Crystal structures of Ca4+xY3–xSi7O15+xN5–x (0 ≤ x ≤ 1) comprising of an isolated [Si7(O,N)19] unit

Kobayashi, M.; Yasunaga, T.; Kato, H.; Fujii, K.; Yashima, M.; Kakihana, M.

doi:10.1107/S2056989019001257

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ISSN: 2056-9890

Volume 75| Part 2| February 2019| Pages 260-263

https://doi.org/10.1107/S2056989019001257

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Crystal structures of Ca_4+xY_3–xSi₇O_15+xN_5–x (0 ≤ x ≤ 1) comprising of an isolated [Si₇(O,N)₁₉] unit

Makoto Kobayashi,^a ^*‡ Takuya Yasunaga,^a Hideki Kato,^a ^* Kotaro Fujii,^b Masatomo Yashima ^b and Masato Kakihana ^a

^aInstitute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577, Japan, and ^bDepartment of Chemistry, School of Science, Tokyo Institute of Technology, 2-12-1-W4-17, Ookayama, Meguro-ku, To-kyo 152-8551, Japan
^*Correspondence e-mail: mkoba@imass.nagoya-u.ac.jp, hideki.kato.e2@tohoku.ac.jp

Edited by M. Weil, Vienna University of Technology, Austria (Received 8 January 2019; accepted 23 January 2019; online 25 January 2019)

Single crystals of the solid solution series Ca_4+xY_3–xSi₇O_15+xN_5–x were obtained by a solid-state reaction method using a flux for x = 0, 0.5 and 1, resulting in Ca₄Y₃Si₇O₁₅N₅ (tetracalcium triyttrium heptasilicon oxynitride), Ca_4.5Y_2.5Si₇O_15.5N_4.5 and Ca₅Y₂Si₇O₁₆N₄ (pentacalcium diyttrium heptasilicon oxynitride). Single-crystal X-ray analysis revealed that the three compounds are isotypic and belong to space-group type P6₃/m. Ca²⁺ and Y³⁺ cations are distributed over two crystallographic sites (site symmetry $[\overline{3}]$ .. and 1) in a disordered manner. The corresponding (Ca,Y)-centred polyhedra are connected by edge-sharing, resulting in the formation of a layer structure extending parallel to (001). Three [Si(O,N)]₄ tetrahedra (two with point group symmetry m.., one with 3.. and half-occupancy) are condensed into an isolated [Si₇(O,N)₁₉] unit, in which an [Si(O,N)]₄ tetrahedron is located at the center of a 12-membered oxynitride ring with composition [Si₆O₁₅N₃]. The present compounds are the first to have such an [Si₇(O,N)₁₉] unit in their structures.

Keywords: oxynitride; silicate; crystal structure.

CCDC references: 1892876; 1892875; 1892874

1. Chemical context

Silicon oxynitrides (or oxynitridosilicates) containing an alkaline-earth or a rare-earth metal cation have been extensively studied due to their potential applications as phosphors for white-light-emitting diodes (Takeda et al., 2018 ). Recently, the exploration range for new silicon oxynitrides has been expanded to compounds with alkaline-earth and rare-earth metal cations. In this regard, Lu₄Ba₂[Si₉ON₁₆]O, Y₄Ba₂[Si₉ON₁₆]O (Maak et al., 2017 ), La₃BaSi₅N₉O₂ (Durach et al., 2015 ), Ca_1.4Ce_2.6Si₁₂O_4.4N_16.6 (Park et al., 2013 ), Ca_1.46La_2.54Si₁₂O_4.45N_16.55 (Park et al., 2012 ) or BaYSi₂O₅N (Kobayashi et al., 2017 ) were synthesized and their crystal structures determined. The corresponding oxide or nitride forms are unknown for these materials. At the same time, the introduction of multiple anions contributes to the formation of otherwise unattainable silicate units in single anion compounds. In addition to the compounds mentioned above, for example, Ce₄[Si₄O₄N₆]O has a hyperbolic layer structure, which is composed of an [SiO₃N] unit connected by three cyclic [Si₃O₃N₆] units through corner-sharing (Irran et al., 2000 ).

While exploring new oxynitrides, we obtained SrSiO_2.64N_0.24 with a single-chain inosilicate structure, which has not been realized for Sr- or Sr-rich metasilicate oxides and nitrides (Kobayashi et al., 2018 ). In the present work, the synthesis and structure determination of three silicon oxynitrides, denoted by the solid solution series Ca_4+xY_3-xSi₇O_15+xN_5–x, with compositions of Ca₄Y₃Si₇O₁₅N₅ (1, x = 0), Ca_4.5Y_2.5Si₇O_15.5N_4.5 (2, x = 0.5) and Ca₅Y₂Si₇O₁₆N₄ (3, x = 1) are reported.

2. Structural commentary

Compounds 1–3 are isotypic and crystallize in space group P6₃/m. Figs. 1–4 show the crystal structures and atomic arrangements of 1–3. There are five sites in the structure associated with oxygen and/or nitrogen positions. Two sites at Wyckoff position 12i, O1 and O2, and one 6h site, O3, are solely occupied by oxygen, and one 6h site, N5, is solely occupied by nitrogen, irrespective of the value for x. Oxygen and nitrogen atoms are disordered for (O,N)4 situated on a 4f site. For 2 and 3, the O:N ratio at this site amounts to 0.25:0.75 for 2 and 0.5:0.5 for 3, respectively, whereas for 1 this site is exclusively occupied by nitrogen atoms.

Figure 1
Crystal structure of Ca₄Y₃Si₇O₁₅N₅ (1) drawn with cation-centered polyhedra. Pink, green, blue, red and black spheres indicate calcium, yttrium, silicon, oxygen, and nitrogen ions, respectively. Mixed colours of the Si3 and associated (N,O) positions indicate the fraction of vacancy/occupancy.

Figure 2
Crystal structure of Ca_4.5Y_2.5Si₇O_15.5N_4.5 (2) drawn with cation-centered polyhedra. Colour code as in Fig. 1

Figure 3
Crystal structure of Ca₅Y₂Si₇O₁₆N₄ (3) drawn with cation-centered polyhedra. Colour code as in Fig. 1

Figure 4
Representative for all structures, the atomic arrangement around Si atoms in the structure of Ca₄Y₃Si₇O₁₅N₅ (1). Displacement ellipsoids are drawn at the 90% probability level. [Symmetry codes: (i) 1 − y, 1 + x − y, z; (ii) −x + y, 1 − x, z; (iii) x, y, $[{1\over 2}]$ − z; (iv) 1 − y, 1 + x − y, $[{1\over 2}]$ − z; (v) −x + y, 1 − x, $[{1\over 2}]$ − z.]

Ca²⁺ and Y³⁺ occupy two sites, viz. M1 with site symmetry $[\overline{3}]$ .. at Wyckoff position 2b and M2 with site symmetry 1 at Wyckoff position 12i. M1 is coordinated by six oxygen atoms in the structures of 1–3 whereas the coordination environment of M2 depends on the value of x. In the structure of 1, six oxygen and two nitrogen atoms define the respective coordination sphere, but there are two possible coordination environments for 2 and 3 because of the disorder of the anionic 4f site, i.e. two nitrogen and six oxygen atoms, and one nitrogen and seven oxygen atoms, respectively. Site occupancies of Ca²⁺ were refined as 0.1379 (14) (1), 0.1338 (14) (2) and 0.2572 (14) (3) for M1, and 0.6437 (2) (1), 0.7277 (2) (2) and 0.7905 (2) (3) for M2. Thus, Ca²⁺ prefers to occupy the larger M2 site, in agreement with the larger ionic radius of Ca²⁺ compared to Y³⁺ for six- (1.00 versus 0.90 Å) and eight-coordination (1.12 versus 1.02 Å; Shannon, 1976 ). [M1O₆] octahedra and [M2(O,N)₈] dodecahedra are linked through their edges, resulting in the formation of a layer structure extending parallel to (001). Adjacent layers are connected along [001] through corner-sharing and by silicon atoms in the interstices. There are three Si sites in the crystal structure: Si1, Si2 and Si3 at Wyckhoff positions 6h (site symmetry m..), 6h, and 4f (3..), respectively. The latter site is disordered and shows half-occupancy. At both 6h sites, [SiO₃N] tetrahedra are present that are condensed into a 12-membered ring, [Si₆O₁₅N₃], by corner-sharing. As a result of the disorder and associated splitting of the 4f site, tetrahedra above and below the ring are present that share three corners with the ring, resulting in the formation of isolated [Si₇(O,N)₁₉] units, as shown in Fig. 4. These units are located at z = ±0.25 and are situated between the layers formed by layers of [M1O₆] octahedra and [M2(O,N)₈] dodecahedra.

Bond lengths of the [Si(O,N)₄] tetrahedra are collated in Table 1. In agreement with the higher electronegativity of oxygen when compared to nitrogen, the Si—N bonds are systematically longer than Si—O bonds.

Table 1
Selected bond lengths (Å)

	1	2	3
Si1—O1	1.634 (2) × 2	1.621 (2) × 2	1.623 (2) × 2
Si1—O3	1.686 (3)	1.669 (4)	1.673 (3)
Si1—N5	1.754 (3)	1.788 (4)	1.781 (3)
Si2—O2	1.635 (2) × 2	1.622 (3) × 2	1.624 (2) × 2
Si2—O3	1.684 (3)	1.673 (4)	1.672 (3)
Si2—N5	1.753 (3)	1.798 (4)	1.782 (3)
Si3—(O,N)4	1.804 (6)	1.769 (8)	1.765 (7)
Si3—N5	1.809 (3) × 3	1.730 (5) × 3	1.732 (3) × 3

3. Synthesis and crystallization

Single crystals of 1–3 were obtained from powders synthesized by a solid-state reaction method. CaCO₃ (Kanto Chemical, 99.99%), Y₂O₃ (Wako Chemical, 99.99%), SiO₂ (Fuso Chemical, 99.999%), Si₃N₄ (Kojundo Chemical, 99.9%), and CeO₂ (Kanto Chemical, 99.5%) in the molar ratio of CaCO₃:Y₂O₃:SiO₂:Si₃N₄ = 5.76:0.62:2.8:1.4 for 2 and of CaCO₃:Y₂O₃:CeO₂:SiO₂:Si₃N₄ = 5.76:0.61:0.01:2.8:1.4 (2 mol% Ce to Y) for 1 and 3 were ground in the presence of 20 wt% CaF₂ (Wako Chemical, 99.9%) as a flux. The mixtures were pelletized at 20 MPa, put on an alumina boat with a carbon sheet dish (Toyo Tanso, 0.1 mm of thickness) and calcined at 1733 K for 4 h under 100 ml min⁻¹ of flowing nitrogen. The reaction mixtures were slowly cooled under different conditions: to 1373 K at a rate of 30 K h⁻¹, to 1173 K at a rate of 100 K h⁻¹ and to RT by turning off the power for 1, and to 1373 K at a rate of 60 K h⁻¹, to 1173 K at a rate of 100 K h⁻¹ and to RT by turning off the power for 2 and 3. After roughly grinding the recrystallized fused pellets, the powders obtained were washed with 5 M HCl(aq.) and distilled water, followed by drying at 353 K. Colourless platelet-like single crystals were selected from the reaction products. Each crystal was cut into two portions. One was affixed to a Mitegen^(R) micro-mount device with a drop of Paratone N oil for single-crystal X-ray analysis. The other part was used for elemental analysis by energy dispersive X-ray (EDX) spectrometry using a scanning electron microscope (Hitachi, SU1510) equipped with an EDX detector (Horiba, X-act). EDX analysis indicated a Ca:Y:Si ratio of 0.266 (9):0.237 (4):0.497 (9) for 1, of 0.325 (9):0.183 (5):0.492 (5) for 2, and of 0.386 (19):0.146 (10):0.468 (10) for 3. The ideal ratios according to the formulae of the three title compounds are 0.286:0.214:0.500, 0.321:0.179:0.500, and 0.357:0.143:0.500, respectively.

4. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 2. In the initial stages of the refinements, all Si3 positions were treated as being located at the the 2d site, corresponding to a triangular environment of three N5 atoms. As a result of the strong anisotropy of the displacement ellipsoids along the c axis, the Si3 sites were subsequently refined as being split with half occupancy and a mirror symmetry element at z = ±0.25. When the occupancies of the disordered Ca²⁺ and Y³⁺ sites were refined freely, the ratios of Ca:Y were 7:86:6.14 for 1, 10.07:3.93 for 2, and 9:88:4.12 for 3. Reliability factors for these refinements are summarized in Table 3. All values are almost the same, and the differences between the refined structures are within standard uncertainties. For the final steps of refinements, values obtained by EDX spectrometry were idealized under consideration of charge neutrality. Incorporation of Ce in single crystals of 1 and 3 was confirmed by their photoluminescence (the data are not shown). However, the contamination was ignored because of the small amount (2 mol% relative to Y, that is, Ca₄Y_2.93Ce_0.06Si₇O₁₅N₅ for 1 and Ca₅Y_1.96Ce_0.04Si₇O₁₅N₅ for 3). Actually, consideration of the presence of Ce had only a marginal effect on refinement parameters and refined structures.

Table 2
Experimental details

	1	2	3
Crystal data
Chemical formula	Ca₄Y₃Si₇O₁₅N₅	Ca_4.5Y_2.5Si₇O_15.5N_4.5	Ca₅Y₂Si₇O₁₆N₄
M_r	933.73	910.31	886.89
Crystal system, space group	Hexagonal, P6₃/m	Hexagonal, P6₃/m	Hexagonal, P6₃/m
Temperature (K)	293	296	293
a, c (Å)	10.0884 (5), 9.9740 (5)	10.0792 (5), 9.9900 (5)	10.0541 (2), 10.0168 (2)
V (Å³)	879.11 (10)	878.92 (10)	876.89 (4)
Z	2	2	2
Radiation type	Mo Kα	Mo Kα	Mo Kα
μ (mm⁻¹)	11.56	10.08	8.63
Crystal size (mm)	0.07 × 0.04 × 0.01	0.07 × 0.06 × 0.01	0.05 × 0.03 × 0.02

Data collection
Diffractometer	Rigaku XtaLAB PRO with a PILATUS 200K	Rigaku R-Axis RAPID II	Rigaku R-Axis RAPID II
Absorption correction	Multi-scan (CrysAlis PRO; Rigaku OD, 2015 )	Multi-scan (ABSCOR; Higashi, 2001 )	Multi-scan (ABSCOR; Higashi, 2001)
T_min, T_max	0.684, 1	0.724, 1.000	0.820, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections	8201, 778, 699	8568, 709, 688	8532, 702, 681
R_int	0.039	0.030	0.027
(sin θ/λ)_max (Å⁻¹)	0.685	0.649	0.648

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.025, 0.058, 1.10	0.033, 0.091, 1.19	0.024, 0.062, 1.09
No. of reflections	778	709	702
No. of parameters	62	63	63
No. of restraints	1	1	1
Δρ_max, Δρ_min (e Å⁻³)	1.25, −0.56	1.83, −0.64	0.50, −0.86
Computer programs: CrysAlis PRO (Rigaku OD, 2015), RAPID-AUTO (Rigaku, 2005 ), SHELXT (Sheldrick, 2015a ), SHELXL2014 (Sheldrick, 2015b ), VESTA (Momma & Izumi, 2011 ), WinGX (Farrugia, 2012 ) and publCIF (Westrip, 2010 ).

Table 3
R[F² > 2σ(F²)], wR(F²), S depending on the refinement of the site occupation factor of Ca and Y

	1	2	3
R[F² > 2σ(F²)], wR(F²), S at free occupancy	0.025, 0.058, 1.10	0.031, 0.088, 1.14	0.023, 0.062, 1.09
R[F² > 2σ(F²)], wR(F²), S at fixed occupancy	0.025, 0.058, 1.10	0.033, 0.091, 1.18	0.024, 0.062, 1.09

Five sites around the silicon atoms were detected. Although it is difficult to distinguish between oxygen and nitrogen atoms by XRD analysis alone, site occupancies of oxygen and nitrogen sites were determined from coordination environments, bond lengths, and bond-valence sums (Morgan, 1986 ; Fuertes, 2006 ; Braun et al., 2010 ; Maak et al., 2017). Following Pauling's second crystal rule, the site at Wyckoff position 6h is coordinated by three Si atoms and thus should be occupied by nitrogen (N5) alone. The relatively long bond length of Si3—(O,N)4, 1.804 (6), 1.769 (8), and 1.765 (7) Å for 1, 2, and 3, respectively, indicate that the (O,N)4 site at the 4f position also might be occupied by nitrogen. Under consideration of charge neutrality for the different compositions in 1–3, this site was refined as being occupationally disordered by oxygen and nitrogen for 2 and 3.

Supporting information

CCDC references: 1892876; 1892875; 1892874

Crystal structure: contains datablocks global, 1, 2, 3, Publ_Block. DOI: https://doi.org/10.1107/S2056989019001257/wm5483sup1.cif

Structure factors: contains datablock 1. DOI: https://doi.org/10.1107/S2056989019001257/wm54831sup2.hkl

Structure factors: contains datablock 2. DOI: https://doi.org/10.1107/S2056989019001257/wm54832sup3.hkl

Structure factors: contains datablock 3. DOI: https://doi.org/10.1107/S2056989019001257/wm54833sup4.hkl

checkCIF report

Computing details top

Data collection: CrysAlis PRO (Rigaku OD, 2015) for (1); RAPID-AUTO (Rigaku, 2005) for (2), (3). Cell refinement: CrysAlis PRO (Rigaku OD, 2015) for (1); RAPID-AUTO (Rigaku, 2005) for (2), (3). Data reduction: CrysAlis PRO (Rigaku OD, 2015) for (1); RAPID-AUTO (Rigaku, 2005) for (2), (3). For all structures, program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: VESTA (Momma & Izumi, 2011); software used to prepare material for publication: WinGX (Farrugia, 2012) and publCIF (Westrip, 2010).

Tetracalcium triyttrium heptasilicon oxynitride (1) top

Crystal data top

Ca₄Y₃Si₇O₁₅N₅	D_x = 3.527 Mg m⁻³
M_r = 933.73	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₃/m	Cell parameters from 2781 reflections
Hall symbol: -P 6c	θ = 3.0–28.8°
a = 10.0884 (5) Å	µ = 11.56 mm⁻¹
c = 9.9740 (5) Å	T = 293 K
V = 879.11 (10) Å³	Platelet, colorless
Z = 2	0.07 × 0.04 × 0.01 mm
F(000) = 900

Data collection top

Rigaku XtaLAB PRO with a PILATUS 200K diffractometer	778 independent reflections
Radiation source: fine-focus sealed X-ray tube	699 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.039
ω scans	θ_max = 29.1°, θ_min = 2.3°
Absorption correction: multi-scan (CrysAlisPro; Rigaku OD, 2015)	h = −13→13
T_min = 0.684, T_max = 1	k = −13→12
8201 measured reflections	l = −13→13

Refinement top

Refinement on F²	1 restraint
Least-squares matrix: full	0 constraints
R[F² > 2σ(F²)] = 0.025	Primary atom site location: structure-invariant direct methods
wR(F²) = 0.058	w = 1/[σ²(F_o²) + (0.0223P)² + 2.2946P] where P = (F_o² + 2F_c²)/3
S = 1.10	(Δ/σ)_max < 0.001
778 reflections	Δρ_max = 1.25 e Å⁻³
62 parameters	Δρ_min = −0.56 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)
Ca1	0	0	0	0.00571 (16)	0.1379 (14)
Y1	0	0	0	0.00571 (16)	0.8620 (14)
Ca2	0.41947 (5)	0.13257 (4)	0.03127 (4)	0.01093 (14)	0.6437 (2)
Y2	0.41947 (5)	0.13257 (4)	0.03127 (4)	0.01093 (14)	0.3563 (2)
Si1	0.10867 (11)	0.31831 (11)	0.25	0.0059 (2)
Si2	0.56028 (12)	0.01024 (11)	0.25	0.0075 (2)
Si3	0.3333	0.6667	0.2191 (2)	0.0107 (8)	0.5
O1	0.0791 (2)	0.2237 (2)	0.10980 (19)	0.0136 (4)
O2	0.4447 (2)	0.3571 (2)	0.1075 (2)	0.0170 (4)
O3	0.3985 (3)	0.0201 (3)	0.25	0.0180 (6)
N4	0.3333	0.6667	0.0382 (6)	0.0242 (11)
N5	0.2961 (4)	0.4743 (4)	0.25	0.0164 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ca1	0.0056 (2)	0.0056 (2)	0.0059 (3)	0.00282 (10)	0	0
Y1	0.0056 (2)	0.0056 (2)	0.0059 (3)	0.00282 (10)	0	0
Ca2	0.0164 (2)	0.0099 (2)	0.0095 (2)	0.00887 (17)	−0.00042 (15)	−0.00065 (14)
Y2	0.0164 (2)	0.0099 (2)	0.0095 (2)	0.00887 (17)	−0.00042 (15)	−0.00065 (14)
Si1	0.0059 (5)	0.0053 (5)	0.0056 (5)	0.0021 (4)	0	0
Si2	0.0061 (5)	0.0069 (5)	0.0087 (5)	0.0026 (4)	0	0
Si3	0.0083 (6)	0.0083 (6)	0.016 (2)	0.0041 (3)	0	0
O1	0.0166 (10)	0.0138 (9)	0.0100 (10)	0.0074 (8)	−0.0004 (8)	−0.0048 (8)
O2	0.0235 (11)	0.0159 (10)	0.0138 (10)	0.0114 (9)	−0.0054 (8)	−0.0069 (8)
O3	0.0171 (15)	0.0169 (15)	0.0204 (16)	0.0089 (12)	0	0
N4	0.0167 (14)	0.0167 (14)	0.039 (3)	0.0083 (7)	0	0
N5	0.0068 (16)	0.0096 (16)	0.032 (2)	0.0038 (13)	0	0

Geometric parameters (Å, º) top

Ca1—O1ⁱ	2.2646 (19)	Si2—Ca2^ix	3.1707 (8)
Ca1—O1ⁱⁱ	2.2646 (19)	Si2—Ca2^viii	3.2065 (6)
Ca1—O1ⁱⁱⁱ	2.2646 (19)	Si2—Y2^viii	3.2065 (6)
Ca1—O1^iv	2.2646 (19)	Si2—Ca2^xiii	3.2065 (6)
Ca1—O1^v	2.2646 (19)	Si2—Y2^xiii	3.2065 (6)
Ca1—O1	2.2646 (19)	Si3—Si3^ix	0.617 (5)
Ca1—Y2ⁱⁱ	3.7596 (4)	Si3—N4	1.804 (6)
Ca1—Ca2ⁱⁱⁱ	3.7596 (4)	Si3—N5^xiv	1.809 (3)
Ca1—Ca2ⁱⁱ	3.7596 (4)	Si3—N5	1.809 (3)
Ca1—Y2ⁱⁱⁱ	3.7596 (4)	Si3—N5^xv	1.809 (4)
Ca1—Ca2ⁱ	3.7596 (4)	Si3—Ca2^xvi	3.3919 (18)
Ca1—Y2ⁱ	3.7596 (4)	Si3—Y2^xvi	3.3919 (18)
Ca2—O2	2.280 (2)	Si3—Ca2ⁱⁱ	3.3919 (18)
Ca2—N4^vi	2.3979 (17)	Si3—Y2ⁱⁱ	3.3919 (18)
Ca2—O2^iv	2.418 (2)	Si3—Ca2^vi	3.3919 (18)
Ca2—O3	2.4189 (14)	Si3—Y2^vi	3.3919 (18)
Ca2—O1^iv	2.477 (2)	O1—Y2ⁱⁱ	2.477 (2)
Ca2—O2^vii	2.624 (2)	O1—Ca2ⁱⁱ	2.477 (2)
Ca2—O1ⁱⁱⁱ	2.634 (2)	O1—Ca2^v	2.634 (2)
Ca2—N5^iv	2.8519 (8)	O1—Y2^v	2.634 (2)
Ca2—Si1ⁱⁱⁱ	3.1641 (8)	O2—Si2^xvii	1.635 (2)
Ca2—Si2	3.1707 (8)	O2—Y2ⁱⁱ	2.418 (2)
Ca2—Si2^viii	3.2065 (6)	O2—Ca2ⁱⁱ	2.418 (2)
Ca2—Si1^iv	3.2109 (6)	O2—Ca2^xvii	2.624 (2)
Si1—O1	1.6342 (19)	O2—Y2^xvii	2.624 (2)
Si1—O1^ix	1.6342 (19)	O3—Si1ⁱⁱⁱ	1.686 (3)
Si1—O3^v	1.686 (3)	O3—Y2^ix	2.4189 (14)
Si1—N5	1.754 (3)	O3—Ca2^ix	2.4189 (14)
Si1—Ca2^v	3.1641 (8)	N4—Y2^xvi	2.3980 (17)
Si1—Y2^v	3.1641 (8)	N4—Ca2^xvi	2.3980 (17)
Si1—Ca2^x	3.1641 (8)	N4—Ca2^vi	2.3980 (17)
Si1—Y2^x	3.1641 (8)	N4—Y2^vi	2.3980 (17)
Si1—Ca2^xi	3.2109 (6)	N4—Y2ⁱⁱ	2.3980 (17)
Si1—Y2^xi	3.2109 (6)	N4—Ca2ⁱⁱ	2.3980 (17)
Si1—Ca2ⁱⁱ	3.2109 (6)	N5—Si2^xvii	1.753 (3)
Si1—Y2ⁱⁱ	3.2109 (6)	N5—Si3^ix	1.809 (3)
Si2—O2^xii	1.635 (2)	N5—Ca2ⁱⁱ	2.8520 (8)
Si2—O2^vii	1.635 (2)	N5—Y2ⁱⁱ	2.8520 (8)
Si2—O3	1.685 (3)	N5—Y2^xi	2.8520 (8)
Si2—N5^vii	1.753 (3)	N5—Ca2^xi	2.8520 (8)
Si2—Y2^ix	3.1707 (8)

O1ⁱ—Ca1—O1ⁱⁱ	98.58 (6)	O2^xii—Si2—O3	104.46 (9)
O1ⁱ—Ca1—O1ⁱⁱⁱ	81.42 (6)	O2^vii—Si2—O3	104.46 (9)
O1ⁱⁱ—Ca1—O1ⁱⁱⁱ	180.00 (11)	O2^xii—Si2—N5^vii	107.17 (9)
O1ⁱ—Ca1—O1^iv	98.58 (6)	O2^vii—Si2—N5^vii	107.17 (9)
O1ⁱⁱ—Ca1—O1^iv	98.58 (6)	O3—Si2—N5^vii	113.01 (16)
O1ⁱⁱⁱ—Ca1—O1^iv	81.42 (6)	O2^xii—Si2—Y2^ix	55.73 (8)
O1ⁱ—Ca1—O1^v	81.42 (6)	O2^vii—Si2—Y2^ix	129.27 (9)
O1ⁱⁱ—Ca1—O1^v	81.42 (6)	O3—Si2—Y2^ix	48.77 (4)
O1ⁱⁱⁱ—Ca1—O1^v	98.58 (6)	N5^vii—Si2—Y2^ix	122.49 (7)
O1^iv—Ca1—O1^v	180.00 (9)	O2^xii—Si2—Ca2^ix	55.73 (8)
O1ⁱ—Ca1—O1	180	O2^vii—Si2—Ca2^ix	129.27 (9)
O1ⁱⁱ—Ca1—O1	81.42 (6)	O3—Si2—Ca2^ix	48.77 (4)
O1ⁱⁱⁱ—Ca1—O1	98.58 (6)	N5^vii—Si2—Ca2^ix	122.49 (7)
O1^iv—Ca1—O1	81.42 (6)	Y2^ix—Si2—Ca2^ix	0
O1^v—Ca1—O1	98.58 (6)	O2^xii—Si2—Ca2	129.27 (9)
O1ⁱ—Ca1—Y2ⁱⁱ	140.44 (5)	O2^vii—Si2—Ca2	55.73 (8)
O1ⁱⁱ—Ca1—Y2ⁱⁱ	80.35 (5)	O3—Si2—Ca2	48.77 (4)
O1ⁱⁱⁱ—Ca1—Y2ⁱⁱ	99.65 (5)	N5^vii—Si2—Ca2	122.49 (7)
O1^iv—Ca1—Y2ⁱⁱ	43.64 (5)	Y2^ix—Si2—Ca2	87
O1^v—Ca1—Y2ⁱⁱ	136.36 (5)	Ca2^ix—Si2—Ca2	86.95 (3)
O1—Ca1—Y2ⁱⁱ	39.56 (5)	O2^xii—Si2—Ca2^viii	147.48 (9)
O1ⁱ—Ca1—Ca2ⁱⁱⁱ	39.56 (5)	O2^vii—Si2—Ca2^viii	47.33 (7)
O1ⁱⁱ—Ca1—Ca2ⁱⁱⁱ	99.65 (5)	O3—Si2—Ca2^viii	107.93 (5)
O1ⁱⁱⁱ—Ca1—Ca2ⁱⁱⁱ	80.35 (5)	N5^vii—Si2—Ca2^viii	62.33 (2)
O1^iv—Ca1—Ca2ⁱⁱⁱ	136.36 (5)	Y2^ix—Si2—Ca2^viii	156.7
O1^v—Ca1—Ca2ⁱⁱⁱ	43.64 (5)	Ca2^ix—Si2—Ca2^viii	156.70 (3)
O1—Ca1—Ca2ⁱⁱⁱ	140.44 (5)	Ca2—Si2—Ca2^viii	73.410 (12)
Y2ⁱⁱ—Ca1—Ca2ⁱⁱⁱ	180	O2^xii—Si2—Y2^viii	147.48 (9)
O1ⁱ—Ca1—Ca2ⁱⁱ	140.44 (5)	O2^vii—Si2—Y2^viii	47.33 (7)
O1ⁱⁱ—Ca1—Ca2ⁱⁱ	80.35 (5)	O3—Si2—Y2^viii	107.93 (5)
O1ⁱⁱⁱ—Ca1—Ca2ⁱⁱ	99.65 (5)	N5^vii—Si2—Y2^viii	62.33 (2)
O1^iv—Ca1—Ca2ⁱⁱ	43.64 (5)	Y2^ix—Si2—Y2^viii	156.70 (3)
O1^v—Ca1—Ca2ⁱⁱ	136.36 (5)	Ca2^ix—Si2—Y2^viii	156.70 (3)
O1—Ca1—Ca2ⁱⁱ	39.56 (5)	Ca2—Si2—Y2^viii	73.4
Y2ⁱⁱ—Ca1—Ca2ⁱⁱ	0	Ca2^viii—Si2—Y2^viii	0.000 (16)
Ca2ⁱⁱⁱ—Ca1—Ca2ⁱⁱ	180.000 (13)	O2^xii—Si2—Ca2^xiii	47.33 (7)
O1ⁱ—Ca1—Y2ⁱⁱⁱ	39.56 (5)	O2^vii—Si2—Ca2^xiii	147.48 (9)
O1ⁱⁱ—Ca1—Y2ⁱⁱⁱ	99.65 (5)	O3—Si2—Ca2^xiii	107.93 (5)
O1ⁱⁱⁱ—Ca1—Y2ⁱⁱⁱ	80.35 (5)	N5^vii—Si2—Ca2^xiii	62.33 (2)
O1^iv—Ca1—Y2ⁱⁱⁱ	136.36 (5)	Y2^ix—Si2—Ca2^xiii	73.4
O1^v—Ca1—Y2ⁱⁱⁱ	43.64 (5)	Ca2^ix—Si2—Ca2^xiii	73.410 (12)
O1—Ca1—Y2ⁱⁱⁱ	140.44 (5)	Ca2—Si2—Ca2^xiii	156.70 (3)
Y2ⁱⁱ—Ca1—Y2ⁱⁱⁱ	180	Ca2^viii—Si2—Ca2^xiii	122.07 (3)
Ca2ⁱⁱⁱ—Ca1—Y2ⁱⁱⁱ	0.000 (16)	Y2^viii—Si2—Ca2^xiii	122.1
Ca2ⁱⁱ—Ca1—Y2ⁱⁱⁱ	180	O2^xii—Si2—Y2^xiii	47.33 (7)
O1ⁱ—Ca1—Ca2ⁱ	80.35 (5)	O2^vii—Si2—Y2^xiii	147.48 (9)
O1ⁱⁱ—Ca1—Ca2ⁱ	43.64 (5)	O3—Si2—Y2^xiii	107.93 (5)
O1ⁱⁱⁱ—Ca1—Ca2ⁱ	136.36 (5)	N5^vii—Si2—Y2^xiii	62.33 (2)
O1^iv—Ca1—Ca2ⁱ	140.44 (5)	Y2^ix—Si2—Y2^xiii	73.410 (12)
O1^v—Ca1—Ca2ⁱ	39.56 (5)	Ca2^ix—Si2—Y2^xiii	73.410 (12)
O1—Ca1—Ca2ⁱ	99.65 (5)	Ca2—Si2—Y2^xiii	156.7
Y2ⁱⁱ—Ca1—Ca2ⁱ	119.3	Ca2^viii—Si2—Y2^xiii	122.07 (3)
Ca2ⁱⁱⁱ—Ca1—Ca2ⁱ	60.681 (2)	Y2^viii—Si2—Y2^xiii	122.07 (3)
Ca2ⁱⁱ—Ca1—Ca2ⁱ	119.319 (2)	Ca2^xiii—Si2—Y2^xiii	0.000 (16)
Y2ⁱⁱⁱ—Ca1—Ca2ⁱ	60.7	Si3^ix—Si3—N4	180
O1ⁱ—Ca1—Y2ⁱ	80.35 (5)	Si3^ix—Si3—N5^xiv	80.19 (7)
O1ⁱⁱ—Ca1—Y2ⁱ	43.64 (5)	N4—Si3—N5^xiv	99.82 (7)
O1ⁱⁱⁱ—Ca1—Y2ⁱ	136.36 (5)	Si3^ix—Si3—N5	80.18 (7)
O1^iv—Ca1—Y2ⁱ	140.44 (5)	N4—Si3—N5	99.82 (7)
O1^v—Ca1—Y2ⁱ	39.56 (5)	N5^xiv—Si3—N5	117.15 (4)
O1—Ca1—Y2ⁱ	99.65 (5)	Si3^ix—Si3—N5^xv	80.18 (8)
Y2ⁱⁱ—Ca1—Y2ⁱ	119.319 (2)	N4—Si3—N5^xv	99.82 (7)
Ca2ⁱⁱⁱ—Ca1—Y2ⁱ	60.681 (2)	N5^xiv—Si3—N5^xv	117.16 (4)
Ca2ⁱⁱ—Ca1—Y2ⁱ	119.319 (2)	N5—Si3—N5^xv	117.15 (4)
Y2ⁱⁱⁱ—Ca1—Y2ⁱ	60.681 (2)	Si3^ix—Si3—Ca2^xvi	137.41 (3)
Ca2ⁱ—Ca1—Y2ⁱ	0.000 (13)	N4—Si3—Ca2^xvi	42.60 (3)
O2—Ca2—N4^vi	72.84 (8)	N5^xiv—Si3—Ca2^xvi	57.22 (5)
O2—Ca2—O2^iv	162.18 (6)	N5—Si3—Ca2^xvi	117.10 (9)
N4^vi—Ca2—O2^iv	107.07 (10)	N5^xv—Si3—Ca2^xvi	117.54 (9)
O2—Ca2—O3	96.04 (8)	Si3^ix—Si3—Y2^xvi	137.41 (3)
N4^vi—Ca2—O3	117.84 (14)	N4—Si3—Y2^xvi	42.60 (3)
O2^iv—Ca2—O3	99.44 (8)	N5^xiv—Si3—Y2^xvi	57.22 (5)
O2—Ca2—O1^iv	80.58 (7)	N5—Si3—Y2^xvi	117.10 (9)
N4^vi—Ca2—O1^iv	108.21 (10)	N5^xv—Si3—Y2^xvi	117.54 (9)
O2^iv—Ca2—O1^iv	82.66 (7)	Ca2^xvi—Si3—Y2^xvi	0.00 (2)
O3—Ca2—O1^iv	130.56 (8)	Si3^ix—Si3—Ca2ⁱⁱ	137.40 (3)
O2—Ca2—O2^vii	113.34 (9)	N4—Si3—Ca2ⁱⁱ	42.60 (3)
N4^vi—Ca2—O2^vii	67.01 (7)	N5^xiv—Si3—Ca2ⁱⁱ	117.54 (9)
O2^iv—Ca2—O2^vii	81.88 (7)	N5—Si3—Ca2ⁱⁱ	57.22 (5)
O3—Ca2—O2^vii	62.54 (8)	N5^xv—Si3—Ca2ⁱⁱ	117.10 (9)
O1^iv—Ca2—O2^vii	161.43 (7)	Ca2^xvi—Si3—Ca2ⁱⁱ	71.77 (4)
O2—Ca2—O1ⁱⁱⁱ	104.80 (7)	Y2^xvi—Si3—Ca2ⁱⁱ	71.8
N4^vi—Ca2—O1ⁱⁱⁱ	177.55 (5)	Si3^ix—Si3—Y2ⁱⁱ	137.40 (3)
O2^iv—Ca2—O1ⁱⁱⁱ	74.97 (6)	N4—Si3—Y2ⁱⁱ	42.60 (3)
O3—Ca2—O1ⁱⁱⁱ	62.73 (8)	N5^xiv—Si3—Y2ⁱⁱ	117.54 (9)
O1^iv—Ca2—O1ⁱⁱⁱ	70.53 (8)	N5—Si3—Y2ⁱⁱ	57.22 (5)
O2^vii—Ca2—O1ⁱⁱⁱ	114.87 (6)	N5^xv—Si3—Y2ⁱⁱ	117.10 (9)
O2—Ca2—N5^iv	104.57 (9)	Ca2^xvi—Si3—Y2ⁱⁱ	71.77 (4)
N4^vi—Ca2—N5^iv	62.85 (14)	Y2^xvi—Si3—Y2ⁱⁱ	71.77 (4)
O2^iv—Ca2—N5^iv	61.67 (8)	Ca2ⁱⁱ—Si3—Y2ⁱⁱ	0.000 (15)
O3—Ca2—N5^iv	158.03 (9)	Si3^ix—Si3—Ca2^vi	137.40 (3)
O1^iv—Ca2—N5^iv	61.86 (8)	N4—Si3—Ca2^vi	42.60 (3)
O2^vii—Ca2—N5^iv	101.48 (8)	N5^xiv—Si3—Ca2^vi	117.10 (9)
O1ⁱⁱⁱ—Ca2—N5^iv	117.64 (8)	N5—Si3—Ca2^vi	117.54 (9)
O2—Ca2—Si1ⁱⁱⁱ	103.50 (6)	N5^xv—Si3—Ca2^vi	57.22 (5)
N4^vi—Ca2—Si1ⁱⁱⁱ	149.56 (12)	Ca2^xvi—Si3—Ca2^vi	71.77 (4)
O2^iv—Ca2—Si1ⁱⁱⁱ	85.50 (5)	Y2^xvi—Si3—Ca2^vi	71.8
O3—Ca2—Si1ⁱⁱⁱ	31.72 (7)	Ca2ⁱⁱ—Si3—Ca2^vi	71.77 (4)
O1^iv—Ca2—Si1ⁱⁱⁱ	100.73 (5)	Y2ⁱⁱ—Si3—Ca2^vi	71.8
O2^vii—Ca2—Si1ⁱⁱⁱ	88.24 (5)	Si3^ix—Si3—Y2^vi	137.40 (3)
O1ⁱⁱⁱ—Ca2—Si1ⁱⁱⁱ	31.06 (4)	N4—Si3—Y2^vi	42.60 (3)
N5^iv—Ca2—Si1ⁱⁱⁱ	143.47 (7)	N5^xiv—Si3—Y2^vi	117.10 (9)
O2—Ca2—Si2	107.94 (6)	N5—Si3—Y2^vi	117.54 (9)
N4^vi—Ca2—Si2	92.78 (9)	N5^xv—Si3—Y2^vi	57.22 (5)
O2^iv—Ca2—Si2	89.88 (5)	Ca2^xvi—Si3—Y2^vi	71.77 (4)
O3—Ca2—Si2	31.59 (7)	Y2^xvi—Si3—Y2^vi	71.77 (4)
O1^iv—Ca2—Si2	158.96 (5)	Ca2ⁱⁱ—Si3—Y2^vi	71.77 (4)
O2^vii—Ca2—Si2	30.98 (5)	Y2ⁱⁱ—Si3—Y2^vi	71.77 (4)
O1ⁱⁱⁱ—Ca2—Si2	88.56 (5)	Ca2^vi—Si3—Y2^vi	0.000 (18)
N5^iv—Ca2—Si2	130.63 (7)	Si1—O1—Ca1	150.03 (12)
Si1ⁱⁱⁱ—Ca2—Si2	58.93 (3)	Si1—O1—Y2ⁱⁱ	100.71 (9)
O2—Ca2—Si2^viii	137.54 (6)	Ca1—O1—Y2ⁱⁱ	104.82 (7)
N4^vi—Ca2—Si2^viii	81.59 (11)	Si1—O1—Ca2ⁱⁱ	100.71 (9)
O2^iv—Ca2—Si2^viii	29.80 (5)	Ca1—O1—Ca2ⁱⁱ	104.82 (7)
O3—Ca2—Si2^viii	126.06 (7)	Y2ⁱⁱ—O1—Ca2ⁱⁱ	0
O1^iv—Ca2—Si2^viii	75.91 (5)	Si1—O1—Ca2^v	92.67 (9)
O2^vii—Ca2—Si2^viii	85.57 (5)	Ca1—O1—Ca2^v	99.97 (7)
O1ⁱⁱⁱ—Ca2—Si2^viii	100.00 (5)	Y2ⁱⁱ—O1—Ca2^v	95.9
N5^iv—Ca2—Si2^viii	32.98 (7)	Ca2ⁱⁱ—O1—Ca2^v	95.94 (7)
Si1ⁱⁱⁱ—Ca2—Si2^viii	115.22 (2)	Si1—O1—Y2^v	92.67 (9)
Si2—Ca2—Si2^viii	106.589 (12)	Ca1—O1—Y2^v	99.97 (7)
O2—Ca2—Si1^iv	86.68 (6)	Y2ⁱⁱ—O1—Y2^v	95.94 (7)
N4^vi—Ca2—Si1^iv	82.26 (11)	Ca2ⁱⁱ—O1—Y2^v	95.94 (7)
O2^iv—Ca2—Si1^iv	75.76 (5)	Ca2^v—O1—Y2^v	0.00 (3)
O3—Ca2—Si1^iv	159.66 (7)	Si2^xvii—O2—Ca2	139.08 (12)
O1^iv—Ca2—Si1^iv	30.01 (5)	Si2^xvii—O2—Y2ⁱⁱ	102.87 (10)
O2^vii—Ca2—Si1^iv	134.39 (5)	Ca2—O2—Y2ⁱⁱ	107.8
O1ⁱⁱⁱ—Ca2—Si1^iv	97.06 (5)	Si2^xvii—O2—Ca2ⁱⁱ	102.87 (10)
N5^iv—Ca2—Si1^iv	32.96 (7)	Ca2—O2—Ca2ⁱⁱ	107.85 (8)
Si1ⁱⁱⁱ—Ca2—Si1^iv	128.11 (3)	Y2ⁱⁱ—O2—Ca2ⁱⁱ	0
Si2—Ca2—Si1^iv	162.54 (2)	Si2^xvii—O2—Ca2^xvii	93.30 (9)
Si2^viii—Ca2—Si1^iv	56.20 (2)	Ca2—O2—Ca2^xvii	108.14 (8)
O1—Si1—O1^ix	117.68 (15)	Y2ⁱⁱ—O2—Ca2^xvii	98.1
O1—Si1—O3^v	105.15 (9)	Ca2ⁱⁱ—O2—Ca2^xvii	98.12 (7)
O1^ix—Si1—O3^v	105.15 (9)	Si2^xvii—O2—Y2^xvii	93.30 (9)
O1—Si1—N5	108.92 (9)	Ca2—O2—Y2^xvii	108.1
O1^ix—Si1—N5	108.92 (9)	Y2ⁱⁱ—O2—Y2^xvii	98.12 (7)
O3^v—Si1—N5	110.87 (16)	Ca2ⁱⁱ—O2—Y2^xvii	98.12 (7)
O1—Si1—Ca2^v	56.27 (7)	Ca2^xvii—O2—Y2^xvii	0.00 (3)
O1^ix—Si1—Ca2^v	128.66 (8)	Si2—O3—Si1ⁱⁱⁱ	135.20 (19)
O3^v—Si1—Ca2^v	48.97 (4)	Si2—O3—Y2^ix	99.64 (8)
N5—Si1—Ca2^v	121.33 (7)	Si1ⁱⁱⁱ—O3—Y2^ix	99.31 (8)
O1—Si1—Y2^v	56.27 (7)	Si2—O3—Ca2^ix	99.64 (8)
O1^ix—Si1—Y2^v	128.66 (8)	Si1ⁱⁱⁱ—O3—Ca2^ix	99.31 (8)
O3^v—Si1—Y2^v	48.97 (4)	Y2^ix—O3—Ca2^ix	0
N5—Si1—Y2^v	121.33 (7)	Si2—O3—Ca2	99.64 (8)
Ca2^v—Si1—Y2^v	0.000 (16)	Si1ⁱⁱⁱ—O3—Ca2	99.31 (8)
O1—Si1—Ca2^x	128.66 (8)	Y2^ix—O3—Ca2	128.8
O1^ix—Si1—Ca2^x	56.27 (7)	Ca2^ix—O3—Ca2	128.82 (13)
O3^v—Si1—Ca2^x	48.97 (4)	Si3—N4—Y2^xvi	106.79 (13)
N5—Si1—Ca2^x	121.33 (7)	Si3—N4—Ca2^xvi	106.79 (13)
Ca2^v—Si1—Ca2^x	87.18 (3)	Y2^xvi—N4—Ca2^xvi	0
Y2^v—Si1—Ca2^x	87.2	Si3—N4—Ca2^vi	106.79 (13)
O1—Si1—Y2^x	128.66 (8)	Y2^xvi—N4—Ca2^vi	112
O1^ix—Si1—Y2^x	56.27 (7)	Ca2^xvi—N4—Ca2^vi	112.01 (12)
O3^v—Si1—Y2^x	48.97 (4)	Si3—N4—Y2^vi	106.79 (13)
N5—Si1—Y2^x	121.33 (7)	Y2^xvi—N4—Y2^vi	112.01 (12)
Ca2^v—Si1—Y2^x	87.18 (3)	Ca2^xvi—N4—Y2^vi	112.01 (12)
Y2^v—Si1—Y2^x	87.18 (3)	Ca2^vi—N4—Y2^vi	0.000 (19)
Ca2^x—Si1—Y2^x	0.000 (11)	Si3—N4—Y2ⁱⁱ	106.79 (13)
O1—Si1—Ca2^xi	147.46 (9)	Y2^xvi—N4—Y2ⁱⁱ	112.01 (12)
O1^ix—Si1—Ca2^xi	49.29 (7)	Ca2^xvi—N4—Y2ⁱⁱ	112.01 (12)
O3^v—Si1—Ca2^xi	107.19 (5)	Ca2^vi—N4—Y2ⁱⁱ	112.01 (12)
N5—Si1—Ca2^xi	62.20 (2)	Y2^vi—N4—Y2ⁱⁱ	112.01 (12)
Ca2^v—Si1—Ca2^xi	156.16 (3)	Si3—N4—Ca2ⁱⁱ	106.79 (13)
Y2^v—Si1—Ca2^xi	156.2	Y2^xvi—N4—Ca2ⁱⁱ	112
Ca2^x—Si1—Ca2^xi	73.134 (8)	Ca2^xvi—N4—Ca2ⁱⁱ	112.01 (12)
Y2^x—Si1—Ca2^xi	73.1	Ca2^vi—N4—Ca2ⁱⁱ	112.01 (12)
O1—Si1—Y2^xi	147.46 (9)	Y2^vi—N4—Ca2ⁱⁱ	112
O1^ix—Si1—Y2^xi	49.29 (7)	Y2ⁱⁱ—N4—Ca2ⁱⁱ	0
O3^v—Si1—Y2^xi	107.19 (5)	Si2^xvii—N5—Si1	119.1 (2)
N5—Si1—Y2^xi	62.20 (2)	Si2^xvii—N5—Si3^ix	118.93 (18)
Ca2^v—Si1—Y2^xi	156.16 (3)	Si1—N5—Si3^ix	121.00 (18)
Y2^v—Si1—Y2^xi	156.16 (3)	Si2^xvii—N5—Si3	118.93 (18)
Ca2^x—Si1—Y2^xi	73.134 (8)	Si1—N5—Si3	121.00 (18)
Y2^x—Si1—Y2^xi	73.134 (8)	Si3^ix—N5—Si3	19.64 (15)
Ca2^xi—Si1—Y2^xi	0.000 (18)	Si2^xvii—N5—Ca2ⁱⁱ	84.69 (7)
O1—Si1—Ca2ⁱⁱ	49.29 (7)	Si1—N5—Ca2ⁱⁱ	84.84 (7)
O1^ix—Si1—Ca2ⁱⁱ	147.46 (9)	Si3^ix—N5—Ca2ⁱⁱ	110.18 (11)
O3^v—Si1—Ca2ⁱⁱ	107.19 (5)	Si3—N5—Ca2ⁱⁱ	90.54 (9)
N5—Si1—Ca2ⁱⁱ	62.20 (2)	Si2^xvii—N5—Y2ⁱⁱ	84.69 (7)
Ca2^v—Si1—Ca2ⁱⁱ	73.134 (8)	Si1—N5—Y2ⁱⁱ	84.84 (7)
Y2^v—Si1—Ca2ⁱⁱ	73.1	Si3^ix—N5—Y2ⁱⁱ	110.18 (11)
Ca2^x—Si1—Ca2ⁱⁱ	156.16 (3)	Si3—N5—Y2ⁱⁱ	90.54 (9)
Y2^x—Si1—Ca2ⁱⁱ	156.2	Ca2ⁱⁱ—N5—Y2ⁱⁱ	0.00 (3)
Ca2^xi—Si1—Ca2ⁱⁱ	121.79 (3)	Si2^xvii—N5—Y2^xi	84.69 (7)
Y2^xi—Si1—Ca2ⁱⁱ	121.8	Si1—N5—Y2^xi	84.84 (7)
O1—Si1—Y2ⁱⁱ	49.29 (7)	Si3^ix—N5—Y2^xi	90.54 (9)
O1^ix—Si1—Y2ⁱⁱ	147.46 (9)	Si3—N5—Y2^xi	110.18 (11)
O3^v—Si1—Y2ⁱⁱ	107.19 (5)	Ca2ⁱⁱ—N5—Y2^xi	159.27 (14)
N5—Si1—Y2ⁱⁱ	62.20 (2)	Y2ⁱⁱ—N5—Y2^xi	159.27 (14)
Ca2^v—Si1—Y2ⁱⁱ	73.134 (8)	Si2^xvii—N5—Ca2^xi	84.69 (7)
Y2^v—Si1—Y2ⁱⁱ	73.134 (8)	Si1—N5—Ca2^xi	84.84 (7)
Ca2^x—Si1—Y2ⁱⁱ	156.16 (3)	Si3^ix—N5—Ca2^xi	90.54 (9)
Y2^x—Si1—Y2ⁱⁱ	156.16 (3)	Si3—N5—Ca2^xi	110.18 (11)
Ca2^xi—Si1—Y2ⁱⁱ	121.79 (3)	Ca2ⁱⁱ—N5—Ca2^xi	159.27 (14)
Y2^xi—Si1—Y2ⁱⁱ	121.79 (3)	Y2ⁱⁱ—N5—Ca2^xi	159.3
Ca2ⁱⁱ—Si1—Y2ⁱⁱ	0.000 (7)	Y2^xi—N5—Ca2^xi	0
O2^xii—Si2—O2^vii	120.73 (16)

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

Calcium yttrium heptasilicon oxynitride (2) top

Crystal data top

Ca_4.5Y_2.5Si₇O_15.5N_4.5	D_x = 3.44 Mg m⁻³
M_r = 910.31	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₃/m	Cell parameters from 6355 reflections
Hall symbol: -P 6c	θ = 3.1–27.5°
a = 10.0792 (5) Å	µ = 10.08 mm⁻¹
c = 9.9900 (5) Å	T = 296 K
V = 878.92 (10) Å³	Platelet, colorless
Z = 2	0.07 × 0.06 × 0.01 mm
F(000) = 882

Data collection top

Rigaku R-Axis RAPID II diffractometer	709 independent reflections
Radiation source: sealed x-ray tube	688 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.030
Detector resolution: 10 pixels mm^-1	θ_max = 27.5°, θ_min = 3.1°
phi or ω oscillation scans	h = −13→12
Absorption correction: multi-scan (ABSCOR; Higashi, 2001)	k = −12→12
T_min = 0.724, T_max = 1.000	l = −12→12
8568 measured reflections

Refinement top

Refinement on F²	0 constraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F² > 2σ(F²)] = 0.033	w = 1/[σ²(F_o²) + (0.0508P)² + 2.6144P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.091	(Δ/σ)_max < 0.001
S = 1.19	Δρ_max = 1.83 e Å⁻³
709 reflections	Δρ_min = −0.64 e Å⁻³
63 parameters	Extinction correction: SHELXL-2014/7 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
1 restraint	Extinction coefficient: 0.028 (2)

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ca1	0	0	0	0.0099 (3)	0.1338 (14)
Y1	0	0	0	0.0099 (3)	0.8662 (14)
Ca2	0.41517 (7)	0.12870 (6)	0.03382 (6)	0.0143 (2)	0.7277 (2)
Y2	0.41517 (7)	0.12870 (6)	0.03382 (6)	0.0143 (2)	0.2723 (2)
Si1	0.11057 (12)	0.31892 (13)	0.25	0.0061 (3)
Si2	0.55909 (13)	0.01171 (14)	0.25	0.0077 (3)
Si3	0.3333	0.6667	0.2216 (2)	0.0035 (9)	0.5
O1	0.0838 (3)	0.2250 (3)	0.1115 (2)	0.0143 (5)
O2	0.4447 (3)	0.3570 (3)	0.1092 (3)	0.0184 (6)
O3	0.3956 (4)	0.0167 (4)	0.25	0.0186 (8)
O4	0.3333	0.6667	0.0445 (8)	0.0358 (15)	0.25
N4	0.3333	0.6667	0.0445 (8)	0.0358 (15)	0.75
N5	0.2989 (4)	0.4828 (5)	0.25	0.0251 (11)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ca1	0.0095 (3)	0.0095 (3)	0.0107 (4)	0.00475 (15)	0	0
Y1	0.0095 (3)	0.0095 (3)	0.0107 (4)	0.00475 (15)	0	0
Ca2	0.0209 (3)	0.0137 (3)	0.0117 (4)	0.0111 (2)	−0.0003 (2)	−0.00032 (19)
Y2	0.0209 (3)	0.0137 (3)	0.0117 (4)	0.0111 (2)	−0.0003 (2)	−0.00032 (19)
Si1	0.0049 (5)	0.0078 (6)	0.0045 (6)	0.0024 (4)	0	0
Si2	0.0060 (5)	0.0101 (6)	0.0072 (6)	0.0042 (4)	0	0
Si3	0.0015 (6)	0.0015 (6)	0.008 (3)	0.0007 (3)	0	0
O1	0.0198 (12)	0.0174 (11)	0.0076 (11)	0.0108 (10)	0.0010 (9)	−0.0036 (9)
O2	0.0295 (14)	0.0159 (11)	0.0107 (12)	0.0120 (10)	−0.0052 (10)	−0.0054 (10)
O3	0.0169 (17)	0.0204 (17)	0.0183 (19)	0.0092 (14)	0	0
O4	0.032 (2)	0.032 (2)	0.044 (4)	0.0159 (10)	0	0
N4	0.032 (2)	0.032 (2)	0.044 (4)	0.0159 (10)	0	0
N5	0.0081 (18)	0.020 (2)	0.044 (3)	0.0048 (16)	0	0

Geometric parameters (Å, º) top

Ca1—O1	2.276 (2)	Si2—Ca2^viii	3.1415 (10)
Ca1—O1ⁱ	2.276 (2)	Si2—Y2^viii	3.1415 (10)
Ca1—O1ⁱⁱ	2.276 (2)	Si2—Ca2^xii	3.2368 (8)
Ca1—O1ⁱⁱⁱ	2.276 (2)	Si2—Y2^xii	3.2368 (8)
Ca1—O1^iv	2.276 (2)	Si2—Y2^xiii	3.2368 (8)
Ca1—O1^v	2.276 (2)	Si2—Ca2^xiii	3.2368 (8)
Ca1—Ca2	3.7255 (6)	Si3—Si3^viii	0.567 (5)
Ca1—Ca2ⁱⁱⁱ	3.7255 (6)	Si3—N5^xiv	1.730 (5)
Ca1—Ca2ⁱⁱ	3.7255 (6)	Si3—N5^xv	1.730 (5)
Ca1—Y2ⁱⁱ	3.7255 (6)	Si3—N5	1.730 (5)
Ca1—Y2ⁱⁱⁱ	3.7255 (6)	Si3—O4	1.769 (8)
Ca2—O2	2.295 (2)	Si3—N4^viii	2.336 (8)
Ca2—O3	2.3990 (17)	Si3—Ca2^xvi	3.4587 (19)
Ca2—O2^iv	2.422 (3)	Si3—Ca2ⁱⁱ	3.4587 (19)
Ca2—O1^iv	2.457 (3)	Si3—Ca2^vi	3.4587 (19)
Ca2—N4^vi	2.463 (3)	O1—Y2ⁱⁱ	2.457 (3)
Ca2—O4^vi	2.463 (3)	O1—Ca2ⁱⁱ	2.457 (3)
Ca2—O1ⁱⁱⁱ	2.627 (2)	O1—Ca2^v	2.627 (2)
Ca2—O2^vii	2.638 (3)	O1—Y2^v	2.627 (2)
Ca2—N5^iv	2.9043 (12)	O2—Si2^xvii	1.622 (3)
Ca2—Si1ⁱⁱⁱ	3.1302 (10)	O2—Y2ⁱⁱ	2.422 (3)
Ca2—Si2	3.1415 (10)	O2—Ca2ⁱⁱ	2.422 (3)
Ca2—Si1^iv	3.2255 (8)	O2—Ca2^xvii	2.638 (3)
Si1—O1^viii	1.621 (2)	O2—Y2^xvii	2.638 (3)
Si1—O1	1.621 (2)	O3—Si1ⁱⁱⁱ	1.669 (4)
Si1—O3^v	1.669 (4)	O3—Ca2^viii	2.3990 (17)
Si1—N5	1.788 (4)	O3—Y2^viii	2.3990 (17)
Si1—Ca2^v	3.1302 (10)	O4—Y2^xvi	2.463 (3)
Si1—Y2^v	3.1302 (10)	O4—Ca2^xvi	2.463 (3)
Si1—Ca2^ix	3.1302 (10)	O4—Ca2^vi	2.463 (3)
Si1—Y2^ix	3.1302 (10)	O4—Y2^vi	2.463 (3)
Si1—Ca2^x	3.2255 (8)	O4—Y2ⁱⁱ	2.463 (3)
Si1—Y2^x	3.2255 (8)	O4—Ca2ⁱⁱ	2.463 (3)
Si1—Y2ⁱⁱ	3.2255 (8)	N5—Si3^viii	1.730 (5)
Si1—Ca2ⁱⁱ	3.2255 (8)	N5—Si2^xvii	1.798 (4)
Si2—O2^xi	1.622 (3)	N5—Ca2ⁱⁱ	2.9042 (12)
Si2—O2^vii	1.622 (3)	N5—Y2ⁱⁱ	2.9042 (12)
Si2—O3	1.673 (4)	N5—Y2^x	2.9042 (12)
Si2—N5^vii	1.798 (4)	N5—Ca2^x	2.9042 (12)

O1—Ca1—O1ⁱ	180	Ca2^x—Si1—Ca2ⁱⁱ	123.06 (4)
O1—Ca1—O1ⁱⁱ	81.90 (8)	Y2^x—Si1—Ca2ⁱⁱ	123.1
O1ⁱ—Ca1—O1ⁱⁱ	98.10 (8)	Y2ⁱⁱ—Si1—Ca2ⁱⁱ	0
O1—Ca1—O1ⁱⁱⁱ	98.10 (8)	O2^xi—Si2—O2^vii	120.21 (19)
O1ⁱ—Ca1—O1ⁱⁱⁱ	81.90 (8)	O2^xi—Si2—O3	105.94 (12)
O1ⁱⁱ—Ca1—O1ⁱⁱⁱ	180.00 (14)	O2^vii—Si2—O3	105.94 (12)
O1—Ca1—O1^iv	81.90 (8)	O2^xi—Si2—N5^vii	107.38 (12)
O1ⁱ—Ca1—O1^iv	98.10 (8)	O2^vii—Si2—N5^vii	107.38 (12)
O1ⁱⁱ—Ca1—O1^iv	98.10 (8)	O3—Si2—N5^vii	109.7 (2)
O1ⁱⁱⁱ—Ca1—O1^iv	81.90 (8)	O2^xi—Si2—Ca2	130.42 (11)
O1—Ca1—O1^v	98.10 (8)	O2^vii—Si2—Ca2	57.07 (10)
O1ⁱ—Ca1—O1^v	81.90 (8)	O3—Si2—Ca2	48.88 (6)
O1ⁱⁱ—Ca1—O1^v	81.90 (8)	N5^vii—Si2—Ca2	120.81 (9)
O1ⁱⁱⁱ—Ca1—O1^v	98.10 (8)	O2^xi—Si2—Ca2^viii	57.07 (10)
O1^iv—Ca1—O1^v	180.0 (2)	O2^vii—Si2—Ca2^viii	130.42 (11)
O1—Ca1—Ca2	79.39 (6)	O3—Si2—Ca2^viii	48.88 (6)
O1ⁱ—Ca1—Ca2	100.61 (6)	N5^vii—Si2—Ca2^viii	120.81 (9)
O1ⁱⁱ—Ca1—Ca2	135.80 (6)	Ca2—Si2—Ca2^viii	86.86 (4)
O1ⁱⁱⁱ—Ca1—Ca2	44.20 (6)	O2^xi—Si2—Y2^viii	57.07 (10)
O1^iv—Ca1—Ca2	39.84 (6)	O2^vii—Si2—Y2^viii	130.42 (11)
O1^v—Ca1—Ca2	140.16 (6)	O3—Si2—Y2^viii	48.88 (6)
O1—Ca1—Ca2ⁱⁱⁱ	140.16 (6)	N5^vii—Si2—Y2^viii	120.81 (9)
O1ⁱ—Ca1—Ca2ⁱⁱⁱ	39.84 (6)	Ca2—Si2—Y2^viii	86.9
O1ⁱⁱ—Ca1—Ca2ⁱⁱⁱ	100.61 (6)	Ca2^viii—Si2—Y2^viii	0.00 (2)
O1ⁱⁱⁱ—Ca1—Ca2ⁱⁱⁱ	79.39 (6)	O2^xi—Si2—Ca2^xii	145.99 (11)
O1^iv—Ca1—Ca2ⁱⁱⁱ	135.80 (6)	O2^vii—Si2—Ca2^xii	46.38 (9)
O1^v—Ca1—Ca2ⁱⁱⁱ	44.20 (6)	O3—Si2—Ca2^xii	107.97 (6)
Ca2—Ca1—Ca2ⁱⁱⁱ	119.187 (3)	N5^vii—Si2—Ca2^xii	63.05 (3)
O1—Ca1—Ca2ⁱⁱ	39.84 (6)	Ca2—Si2—Ca2^xii	73.437 (16)
O1ⁱ—Ca1—Ca2ⁱⁱ	140.16 (6)	Ca2^viii—Si2—Ca2^xii	156.83 (4)
O1ⁱⁱ—Ca1—Ca2ⁱⁱ	79.39 (6)	Y2^viii—Si2—Ca2^xii	156.8
O1ⁱⁱⁱ—Ca1—Ca2ⁱⁱ	100.61 (6)	O2^xi—Si2—Y2^xii	145.99 (11)
O1^iv—Ca1—Ca2ⁱⁱ	44.20 (6)	O2^vii—Si2—Y2^xii	46.38 (9)
O1^v—Ca1—Ca2ⁱⁱ	135.80 (6)	O3—Si2—Y2^xii	107.97 (6)
Ca2—Ca1—Ca2ⁱⁱ	60.813 (3)	N5^vii—Si2—Y2^xii	63.05 (3)
Ca2ⁱⁱⁱ—Ca1—Ca2ⁱⁱ	180.000 (18)	Ca2—Si2—Y2^xii	73.4
O1—Ca1—Y2ⁱⁱ	39.84 (6)	Ca2^viii—Si2—Y2^xii	156.83 (4)
O1ⁱ—Ca1—Y2ⁱⁱ	140.16 (6)	Y2^viii—Si2—Y2^xii	156.83 (4)
O1ⁱⁱ—Ca1—Y2ⁱⁱ	79.39 (6)	Ca2^xii—Si2—Y2^xii	0.00 (4)
O1ⁱⁱⁱ—Ca1—Y2ⁱⁱ	100.61 (6)	O2^xi—Si2—Y2^xiii	46.38 (9)
O1^iv—Ca1—Y2ⁱⁱ	44.20 (6)	O2^vii—Si2—Y2^xiii	145.99 (11)
O1^v—Ca1—Y2ⁱⁱ	135.80 (6)	O3—Si2—Y2^xiii	107.97 (6)
Ca2—Ca1—Y2ⁱⁱ	60.8	N5^vii—Si2—Y2^xiii	63.05 (3)
Ca2ⁱⁱⁱ—Ca1—Y2ⁱⁱ	180.000 (18)	Ca2—Si2—Y2^xiii	156.8
Ca2ⁱⁱ—Ca1—Y2ⁱⁱ	0.00 (3)	Ca2^viii—Si2—Y2^xiii	73.437 (16)
O1—Ca1—Y2ⁱⁱⁱ	140.16 (6)	Y2^viii—Si2—Y2^xiii	73.437 (16)
O1ⁱ—Ca1—Y2ⁱⁱⁱ	39.84 (6)	Ca2^xii—Si2—Y2^xiii	122.32 (4)
O1ⁱⁱ—Ca1—Y2ⁱⁱⁱ	100.61 (6)	Y2^xii—Si2—Y2^xiii	122.32 (4)
O1ⁱⁱⁱ—Ca1—Y2ⁱⁱⁱ	79.39 (6)	O2^xi—Si2—Ca2^xiii	46.38 (9)
O1^iv—Ca1—Y2ⁱⁱⁱ	135.80 (6)	O2^vii—Si2—Ca2^xiii	145.99 (11)
O1^v—Ca1—Y2ⁱⁱⁱ	44.20 (6)	O3—Si2—Ca2^xiii	107.97 (6)
Ca2—Ca1—Y2ⁱⁱⁱ	119.2	N5^vii—Si2—Ca2^xiii	63.05 (3)
Ca2ⁱⁱⁱ—Ca1—Y2ⁱⁱⁱ	0.00 (2)	Ca2—Si2—Ca2^xiii	156.83 (4)
Ca2ⁱⁱ—Ca1—Y2ⁱⁱⁱ	180.000 (14)	Ca2^viii—Si2—Ca2^xiii	73.437 (16)
Y2ⁱⁱ—Ca1—Y2ⁱⁱⁱ	180.000 (14)	Y2^viii—Si2—Ca2^xiii	73.4
O2—Ca2—O3	96.63 (11)	Ca2^xii—Si2—Ca2^xiii	122.32 (4)
O2—Ca2—O2^iv	161.52 (8)	Y2^xii—Si2—Ca2^xiii	122.3
O3—Ca2—O2^iv	100.46 (10)	Y2^xiii—Si2—Ca2^xiii	0
O2—Ca2—O1^iv	81.73 (8)	Si3^viii—Si3—N5^xiv	80.57 (8)
O3—Ca2—O1^iv	132.32 (10)	Si3^viii—Si3—N5^xv	80.56 (9)
O2^iv—Ca2—O1^iv	81.59 (9)	N5^xiv—Si3—N5^xv	117.37 (5)
O2—Ca2—N4^vi	72.63 (11)	Si3^viii—Si3—N5	80.56 (8)
O3—Ca2—N4^vi	119.23 (18)	N5^xiv—Si3—N5	117.37 (5)
O2^iv—Ca2—N4^vi	104.53 (14)	N5^xv—Si3—N5	117.36 (5)
O1^iv—Ca2—N4^vi	105.78 (14)	Si3^viii—Si3—O4	180
O2—Ca2—O4^vi	72.63 (11)	N5^xiv—Si3—O4	99.44 (8)
O3—Ca2—O4^vi	119.23 (18)	N5^xv—Si3—O4	99.44 (8)
O2^iv—Ca2—O4^vi	104.53 (14)	N5—Si3—O4	99.44 (8)
O1^iv—Ca2—O4^vi	105.78 (14)	Si3^viii—Si3—N4^viii	0.0040 (10)
N4^vi—Ca2—O4^vi	0	N5^xiv—Si3—N4^viii	80.56 (8)
O2—Ca2—O1ⁱⁱⁱ	106.08 (9)	N5^xv—Si3—N4^viii	80.56 (8)
O3—Ca2—O1ⁱⁱⁱ	62.93 (10)	N5—Si3—N4^viii	80.56 (8)
O2^iv—Ca2—O1ⁱⁱⁱ	75.98 (8)	O4—Si3—N4^viii	180
O1^iv—Ca2—O1ⁱⁱⁱ	71.77 (10)	Si3^viii—Si3—Ca2^xvi	137.55 (3)
N4^vi—Ca2—O1ⁱⁱⁱ	177.46 (11)	N5^xiv—Si3—Ca2^xvi	56.98 (6)
O4^vi—Ca2—O1ⁱⁱⁱ	177.46 (11)	N5^xv—Si3—Ca2^xvi	117.04 (11)
O2—Ca2—O2^vii	112.13 (12)	N5—Si3—Ca2^xvi	116.96 (11)
O3—Ca2—O2^vii	62.75 (10)	O4—Si3—Ca2^xvi	42.46 (3)
O2^iv—Ca2—O2^vii	82.24 (9)	N4^viii—Si3—Ca2^xvi	137.54 (3)
O1^iv—Ca2—O2^vii	159.89 (8)	Si3^viii—Si3—Ca2ⁱⁱ	137.54 (3)
N4^vi—Ca2—O2^vii	67.05 (10)	N5^xiv—Si3—Ca2ⁱⁱ	117.04 (11)
O4^vi—Ca2—O2^vii	67.05 (10)	N5^xv—Si3—Ca2ⁱⁱ	116.96 (11)
O1ⁱⁱⁱ—Ca2—O2^vii	115.49 (8)	N5—Si3—Ca2ⁱⁱ	56.98 (6)
O2—Ca2—N5^iv	103.18 (11)	O4—Si3—Ca2ⁱⁱ	42.46 (3)
O3—Ca2—N5^iv	157.70 (11)	N4^viii—Si3—Ca2ⁱⁱ	137.54 (3)
O2^iv—Ca2—N5^iv	61.59 (11)	Ca2^xvi—Si3—Ca2ⁱⁱ	71.55 (5)
O1^iv—Ca2—N5^iv	61.83 (10)	Si3^viii—Si3—Ca2^vi	137.54 (3)
N4^vi—Ca2—N5^iv	59.0 (2)	N5^xiv—Si3—Ca2^vi	116.96 (11)
O4^vi—Ca2—N5^iv	59.0 (2)	N5^xv—Si3—Ca2^vi	56.98 (6)
O1ⁱⁱⁱ—Ca2—N5^iv	119.67 (11)	N5—Si3—Ca2^vi	117.04 (11)
O2^vii—Ca2—N5^iv	99.76 (10)	O4—Si3—Ca2^vi	42.46 (3)
O2—Ca2—Si1ⁱⁱⁱ	104.39 (7)	N4^viii—Si3—Ca2^vi	137.54 (3)
O3—Ca2—Si1ⁱⁱⁱ	31.79 (9)	Ca2^xvi—Si3—Ca2^vi	71.55 (5)
O2^iv—Ca2—Si1ⁱⁱⁱ	86.87 (6)	Ca2ⁱⁱ—Si3—Ca2^vi	71.55 (5)
O1^iv—Ca2—Si1ⁱⁱⁱ	102.18 (6)	Si1—O1—Ca1	150.45 (15)
N4^vi—Ca2—Si1ⁱⁱⁱ	151.01 (16)	Si1—O1—Y2ⁱⁱ	102.59 (12)
O4^vi—Ca2—Si1ⁱⁱⁱ	151.01 (16)	Ca1—O1—Y2ⁱⁱ	103.76 (9)
O1ⁱⁱⁱ—Ca2—Si1ⁱⁱⁱ	31.18 (5)	Si1—O1—Ca2ⁱⁱ	102.59 (12)
O2^vii—Ca2—Si1ⁱⁱⁱ	88.78 (6)	Ca1—O1—Ca2ⁱⁱ	103.76 (9)
N5^iv—Ca2—Si1ⁱⁱⁱ	145.42 (10)	Y2ⁱⁱ—O1—Ca2ⁱⁱ	0
O2—Ca2—Si2	107.34 (7)	Si1—O1—Ca2^v	91.80 (10)
O3—Ca2—Si2	31.69 (8)	Ca1—O1—Ca2^v	98.64 (9)
O2^iv—Ca2—Si2	90.97 (7)	Y2ⁱⁱ—O1—Ca2^v	95.7
O1^iv—Ca2—Si2	160.68 (6)	Ca2ⁱⁱ—O1—Ca2^v	95.69 (8)
N4^vi—Ca2—Si2	93.31 (13)	Si1—O1—Y2^v	91.80 (10)
O4^vi—Ca2—Si2	93.31 (13)	Ca1—O1—Y2^v	98.64 (9)
O1ⁱⁱⁱ—Ca2—Si2	89.16 (6)	Y2ⁱⁱ—O1—Y2^v	95.69 (8)
O2^vii—Ca2—Si2	31.07 (6)	Ca2ⁱⁱ—O1—Y2^v	95.69 (8)
N5^iv—Ca2—Si2	129.41 (8)	Ca2^v—O1—Y2^v	0.00 (4)
Si1ⁱⁱⁱ—Ca2—Si2	59.41 (3)	Si2^xvii—O2—Ca2	139.04 (15)
O2—Ca2—Si1^iv	86.75 (7)	Si2^xvii—O2—Y2ⁱⁱ	104.62 (12)
O3—Ca2—Si1^iv	160.80 (9)	Ca2—O2—Y2ⁱⁱ	106.1
O2^iv—Ca2—Si1^iv	74.80 (7)	Si2^xvii—O2—Ca2ⁱⁱ	104.62 (12)
O1^iv—Ca2—Si1^iv	29.38 (6)	Ca2—O2—Ca2ⁱⁱ	106.14 (10)
N4^vi—Ca2—Si1^iv	79.85 (16)	Y2ⁱⁱ—O2—Ca2ⁱⁱ	0
O4^vi—Ca2—Si1^iv	79.85 (16)	Si2^xvii—O2—Ca2^xvii	91.86 (11)
O1ⁱⁱⁱ—Ca2—Si1^iv	97.94 (6)	Ca2—O2—Ca2^xvii	109.92 (11)
O2^vii—Ca2—Si1^iv	133.13 (6)	Y2ⁱⁱ—O2—Ca2^xvii	97.8
N5^iv—Ca2—Si1^iv	33.39 (8)	Ca2ⁱⁱ—O2—Ca2^xvii	97.76 (9)
Si1ⁱⁱⁱ—Ca2—Si1^iv	129.12 (4)	Si2^xvii—O2—Y2^xvii	91.86 (11)
Si2—Ca2—Si1^iv	161.90 (3)	Ca2—O2—Y2^xvii	109.9
O1^viii—Si1—O1	117.18 (18)	Y2ⁱⁱ—O2—Y2^xvii	97.76 (9)
O1^viii—Si1—O3^v	106.15 (11)	Ca2ⁱⁱ—O2—Y2^xvii	97.76 (9)
O1—Si1—O3^v	106.15 (11)	Ca2^xvii—O2—Y2^xvii	0.00 (2)
O1^viii—Si1—N5	109.23 (11)	Si1ⁱⁱⁱ—O3—Si2	136.8 (2)
O1—Si1—N5	109.23 (11)	Si1ⁱⁱⁱ—O3—Ca2	99.02 (10)
O3^v—Si1—N5	108.6 (2)	Si2—O3—Ca2	99.42 (10)
O1^viii—Si1—Ca2^v	129.30 (10)	Si1ⁱⁱⁱ—O3—Ca2^viii	99.02 (10)
O1—Si1—Ca2^v	57.02 (9)	Si2—O3—Ca2^viii	99.42 (10)
O3^v—Si1—Ca2^v	49.19 (6)	Ca2—O3—Ca2^viii	128.37 (16)
N5—Si1—Ca2^v	120.21 (10)	Si1ⁱⁱⁱ—O3—Y2^viii	99.02 (10)
O1^viii—Si1—Y2^v	129.30 (10)	Si2—O3—Y2^viii	99.42 (10)
O1—Si1—Y2^v	57.02 (9)	Ca2—O3—Y2^viii	128.4
O3^v—Si1—Y2^v	49.19 (6)	Ca2^viii—O3—Y2^viii	0.00 (3)
N5—Si1—Y2^v	120.21 (10)	Si3—O4—Y2^xvi	108.54 (18)
Ca2^v—Si1—Y2^v	0.00 (3)	Si3—O4—Ca2^xvi	108.54 (18)
O1^viii—Si1—Ca2^ix	57.02 (9)	Y2^xvi—O4—Ca2^xvi	0
O1—Si1—Ca2^ix	129.30 (10)	Si3—O4—Ca2^vi	108.54 (18)
O3^v—Si1—Ca2^ix	49.19 (6)	Y2^xvi—O4—Ca2^vi	110.4
N5—Si1—Ca2^ix	120.21 (10)	Ca2^xvi—O4—Ca2^vi	110.39 (17)
Ca2^v—Si1—Ca2^ix	87.25 (3)	Si3—O4—Y2^vi	108.54 (18)
Y2^v—Si1—Ca2^ix	87.2	Y2^xvi—O4—Y2^vi	110.39 (17)
O1^viii—Si1—Y2^ix	57.02 (9)	Ca2^xvi—O4—Y2^vi	110.39 (17)
O1—Si1—Y2^ix	129.30 (10)	Ca2^vi—O4—Y2^vi	0.00 (3)
O3^v—Si1—Y2^ix	49.19 (6)	Si3—O4—Y2ⁱⁱ	108.54 (18)
N5—Si1—Y2^ix	120.21 (10)	Y2^xvi—O4—Y2ⁱⁱ	110.39 (17)
Ca2^v—Si1—Y2^ix	87.25 (3)	Ca2^xvi—O4—Y2ⁱⁱ	110.39 (17)
Y2^v—Si1—Y2^ix	87.25 (3)	Ca2^vi—O4—Y2ⁱⁱ	110.39 (17)
Ca2^ix—Si1—Y2^ix	0.00 (3)	Y2^vi—O4—Y2ⁱⁱ	110.39 (17)
O1^viii—Si1—Ca2^x	48.03 (9)	Si3—O4—Ca2ⁱⁱ	108.54 (18)
O1—Si1—Ca2^x	146.28 (10)	Y2^xvi—O4—Ca2ⁱⁱ	110.4
O3^v—Si1—Ca2^x	107.30 (6)	Ca2^xvi—O4—Ca2ⁱⁱ	110.39 (17)
N5—Si1—Ca2^x	63.39 (3)	Ca2^vi—O4—Ca2ⁱⁱ	110.39 (17)
Ca2^v—Si1—Ca2^x	156.46 (4)	Y2^vi—O4—Ca2ⁱⁱ	110.4
Y2^v—Si1—Ca2^x	156.5	Y2ⁱⁱ—O4—Ca2ⁱⁱ	0
Ca2^ix—Si1—Ca2^x	72.773 (9)	Si3^viii—N5—Si3	18.88 (17)
Y2^ix—Si1—Ca2^x	72.8	Si3^viii—N5—Si1	122.8 (2)
O1^viii—Si1—Y2^x	48.03 (9)	Si3—N5—Si1	122.8 (2)
O1—Si1—Y2^x	146.28 (10)	Si3^viii—N5—Si2^xvii	121.1 (2)
O3^v—Si1—Y2^x	107.30 (6)	Si3—N5—Si2^xvii	121.1 (2)
N5—Si1—Y2^x	63.39 (3)	Si1—N5—Si2^xvii	115.1 (3)
Ca2^v—Si1—Y2^x	156.46 (4)	Si3^viii—N5—Ca2ⁱⁱ	111.94 (15)
Y2^v—Si1—Y2^x	156.46 (4)	Si3—N5—Ca2ⁱⁱ	93.06 (10)
Ca2^ix—Si1—Y2^x	72.773 (9)	Si1—N5—Ca2ⁱⁱ	83.21 (9)
Y2^ix—Si1—Y2^x	72.773 (9)	Si2^xvii—N5—Ca2ⁱⁱ	83.45 (9)
Ca2^x—Si1—Y2^x	0.00 (3)	Si3^viii—N5—Y2ⁱⁱ	111.94 (15)
O1^viii—Si1—Y2ⁱⁱ	146.28 (10)	Si3—N5—Y2ⁱⁱ	93.06 (10)
O1—Si1—Y2ⁱⁱ	48.03 (9)	Si1—N5—Y2ⁱⁱ	83.21 (9)
O3^v—Si1—Y2ⁱⁱ	107.30 (6)	Si2^xvii—N5—Y2ⁱⁱ	83.45 (9)
N5—Si1—Y2ⁱⁱ	63.39 (3)	Ca2ⁱⁱ—N5—Y2ⁱⁱ	0.00 (4)
Ca2^v—Si1—Y2ⁱⁱ	72.773 (9)	Si3^viii—N5—Y2^x	93.06 (10)
Y2^v—Si1—Y2ⁱⁱ	72.773 (9)	Si3—N5—Y2^x	111.94 (15)
Ca2^ix—Si1—Y2ⁱⁱ	156.46 (4)	Si1—N5—Y2^x	83.21 (9)
Y2^ix—Si1—Y2ⁱⁱ	156.46 (4)	Si2^xvii—N5—Y2^x	83.45 (9)
Ca2^x—Si1—Y2ⁱⁱ	123.06 (4)	Ca2ⁱⁱ—N5—Y2^x	155.00 (19)
Y2^x—Si1—Y2ⁱⁱ	123.06 (4)	Y2ⁱⁱ—N5—Y2^x	155.00 (19)
O1^viii—Si1—Ca2ⁱⁱ	146.28 (10)	Si3^viii—N5—Ca2^x	93.06 (10)
O1—Si1—Ca2ⁱⁱ	48.03 (9)	Si3—N5—Ca2^x	111.94 (15)
O3^v—Si1—Ca2ⁱⁱ	107.30 (6)	Si1—N5—Ca2^x	83.21 (9)
N5—Si1—Ca2ⁱⁱ	63.39 (3)	Si2^xvii—N5—Ca2^x	83.45 (9)
Ca2^v—Si1—Ca2ⁱⁱ	72.773 (9)	Ca2ⁱⁱ—N5—Ca2^x	155.00 (19)
Y2^v—Si1—Ca2ⁱⁱ	72.8	Y2ⁱⁱ—N5—Ca2^x	155
Ca2^ix—Si1—Ca2ⁱⁱ	156.46 (4)	Y2^x—N5—Ca2^x	0
Y2^ix—Si1—Ca2ⁱⁱ	156.5

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

Pentacalcium diyttrium heptasilicon oxynitride (3) top

Crystal data top

Ca₅Y₂Si₇O₁₆N₄	D_x = 3.359 Mg m⁻³
M_r = 886.89	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₃/m	Cell parameters from 7553 reflections
Hall symbol: -P 6c	θ = 3.1–27.4°
a = 10.0541 (2) Å	µ = 8.63 mm⁻¹
c = 10.0168 (2) Å	T = 293 K
V = 876.89 (4) Å³	Platelet, colorless
Z = 2	0.05 × 0.03 × 0.02 mm
F(000) = 864

Data collection top

Rigaku R-Axis RAPID II diffractometer	702 independent reflections
Radiation source: sealed x-ray tube	681 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.027
Detector resolution: 10 pixels mm^-1	θ_max = 27.4°, θ_min = 3.1°
phi or ω oscillation scans	h = −13→13
Absorption correction: multi-scan (ABSCOR; Higashi, 2001)	k = −13→13
T_min = 0.820, T_max = 1.000	l = −12→12
8532 measured reflections

Refinement top

Refinement on F²	0 constraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F² > 2σ(F²)] = 0.024	w = 1/[σ²(F_o²) + (0.0366P)² + 1.4061P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.062	(Δ/σ)_max < 0.001
S = 1.09	Δρ_max = 0.50 e Å⁻³
702 reflections	Δρ_min = −0.86 e Å⁻³
63 parameters	Extinction correction: SHELXL-2014/7 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
1 restraint	Extinction coefficient: 0.0135 (11)

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ca1	0	0	0	0.00811 (18)	0.2572 (14)
Y1	0	0	0	0.00811 (18)	0.7428 (14)
Ca2	0.41677 (5)	0.13055 (4)	0.03368 (4)	0.01268 (17)	0.7905 (2)
Y2	0.41677 (5)	0.13055 (4)	0.03368 (4)	0.01268 (17)	0.2095 (2)
Si1	0.11074 (9)	0.31954 (9)	0.25	0.0073 (2)
Si2	0.55788 (9)	0.00978 (9)	0.25	0.0087 (2)
Si3	0.3333	0.6667	0.21626 (19)	0.0077 (5)	0.5
O1	0.08563 (19)	0.22613 (19)	0.11149 (17)	0.0150 (4)
O2	0.4430 (2)	0.35772 (19)	0.10933 (18)	0.0187 (4)
O3	0.3963 (3)	0.0190 (3)	0.25	0.0197 (5)
O4	0.3333	0.6667	0.0400 (6)	0.0452 (13)	0.5
N4	0.3333	0.6667	0.0400 (6)	0.0452 (13)	0.5
N5	0.2988 (3)	0.4832 (3)	0.25	0.0208 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ca1	0.0084 (2)	0.0084 (2)	0.0076 (3)	0.00418 (10)	0	0
Y1	0.0084 (2)	0.0084 (2)	0.0076 (3)	0.00418 (10)	0	0
Ca2	0.0191 (2)	0.0123 (2)	0.0098 (2)	0.01028 (16)	−0.00029 (14)	−0.00046 (13)
Y2	0.0191 (2)	0.0123 (2)	0.0098 (2)	0.01028 (16)	−0.00029 (14)	−0.00046 (13)
Si1	0.0074 (4)	0.0071 (4)	0.0064 (4)	0.0029 (3)	0	0
Si2	0.0070 (4)	0.0089 (4)	0.0097 (4)	0.0035 (3)	0	0
Si3	0.0054 (5)	0.0054 (5)	0.0123 (14)	0.0027 (2)	0	0
O1	0.0173 (8)	0.0165 (8)	0.0097 (8)	0.0073 (7)	−0.0001 (6)	−0.0043 (7)
O2	0.0257 (9)	0.0186 (8)	0.0143 (8)	0.0130 (7)	−0.0049 (7)	−0.0055 (7)
O3	0.0185 (12)	0.0207 (12)	0.0206 (13)	0.0103 (10)	0	0
O4	0.0318 (14)	0.0318 (14)	0.072 (4)	0.0159 (7)	0	0
N4	0.0318 (14)	0.0318 (14)	0.072 (4)	0.0159 (7)	0	0
N5	0.0077 (12)	0.0102 (13)	0.043 (2)	0.0033 (10)	0	0

Geometric parameters (Å, º) top

Ca1—O1ⁱ	2.2804 (16)	Si2—Ca2^viii	3.1472 (7)
Ca1—O1ⁱⁱ	2.2804 (16)	Si2—Ca2^xii	3.2387 (5)
Ca1—O1	2.2804 (16)	Si2—Y2^xii	3.2387 (5)
Ca1—O1ⁱⁱⁱ	2.2804 (16)	Si2—Ca2^xiii	3.2387 (5)
Ca1—O1^iv	2.2804 (16)	Si2—Y2^xiii	3.2387 (5)
Ca1—O1^v	2.2804 (16)	Si3—Si3^viii	0.676 (4)
Ca1—Ca2	3.7276 (4)	Si3—N5^xiv	1.732 (3)
Ca1—Ca2ⁱⁱ	3.7276 (4)	Si3—N5^xv	1.732 (3)
Ca1—Ca2ⁱ	3.7276 (4)	Si3—N5	1.732 (3)
Ca1—Y2ⁱ	3.7276 (4)	Si3—O4	1.765 (7)
Ca1—Y2ⁱⁱ	3.7276 (4)	Si3—Ca2^xvi	3.4080 (15)
Ca2—O2	2.2930 (17)	Si3—Y2^xvi	3.4080 (15)
Ca2—O3	2.4010 (12)	Si3—Ca2ⁱ	3.4080 (15)
Ca2—O2ⁱⁱⁱ	2.4136 (18)	Si3—Y2ⁱ	3.4080 (15)
Ca2—N4^vi	2.4274 (19)	Si3—Y2^vi	3.4080 (15)
Ca2—O4^vi	2.4274 (19)	Si3—Ca2^vi	3.4080 (15)
Ca2—O1ⁱⁱⁱ	2.4475 (17)	O1—Y2ⁱ	2.4475 (17)
Ca2—O2^vii	2.6369 (18)	O1—Ca2ⁱ	2.4475 (17)
Ca2—O1ⁱⁱ	2.6475 (17)	O1—Ca2^iv	2.6475 (17)
Ca2—N5ⁱⁱⁱ	2.9071 (7)	O1—Y2^iv	2.6475 (17)
Ca2—Si1ⁱⁱ	3.1432 (7)	O2—Si2^xvii	1.6241 (18)
Ca2—Si2	3.1472 (7)	O2—Y2ⁱ	2.4136 (18)
Ca2—Si1ⁱⁱⁱ	3.2277 (5)	O2—Ca2ⁱ	2.4136 (18)
Si1—O1^viii	1.6227 (17)	O2—Ca2^xvii	2.6370 (18)
Si1—O1	1.6228 (17)	O2—Y2^xvii	2.6370 (18)
Si1—O3^iv	1.673 (3)	O3—Si1ⁱⁱ	1.673 (3)
Si1—N5	1.781 (3)	O3—Ca2^viii	2.4011 (12)
Si1—Ca2^iv	3.1433 (7)	O3—Y2^viii	2.4011 (12)
Si1—Y2^iv	3.1433 (7)	O4—Y2^xvi	2.4273 (19)
Si1—Ca2^ix	3.1433 (7)	O4—Ca2^xvi	2.4273 (19)
Si1—Y2^ix	3.1433 (7)	O4—Ca2^vi	2.4273 (19)
Si1—Ca2^x	3.2277 (5)	O4—Y2^vi	2.4273 (19)
Si1—Y2^x	3.2277 (5)	O4—Y2ⁱ	2.4273 (19)
Si1—Y2ⁱ	3.2277 (5)	O4—Ca2ⁱ	2.4273 (19)
Si1—Ca2ⁱ	3.2277 (5)	N5—Si3^viii	1.732 (3)
Si2—O2^xi	1.6241 (18)	N5—Si2^xvii	1.782 (3)
Si2—O2^vii	1.6241 (18)	N5—Ca2ⁱ	2.9071 (7)
Si2—O3	1.672 (3)	N5—Y2ⁱ	2.9071 (7)
Si2—N5^vii	1.782 (3)	N5—Y2^x	2.9071 (7)
Si2—Y2^viii	3.1472 (7)	N5—Ca2^x	2.9071 (7)

O1ⁱ—Ca1—O1ⁱⁱ	180.00 (9)	O2^xi—Si2—Y2^viii	56.86 (7)
O1ⁱ—Ca1—O1	81.94 (6)	O2^vii—Si2—Y2^viii	130.39 (7)
O1ⁱⁱ—Ca1—O1	98.06 (6)	O3—Si2—Y2^viii	48.78 (4)
O1ⁱ—Ca1—O1ⁱⁱⁱ	98.06 (6)	N5^vii—Si2—Y2^viii	121.36 (6)
O1ⁱⁱ—Ca1—O1ⁱⁱⁱ	81.94 (6)	O2^xi—Si2—Ca2^viii	56.86 (7)
O1—Ca1—O1ⁱⁱⁱ	81.94 (6)	O2^vii—Si2—Ca2^viii	130.39 (7)
O1ⁱ—Ca1—O1^iv	81.94 (6)	O3—Si2—Ca2^viii	48.78 (4)
O1ⁱⁱ—Ca1—O1^iv	98.06 (6)	N5^vii—Si2—Ca2^viii	121.36 (6)
O1—Ca1—O1^iv	98.06 (6)	Y2^viii—Si2—Ca2^viii	0
O1ⁱⁱⁱ—Ca1—O1^iv	180.00 (12)	O2^xi—Si2—Ca2	130.39 (7)
O1ⁱ—Ca1—O1^v	98.06 (6)	O2^vii—Si2—Ca2	56.86 (7)
O1ⁱⁱ—Ca1—O1^v	81.94 (6)	O3—Si2—Ca2	48.78 (4)
O1—Ca1—O1^v	180	N5^vii—Si2—Ca2	121.36 (6)
O1ⁱⁱⁱ—Ca1—O1^v	98.06 (6)	Y2^viii—Si2—Ca2	87
O1^iv—Ca1—O1^v	81.94 (6)	Ca2^viii—Si2—Ca2	87.02 (2)
O1ⁱ—Ca1—Ca2	135.31 (4)	O2^xi—Si2—Ca2^xii	145.93 (8)
O1ⁱⁱ—Ca1—Ca2	44.69 (4)	O2^vii—Si2—Ca2^xii	46.05 (6)
O1—Ca1—Ca2	78.88 (4)	O3—Si2—Ca2^xii	108.32 (4)
O1ⁱⁱⁱ—Ca1—Ca2	39.57 (4)	N5^vii—Si2—Ca2^xii	63.15 (2)
O1^iv—Ca1—Ca2	140.43 (4)	Y2^viii—Si2—Ca2^xii	157.1
O1^v—Ca1—Ca2	101.12 (4)	Ca2^viii—Si2—Ca2^xii	157.07 (3)
O1ⁱ—Ca1—Ca2ⁱⁱ	101.12 (4)	Ca2—Si2—Ca2^xii	73.312 (11)
O1ⁱⁱ—Ca1—Ca2ⁱⁱ	78.88 (4)	O2^xi—Si2—Y2^xii	145.93 (8)
O1—Ca1—Ca2ⁱⁱ	140.43 (4)	O2^vii—Si2—Y2^xii	46.05 (6)
O1ⁱⁱⁱ—Ca1—Ca2ⁱⁱ	135.31 (4)	O3—Si2—Y2^xii	108.32 (4)
O1^iv—Ca1—Ca2ⁱⁱ	44.69 (4)	N5^vii—Si2—Y2^xii	63.15 (2)
O1^v—Ca1—Ca2ⁱⁱ	39.57 (4)	Y2^viii—Si2—Y2^xii	157.07 (3)
Ca2—Ca1—Ca2ⁱⁱ	119.190 (2)	Ca2^viii—Si2—Y2^xii	157.07 (3)
O1ⁱ—Ca1—Ca2ⁱ	78.88 (4)	Ca2—Si2—Y2^xii	73.3
O1ⁱⁱ—Ca1—Ca2ⁱ	101.12 (4)	Ca2^xii—Si2—Y2^xii	0.000 (15)
O1—Ca1—Ca2ⁱ	39.57 (4)	O2^xi—Si2—Ca2^xiii	46.05 (6)
O1ⁱⁱⁱ—Ca1—Ca2ⁱ	44.69 (4)	O2^vii—Si2—Ca2^xiii	145.93 (8)
O1^iv—Ca1—Ca2ⁱ	135.31 (4)	O3—Si2—Ca2^xiii	108.32 (4)
O1^v—Ca1—Ca2ⁱ	140.43 (4)	N5^vii—Si2—Ca2^xiii	63.15 (2)
Ca2—Ca1—Ca2ⁱ	60.810 (2)	Y2^viii—Si2—Ca2^xiii	73.3
Ca2ⁱⁱ—Ca1—Ca2ⁱ	180.000 (12)	Ca2^viii—Si2—Ca2^xiii	73.312 (11)
O1ⁱ—Ca1—Y2ⁱ	78.88 (4)	Ca2—Si2—Ca2^xiii	157.07 (3)
O1ⁱⁱ—Ca1—Y2ⁱ	101.12 (4)	Ca2^xii—Si2—Ca2^xiii	122.65 (3)
O1—Ca1—Y2ⁱ	39.57 (4)	Y2^xii—Si2—Ca2^xiii	122.7
O1ⁱⁱⁱ—Ca1—Y2ⁱ	44.69 (4)	O2^xi—Si2—Y2^xiii	46.05 (6)
O1^iv—Ca1—Y2ⁱ	135.31 (4)	O2^vii—Si2—Y2^xiii	145.93 (8)
O1^v—Ca1—Y2ⁱ	140.43 (4)	O3—Si2—Y2^xiii	108.32 (4)
Ca2—Ca1—Y2ⁱ	60.8	N5^vii—Si2—Y2^xiii	63.15 (2)
Ca2ⁱⁱ—Ca1—Y2ⁱ	180.000 (12)	Y2^viii—Si2—Y2^xiii	73.312 (11)
Ca2ⁱ—Ca1—Y2ⁱ	0.000 (12)	Ca2^viii—Si2—Y2^xiii	73.312 (11)
O1ⁱ—Ca1—Y2ⁱⁱ	101.12 (4)	Ca2—Si2—Y2^xiii	157.1
O1ⁱⁱ—Ca1—Y2ⁱⁱ	78.88 (4)	Ca2^xii—Si2—Y2^xiii	122.65 (3)
O1—Ca1—Y2ⁱⁱ	140.43 (4)	Y2^xii—Si2—Y2^xiii	122.65 (3)
O1ⁱⁱⁱ—Ca1—Y2ⁱⁱ	135.31 (4)	Ca2^xiii—Si2—Y2^xiii	0.000 (16)
O1^iv—Ca1—Y2ⁱⁱ	44.69 (4)	Si3^viii—Si3—N5^xiv	78.75 (7)
O1^v—Ca1—Y2ⁱⁱ	39.57 (4)	Si3^viii—Si3—N5^xv	78.74 (7)
Ca2—Ca1—Y2ⁱⁱ	119.2	N5^xiv—Si3—N5^xv	116.29 (4)
Ca2ⁱⁱ—Ca1—Y2ⁱⁱ	0.000 (16)	Si3^viii—Si3—N5	78.74 (6)
Ca2ⁱ—Ca1—Y2ⁱⁱ	180	N5^xiv—Si3—N5	116.29 (4)
Y2ⁱ—Ca1—Y2ⁱⁱ	180	N5^xv—Si3—N5	116.29 (4)
O2—Ca2—O3	96.16 (7)	Si3^viii—Si3—O4	180
O2—Ca2—O2ⁱⁱⁱ	161.05 (5)	N5^xiv—Si3—O4	101.25 (6)
O3—Ca2—O2ⁱⁱⁱ	100.98 (7)	N5^xv—Si3—O4	101.25 (6)
O2—Ca2—N4^vi	73.06 (8)	N5—Si3—O4	101.25 (6)
O3—Ca2—N4^vi	118.54 (14)	Si3^viii—Si3—Ca2^xvi	137.28 (2)
O2ⁱⁱⁱ—Ca2—N4^vi	105.11 (11)	N5^xiv—Si3—Ca2^xvi	58.53 (4)
O2—Ca2—O4^vi	73.06 (8)	N5^xv—Si3—Ca2^xvi	118.42 (8)
O3—Ca2—O4^vi	118.54 (14)	N5—Si3—Ca2^xvi	118.45 (8)
O2ⁱⁱⁱ—Ca2—O4^vi	105.11 (11)	O4—Si3—Ca2^xvi	42.73 (2)
N4^vi—Ca2—O4^vi	0	Si3^viii—Si3—Y2^xvi	137.28 (2)
O2—Ca2—O1ⁱⁱⁱ	81.84 (6)	N5^xiv—Si3—Y2^xvi	58.53 (4)
O3—Ca2—O1ⁱⁱⁱ	132.03 (7)	N5^xv—Si3—Y2^xvi	118.42 (8)
O2ⁱⁱⁱ—Ca2—O1ⁱⁱⁱ	80.71 (6)	N5—Si3—Y2^xvi	118.45 (8)
N4^vi—Ca2—O1ⁱⁱⁱ	106.72 (11)	O4—Si3—Y2^xvi	42.73 (2)
O4^vi—Ca2—O1ⁱⁱⁱ	106.72 (11)	Ca2^xvi—Si3—Y2^xvi	0.00 (2)
O2—Ca2—O2^vii	113.34 (8)	Si3^viii—Si3—Ca2ⁱ	137.27 (2)
O3—Ca2—O2^vii	62.62 (7)	N5^xiv—Si3—Ca2ⁱ	118.42 (8)
O2ⁱⁱⁱ—Ca2—O2^vii	82.05 (6)	N5^xv—Si3—Ca2ⁱ	118.45 (8)
N4^vi—Ca2—O2^vii	67.30 (8)	N5—Si3—Ca2ⁱ	58.53 (4)
O4^vi—Ca2—O2^vii	67.30 (8)	O4—Si3—Ca2ⁱ	42.73 (2)
O1ⁱⁱⁱ—Ca2—O2^vii	159.44 (6)	Ca2^xvi—Si3—Ca2ⁱ	71.97 (4)
O2—Ca2—O1ⁱⁱ	105.75 (6)	Y2^xvi—Si3—Ca2ⁱ	72
O3—Ca2—O1ⁱⁱ	62.69 (7)	Si3^viii—Si3—Y2ⁱ	137.27 (2)
O2ⁱⁱⁱ—Ca2—O1ⁱⁱ	75.59 (5)	N5^xiv—Si3—Y2ⁱ	118.42 (8)
N4^vi—Ca2—O1ⁱⁱ	178.26 (6)	N5^xv—Si3—Y2ⁱ	118.45 (8)
O4^vi—Ca2—O1ⁱⁱ	178.26 (6)	N5—Si3—Y2ⁱ	58.53 (4)
O1ⁱⁱⁱ—Ca2—O1ⁱⁱ	71.75 (7)	O4—Si3—Y2ⁱ	42.73 (2)
O2^vii—Ca2—O1ⁱⁱ	114.42 (5)	Ca2^xvi—Si3—Y2ⁱ	71.97 (4)
O2—Ca2—N5ⁱⁱⁱ	103.67 (7)	Y2^xvi—Si3—Y2ⁱ	71.97 (4)
O3—Ca2—N5ⁱⁱⁱ	157.98 (8)	Ca2ⁱ—Si3—Y2ⁱ	0.00 (2)
O2ⁱⁱⁱ—Ca2—N5ⁱⁱⁱ	61.16 (7)	Si3^viii—Si3—Y2^vi	137.27 (2)
N4^vi—Ca2—N5ⁱⁱⁱ	60.10 (15)	N5^xiv—Si3—Y2^vi	118.45 (8)
O4^vi—Ca2—N5ⁱⁱⁱ	60.10 (15)	N5^xv—Si3—Y2^vi	58.53 (4)
O1ⁱⁱⁱ—Ca2—N5ⁱⁱⁱ	61.53 (7)	N5—Si3—Y2^vi	118.42 (8)
O2^vii—Ca2—N5ⁱⁱⁱ	100.12 (7)	O4—Si3—Y2^vi	42.73 (2)
O1ⁱⁱ—Ca2—N5ⁱⁱⁱ	119.31 (7)	Ca2^xvi—Si3—Y2^vi	71.97 (4)
O2—Ca2—Si1ⁱⁱ	103.99 (5)	Y2^xvi—Si3—Y2^vi	71.97 (4)
O3—Ca2—Si1ⁱⁱ	31.66 (6)	Ca2ⁱ—Si3—Y2^vi	71.97 (4)
O2ⁱⁱⁱ—Ca2—Si1ⁱⁱ	86.88 (4)	Y2ⁱ—Si3—Y2^vi	71.97 (4)
N4^vi—Ca2—Si1ⁱⁱ	150.19 (13)	Si3^viii—Si3—Ca2^vi	137.27 (2)
O4^vi—Ca2—Si1ⁱⁱ	150.19 (13)	N5^xiv—Si3—Ca2^vi	118.45 (8)
O1ⁱⁱⁱ—Ca2—Si1ⁱⁱ	102.05 (4)	N5^xv—Si3—Ca2^vi	58.53 (4)
O2^vii—Ca2—Si1ⁱⁱ	88.07 (4)	N5—Si3—Ca2^vi	118.42 (8)
O1ⁱⁱ—Ca2—Si1ⁱⁱ	31.07 (4)	O4—Si3—Ca2^vi	42.73 (2)
N5ⁱⁱⁱ—Ca2—Si1ⁱⁱ	145.05 (6)	Ca2^xvi—Si3—Ca2^vi	71.97 (4)
O2—Ca2—Si2	107.89 (5)	Y2^xvi—Si3—Ca2^vi	72
O3—Ca2—Si2	31.59 (6)	Ca2ⁱ—Si3—Ca2^vi	71.97 (4)
O2ⁱⁱⁱ—Ca2—Si2	91.00 (5)	Y2ⁱ—Si3—Ca2^vi	72
N4^vi—Ca2—Si2	93.24 (10)	Y2^vi—Si3—Ca2^vi	0
O4^vi—Ca2—Si2	93.24 (10)	Si1—O1—Ca1	150.18 (10)
O1ⁱⁱⁱ—Ca2—Si2	159.75 (4)	Si1—O1—Y2ⁱ	103.06 (8)
O2^vii—Ca2—Si2	31.04 (4)	Ca1—O1—Y2ⁱ	104.02 (6)
O1ⁱⁱ—Ca2—Si2	88.33 (4)	Si1—O1—Ca2ⁱ	103.06 (8)
N5ⁱⁱⁱ—Ca2—Si2	129.71 (5)	Ca1—O1—Ca2ⁱ	104.02 (6)
Si1ⁱⁱ—Ca2—Si2	58.79 (2)	Y2ⁱ—O1—Ca2ⁱ	0
O2—Ca2—Si1ⁱⁱⁱ	86.92 (5)	Si1—O1—Ca2^iv	91.58 (7)
O3—Ca2—Si1ⁱⁱⁱ	160.52 (6)	Ca1—O1—Ca2^iv	98.02 (6)
O2ⁱⁱⁱ—Ca2—Si1ⁱⁱⁱ	74.24 (5)	Y2ⁱ—O1—Ca2^iv	95.5
N4^vi—Ca2—Si1ⁱⁱⁱ	80.79 (13)	Ca2ⁱ—O1—Ca2^iv	95.48 (6)
O4^vi—Ca2—Si1ⁱⁱⁱ	80.79 (13)	Si1—O1—Y2^iv	91.58 (7)
O1ⁱⁱⁱ—Ca2—Si1ⁱⁱⁱ	29.32 (4)	Ca1—O1—Y2^iv	98.02 (6)
O2^vii—Ca2—Si1ⁱⁱⁱ	133.34 (4)	Y2ⁱ—O1—Y2^iv	95.48 (6)
O1ⁱⁱ—Ca2—Si1ⁱⁱⁱ	97.93 (4)	Ca2ⁱ—O1—Y2^iv	95.48 (6)
N5ⁱⁱⁱ—Ca2—Si1ⁱⁱⁱ	33.23 (5)	Ca2^iv—O1—Y2^iv	0.000 (18)
Si1ⁱⁱ—Ca2—Si1ⁱⁱⁱ	129.00 (3)	Si2^xvii—O2—Ca2	139.12 (11)
Si2—Ca2—Si1ⁱⁱⁱ	161.82 (2)	Si2^xvii—O2—Y2ⁱ	104.98 (8)
O1^viii—Si1—O1	117.51 (13)	Ca2—O2—Y2ⁱ	106.5
O1^viii—Si1—O3^iv	106.16 (8)	Si2^xvii—O2—Ca2ⁱ	104.98 (8)
O1—Si1—O3^iv	106.16 (8)	Ca2—O2—Ca2ⁱ	106.55 (7)
O1^viii—Si1—N5	108.71 (8)	Y2ⁱ—O2—Ca2ⁱ	0
O1—Si1—N5	108.71 (8)	Si2^xvii—O2—Ca2^xvii	92.10 (8)
O3^iv—Si1—N5	109.35 (13)	Ca2—O2—Ca2^xvii	108.46 (7)
O1^viii—Si1—Ca2^iv	129.73 (7)	Y2ⁱ—O2—Ca2^xvii	98
O1—Si1—Ca2^iv	57.35 (6)	Ca2ⁱ—O2—Ca2^xvii	97.95 (6)
O3^iv—Si1—Ca2^iv	48.90 (4)	Si2^xvii—O2—Y2^xvii	92.10 (8)
N5—Si1—Ca2^iv	120.32 (6)	Ca2—O2—Y2^xvii	108.5
O1^viii—Si1—Y2^iv	129.73 (7)	Y2ⁱ—O2—Y2^xvii	97.95 (6)
O1—Si1—Y2^iv	57.35 (6)	Ca2ⁱ—O2—Y2^xvii	97.95 (6)
O3^iv—Si1—Y2^iv	48.90 (4)	Ca2^xvii—O2—Y2^xvii	0.00 (2)
N5—Si1—Y2^iv	120.32 (6)	Si2—O3—Si1ⁱⁱ	134.77 (16)
Ca2^iv—Si1—Y2^iv	0.00 (2)	Si2—O3—Ca2	99.63 (7)
O1^viii—Si1—Ca2^ix	57.35 (6)	Si1ⁱⁱ—O3—Ca2	99.44 (7)
O1—Si1—Ca2^ix	129.73 (7)	Si2—O3—Ca2^viii	99.63 (7)
O3^iv—Si1—Ca2^ix	48.90 (4)	Si1ⁱⁱ—O3—Ca2^viii	99.44 (7)
N5—Si1—Ca2^ix	120.32 (6)	Ca2—O3—Ca2^viii	128.97 (11)
Ca2^iv—Si1—Ca2^ix	87.16 (2)	Si2—O3—Y2^viii	99.63 (7)
Y2^iv—Si1—Ca2^ix	87.2	Si1ⁱⁱ—O3—Y2^viii	99.44 (7)
O1^viii—Si1—Y2^ix	57.35 (6)	Ca2—O3—Y2^viii	129
O1—Si1—Y2^ix	129.73 (7)	Ca2^viii—O3—Y2^viii	0.00 (4)
O3^iv—Si1—Y2^ix	48.90 (4)	Si3—O4—Y2^xvi	107.71 (14)
N5—Si1—Y2^ix	120.32 (6)	Si3—O4—Ca2^xvi	107.71 (14)
Ca2^iv—Si1—Y2^ix	87.16 (2)	Y2^xvi—O4—Ca2^xvi	0
Y2^iv—Si1—Y2^ix	87.16 (2)	Si3—O4—Ca2^vi	107.71 (14)
Ca2^ix—Si1—Y2^ix	0.00 (2)	Y2^xvi—O4—Ca2^vi	111.2
O1^viii—Si1—Ca2^x	47.62 (6)	Ca2^xvi—O4—Ca2^vi	111.18 (13)
O1—Si1—Ca2^x	146.23 (7)	Si3—O4—Y2^vi	107.71 (14)
O3^iv—Si1—Ca2^x	107.33 (4)	Y2^xvi—O4—Y2^vi	111.18 (13)
N5—Si1—Ca2^x	63.45 (2)	Ca2^xvi—O4—Y2^vi	111.18 (13)
Ca2^iv—Si1—Ca2^x	156.21 (3)	Ca2^vi—O4—Y2^vi	0.00 (3)
Y2^iv—Si1—Ca2^x	156.2	Si3—O4—Y2ⁱ	107.71 (14)
Ca2^ix—Si1—Ca2^x	72.618 (6)	Y2^xvi—O4—Y2ⁱ	111.18 (13)
Y2^ix—Si1—Ca2^x	72.6	Ca2^xvi—O4—Y2ⁱ	111.18 (13)
O1^viii—Si1—Y2^x	47.62 (6)	Ca2^vi—O4—Y2ⁱ	111.18 (13)
O1—Si1—Y2^x	146.23 (7)	Y2^vi—O4—Y2ⁱ	111.18 (13)
O3^iv—Si1—Y2^x	107.33 (4)	Si3—O4—Ca2ⁱ	107.71 (14)
N5—Si1—Y2^x	63.45 (2)	Y2^xvi—O4—Ca2ⁱ	111.2
Ca2^iv—Si1—Y2^x	156.21 (3)	Ca2^xvi—O4—Ca2ⁱ	111.18 (13)
Y2^iv—Si1—Y2^x	156.21 (3)	Ca2^vi—O4—Ca2ⁱ	111.18 (13)
Ca2^ix—Si1—Y2^x	72.618 (6)	Y2^vi—O4—Ca2ⁱ	111.2
Y2^ix—Si1—Y2^x	72.618 (6)	Y2ⁱ—O4—Ca2ⁱ	0
Ca2^x—Si1—Y2^x	0.00 (3)	Si3^viii—N5—Si3	22.51 (13)
O1^viii—Si1—Y2ⁱ	146.23 (7)	Si3^viii—N5—Si1	122.61 (15)
O1—Si1—Y2ⁱ	47.62 (6)	Si3—N5—Si1	122.61 (15)
O3^iv—Si1—Y2ⁱ	107.33 (4)	Si3^viii—N5—Si2^xvii	120.70 (15)
N5—Si1—Y2ⁱ	63.45 (2)	Si3—N5—Si2^xvii	120.70 (15)
Ca2^iv—Si1—Y2ⁱ	72.618 (6)	Si1—N5—Si2^xvii	115.29 (16)
Y2^iv—Si1—Y2ⁱ	72.618 (6)	Si3^viii—N5—Ca2ⁱ	113.45 (10)
Ca2^ix—Si1—Y2ⁱ	156.21 (3)	Si3—N5—Ca2ⁱ	90.94 (7)
Y2^ix—Si1—Y2ⁱ	156.21 (3)	Si1—N5—Ca2ⁱ	83.32 (6)
Ca2^x—Si1—Y2ⁱ	123.37 (3)	Si2^xvii—N5—Ca2ⁱ	83.70 (6)
Y2^x—Si1—Y2ⁱ	123.37 (3)	Si3^viii—N5—Y2ⁱ	113.45 (10)
O1^viii—Si1—Ca2ⁱ	146.23 (7)	Si3—N5—Y2ⁱ	90.94 (7)
O1—Si1—Ca2ⁱ	47.62 (6)	Si1—N5—Y2ⁱ	83.32 (6)
O3^iv—Si1—Ca2ⁱ	107.33 (4)	Si2^xvii—N5—Y2ⁱ	83.70 (6)
N5—Si1—Ca2ⁱ	63.45 (2)	Ca2ⁱ—N5—Y2ⁱ	0.00 (3)
Ca2^iv—Si1—Ca2ⁱ	72.618 (6)	Si3^viii—N5—Y2^x	90.94 (7)
Y2^iv—Si1—Ca2ⁱ	72.6	Si3—N5—Y2^x	113.45 (10)
Ca2^ix—Si1—Ca2ⁱ	156.21 (3)	Si1—N5—Y2^x	83.32 (6)
Y2^ix—Si1—Ca2ⁱ	156.2	Si2^xvii—N5—Y2^x	83.70 (6)
Ca2^x—Si1—Ca2ⁱ	123.37 (3)	Ca2ⁱ—N5—Y2^x	155.61 (11)
Y2^x—Si1—Ca2ⁱ	123.4	Y2ⁱ—N5—Y2^x	155.61 (11)
Y2ⁱ—Si1—Ca2ⁱ	0	Si3^viii—N5—Ca2^x	90.94 (7)
O2^xi—Si2—O2^vii	120.36 (13)	Si3—N5—Ca2^x	113.45 (10)
O2^xi—Si2—O3	105.60 (8)	Si1—N5—Ca2^x	83.32 (6)
O2^vii—Si2—O3	105.60 (8)	Si2^xvii—N5—Ca2^x	83.70 (6)
O2^xi—Si2—N5^vii	107.03 (8)	Ca2ⁱ—N5—Ca2^x	155.61 (11)
O2^vii—Si2—N5^vii	107.03 (8)	Y2ⁱ—N5—Ca2^x	155.6
O3—Si2—N5^vii	111.18 (13)	Y2^x—N5—Ca2^x	0

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

Selected bond lengths (Å) top

	1	2	3
Si1—O1	1.634 (2) × 2	1.621 (2) × 2	1.623 (2) × 2
Si1—O3	1.686 (3)	1.669 (4)	1.673 (3)
Si1—N5	1.754 (3)	1.788 (4)	1.781 (3)
Si2—O2	1.635 (2) × 2	1.622 (3) × 2	1.624 (2) × 2
Si2—O3	1.685 (3)	1.673 (4)	1.672 (3)
Si2—N5	1.753 (3)	1.798 (4)	1.782 (3)
Si3—(O,N)4	1.804 (6)	1.769 (8)	1.765 (7)
Si3—N5	1.809 (3) × 3	1.730 (5) × 3	1.732 (3) × 3

R[F² > 2σ(F²)], wR(F²), S depending on the refinement of the site occupation factor of Ca and Y. top

	1	2	3
R[F² > 2σ(F²)], wR(F²), S at free occupancy	0.025, 0.058, 1.10	0.031, 0.088, 1.14	0.023, 0.062, 1.09
R[F² > 2σ(F²)], wR(F²), S at fixed occupancy	0.025, 0.058, 1.10	0.033, 0.091, 1.18	0.024, 0.062, 1.09

Footnotes

‡Present address: Institute of Materials and Systems for Sustainability, Nagoya University, Furo-cho, Chikusa-ku, Nagoya 464-8601, Japan.

Funding information

Funding for this research was provided by: Ministry of Education, Culture, Sports, Science and Technology (grant Nos. JP16H06438, JP16H06439 and JP16H06440); Nippon Sheet Glass Foundation for Materials Science and Engineering; Dynamic Alliance for Open Innovation Bridging Human, Environment and Materials.

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ISSN: 2056-9890

Volume 75| Part 2| February 2019| Pages 260-263

https://doi.org/10.1107/S2056989019001257

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