)
O1	0.2544 (3)	0	0.5	0.0084 (5)
O2	0	−0.1588 (2)	−0.2390 (2)	0.0062 (3)
O3	−0.1223 (2)	−0.0828 (2)	0.2444 (2)	0.0092 (2)
O5	−0.25	0.1692 (2)	0.25	0.0062 (4)
O6	0.1219 (2)	0.2516 (2)	0.4914 (2)	0.0095 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Eu	0.0176 (6)	0.0154 (8)	0.0089 (2)	0	0	−0.0034 (5)
Mo1	0.0033 (1)	0.0067 (1)	0.0036 (1)	0.0004 (1)	−0.0004 (1)	0.0013 (1)
Mo3	0.0081 (1)	0.0043 (1)	0.0032 (1)	0	0	0.0002 (1)
Mo4	0.0173 (7)	0.0080 (5)	0.0105 (5)	−0.0049 (1)	−0.0095 (6)	0.0041 (5)

Bond lengths (Å) top

Eu—Eu	0.6063 (9)	Mo4—O3	1.938 (4)
Eu—Mo4	3.338 (3)	Mo4—O3	2.077 (4)
Eu—Mo4	3.338 (3)	Mo4—O5	2.042 (4)
Eu—O1	3.082 (3)	Mo4—O6	2.116 (4)
Eu—O1	2.475 (3)	Mo4—O6	2.027 (4)
Eu—O2	2.745 (2)	O1—O3	2.921 (2)
Eu—O2	2.745 (2)	O1—O3	2.921 (2)
Eu—O3	2.944 (2)	O1—O3	2.786 (2)
Eu—O3	2.643 (2)	O1—O3	2.786 (2)
Eu—O3	2.643 (2)	O1—O5	2.872 (1)
Eu—O3	2.944 (2)	O1—O5	2.872 (1)
Eu—O6	2.717 (2)	O1—O6	2.937 (2)
Eu—O6	3.009 (2)	O1—O6	2.860 (2)
Eu—O6	3.009 (2)	O1—O6	2.860 (2)
Eu—O6	2.717 (2)	O1—O6	2.937 (2)
Mo1—Mo1	2.7302 (3)	O2—O3	2.793 (2)
Mo1—Mo1	2.7538 (3)	O2—O3	2.793 (2)
Mo1—Mo3	2.7558 (3)	O2—O3	2.943 (2)
Mo1—Mo3	2.7478 (3)	O2—O3	2.943 (2)
Mo1—Mo4	3.060 (2)	O2—O5	2.8325 (1)
Mo1—Mo4	2.799 (5)	O2—O5	2.8325 (1)
Mo1—Mo4	2.751 (2)	O2—O6	2.870 (3)
Mo1—O1	2.046 (2)	O2—O6	2.870 (3)
Mo1—O2	2.043 (2)	O2—O6	2.824 (3)
Mo1—O3	2.030 (2)	O2—O6	2.824 (3)
Mo1—O5	2.093 (1)	O3—O3	2.768 (2)
Mo1—O6	2.038 (2)	O3—O3	2.891 (2)
Mo3—Mo4	2.692 (2)	O3—O5	2.913 (2)
Mo3—Mo4	2.692 (2)	O3—O5	2.878 (2)
Mo3—O2	2.126 (2)	O3—O6	2.977 (2)
Mo3—O3	2.033 (2)	O3—O6	2.745 (2)
Mo3—O3	2.033 (2)	O5—O6	2.790 (2)
Mo3—O6	2.032 (2)	O5—O6	2.911 (2)
Mo3—O6	2.032 (2)	O5—O6	2.911 (2)
Mo4—Mo4	2.958 (7)	O5—O6	2.790 (2)
Mo4—Mo4	2.288 (9)	O6—O6	2.902 (2)
Mo4—O1	2.021 (4)	O6—O6	2.760 (2)

Experimental details

	(Crystal1)	(Crystal2)	(Crystal3)
Crystal data
Chemical formula	Eu_0.976(6)V_1.13(5)Mo_7.10(5)O₁₄	Eu_0.986(4)V_1.10(3)Mo_7.30(1)O₁₄	EuMo_7.96(1)O₁₄
M_r	?	?	?
Crystal system, space group	Orthorhombic, ?	Orthorhombic, ?	Orthorhombic, ?
Temperature (K)	293	293	293
Wave vectors	q = 0.195(2)c*	q = 0.245(2)c*	q = 0.286(3)c*
a, b, c (Å)	11.306 (1), 10.025 (1), 9.254 (1)	11.325 (1), 10.024 (1), 9.240 (1)	11.315 (1), 10.035 (1, 9.265 (1)
V (Å³)	1048.9 (2)	1048.9 (2)	1052 (2)
Z	4	4	4
Radiation type	Mo Kα	Mo Kα	Mo Kα
µ (mm⁻¹)	14.8	15.2	14.9
Crystal size (mm)	× ×	× ×	× ×

Data collection
Diffractometer	CAD4 diffractometer	CAD4 diffractometer	CAD4 diffractometer
Absorption correction	Gaussian	Gaussian	Gaussian
T_min, T_max	0.26, 0.42	0.23, 0.49	0.21, 0.52
No. of measured, independent and observed [I > 3σ(I)] reflections	13556, ?, 2711	13556, ?, 2423	13556, ?, 2695
R_int	0.030	0.031	0.029
(sin θ/λ)_max (Å⁻¹)	0.995	0.995	0.995

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.041, 0.0481, ?	0.041, 0.0449, ?	0.048, 0.0553, ?
No. of reflections	?	?	?
No. of parameters	132	134	120
No. of restraints	?	?	?
Δρ_max, Δρ_min (e Å⁻³)	3.5, −3.6	3.0, −3.7	4.0, −4.4

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Format		BIBTeX
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