Eu3Si15 − xAl1 + xOxN23 − x (x ≃ 5/3) as a commensurate composite crystal

Michiue, Y.; Shioi, K.; Hirosaki, N.; Takeda, T.; Xie, R.-J.; Sato, A.; Onoda, M.; Matsushita, Y.

doi:10.1107/S0108768109030419

Eu₃Si_15 − xAl_1 + xO_xN_23 − x (x ≃ 5/3) as a commensurate composite crystal

Y. Michiue, K. Shioi, N. Hirosaki, T. Takeda, R.-J. Xie, A. Sato, M. Onoda and Y. Matsushita

A new Eu-SiAlON crystal, Eu₃Si_15 − xAl_1 + xO_xN_23 − x (x ≃ 5/3), was found and the structure was determined by an X-ray diffraction technique using a twinned sample. The structure consists of a host framework, which is constructed by the connection of MX₄ tetrahedra (M: Si or Al; X: O or N), and Eu ions as the guest ions. The structure is considered to be a commensurate composite crystal. The basic vectors are a₁ = a/3, b and c for the first substructure, and a₂ = a/5, b and c for the second substructure. The first substructure consists of part of the host framework and the Eu ions, while the remainder of the host structure is taken as the second substructure. Possible phases belonging to the series are proposed using the composite crystal model in (3 + 1)-dimensional superspace. Chemical composition, possible space groups, cell parameters, and the basic model for those phases are presented.

Keywords: composite crystal; superspace description; twinning.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768109030419/sn5084sup1.cif Contains datablocks global, 3d, 4d
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768109030419/sn50843dsup2.hkl Contains datablock 3d
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768109030419/sn50844dsup3.hkl Contains datablock 4d

Computing details top

Program(s) used to refine structure: Jana2006 (Petricek, Dusek & Palatinus, 2006) for (3d); (Jana2000; Petricek and Dusek, 2000) for (4d). Software used to prepare material for publication: Jana2006 (Petricek, Dusek & Palatinus, 2006) for (3d); (Jana2000; Petricek and Dusek, 2000) for (4d).

Figures top

(3d) top

Crystal data top

Al_2.667Eu₃N_21.333O_1.667Si_13.333	Z = 2
M_r = 1227.8	F(000) = 1146
Monoclinic, P2₁	D_x = 4.110 Mg m⁻³
Hall symbol: P 2yb	Mo Kα radiation, λ = 0.71069 Å
a = 14.6970 (9) Å	µ = 10.37 mm⁻¹
b = 9.036 (2) Å	T = 295 K
c = 7.4677 (7) Å	Plate, pale yellow
β = 90.224 (1)°	0.30 × 0.25 × 0.05 mm
V = 991.7 (2) Å³

Data collection top

Bruker SMART APEX CCDarea-detector diffractometer	10994 independent reflections
Radiation source: fine-focus sealed tube	10354 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.033
ω scans	θ_max = 40.4°, θ_min = 1.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	h = −25→26
T_min = 0.035, T_max = 0.432	k = −16→16
22393 measured reflections	l = −13→10

Refinement top

Refinement on F²	0 restraints
R[F² > 2σ(F²)] = 0.053	161 constraints
wR(F²) = 0.115	Weighting scheme based on measured s.u.'s w = 1/(σ²(I) + 0.000004I²)
S = 2.15	(Δ/σ)_max = 0.020
10994 reflections	Δρ_max = 5.13 e Å⁻³
266 parameters	Δρ_min = −3.47 e Å⁻³

Crystal data top

Al_2.667Eu₃N_21.333O_1.667Si_13.333	V = 991.7 (2) Å³
M_r = 1227.8	Z = 2
Monoclinic, P2₁	Mo Kα radiation
a = 14.6970 (9) Å	µ = 10.37 mm⁻¹
b = 9.036 (2) Å	T = 295 K
c = 7.4677 (7) Å	0.30 × 0.25 × 0.05 mm
β = 90.224 (1)°

Data collection top

Bruker SMART APEX CCDarea-detector diffractometer	10994 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	10354 reflections with I > 2σ(I)
T_min = 0.035, T_max = 0.432	R_int = 0.033
22393 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.053	266 parameters
wR(F²) = 0.115	0 restraints
S = 2.15	Δρ_max = 5.13 e Å⁻³
10994 reflections	Δρ_min = −3.47 e Å⁻³

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Eu1	0.08342 (5)	0.5	0.25328 (7)	0.03310 (16)
Eu2	0.41856 (4)	0.46605 (5)	0.26321 (6)	0.03438 (17)
Eu3	0.74871 (5)	0.48118 (11)	0.24819 (6)	0.02618 (8)
Si1	0.08997 (18)	0.1734 (2)	0.5566 (3)	0.0121 (5)	0.8333
Si2	0.40923 (17)	0.1485 (2)	0.4895 (3)	0.0093 (4)	0.8333
Si3a	0.7768 (3)	0.1504 (4)	0.4897 (5)	0.0059 (8)*	0.439 (6)
Si3b	0.7205 (3)	0.1675 (5)	0.5596 (7)	0.0114 (10)*	0.395 (6)
Si4	0.59182 (19)	0.2950 (2)	0.4426 (3)	0.0124 (5)	0.8333
Si5	0.90848 (19)	0.3230 (2)	0.5149 (3)	0.0116 (4)	0.8333
Si6a	0.2776 (3)	0.3220 (5)	0.5133 (6)	0.0099 (9)*	0.439 (6)
Si6b	0.2222 (3)	0.3010 (5)	0.4433 (6)	0.0071 (9)*	0.394 (6)
Si7	0.10085 (17)	0.6257 (2)	0.8478 (3)	0.0104 (4)	0.8333
Si8	0.30079 (19)	0.6243 (3)	0.8636 (3)	0.0119 (5)	0.8333
Si9	0.50042 (16)	0.6194 (2)	0.8653 (3)	0.0086 (5)	0.8333
Si10	0.69905 (16)	0.6218 (3)	0.8549 (3)	0.0087 (4)	0.8333
Si11	0.89925 (18)	0.6298 (2)	0.8569 (3)	0.0098 (4)	0.8333
Si12	−0.00006 (17)	0.8313 (3)	0.1244 (3)	0.0088 (5)	0.8333
Si13	0.19813 (18)	0.8277 (3)	0.1308 (3)	0.0096 (5)	0.8333
Si14	0.39969 (18)	0.8210 (2)	0.1319 (3)	0.0108 (4)	0.8333
Si15	0.60138 (18)	0.8225 (3)	0.1386 (3)	0.0118 (5)	0.8333
Si16	0.80161 (15)	0.8270 (3)	0.1270 (3)	0.0081 (4)	0.8333
Al1	0.08997 (18)	0.1734 (2)	0.5566 (3)	0.0121 (5)	0.1667
Al2	0.40923 (17)	0.1485 (2)	0.4895 (3)	0.0093 (4)	0.1667
Al3a	0.7768 (3)	0.1504 (4)	0.4897 (5)	0.0059 (8)*	0.0877 (12)
Al3b	0.7205 (3)	0.1675 (5)	0.5596 (7)	0.0114 (10)*	0.0789 (12)
Al4	0.59182 (19)	0.2950 (2)	0.4426 (3)	0.0124 (5)	0.1667
Al5	0.90848 (19)	0.3230 (2)	0.5149 (3)	0.0116 (4)	0.1667
Al6a	0.2776 (3)	0.3220 (5)	0.5133 (6)	0.0099 (9)*	0.0878 (12)
Al6b	0.2222 (3)	0.3010 (5)	0.4433 (6)	0.0071 (9)*	0.0788 (12)
Al7	0.10085 (17)	0.6257 (2)	0.8478 (3)	0.0104 (4)	0.1667
Al8	0.30079 (19)	0.6243 (3)	0.8636 (3)	0.0119 (5)	0.1667
Al9	0.50042 (16)	0.6194 (2)	0.8653 (3)	0.0086 (5)	0.1667
Al10	0.69905 (16)	0.6218 (3)	0.8549 (3)	0.0087 (4)	0.1667
Al11	0.89925 (18)	0.6298 (2)	0.8569 (3)	0.0098 (4)	0.1667
Al12	−0.00006 (17)	0.8313 (3)	0.1244 (3)	0.0088 (5)	0.1667
Al13	0.19813 (18)	0.8277 (3)	0.1308 (3)	0.0096 (5)	0.1667
Al14	0.39969 (18)	0.8210 (2)	0.1319 (3)	0.0108 (4)	0.1667
Al15	0.60138 (18)	0.8225 (3)	0.1386 (3)	0.0118 (5)	0.1667
Al16	0.80161 (15)	0.8270 (3)	0.1270 (3)	0.0081 (4)	0.1667
N1	0.0903 (4)	0.9889 (5)	0.5900 (6)	0.0148 (8)*	0.4444
N2	0.4236 (4)	0.9811 (7)	0.5901 (7)	0.0202 (12)*	0.4444
N3	0.7596 (4)	0.9858 (8)	0.5918 (7)	0.0201 (10)*	0.4444
N4	0.1118 (4)	0.2301 (6)	0.3426 (8)	0.0113 (9)*
N5	0.3120 (4)	0.1915 (6)	0.3591 (7)	0.0046 (7)*
N6	0.4980 (5)	0.2099 (7)	0.3455 (10)	0.0158 (12)*
N7	0.6890 (5)	0.2132 (8)	0.3490 (11)	0.0173 (13)*
N8	0.8970 (6)	0.1873 (8)	0.3637 (10)	0.0262 (15)*
N9	−0.0012 (4)	0.2710 (6)	0.6516 (7)	0.0065 (8)*
N10	0.1905 (4)	0.2468 (6)	0.6571 (8)	0.0083 (9)*
N11	0.3836 (4)	0.2900 (6)	0.6392 (8)	0.0111 (10)*
N12	0.6011 (5)	0.2411 (7)	0.6597 (8)	0.0172 (11)*
N13	0.8086 (6)	0.2821 (10)	0.6446 (13)	0.0259 (18)*
N14	0.0996 (5)	0.2734 (5)	0.9850 (7)	0.0143 (8)*
N15	0.2980 (4)	0.2530 (6)	0.9697 (8)	0.0165 (10)*
N16	0.4982 (5)	0.2528 (6)	0.9712 (8)	0.0152 (9)*
N17	0.7043 (4)	0.2646 (6)	0.9777 (8)	0.0148 (9)*
N18	0.8986 (4)	0.2602 (5)	0.9798 (6)	0.0122 (8)*
N19	0.0003 (4)	0.0225 (6)	0.1155 (8)	0.0151 (9)*
N20	0.2008 (4)	0.0221 (5)	0.1078 (7)	0.0113 (8)*
N21	0.4011 (5)	0.0151 (5)	0.1204 (6)	0.0143 (8)*
N22	0.6014 (4)	0.0159 (5)	0.0967 (6)	0.0129 (8)*
N23	0.7980 (4)	0.0189 (5)	0.1222 (7)	0.0111 (8)*
O1	0.0903 (4)	0.9889 (5)	0.5900 (6)	0.0148 (8)*	0.5556
O2	0.4236 (4)	0.9811 (7)	0.5901 (7)	0.0202 (12)*	0.5556
O3	0.7596 (4)	0.9858 (8)	0.5918 (7)	0.0201 (10)*	0.5556

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Eu1	0.0618 (4)	0.0177 (2)	0.01984 (18)	0.0007 (2)	0.0084 (4)	−0.00048 (16)
Eu2	0.0549 (3)	0.01547 (18)	0.0326 (3)	0.0079 (2)	−0.0228 (3)	−0.00263 (19)
Eu3	0.03942 (19)	0.02678 (12)	0.01233 (11)	−0.01618 (13)	−0.0003 (3)	−0.0052 (2)
Si1	0.0157 (10)	0.0104 (7)	0.0100 (7)	0.0115 (8)	−0.0038 (9)	−0.0012 (5)
Si2	0.0102 (8)	0.0092 (6)	0.0085 (6)	0.0016 (8)	0.0024 (9)	0.0003 (5)
Si4	0.0164 (10)	0.0115 (7)	0.0094 (7)	0.0039 (8)	−0.0059 (10)	−0.0007 (5)
Si5	0.0189 (10)	0.0091 (6)	0.0069 (6)	0.0027 (9)	0.0016 (10)	0.0004 (5)
Si7	0.0102 (9)	0.0112 (7)	0.0098 (7)	−0.0011 (7)	0.0026 (8)	0.0010 (5)
Si8	0.0174 (10)	0.0114 (8)	0.0069 (9)	−0.0015 (8)	−0.0007 (8)	0.0023 (6)
Si9	0.0069 (8)	0.0092 (7)	0.0096 (9)	−0.0005 (7)	0.0013 (8)	0.0013 (6)
Si10	0.0071 (8)	0.0128 (8)	0.0062 (8)	−0.0013 (7)	0.0005 (7)	0.0001 (6)
Si11	0.0101 (8)	0.0108 (7)	0.0087 (7)	−0.0043 (7)	0.0040 (8)	−0.0008 (5)
Si12	0.0099 (8)	0.0101 (7)	0.0063 (8)	0.0006 (7)	0.0025 (8)	0.0004 (6)
Si13	0.0128 (9)	0.0081 (7)	0.0079 (8)	0.0018 (7)	0.0048 (8)	0.0009 (6)
Si14	0.0146 (9)	0.0096 (6)	0.0082 (7)	−0.0027 (8)	0.0040 (9)	0.0008 (5)
Si15	0.0117 (9)	0.0129 (7)	0.0109 (7)	0.0037 (8)	0.0012 (8)	0.0017 (5)
Si16	0.0017 (7)	0.0139 (8)	0.0088 (9)	0.0024 (7)	0.0005 (7)	−0.0017 (6)
Al1	0.0157 (10)	0.0104 (7)	0.0100 (7)	0.0115 (8)	−0.0038 (9)	−0.0012 (5)
Al2	0.0102 (8)	0.0092 (6)	0.0085 (6)	0.0016 (8)	0.0024 (9)	0.0003 (5)
Al4	0.0164 (10)	0.0115 (7)	0.0094 (7)	0.0039 (8)	−0.0059 (10)	−0.0007 (5)
Al5	0.0189 (10)	0.0091 (6)	0.0069 (6)	0.0027 (9)	0.0016 (10)	0.0004 (5)
Al7	0.0102 (9)	0.0112 (7)	0.0098 (7)	−0.0011 (7)	0.0026 (8)	0.0010 (5)
Al8	0.0174 (10)	0.0114 (8)	0.0069 (9)	−0.0015 (8)	−0.0007 (8)	0.0023 (6)
Al9	0.0069 (8)	0.0092 (7)	0.0096 (9)	−0.0005 (7)	0.0013 (8)	0.0013 (6)
Al10	0.0071 (8)	0.0128 (8)	0.0062 (8)	−0.0013 (7)	0.0005 (7)	0.0001 (6)
Al11	0.0101 (8)	0.0108 (7)	0.0087 (7)	−0.0043 (7)	0.0040 (8)	−0.0008 (5)
Al12	0.0099 (8)	0.0101 (7)	0.0063 (8)	0.0006 (7)	0.0025 (8)	0.0004 (6)
Al13	0.0128 (9)	0.0081 (7)	0.0079 (8)	0.0018 (7)	0.0048 (8)	0.0009 (6)
Al14	0.0146 (9)	0.0096 (6)	0.0082 (7)	−0.0027 (8)	0.0040 (9)	0.0008 (5)
Al15	0.0117 (9)	0.0129 (7)	0.0109 (7)	0.0037 (8)	0.0012 (8)	0.0017 (5)
Al16	0.0017 (7)	0.0139 (8)	0.0088 (9)	0.0024 (7)	0.0005 (7)	−0.0017 (6)

Geometric parameters (Å, º) top

Eu1—N1ⁱ	2.811 (6)	Si5—N8	1.675 (8)
Eu1—N3ⁱⁱ	2.584 (6)	Si5—N9^ix	1.736 (6)
Eu1—N4	2.563 (6)	Si5—N13	1.800 (10)
Eu1—N9ⁱⁱⁱ	2.821 (6)	Si5—O1ⁱⁱ	1.692 (5)
Eu1—N13^iv	3.098 (9)	Si6a—N3ⁱⁱ	1.761 (8)
Eu1—N14^v	2.874 (5)	Si6a—N5	1.725 (7)
Eu1—N18^iv	2.937 (5)	Si6a—N10	1.806 (7)
Eu1—N19^vi	3.023 (6)	Si6a—N11	1.840 (7)
Eu1—O1ⁱ	2.811 (6)	Si6a—O3ⁱⁱ	1.761 (8)
Eu1—O3ⁱⁱ	2.584 (6)	Si6b—N3ⁱⁱ	1.711 (9)
Eu2—N2ⁱⁱ	2.568 (6)	Si6b—N4	1.897 (7)
Eu2—N3ⁱⁱ	2.839 (6)	Si6b—N5	1.768 (7)
Eu2—N5	3.020 (5)	Si6b—N10	1.735 (8)
Eu2—N6	2.664 (7)	Si6b—O3ⁱⁱ	1.711 (9)
Eu2—N11	3.268 (6)	Si7—N8^iv	1.675 (8)
Eu2—N12^iv	2.568 (6)	Si7—N18^x	1.770 (5)
Eu2—N16^v	3.137 (6)	Si7—N19ⁱⁱⁱ	1.777 (6)
Eu2—N22^vii	2.741 (5)	Si7—N23^iv	1.786 (6)
Eu2—O2ⁱⁱ	2.568 (6)	Si8—N7^iv	1.786 (8)
Eu2—O3ⁱⁱ	2.839 (6)	Si8—N17^x	1.737 (6)
Eu3—N1ⁱⁱ	2.657 (6)	Si8—N22^iv	1.763 (6)
Eu3—N2ⁱⁱ	2.806 (6)	Si8—N23^iv	1.739 (6)
Eu3—N7	2.683 (7)	Si9—N6^iv	1.774 (7)
Eu3—N10^iv	2.657 (6)	Si9—N16^x	1.716 (6)
Eu3—N15^iv	3.025 (6)	Si9—N21^iv	1.730 (7)
Eu3—N17^v	2.887 (6)	Si9—N22^iv	1.789 (6)
Eu3—N20^vii	2.785 (5)	Si10—N5^iv	1.725 (6)
Eu3—O1ⁱⁱ	2.657 (6)	Si10—N15^x	1.767 (6)
Eu3—O2ⁱⁱ	2.806 (6)	Si10—N20^iv	1.747 (6)
Si1—N1^viii	1.686 (5)	Si10—N21^iv	1.770 (7)
Si1—N4	1.709 (6)	Si11—N4^iv	1.751 (6)
Si1—N9	1.756 (6)	Si11—N14^x	1.755 (5)
Si1—N10	1.783 (6)	Si11—N19^iv	1.778 (6)
Si1—O1^viii	1.686 (5)	Si11—N20^iv	1.783 (6)
Si2—N2^viii	1.702 (6)	Si12—N9ⁱⁱⁱ	1.760 (6)
Si2—N5	1.769 (6)	Si12—N14ⁱⁱⁱ	1.753 (7)
Si2—N6	1.783 (8)	Si12—N18^iv	1.803 (6)
Si2—N11	1.740 (6)	Si12—N19^xi	1.729 (6)
Si2—O2^viii	1.702 (6)	Si13—N13^iv	1.731 (10)
Si3a—N3^viii	1.691 (8)	Si13—N17^iv	1.746 (7)
Si3a—N7	1.755 (9)	Si13—N18^iv	1.751 (6)
Si3a—N8	2.033 (9)	Si13—N20^xi	1.766 (5)
Si3a—N13	1.723 (10)	Si14—N12^iv	1.716 (6)
Si3a—O3^viii	1.691 (8)	Si14—N16^iv	1.799 (7)
Si3b—N3^viii	1.756 (9)	Si14—N17^iv	1.804 (7)
Si3b—N7	1.689 (10)	Si14—N21^xi	1.756 (5)
Si3b—N12	2.023 (9)	Si15—N11^iv	1.699 (6)
Si3b—N13	1.774 (10)	Si15—N15^iv	1.801 (7)
Si3b—O3^viii	1.756 (9)	Si15—N16^iv	1.789 (7)
Si4—N2ⁱⁱ	1.715 (7)	Si15—N22^xi	1.775 (5)
Si4—N6	1.735 (8)	Si16—N10^iv	1.771 (6)
Si4—N7	1.756 (8)	Si16—N14^iv	1.746 (7)
Si4—N12	1.698 (6)	Si16—N15^iv	1.762 (7)
Si4—O2ⁱⁱ	1.715 (7)	Si16—N23^xi	1.735 (5)
Si5—N1ⁱⁱ	1.692 (5)

N1ⁱ—Eu1—N3ⁱⁱ	128.52 (15)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x+1, y−1/2, −z+1; (iii) −x, y+1/2, −z+1; (iv) −x+1, y+1/2, −z+1; (v) x, y, z−1; (vi) −x, y+1/2, −z; (vii) −x+1, y+1/2, −z; (viii) x, y−1, z; (ix) x+1, y, z; (x) −x+1, y+1/2, −z+2; (xi) x, y+1, z.

(4d) top

Crystal data top

Al_1.778Eu₂N_14.222O_1.111Si_8.889	Z = 1
M_r = 818.5	F(000) = 382
Orthorhombic, Pm21n(α00)000†	D_x = 4.110 Mg m⁻³
q = 1.66667a*‡	Mo Kα radiation, λ = 0.71069 Å
a = 4.8990 (3) Å	µ = 10.37 mm⁻¹
b = 9.036 (2) Å	T = 295 K
c = 7.4677 (7) Å	Plate, pale yellow
V = 330.58 (8) Å³	0.30 × 0.25 × 0.05 mm

† Symmetry operations: (1) x₁, x₂, x₃, x₄; (2) 1/2+x₁, 1/2+x₂, −x₃, x₄; (3) 1/2−x₁, x₂, x₃, −x₄; (4) −x₁, 1/2+x₂, −x₃, −x₄.

‡

;

Data collection top

Bruker SMART APEX CCDarea-detector diffractometer	10994 independent reflections
Radiation source: fine-focus sealed tube	10354 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.033
ω scans	θ_max = 40.4°, θ_min = 1.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	h = −8→8
T_min = 0.035, T_max = 0.432	k = −16→16
22393 measured reflections	l = −13→10

Refinement top

Refinement on F²	248 parameters
R[F² > 2σ(F²)] = 0.055	Weighting scheme based on measured s.u.'s w = 1/(σ²(I) + 0.000004I²)
wR(F²) = 0.119	(Δ/σ)_max = 0.042
S = 2.23	Δρ_max = 4.59 e Å⁻³
10994 reflections	Δρ_min = −4.18 e Å⁻³

Crystal data top

Al_1.778Eu₂N_14.222O_1.111Si_8.889	V = 330.58 (8) Å³
M_r = 818.5	Z = 1
Orthorhombic, Pm21n(α00)000†	Mo Kα radiation
q = 1.66667a*‡	µ = 10.37 mm⁻¹
a = 4.8990 (3) Å	T = 295 K
b = 9.036 (2) Å	0.30 × 0.25 × 0.05 mm
c = 7.4677 (7) Å

† Symmetry operations: (1) x₁, x₂, x₃, x₄; (2) 1/2+x₁, 1/2+x₂, −x₃, x₄; (3) 1/2−x₁, x₂, x₃, −x₄; (4) −x₁, 1/2+x₂, −x₃, −x₄.

‡

;

Data collection top

Bruker SMART APEX CCDarea-detector diffractometer	10994 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	10354 reflections with I > 2σ(I)
T_min = 0.035, T_max = 0.432	R_int = 0.033
22393 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.055	248 parameters
wR(F²) = 0.119	Δρ_max = 4.59 e Å⁻³
S = 2.23	Δρ_min = −4.18 e Å⁻³
10994 reflections

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Eu11	0.25	0.5	0.25486 (3)	0.03111 (7)
Si11a	0.25	0.1662 (3)	0.4901 (3)	0.0113 (5)	0.8333
Si11b	0.25	0.1911 (3)	0.5558 (3)	0.0138 (5)	0.8333
Si11c	0.1678 (8)	0.1674 (4)	0.4895 (5)	0.0009 (7)*	0.441 (6)
Si11d	0.3348 (11)	0.1845 (5)	0.5596 (7)	0.0053 (10)*	0.392 (6)
Si12a	0.75	0.3404 (2)	0.5149 (3)	0.0110 (4)	0.8333
Si12b	0.75	0.3126 (2)	0.4419 (3)	0.0115 (5)	0.8333
Si12c	0.8293 (9)	0.3387 (5)	0.5134 (6)	0.0105 (9)*	0.442 (6)
Si12d	0.6644 (10)	0.3182 (5)	0.4443 (6)	0.0070 (9)*	0.391 (6)
Al11a	0.25	0.166167	0.490075	0.0113 (5)	0.1667
Al11b	0.25	0.19115	0.555797	0.0138 (5)	0.1667
Al11c	0.167833	0.167406	0.489479	0.0009 (7)*	0.0882 (13)
Al11d	0.3348	0.184457	0.559631	0.0053 (10)*	0.0785 (13)
Al12a	0.75	0.340416	0.514937	0.0110 (4)	0.1667
Al12b	0.75	0.312581	0.441946	0.0115 (5)	0.1667
Al12c	0.829298	0.338669	0.513421	0.0105 (9)*	0.0884 (12)
Al12d	0.664376	0.318156	0.444298	0.0070 (9)*	0.0783 (12)
N11	0.25	0.0019 (5)	0.5905 (3)	0.0189 (5)*	0.4444
O11	0.25	0.001894	0.590478	0.0189 (5)*	0.5556
Si21	0.5	0.64182 (10)	0.85767 (9)	0.00978 (16)	0.8333
Si22	0	0.84351 (10)	0.13046 (9)	0.00973 (16)	0.8333
Al21	0.5	0.641818	0.857673	0.00978 (16)	0.1667
Al22	0	0.843511	0.130462	0.00973 (16)	0.1667
N21	0.5	0.2237 (3)	0.3520 (3)	0.0152 (5)*
N22	0	0.2837 (3)	0.6502 (3)	0.0122 (4)*
N23	0.5	0.2781 (2)	0.9769 (3)	0.0144 (3)*
N24	0	0.0365 (2)	0.1125 (3)	0.0128 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Eu11	0.05212 (17)	0.01990 (7)	0.02132 (11)	0	0	−0.00303 (9)
Si11a	0.0078 (9)	0.0138 (8)	0.0124 (8)	0	0	0.0007 (6)
Si11b	0.0161 (11)	0.0132 (8)	0.0121 (8)	0	0	−0.0003 (6)
Si12a	0.0181 (10)	0.0081 (6)	0.0070 (6)	0	0	0.0000 (5)
Si12b	0.0141 (10)	0.0112 (7)	0.0092 (7)	0	0	−0.0008 (5)
Al11a	0.0078 (9)	0.0138 (8)	0.0124 (8)	0	0	0.0007 (6)
Al11b	0.0161 (11)	0.0132 (8)	0.0121 (8)	0	0	−0.0003 (6)
Al12a	0.0181 (10)	0.0081 (6)	0.0070 (6)	0	0	0.0000 (5)
Al12b	0.0141 (10)	0.0112 (7)	0.0092 (7)	0	0	−0.0008 (5)
Si21	0.0104 (3)	0.0109 (2)	0.0080 (3)	0	0	0.00067 (19)
Si22	0.0097 (3)	0.0113 (2)	0.0082 (3)	0	0	0.00031 (19)
Al21	0.0104 (3)	0.0109 (2)	0.0080 (3)	0	0	0.00067 (19)
Al22	0.0097 (3)	0.0113 (2)	0.0082 (3)	0	0	0.00031 (19)

Bond lengths (Å) top

	Average	Minimum	Maximum
Si11a—N11	1.710 (6)	1.710 (6)	1.710 (6)

Experimental details

	(3d)	(4d)
Crystal data
Chemical formula	Al_2.667Eu₃N_21.333O_1.667Si_13.333	Al_1.778Eu₂N_14.222O_1.111Si_8.889
M_r	1227.8	818.5
Crystal system, space group	Monoclinic, P2₁	Orthorhombic, Pm21n(α00)000†
Temperature (K)	295	295
a, b, c (Å)	14.6970 (9), 9.036 (2), 7.4677 (7)	?
α, β, γ (°)	90, 90.224 (1), 90	4.8990 (3), 9.036 (2), 7.4677 (7)
V (Å³)	991.7 (2)	90, 90, 90
Z	2	330.58 (8)
Radiation type	Mo Kα	?
µ (mm⁻¹)	10.37	?
Crystal size (mm)	0.30 × 0.25 × 0.05	Pale yellow

Data collection
Diffractometer	Bruker SMART APEX CCDarea-detector diffractometer	Bruker SMART APEX CCDarea-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2004)	Multi-scan (SADABS; Sheldrick, 2004)
T_min, T_max	0.035, 0.432	0.035, 0.432
No. of measured, independent and observed [I > 2σ(I)] reflections	22393, 10994, 10354	22393, 10994, 10354
R_int	0.033	0.033
(sin θ/λ)_max (Å⁻¹)	0.912	0.912

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.053, 0.115, 2.15	0.055, 0.119, 2.23
No. of reflections	10994	10994
No. of parameters	266	248
No. of restraints	0	?
Δρ_max, Δρ_min (e Å⁻³)	5.13, −3.47	4.59, −4.18

† Symmetry operations: (1) x₁, x₂, x₃, x₄; (2) 1/2+x₁, 1/2+x₂, −x₃, x₄; (3) 1/2−x₁, x₂, x₃, −x₄; (4) −x₁, 1/2+x₂, −x₃, −x₄.

Computer programs: Jana2006 (Petricek, Dusek & Palatinus, 2006), (Jana2000; Petricek and Dusek, 2000).

Selected bond lengths (Å) for (3d) top

Eu1—N1ⁱ	2.811 (6)	Si5—N8	1.675 (8)
Eu1—N3ⁱⁱ	2.584 (6)	Si5—N9^ix	1.736 (6)
Eu1—N4	2.563 (6)	Si5—N13	1.800 (10)
Eu1—N9ⁱⁱⁱ	2.821 (6)	Si5—O1ⁱⁱ	1.692 (5)
Eu1—N13^iv	3.098 (9)	Si6a—N3ⁱⁱ	1.761 (8)
Eu1—N14^v	2.874 (5)	Si6a—N5	1.725 (7)
Eu1—N18^iv	2.937 (5)	Si6a—N10	1.806 (7)
Eu1—N19^vi	3.023 (6)	Si6a—N11	1.840 (7)
Eu1—O1ⁱ	2.811 (6)	Si6a—O3ⁱⁱ	1.761 (8)
Eu1—O3ⁱⁱ	2.584 (6)	Si6b—N3ⁱⁱ	1.711 (9)
Eu2—N2ⁱⁱ	2.568 (6)	Si6b—N4	1.897 (7)
Eu2—N3ⁱⁱ	2.839 (6)	Si6b—N5	1.768 (7)
Eu2—N5	3.020 (5)	Si6b—N10	1.735 (8)
Eu2—N6	2.664 (7)	Si6b—O3ⁱⁱ	1.711 (9)
Eu2—N11	3.268 (6)	Si7—N8^iv	1.675 (8)
Eu2—N12^iv	2.568 (6)	Si7—N18^x	1.770 (5)
Eu2—N16^v	3.137 (6)	Si7—N19ⁱⁱⁱ	1.777 (6)
Eu2—N22^vii	2.741 (5)	Si7—N23^iv	1.786 (6)
Eu2—O2ⁱⁱ	2.568 (6)	Si8—N7^iv	1.786 (8)
Eu2—O3ⁱⁱ	2.839 (6)	Si8—N17^x	1.737 (6)
Eu3—N1ⁱⁱ	2.657 (6)	Si8—N22^iv	1.763 (6)
Eu3—N2ⁱⁱ	2.806 (6)	Si8—N23^iv	1.739 (6)
Eu3—N7	2.683 (7)	Si9—N6^iv	1.774 (7)
Eu3—N10^iv	2.657 (6)	Si9—N16^x	1.716 (6)
Eu3—N15^iv	3.025 (6)	Si9—N21^iv	1.730 (7)
Eu3—N17^v	2.887 (6)	Si9—N22^iv	1.789 (6)
Eu3—N20^vii	2.785 (5)	Si10—N5^iv	1.725 (6)
Eu3—O1ⁱⁱ	2.657 (6)	Si10—N15^x	1.767 (6)
Eu3—O2ⁱⁱ	2.806 (6)	Si10—N20^iv	1.747 (6)
Si1—N1^viii	1.686 (5)	Si10—N21^iv	1.770 (7)
Si1—N4	1.709 (6)	Si11—N4^iv	1.751 (6)
Si1—N9	1.756 (6)	Si11—N14^x	1.755 (5)
Si1—N10	1.783 (6)	Si11—N19^iv	1.778 (6)
Si1—O1^viii	1.686 (5)	Si11—N20^iv	1.783 (6)
Si2—N2^viii	1.702 (6)	Si12—N9ⁱⁱⁱ	1.760 (6)
Si2—N5	1.769 (6)	Si12—N14ⁱⁱⁱ	1.753 (7)
Si2—N6	1.783 (8)	Si12—N18^iv	1.803 (6)
Si2—N11	1.740 (6)	Si12—N19^xi	1.729 (6)
Si2—O2^viii	1.702 (6)	Si13—N13^iv	1.731 (10)
Si3a—N3^viii	1.691 (8)	Si13—N17^iv	1.746 (7)
Si3a—N7	1.755 (9)	Si13—N18^iv	1.751 (6)
Si3a—N8	2.033 (9)	Si13—N20^xi	1.766 (5)
Si3a—N13	1.723 (10)	Si14—N12^iv	1.716 (6)
Si3a—O3^viii	1.691 (8)	Si14—N16^iv	1.799 (7)
Si3b—N3^viii	1.756 (9)	Si14—N17^iv	1.804 (7)
Si3b—N7	1.689 (10)	Si14—N21^xi	1.756 (5)
Si3b—N12	2.023 (9)	Si15—N11^iv	1.699 (6)
Si3b—N13	1.774 (10)	Si15—N15^iv	1.801 (7)
Si3b—O3^viii	1.756 (9)	Si15—N16^iv	1.789 (7)
Si4—N2ⁱⁱ	1.715 (7)	Si15—N22^xi	1.775 (5)
Si4—N6	1.735 (8)	Si16—N10^iv	1.771 (6)
Si4—N7	1.756 (8)	Si16—N14^iv	1.746 (7)
Si4—N12	1.698 (6)	Si16—N15^iv	1.762 (7)
Si4—O2ⁱⁱ	1.715 (7)	Si16—N23^xi	1.735 (5)
Si5—N1ⁱⁱ	1.692 (5)

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