Crystal structures of the solid solutions Na3Zn0.912Cd0.088B5O10 and Na3Zn0.845Mg0.155B5O10

Chen, X.-A.; Zhang, Y.-H.; Chang, X.-A.; Xiao, W.-Q.

doi:10.1107/S2056989017015249

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Volume 73| Part 11| November 2017| Pages 1774-1778

https://doi.org/10.1107/S2056989017015249

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Crystal structures of the solid solutions Na₃Zn_0.912Cd_0.088B₅O₁₀ and Na₃Zn_0.845Mg_0.155B₅O₁₀

Xue-An Chen,^a ^* Ya-Hua Zhang,^a Xin-An Chang ^a and Wei-Qiang Xiao ^b

^aCollege of Materials Science and Engineering, Beijing University of Technology, Ping Le Yuan 100, Beijing 100124, People's Republic of China, and ^bInstitute of Microstructure and Property of Advanced Materials, Beijing University of Technology, Ping Le Yuan 100, Beijing 100124, People's Republic of China
^*Correspondence e-mail: xueanchen@bjut.edu.cn

Edited by M. Weil, Vienna University of Technology, Austria (Received 11 October 2017; accepted 19 October 2017; online 24 October 2017)

Two new pentaborates, trisodium zinc cadmium pentaborate, Na₃Zn_0.912Cd_0.088B₅O₁₀, and trisodium zinc magnesium pentaborate, Na₃Zn_0.845Mg_0.155B₅O₁₀, have been synthesized by high-temperature solution reactions at 1023 K. Their crystal structures were determined by single-crystal X-ray diffraction. Both solid solutions crystallize in the orthorhombic form of the parent compound Na₃ZnB₅O₁₀ (space group type Pbca, Z = 8) and contain the double ring [B₅O₁₀]⁵⁻ anion composed of one BO₄ tetrahedron and four BO₃ triangles as the basic structural motif. The anions are bridged by tetrahedrally coordinated and occupationally disordered M²⁺ (M = Zn/Cd, Zn/Mg) cations via common O atoms to form [MB₅O₁₀]_n³ⁿ⁻ layers. The intralayer intersecting channels and the interlayer voids are occupied by Na⁺ cations to balance the charge.

Keywords: crystal structure; Na₃ZnB₅O₁₀; solid solution; borate; isotypism.

CCDC references: 1580783; 1580782

1. Chemical context

Over the past few decades, borate materials have attracted increasing interest owing to their promising applications in non-linear optical materials, birefringent materials, ferroelectric and piezoelectric materials, and host materials for luminescence (Becker, 1998 ; Chen et al., 1999 ). In general, boron atoms can be coordinated by either three or four oxygen atoms forming BO₃ or BO₄ groups, respectively. These groups may interconnect with each other via common oxygen atoms to produce polyborate anionic groups that can adopt different coordination modes to bind to metal cations. The crystal chemistry of the resultant borates is rich, including infinite chains, sheets or networks for the anionic groups. For instance, in a series of pentaborates with general composition A₃MB₅O₁₀ (A = Na, K; M = Mg, Zn, Cd, Co, and Fe), at least three kinds of structure types have been reported, including K₂NaZnB₅O₁₀ in space group C2/c (Chen et al., 2010 ), α-Na₃ZnB₅O₁₀, Na₃CoB₅O₁₀ and K₃MB₅O₁₀ (M = Zn, Cd) in space group P2₁/n (Chen et al., 2007a ; Strauss et al., 2016 ; Wu et al., 2012 ; Yu et al., 2011 ), and β-Na₃ZnB₅O₁₀ as well as Na₃MB₅O₁₀ (M = Mg, Fe) in space group Pbca (Chen et al., 2007b , 2012 ; Strauss et al., 2016). All of the structures contain polyborate anionic groups [B₅O₁₀]⁵⁻, which combine with different A⁺ and M²⁺ cations. During our exploratory syntheses of novel borate materials to study their structure–property relationships, we have obtained two new members of this family of compounds, viz. the solid solutions Na₃Zn_0.912Cd_0.088B₅O₁₀ and Na₃Zn_0.845Mg_0.155B₅O₁₀. Single crystal X-ray structure analyses revealed that these two compounds crystallize in the orthorhombic Na₃MB₅O₁₀ (M = Mg, Fe, Zn) structure type. Herein we describe their syntheses and crystal structures.

2. Structural commentary

Since Na₃Zn_0.912Cd_0.088B₅O₁₀ and Na₃Zn_0.845Mg_0.155B₅O₁₀ have similar structures, the discussion will be based mainly on the cadmium-containing compound. The fundamental building blocks in this structure are [(Zn/Cd)O₄] tetrahedra and [B₅O₁₀]⁵⁻ groups, as illustrated in Fig. 1. Each [B₅O₁₀]⁵⁻ group has one BO₄ tetrahedron (T) and four BO₃ triangles (Δ) condensed to a double ring via a common tetrahedron, the connectivity of which can be formulated as 4Δ1T:<2ΔT> − <2ΔT> according to the nomenclature introduced by Burns et al. (1995 ). The pentaborate group comprises four terminal O atoms in its isolated form. Each [B₅O₁₀]⁵⁻ group is linked to four different [(Zn/Cd)O₄] tetrahedra and likewise each [(Zn/Cd)O₄] tetrahedron is connected to four neighbouring [B₅O₁₀]⁵⁻ groups through sharing all of the terminal O atoms, thus forming infinite sheets with an overall composition of [(Zn/Cd)B₅O₁₀]_n³ⁿ⁻, as depicted in Fig. 2. The symmetry-equivalent (zinc/cadmium) borate sheets propagate in the ab plane and stack along the c axis. The sheets also afford intersecting open channels running parallel to the a- and b-axis directions. Fig. 3 shows a projection of the structure along [100]. Na2⁺ cations reside in these channels and Na1⁺ and Na3⁺ cations are situated at the voids between the sheets to provide charge compensation.

Figure 1
The asymmetric unit of Na₃Zn_0.912Cd_0.088B₅O₁₀ supplemented by additional oxygen atoms to show the full coordination around the disordered M site (M = Zn_0.912 (4)Cd_0.088 (4)). Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (i) $[{1\over 2}]$ − x, $[{1\over 2}]$ + y, z; (ii) $[{3\over 2}]$ − x, $[{1\over 2}]$ + y, z; (iii) 1 − x, $[{1\over 2}]$ + y, $[{1\over 2}]$ − z.]

Figure 2
View of the [(Zn/Cd)B₅O₁₀]_n³ⁿ⁻ layer approximately along [001]. (Zn/Cd) site: green spheres; BO₃ groups: navy triangles; BO₄ groups: magenta tetrahedra.

Figure 3
The crystal structure of Na₃Zn_0.912Cd_0.088B₅O₁₀ projected along [100]. Na1 atoms: violet spheres; Na2 atoms: blue spheres; Na3 atoms: grey spheres; (Zn/Cd) atoms: green spheres; BO₃ groups: navy triangles; BO₄ groups: magenta tetrahedra.

The asymmetric unit of Na₃Zn_0.912Cd_0.088B₅O₁₀ comprises 19 independent sites, i.e. three Na, one disordered (Zn/Cd), five B, and ten O sites, all occupying general positions. Of the three unique Na sites, Na1 is surrounded by seven O atoms with Na—O distances divided into two sets: a set of five short ones is in the range 2.310 (3)–2.700 (3) Å, while another set includes two longer separations [3.054 (3)–3.059 (3) Å, Table 1]. Bond-valence-sum (BVS) calculations using Brown's formula (Brown & Altermatt, 1985 ) gave a BVS value of 0.89 valence units (v.u.) for the seven-coordinated Na1 cation, confirming that the long bonds participate in the overall metal coordination sphere. The coordination environment can be described as an irregular polyhedron. Similarly, Na2 and Na3 atoms have also adopted the seven-coordinated irregular polyhedral arrangement. This is different from the situation in monoclinic α-Na₃ZnB₅O₁₀, where three distinct Na sites have coordination numbers of six, seven, and eight, respectively (Chen et al., 2007a). In the Na₃Zn_0.912Cd_0.088B₅O₁₀ structure, the Na—O distances fall in the range 2.273 (3)–3.059 (3) Å (average range for the three sites 2.553–2.657 Å), which is similar to the value reported for the seven-coordinated Na⁺ cation in α-Na₃ZnB₅O₁₀ [2.318 (2)–2.859 (3) Å, average 2.531 Å] (Chen et al., 2007a), and in agreement with the value of 2.50 Å computed from crystal radii sums for seven-coordinated Na⁺ and four-coordinated O²⁻ ions (Shannon, 1976 ). In the Na₃Zn_0.912Cd_0.088B₅O₁₀ structure, the M1 site is statistically disordered with Zn²⁺ and Cd²⁺ cations. The [Zn_0.912 (4)Cd_0.088 (4)O₄] tetrahedron exhibits a mean O—M1—O angle of 109.14°, close to the ideal value of 109.5°. M1—O bond lengths [1.974 (2)–2.000 (2) Å] are normal when compared with those observed in the related structures of CdZn₂(BO₃)₂ [(Zn_0.67Cd_0.33)–O = 1.995 (14)–2.130 (15) Å, CN = 4] (Zhang et al., 2008 ), Cd₃Zn₃(BO₃)₄ [(Zn_0.5Cd_0.5)–O = 2.015 (3)–2.131 (4) Å, CN = 4] (Sun et al., 2003 ), and Cd_1.17Zn_0.83B₂O₅ [(Zn_0.753Cd_0.247)–O = 1.997 (7)–2.109 (6) Å, CN = 4] (Yuan et al., 2005 ). Of the boron sites, B3 has a tetrahedral configuration, while other B sites are in triangular configurations. The BO₄ and BO₃ groups are rather regular, with average O—B—O angles being close to 109.5 or 120°, respectively. The B—O bond lengths in the tetrahedron cover the range between 1.467 (4) and 1.472 (4) Å, and those in the triangles between 1.305 (5) and 1.407 (4) Å. The average B—O bond lengths (1.469 Å and 1.366–1.373 Å, respectively) are in good agreement with the data reviewed by Hawthorne et al. (1996 ). The calculated BVS values concerning B atoms are around 3 v.u., ranging from 2.99 v.u. for B1 to 3.07 v.u. for B3.

Table 1
Selected geometric parameters (Å, °) for (I)

Na1—O1ⁱ	2.310 (3)	Zn1—O5ⁱⁱⁱ	1.974 (2)
Na1—O9ⁱⁱ	2.404 (3)	Zn1—O9^iv	1.985 (2)
Na1—O4	2.487 (3)	Zn1—O10	2.000 (2)
Na1—O7	2.587 (3)	Zn1—O1^vi	2.000 (2)
Na1—O3ⁱⁱⁱ	2.700 (3)	B1—O1	1.335 (4)
Na1—O3ⁱ	3.054 (3)	B1—O2	1.384 (4)
Na1—O8ⁱⁱ	3.059 (3)	B1—O3	1.400 (4)
Na2—O2^iv	2.355 (3)	B2—O5	1.324 (4)
Na2—O6ⁱⁱⁱ	2.381 (3)	B2—O4	1.376 (4)
Na2—O10ⁱⁱ	2.388 (3)	B2—O3	1.407 (4)
Na2—O6^iv	2.550 (3)	B3—O4	1.467 (4)
Na2—O4ⁱⁱⁱ	2.618 (3)	B3—O2	1.468 (4)
Na2—O10	2.719 (3)	B3—O7	1.468 (4)
Na2—O8	2.859 (3)	B3—O6	1.472 (4)
Na3—O5^v	2.273 (3)	B4—O9	1.337 (4)
Na3—O9	2.361 (3)	B4—O6	1.369 (4)
Na3—O7ⁱⁱ	2.438 (3)	B4—O8	1.395 (4)
Na3—O1^iv	2.458 (3)	B5—O10	1.305 (5)
Na3—O3^v	2.786 (3)	B5—O7	1.388 (4)
Na3—O10ⁱⁱ	2.868 (3)	B5—O8	1.405 (5)
Na3—O2ⁱⁱ	2.910 (3)

O5ⁱⁱⁱ—Zn1—O9^iv	111.39 (10)	O4—B3—O2	110.6 (3)
O5ⁱⁱⁱ—Zn1—O10	103.73 (11)	O4—B3—O7	109.8 (3)
O9^iv—Zn1—O10	112.42 (10)	O2—B3—O7	109.4 (3)
O5ⁱⁱⁱ—Zn1—O1^vi	110.40 (9)	O4—B3—O6	107.9 (3)
O9^iv—Zn1—O1^vi	120.23 (10)	O2—B3—O6	108.8 (3)
O10—Zn1—O1^vi	96.64 (12)	O7—B3—O6	110.4 (3)
O1—B1—O2	121.5 (3)	O9—B4—O6	123.6 (3)
O1—B1—O3	120.0 (3)	O9—B4—O8	118.8 (3)
O2—B1—O3	118.4 (3)	O6—B4—O8	117.6 (3)
O5—B2—O4	123.4 (3)	O10—B5—O7	123.2 (3)
O5—B2—O3	117.4 (3)	O10—B5—O8	118.1 (3)
O4—B2—O3	119.1 (3)	O7—B5—O8	118.7 (3)
Symmetry codes: (i) $[x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z]$ ; (ii) $[x+{\script{1\over 2}}, y, -z+{\script{1\over 2}}]$ ; (iii) $[-x+{\script{3\over 2}}, y+{\script{1\over 2}}, z]$ ; (iv) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (v) $[x, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (vi) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, z]$ .

A comparison between the Na₃Zn_0.845Mg_0.155B₅O₁₀ and Na₃Zn_0.912Cd_0.088B₅O₁₀ structures reveals that the isovalent substitution of Mg²⁺ for Cd²⁺ ions in Na₃Zn_0.912Cd_0.088B₅O₁₀ leads to a significant decrease in the cell volume [V = 1749.7 (3) Å³ for the (Zn/Mg) vs 1763.7 (5) Å³ for the (Zn/Cd) phase; V = 1745.50 (17) Å³ for unsubstituted Na₃ZnB₅O₁₀ (Chen et al., 2012)]. In the two solid solutions, the [B₅O₁₀]⁵⁻ groups show a similar configuration, with the dihedral angles between two hexagonal ring planes being identical within the experimental error [84.7 (1) vs 84.9 (1)°]. The geometric parameters of BO₃ triangles and BO₄ tetrahedra remain basically unchanged from the (Zn/Cd) to the (Zn/Mg) phase, while the [NaO₇] polyhedra in the (Zn/Mg) compound are slightly smaller compared with the corresponding ones in the (Zn/Cd) compound. In contrast, a remarkable difference in the coordination geometry around the divalent metal ions exists. The average (Zn/Mg)—O bond length is 1.962 Å, shorter than the average (Zn/Cd)—O bond length of 1.990 Å. The O—(Zn/Mg)—O angles are 98.11 (13)–119.58 (11)°, distinctly narrower than the O—(Zn/Cd)—O angles of 96.64 (12)–120.23 (10)°. The [(Zn/Mg)O₄] tetrahedron appears to be smaller and more regular than the [(Zn/Cd)O₄] tetrahedron, which follows the general trend of the respective ionic radii [r(Mg²⁺) = 0.72 < r(Zn²⁺) = 0.74 < r(Cd²⁺) = 0.92 Å, CN = 4] (Shannon, 1976).

As mentioned above, Na₃ZnB₅O₁₀ was reported to exist in two structural variants, which we name in the following the α- and β-phases, respectively. The α-form crystallizes in space group P2₁/n, while the β-form in space group Pbca (Chen et al., 2007a, 2012). The relationship between their crystal structures follows a group–subgroup relation: β-Na₃ZnB₅O₁₀ (Pbca, a, b, c, Z = 8) → α-Na₃ZnB₅O₁₀ (P2₁/n, which is a maximal non-isomorphic subgroup of index 2 of Pbca, 0.5a + 0.5b, c, 0.5a − 0.5b, Z = 4). β-Na₃ZnB₅O₁₀ is isotypic with Na₃MB₅O₁₀ (M = Mg, Fe), and the title compounds which are substitutional solid solutions of β-Na₃ZnB₅O₁₀. All structures comprise identical [MB₅O₁₀]_n³ⁿ⁻ (M = Zn, Mg, Fe, (Zn/Mg), (Zn/Cd)) layers constructed by [B₅O₁₀]⁵⁻ groups and MO₄ tetrahedra via common O atoms, and the coordination environments around all cationic sites are very similar. The main differences pertain to the [MO₄] tetrahedra. For example, the average M—O bond lengths are 1.963, 1.963, 1.962, and 1.990 Å for β-Na₃ZnB₅O₁₀, Na₃MgB₅O₁₀, Na₃Zn_0.845Mg_0.155B₅O₁₀, and Na₃Zn_0.912Cd_0.088B₅O₁₀, respectively. The cell volumes show a similar trend.

For Na₃ZnB₅O₁₀, the present study indicates that a partial replacement of Zn²⁺ by Cd²⁺ or Mg²⁺ is favourable for the formation of the orthorhombic Pbca phase. However, keeping the Na⁺ ions unchanged, the complete replacement of Zn²⁺ by larger Cd²⁺ ions does not result in the isotypic cadmium analogue. We have attempted to prepare a hypothetical compound with nominal composition `Na₃CdB₅O₁₀' via a standard solid-state synthetic route by mixing stoichiometric amounts of Na₂CO₃, CdO, and H₃BO₃ powders followed by annealing the mixture at a temperature of 873 K in air for several weeks. No `Na₃CdB₅O₁₀' has been obtained, only a mixture of known phases, viz. NaBO₂ and Cd₂B₂O₅, was formed instead, according to powder X-ray diffraction analyses. This indicates that the structural variants in the family of compounds A₃MB₅O₁₀ depend strongly on sizes of A⁺ and M²⁺ cations.

3. Synthesis and crystallization

In a typical synthesis of the cadmium-containing compound, a powder mixture of the starting materials Na₂B₄O₇·10H₂O, ZnO, CdO, H₃BO₃ in the molar ratio Na:Zn:Cd:B = 3:2:1:7 was transferred to a platinum crucible of 40 mm in diameter and 40 mm in height. The sample was melted at 1023 K for one week, then cooled down to 773 K at a rate of 0.5 K h⁻¹, to 573 K at 1.0 K h⁻¹, followed by cooling to room temperature at 20 K h⁻¹. Colourless prismatic crystals were isolated from the solidified melt. Energy-dispersive X-ray analyses (EDX) in a scanning electron microscope confirmed the existence of the heavy elements zinc and cadmium with an approximate atomic ratio of 8.2:1.5, close to the refined composition of the crystal (9.12: 0.88) (see Figs. S1–S2 and Table S1 in the Supporting information). The magnesium-containing compound was prepared in the same way, except that the starting materials were Na₂B₄O₇·10H₂O, ZnO, MgO, H₃BO₃ in the molar ratio Na:Zn:Mg:B = 2:2:1:6. EDX measurements for the Na₃Zn_0.845Mg_0.155B₅O₁₀ crystal gave an approximate atomic ratio of Zn:Mg = 4.9:3.8, deviating significantly from the refined composition (8.45:1.55) (see Figs. S3–S4 and Table S2). This may be due to the fact that the Mg-peak in the EDX spectrum is very close to the main peak of Zn, which leads the calculations of the integrated intensities of the Zn and Mg peaks to be inaccurate, consequently producing an inaccurate Zn/Mg atomic ratio. The powder X-ray diffraction pattern of the ground crystals are in good agreement with those calculated from the single-crystal data.

The infrared spectra exhibit the characteristic absorption bands of both BO₃ and BO₄ groups for Na₃Zn_0.912Cd_0.088B₅O₁₀ (Na₃Zn_0.845Mg_0.155B₅O₁₀), i.e. BO₃ asymmetric stretching vibrations in the frequency range 1400–1206 (1400–1201) cm⁻¹, BO₄ asymmetric stretching modes from 1077 to 1025 (1079 to 1026) cm⁻¹, BO₃ symmetric stretching modes lying at around 938 (939) cm⁻¹, BO₄ symmetric stretching mixed with BO₃ out-of plane bending modes locating at about 776 (777) cm⁻¹, and the overlapped BO₃ and BO₄ bending vibrations occurring below 722 (723) cm⁻¹. These values correspond well to those reported in the literature (Filatov et al., 2004 ). UV–VIS diffuse reflectance spectra indicated insulator character, with optical band gaps of about 2.95 and 3.10 eV for Na₃Zn_0.912Cd_0.088B₅O₁₀ and Na₃Zn_0.845Mg_0.155B₅O₁₀, respectively.

4. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 2. Based on the EDX measurements, cadmium and magnesium, respectively, was incorporated in the crystals. In fact, refinements of the occupancies of the zinc sites in the two structures revealed a small incorporation of cadmium and a somewhat higher incorporation of magnesium, respectively. For the final models, the occupancies of the disordered M sites (M = Zn, Cd and Zn, Mg, respectively) were constrained to 1.0, with the same coordinates and displacement parameters for the two types of metals. The refined ratios were Zn_0.912 (4):Cd_0.088 (4) and Zn_0.845 (5):Mg_0.155 (5), respectively. The largest residual electron densities in the final difference-Fourier map are below 1.59 e Å⁻³.

Table 2
Experimental details

	Na₃Zn_0.912Cd_0.088B₅O₁₀	Na₃Zn_0.845Mg_0.155B₅O₁₀
Crystal data
M_r	352.53	342.03
Crystal system, space group	Orthorhombic, Pbca	Orthorhombic, Pbca
Temperature (K)	293	293
a, b, c (Å)	7.9407 (14), 12.293 (2), 18.0684 (19)	7.8931 (12), 12.2555 (12), 18.0874 (11)
V (Å³)	1763.7 (5)	1749.7 (3)
Z	8	8
Radiation type	Mo Kα	Mo Kα
μ (mm⁻¹)	2.95	2.60
Crystal size (mm)	0.30 × 0.10 × 0.10	0.30 × 0.20 × 0.20

Data collection
Diffractometer	Rigaku AFC-7R	Rigaku AFC-7R
Absorption correction	ψ scan (Kopfmann & Huber, 1968 )	ψ scan (Kopfmann & Huber, 1968)
T_min, T_max	0.703, 0.752	0.532, 0.603
No. of measured, independent and observed [I > 2σ(I)] reflections	3006, 2562, 1557	2982, 2542, 1496
R_int	0.061	0.053
(sin θ/λ)_max (Å⁻¹)	0.703	0.703

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.072, 0.91	0.044, 0.113, 0.87
No. of reflections	2562	2542
No. of parameters	174	173
Δρ_max, Δρ_min (e Å⁻³)	0.45, −0.45	1.59, −0.70
Computer programs: Rigaku/AFC Diffractometer Control Software (Rigaku Corporation, 1994 $[Rigaku Corporation (1994). Rigaku/AFC Diffractometer Control Software. Rigaku Corporation, Tokyo, Japan.]$ ), SHELXS97 (Sheldrick, 2008 ), SHELXL2014 (Sheldrick, 2015 ), ATOMS (Dowty, 1999 ) and publCIF (Westrip, 2010 ).

Supporting information

CCDC references: 1580783; 1580782

Crystal structure: contains datablocks I, II, global. DOI: https://doi.org/10.1107/S2056989017015249/wm5422sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989017015249/wm5422Isup2.hkl

Structure factors: contains datablock II. DOI: https://doi.org/10.1107/S2056989017015249/wm5422IIsup3.hkl

checkCIF report

Computing details top

For both structures, data collection: Rigaku/AFC Diffractometer Control Software (Rigaku Corporation, 1994); cell refinement: Rigaku/AFC Diffractometer Control Software (Rigaku Corporation, 1994); data reduction: Rigaku/AFC Diffractometer Control Software (Rigaku Corporation, 1994); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: ATOMS (Dowty, 1999); software used to prepare material for publication: publCIF (Westrip, 2010).

Trisodium zinc cadmium pentaborate (I) top

Crystal data top

Na₃Zn_0.912Cd_0.088B₅O₁₀	D_x = 2.655 Mg m⁻³
M_r = 352.53	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pbca	Cell parameters from 25 reflections
a = 7.9407 (14) Å	θ = 12.1–22.2°
b = 12.293 (2) Å	µ = 2.95 mm⁻¹
c = 18.0684 (19) Å	T = 293 K
V = 1763.7 (5) Å³	Prism, colorless
Z = 8	0.30 × 0.10 × 0.10 mm
F(000) = 1356.7

Data collection top

Rigaku AFC-7R diffractometer	R_int = 0.061
Radiation source: fine-focus sealed tube	θ_max = 30.0°, θ_min = 2.3°
2θ – ω scans	h = 0→11
Absorption correction: ψ scan (Kopfmann & Huber, 1968)	k = 0→17
T_min = 0.703, T_max = 0.752	l = 0→25
3006 measured reflections	3 standard reflections every 150 reflections
2562 independent reflections	intensity decay: 2.2%
1557 reflections with I > 2σ(I)

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0224P)²] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.037	(Δ/σ)_max = 0.001
wR(F²) = 0.072	Δρ_max = 0.45 e Å⁻³
S = 0.91	Δρ_min = −0.45 e Å⁻³
2562 reflections	Extinction correction: SHELXL2014 (Sheldrick, 2015), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
174 parameters	Extinction coefficient: 0.00127 (16)

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)
Na1	0.8291 (2)	0.41887 (12)	0.07922 (8)	0.0318 (4)
Na2	0.69268 (17)	0.65268 (11)	0.25478 (7)	0.0248 (3)
Na3	0.79023 (18)	0.42762 (12)	0.42997 (7)	0.0271 (4)
Zn1	0.42413 (4)	0.67826 (3)	0.09632 (2)	0.01812 (12)	0.912 (4)
Cd1	0.42413 (4)	0.67826 (3)	0.09632 (2)	0.01812 (12)	0.088 (4)
B1	0.4192 (5)	0.1571 (3)	0.0744 (2)	0.0195 (8)
B2	0.7256 (5)	0.1729 (4)	0.07257 (19)	0.0198 (8)
B3	0.5612 (5)	0.2868 (3)	0.16320 (19)	0.0174 (7)
B4	0.5534 (5)	0.3497 (3)	0.2967 (2)	0.0206 (8)
B5	0.4884 (6)	0.4782 (3)	0.1978 (2)	0.0239 (9)
O1	0.2779 (3)	0.1189 (2)	0.04400 (13)	0.0260 (6)
O2	0.4154 (3)	0.22647 (18)	0.13473 (12)	0.0211 (5)
O3	0.5761 (3)	0.1244 (2)	0.04691 (13)	0.0261 (6)
O4	0.7176 (3)	0.2455 (2)	0.13046 (12)	0.0215 (5)
O5	0.8686 (3)	0.1418 (2)	0.04139 (13)	0.0286 (6)
O6	0.5712 (3)	0.27092 (17)	0.24380 (12)	0.0220 (5)
O7	0.5416 (3)	0.40273 (18)	0.14568 (12)	0.0226 (6)
O8	0.5100 (4)	0.4541 (2)	0.27321 (13)	0.0380 (8)
O9	0.5732 (3)	0.33154 (19)	0.36916 (11)	0.0241 (5)
O10	0.4228 (4)	0.5721 (2)	0.18019 (14)	0.0390 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.0399 (9)	0.0298 (8)	0.0258 (8)	−0.0017 (7)	−0.0048 (7)	0.0019 (6)
Na2	0.0245 (7)	0.0292 (7)	0.0206 (6)	−0.0011 (7)	0.0013 (6)	−0.0035 (7)
Na3	0.0333 (8)	0.0298 (8)	0.0184 (6)	0.0006 (7)	−0.0012 (6)	0.0029 (6)
Zn1	0.01764 (18)	0.01970 (19)	0.01702 (17)	−0.00189 (18)	0.00014 (17)	−0.00138 (16)
Cd1	0.01764 (18)	0.01970 (19)	0.01702 (17)	−0.00189 (18)	0.00014 (17)	−0.00138 (16)
B1	0.0197 (17)	0.0201 (19)	0.0188 (16)	−0.0030 (19)	−0.0011 (17)	−0.0027 (14)
B2	0.0202 (18)	0.026 (2)	0.0135 (15)	0.0030 (19)	−0.0009 (14)	−0.0027 (17)
B3	0.0195 (18)	0.0194 (16)	0.0134 (15)	−0.0001 (16)	−0.0001 (16)	−0.0009 (13)
B4	0.0191 (19)	0.027 (2)	0.0160 (17)	0.0037 (17)	−0.0023 (15)	−0.0037 (15)
B5	0.028 (2)	0.019 (2)	0.025 (2)	0.0007 (17)	−0.0021 (18)	−0.0050 (17)
O1	0.0208 (13)	0.0307 (14)	0.0266 (13)	−0.0029 (12)	−0.0025 (12)	−0.0080 (11)
O2	0.0178 (11)	0.0250 (12)	0.0204 (11)	−0.0016 (11)	−0.0011 (11)	−0.0049 (9)
O3	0.0212 (12)	0.0332 (14)	0.0239 (12)	0.0000 (13)	0.0006 (12)	−0.0142 (11)
O4	0.0187 (12)	0.0255 (13)	0.0204 (11)	0.0009 (11)	−0.0005 (10)	−0.0092 (11)
O5	0.0214 (12)	0.0390 (15)	0.0253 (13)	0.0061 (12)	0.0001 (11)	−0.0140 (12)
O6	0.0318 (13)	0.0200 (11)	0.0142 (10)	0.0056 (12)	0.0008 (11)	−0.0002 (9)
O7	0.0358 (16)	0.0149 (11)	0.0173 (11)	0.0007 (11)	−0.0015 (10)	−0.0009 (9)
O8	0.068 (2)	0.0257 (14)	0.0206 (13)	0.0200 (14)	−0.0123 (14)	−0.0084 (11)
O9	0.0271 (12)	0.0320 (13)	0.0133 (10)	0.0012 (14)	−0.0030 (11)	−0.0030 (10)
O10	0.061 (2)	0.0242 (13)	0.0322 (14)	0.0203 (15)	0.0125 (15)	0.0114 (11)

Geometric parameters (Å, º) top

Na1—O1ⁱ	2.310 (3)	Zn1—Na1ⁱⁱⁱ	3.5615 (16)
Na1—O9ⁱⁱ	2.404 (3)	B1—O1	1.335 (4)
Na1—O4	2.487 (3)	B1—O2	1.384 (4)
Na1—O7	2.587 (3)	B1—O3	1.400 (4)
Na1—O3ⁱⁱⁱ	2.700 (3)	B1—Cd1^xi	2.767 (4)
Na1—B4ⁱⁱ	2.986 (4)	B1—Na1^xii	3.015 (4)
Na1—B1ⁱ	3.015 (4)	B2—O5	1.324 (4)
Na1—O3ⁱ	3.054 (3)	B2—O4	1.376 (4)
Na1—O8ⁱⁱ	3.059 (3)	B2—O3	1.407 (4)
Na1—B3	3.076 (4)	B2—Na3^xiii	2.903 (4)
Na1—B2	3.135 (5)	B2—Na1^v	3.155 (5)
Na1—B2ⁱⁱⁱ	3.155 (5)	B3—O4	1.467 (4)
Na1—Na3^iv	3.4250 (19)	B3—O2	1.468 (4)
Na1—Cd1^v	3.5614 (16)	B3—O7	1.468 (4)
Na2—O2^vi	2.355 (3)	B3—O6	1.472 (4)
Na2—O6ⁱⁱⁱ	2.381 (3)	B3—Na2^xiv	2.996 (4)
Na2—O10ⁱⁱ	2.388 (3)	B3—Na2^v	3.046 (4)
Na2—O6^vi	2.550 (3)	B4—O9	1.337 (4)
Na2—O4ⁱⁱⁱ	2.618 (3)	B4—O6	1.369 (4)
Na2—O10	2.719 (3)	B4—O8	1.395 (4)
Na2—O8	2.859 (3)	B4—Na1^x	2.986 (4)
Na2—B5	2.879 (4)	B5—O10	1.305 (5)
Na2—B3^vi	2.996 (4)	B5—O7	1.388 (4)
Na2—B3ⁱⁱⁱ	3.046 (4)	B5—O8	1.405 (5)
Na2—Zn1ⁱⁱ	3.2734 (14)	B5—Na3^x	2.862 (4)
Na2—Cd1ⁱⁱ	3.2734 (14)	O1—Cd1^xi	2.000 (2)
Na3—O5^vii	2.273 (3)	O1—Zn1^xi	2.000 (2)
Na3—O9	2.361 (3)	O1—Na1^xii	2.310 (3)
Na3—O7ⁱⁱ	2.438 (3)	O1—Na3^xiv	2.458 (3)
Na3—O1^vi	2.458 (3)	O2—Na2^xiv	2.355 (3)
Na3—O3^vii	2.786 (3)	O2—Na3^x	2.910 (3)
Na3—B5ⁱⁱ	2.862 (4)	O3—Na1^v	2.700 (3)
Na3—O10ⁱⁱ	2.868 (3)	O3—Na3^xiii	2.786 (3)
Na3—B2^vii	2.903 (4)	O4—Na2^v	2.618 (3)
Na3—O2ⁱⁱ	2.910 (3)	O5—Cd1^v	1.974 (2)
Na3—Cd1ⁱⁱ	3.2938 (16)	O5—Zn1^v	1.974 (2)
Na3—Zn1ⁱⁱ	3.2938 (16)	O5—Na3^xiii	2.273 (3)
Na3—Na1^viii	3.4250 (19)	O6—Na2^v	2.381 (3)
Zn1—O5ⁱⁱⁱ	1.974 (2)	O6—Na2^xiv	2.550 (3)
Zn1—O9^vi	1.985 (2)	O7—Na3^x	2.438 (3)
Zn1—O10	2.000 (2)	O9—Cd1^xiv	1.985 (2)
Zn1—O1^ix	2.000 (2)	O9—Zn1^xiv	1.985 (2)
Zn1—Na2^x	3.2733 (14)	O9—Na1^x	2.404 (3)
Zn1—Na3^x	3.2938 (16)	O10—Na2^x	2.388 (3)
Zn1—Na3^vi	3.5382 (16)	O10—Na3^x	2.868 (3)

O1ⁱ—Na1—O9ⁱⁱ	115.21 (10)	O10ⁱⁱ—Na3—Zn1ⁱⁱ	37.07 (5)
O1ⁱ—Na1—O4	97.12 (10)	B2^vii—Na3—Zn1ⁱⁱ	125.68 (9)
O9ⁱⁱ—Na1—O4	76.10 (9)	O2ⁱⁱ—Na3—Zn1ⁱⁱ	128.80 (7)
O1ⁱ—Na1—O7	106.07 (10)	Cd1ⁱⁱ—Na3—Zn1ⁱⁱ	0.000 (13)
O9ⁱⁱ—Na1—O7	119.81 (9)	O5^vii—Na3—Na1^viii	65.50 (8)
O4—Na1—O7	56.45 (8)	O9—Na3—Na1^viii	116.11 (8)
O1ⁱ—Na1—O3ⁱⁱⁱ	91.64 (9)	O7ⁱⁱ—Na3—Na1^viii	137.47 (8)
O9ⁱⁱ—Na1—O3ⁱⁱⁱ	106.08 (10)	O1^vi—Na3—Na1^viii	42.40 (6)
O4—Na1—O3ⁱⁱⁱ	169.04 (9)	O3^vii—Na3—Na1^viii	50.25 (6)
O7—Na1—O3ⁱⁱⁱ	114.72 (9)	B5ⁱⁱ—Na3—Na1^viii	131.86 (10)
O1ⁱ—Na1—B4ⁱⁱ	140.44 (12)	O10ⁱⁱ—Na3—Na1^viii	107.87 (7)
O9ⁱⁱ—Na1—B4ⁱⁱ	25.95 (9)	B2^vii—Na3—Na1^viii	59.13 (9)
O4—Na1—B4ⁱⁱ	71.88 (10)	O2ⁱⁱ—Na3—Na1^viii	151.51 (7)
O7—Na1—B4ⁱⁱ	98.98 (10)	Cd1ⁱⁱ—Na3—Na1^viii	71.79 (4)
O3ⁱⁱⁱ—Na1—B4ⁱⁱ	105.21 (10)	Zn1ⁱⁱ—Na3—Na1^viii	71.79 (4)
O1ⁱ—Na1—B1ⁱ	24.80 (10)	O5ⁱⁱⁱ—Zn1—O9^vi	111.39 (10)
O9ⁱⁱ—Na1—B1ⁱ	91.57 (10)	O5ⁱⁱⁱ—Zn1—O10	103.73 (11)
O4—Na1—B1ⁱ	99.30 (10)	O9^vi—Zn1—O10	112.42 (10)
O7—Na1—B1ⁱ	127.81 (11)	O5ⁱⁱⁱ—Zn1—O1^ix	110.40 (9)
O3ⁱⁱⁱ—Na1—B1ⁱ	91.42 (10)	O9^vi—Zn1—O1^ix	120.23 (10)
B4ⁱⁱ—Na1—B1ⁱ	117.46 (12)	O10—Zn1—O1^ix	96.64 (12)
O1ⁱ—Na1—B3	104.34 (11)	O5ⁱⁱⁱ—Zn1—Na2^x	149.29 (8)
O9ⁱⁱ—Na1—B3	97.50 (10)	O9^vi—Zn1—Na2^x	80.73 (7)
O4—Na1—B3	28.10 (9)	O10—Zn1—Na2^x	46.49 (8)
O7—Na1—B3	28.40 (9)	O1^ix—Zn1—Na2^x	84.43 (7)
O3ⁱⁱⁱ—Na1—B3	142.49 (10)	O5ⁱⁱⁱ—Zn1—Na3^x	89.10 (8)
B4ⁱⁱ—Na1—B3	83.80 (11)	O9^vi—Zn1—Na3^x	159.51 (8)
B1ⁱ—Na1—B3	117.05 (11)	O10—Zn1—Na3^x	59.81 (9)
O1ⁱ—Na1—B2	73.94 (10)	O1^ix—Zn1—Na3^x	48.05 (8)
O9ⁱⁱ—Na1—B2	78.20 (10)	Na2^x—Zn1—Na3^x	81.22 (3)
O4—Na1—B2	25.10 (8)	O5ⁱⁱⁱ—Zn1—Na3^vi	122.04 (8)
O7—Na1—B2	73.29 (9)	O9^vi—Zn1—Na3^vi	39.19 (7)
O3ⁱⁱⁱ—Na1—B2	165.25 (10)	O10—Zn1—Na3^vi	131.64 (8)
B4ⁱⁱ—Na1—B2	84.87 (11)	O1^ix—Zn1—Na3^vi	82.34 (8)
B1ⁱ—Na1—B2	74.22 (10)	Na2^x—Zn1—Na3^vi	85.61 (3)
B3—Na1—B2	47.84 (10)	Na3^x—Zn1—Na3^vi	129.47 (2)
O1ⁱ—Na1—B2ⁱⁱⁱ	97.93 (10)	O5ⁱⁱⁱ—Zn1—Na1ⁱⁱⁱ	71.71 (8)
O9ⁱⁱ—Na1—B2ⁱⁱⁱ	124.59 (10)	O9^vi—Zn1—Na1ⁱⁱⁱ	39.91 (7)
O4—Na1—B2ⁱⁱⁱ	144.44 (10)	O10—Zn1—Na1ⁱⁱⁱ	127.64 (9)
O7—Na1—B2ⁱⁱⁱ	88.40 (10)	O1^ix—Zn1—Na1ⁱⁱⁱ	134.71 (8)
O3ⁱⁱⁱ—Na1—B2ⁱⁱⁱ	26.37 (8)	Na2^x—Zn1—Na1ⁱⁱⁱ	117.39 (3)
B4ⁱⁱ—Na1—B2ⁱⁱⁱ	113.11 (11)	Na3^x—Zn1—Na1ⁱⁱⁱ	160.39 (3)
B1ⁱ—Na1—B2ⁱⁱⁱ	107.72 (11)	Na3^vi—Zn1—Na1ⁱⁱⁱ	62.20 (4)
B3—Na1—B2ⁱⁱⁱ	116.48 (11)	O5ⁱⁱⁱ—Zn1—Na2	83.43 (8)
B2—Na1—B2ⁱⁱⁱ	156.47 (6)	O9^vi—Zn1—Na2	79.97 (7)
O1ⁱ—Na1—Na3^iv	45.83 (7)	O10—Zn1—Na2	48.75 (9)
O9ⁱⁱ—Na1—Na3^iv	140.76 (8)	O1^ix—Zn1—Na2	145.37 (8)
O4—Na1—Na3^iv	131.83 (8)	Na2^x—Zn1—Na2	70.674 (14)
O7—Na1—Na3^iv	99.41 (7)	Na3^x—Zn1—Na2	103.02 (3)
O3ⁱⁱⁱ—Na1—Na3^iv	52.51 (6)	Na3^vi—Zn1—Na2	118.00 (3)
B4ⁱⁱ—Na1—Na3^iv	155.89 (9)	Na1ⁱⁱⁱ—Zn1—Na2	79.33 (3)
B1ⁱ—Na1—Na3^iv	60.76 (8)	O1—B1—O2	121.5 (3)
B3—Na1—Na3^iv	119.19 (9)	O1—B1—O3	120.0 (3)
B2—Na1—Na3^iv	115.38 (8)	O2—B1—O3	118.4 (3)
B2ⁱⁱⁱ—Na1—Na3^iv	52.17 (7)	O1—B1—Cd1^xi	42.59 (16)
O1ⁱ—Na1—Cd1^v	90.77 (8)	O2—B1—Cd1^xi	78.9 (2)
O9ⁱⁱ—Na1—Cd1^v	31.99 (6)	O3—B1—Cd1^xi	162.6 (2)
O4—Na1—Cd1^v	56.75 (6)	O1—B1—Na1^xii	46.55 (16)
O7—Na1—Cd1^v	112.43 (7)	O2—B1—Na1^xii	155.6 (3)
O3ⁱⁱⁱ—Na1—Cd1^v	129.97 (8)	O3—B1—Na1^xii	78.18 (18)
B4ⁱⁱ—Na1—Cd1^v	50.97 (8)	Cd1^xi—B1—Na1^xii	85.80 (11)
B1ⁱ—Na1—Cd1^v	72.05 (8)	O5—B2—O4	123.4 (3)
B3—Na1—Cd1^v	84.23 (8)	O5—B2—O3	117.4 (3)
B2—Na1—Cd1^v	49.21 (8)	O4—B2—O3	119.1 (3)
B2ⁱⁱⁱ—Na1—Cd1^v	154.29 (9)	O5—B2—Na3^xiii	49.29 (16)
Na3^iv—Na1—Cd1^v	132.69 (5)	O4—B2—Na3^xiii	163.5 (3)
O2^vi—Na2—O6ⁱⁱⁱ	97.04 (9)	O3—B2—Na3^xiii	71.11 (17)
O2^vi—Na2—O10ⁱⁱ	91.24 (9)	O5—B2—Na1	94.0 (2)
O6ⁱⁱⁱ—Na2—O10ⁱⁱ	72.03 (10)	O4—B2—Na1	50.05 (18)
O2^vi—Na2—O6^vi	58.16 (8)	O3—B2—Na1	130.0 (2)
O6ⁱⁱⁱ—Na2—O6^vi	107.46 (9)	Na3^xiii—B2—Na1	113.46 (13)
O10ⁱⁱ—Na2—O6^vi	149.35 (10)	O5—B2—Na1^v	81.3 (2)
O2^vi—Na2—O4ⁱⁱⁱ	131.20 (9)	O4—B2—Na1^v	127.3 (2)
O6ⁱⁱⁱ—Na2—O4ⁱⁱⁱ	56.51 (8)	O3—B2—Na1^v	58.45 (19)
O10ⁱⁱ—Na2—O4ⁱⁱⁱ	113.25 (11)	Na3^xiii—B2—Na1^v	68.70 (10)
O6^vi—Na2—O4ⁱⁱⁱ	89.07 (8)	Na1—B2—Na1^v	171.50 (14)
O2^vi—Na2—O10	105.86 (10)	O4—B3—O2	110.6 (3)
O6ⁱⁱⁱ—Na2—O10	143.33 (9)	O4—B3—O7	109.8 (3)
O10ⁱⁱ—Na2—O10	134.11 (12)	O2—B3—O7	109.4 (3)
O6^vi—Na2—O10	64.21 (8)	O4—B3—O6	107.9 (3)
O4ⁱⁱⁱ—Na2—O10	87.01 (8)	O2—B3—O6	108.8 (3)
O2^vi—Na2—O8	92.59 (8)	O7—B3—O6	110.4 (3)
O6ⁱⁱⁱ—Na2—O8	158.52 (10)	O4—B3—Na2^xiv	125.4 (2)
O10ⁱⁱ—Na2—O8	88.67 (10)	O2—B3—Na2^xiv	50.56 (15)
O6^vi—Na2—O8	93.94 (9)	O7—B3—Na2^xiv	124.7 (2)
O4ⁱⁱⁱ—Na2—O8	127.59 (8)	O6—B3—Na2^xiv	58.25 (17)
O10—Na2—O8	49.20 (7)	O4—B3—Na2^v	59.21 (16)
O2^vi—Na2—B5	112.63 (11)	O2—B3—Na2^v	115.0 (2)
O6ⁱⁱⁱ—Na2—B5	150.29 (11)	O7—B3—Na2^v	135.3 (2)
O10ⁱⁱ—Na2—B5	107.34 (12)	O6—B3—Na2^v	49.90 (16)
O6^vi—Na2—B5	88.01 (11)	Na2^xiv—B3—Na2^v	82.25 (9)
O4ⁱⁱⁱ—Na2—B5	99.84 (10)	O4—B3—Na1	52.99 (16)
O10—Na2—B5	26.77 (10)	O2—B3—Na1	129.7 (2)
O8—Na2—B5	28.35 (9)	O7—B3—Na1	56.95 (17)
O2^vi—Na2—B3^vi	28.77 (9)	O6—B3—Na1	121.4 (2)
O6ⁱⁱⁱ—Na2—B3^vi	103.60 (10)	Na2^xiv—B3—Na1	178.31 (15)
O10ⁱⁱ—Na2—B3^vi	119.98 (10)	Na2^v—B3—Na1	96.30 (12)
O6^vi—Na2—B3^vi	29.39 (8)	O9—B4—O6	123.6 (3)
O4ⁱⁱⁱ—Na2—B3^vi	111.57 (10)	O9—B4—O8	118.8 (3)
O10—Na2—B3^vi	85.15 (10)	O6—B4—O8	117.6 (3)
O8—Na2—B3^vi	94.07 (10)	O9—B4—Na1^x	51.91 (17)
B5—Na2—B3^vi	102.00 (12)	O6—B4—Na1^x	142.0 (3)
O2^vi—Na2—B3ⁱⁱⁱ	119.08 (10)	O8—B4—Na1^x	79.6 (2)
O6ⁱⁱⁱ—Na2—B3ⁱⁱⁱ	28.21 (9)	O10—B5—O7	123.2 (3)
O10ⁱⁱ—Na2—B3ⁱⁱⁱ	90.05 (11)	O10—B5—O8	118.1 (3)
O6^vi—Na2—B3ⁱⁱⁱ	102.95 (10)	O7—B5—O8	118.7 (3)
O4ⁱⁱⁱ—Na2—B3ⁱⁱⁱ	28.77 (8)	O10—B5—Na3^x	77.1 (2)
O10—Na2—B3ⁱⁱⁱ	115.71 (10)	O7—B5—Na3^x	58.31 (18)
O8—Na2—B3ⁱⁱⁱ	148.33 (10)	O8—B5—Na3^x	143.4 (3)
B5—Na2—B3ⁱⁱⁱ	124.77 (12)	O10—B5—Na2	69.8 (2)
B3^vi—Na2—B3ⁱⁱⁱ	113.74 (13)	O7—B5—Na2	124.7 (3)
O2^vi—Na2—Zn1ⁱⁱ	58.06 (6)	O8—B5—Na2	75.0 (2)
O6ⁱⁱⁱ—Na2—Zn1ⁱⁱ	64.38 (6)	Na3^x—B5—Na2	139.48 (16)
O10ⁱⁱ—Na2—Zn1ⁱⁱ	37.41 (6)	B1—O1—Cd1^xi	110.6 (2)
O6^vi—Na2—Zn1ⁱⁱ	113.47 (7)	B1—O1—Zn1^xi	110.6 (2)
O4ⁱⁱⁱ—Na2—Zn1ⁱⁱ	120.70 (7)	Cd1^xi—O1—Zn1^xi	0.00 (2)
O10—Na2—Zn1ⁱⁱ	152.26 (7)	B1—O1—Na1^xii	108.6 (2)
O8—Na2—Zn1ⁱⁱ	105.74 (6)	Cd1^xi—O1—Na1^xii	132.05 (12)
B5—Na2—Zn1ⁱⁱ	132.99 (9)	Zn1^xi—O1—Na1^xii	132.05 (12)
B3^vi—Na2—Zn1ⁱⁱ	85.32 (8)	B1—O1—Na3^xiv	116.3 (2)
B3ⁱⁱⁱ—Na2—Zn1ⁱⁱ	91.96 (8)	Cd1^xi—O1—Na3^xiv	94.70 (10)
O2^vi—Na2—Cd1ⁱⁱ	58.06 (6)	Zn1^xi—O1—Na3^xiv	94.70 (10)
O6ⁱⁱⁱ—Na2—Cd1ⁱⁱ	64.38 (6)	Na1^xii—O1—Na3^xiv	91.77 (10)
O10ⁱⁱ—Na2—Cd1ⁱⁱ	37.41 (6)	B1—O2—B3	124.8 (3)
O6^vi—Na2—Cd1ⁱⁱ	113.47 (7)	B1—O2—Na2^xiv	116.0 (2)
O4ⁱⁱⁱ—Na2—Cd1ⁱⁱ	120.70 (7)	B3—O2—Na2^xiv	100.66 (18)
O10—Na2—Cd1ⁱⁱ	152.26 (7)	B1—O2—Na3^x	102.4 (2)
O8—Na2—Cd1ⁱⁱ	105.74 (6)	B3—O2—Na3^x	88.90 (18)
B5—Na2—Cd1ⁱⁱ	132.99 (9)	Na2^xiv—O2—Na3^x	122.91 (10)
B3^vi—Na2—Cd1ⁱⁱ	85.32 (8)	B1—O3—B2	120.8 (3)
B3ⁱⁱⁱ—Na2—Cd1ⁱⁱ	91.96 (8)	B1—O3—Na1^v	116.1 (2)
Zn1ⁱⁱ—Na2—Cd1ⁱⁱ	0.000 (14)	B2—O3—Na1^v	95.2 (2)
O5^vii—Na3—O9	115.10 (10)	B1—O3—Na3^xiii	151.4 (2)
O5^vii—Na3—O7ⁱⁱ	103.02 (10)	B2—O3—Na3^xiii	80.35 (18)
O9—Na3—O7ⁱⁱ	105.90 (9)	Na1^v—O3—Na3^xiii	77.25 (7)
O5^vii—Na3—O1^vi	104.47 (10)	B2—O4—B3	124.8 (3)
O9—Na3—O1^vi	114.00 (10)	B2—O4—Na1	104.9 (2)
O7ⁱⁱ—Na3—O1^vi	114.05 (9)	B3—O4—Na1	98.91 (19)
O5^vii—Na3—O3^vii	53.80 (8)	B2—O4—Na2^v	110.9 (2)
O9—Na3—O3^vii	78.04 (8)	B3—O4—Na2^v	92.02 (17)
O7ⁱⁱ—Na3—O3^vii	153.61 (9)	Na1—O4—Na2^v	126.59 (10)
O1^vi—Na3—O3^vii	86.56 (8)	B2—O5—Cd1^v	115.8 (2)
O5^vii—Na3—B5ⁱⁱ	130.19 (12)	B2—O5—Zn1^v	115.8 (2)
O9—Na3—B5ⁱⁱ	97.75 (11)	Cd1^v—O5—Zn1^v	0.00 (2)
O7ⁱⁱ—Na3—B5ⁱⁱ	28.97 (10)	B2—O5—Na3^xiii	104.5 (2)
O1^vi—Na3—B5ⁱⁱ	93.86 (11)	Cd1^v—O5—Na3^xiii	139.36 (13)
O3^vii—Na3—B5ⁱⁱ	175.52 (12)	Zn1^v—O5—Na3^xiii	139.36 (13)
O5^vii—Na3—O10ⁱⁱ	138.30 (11)	B4—O6—B3	126.3 (3)
O9—Na3—O10ⁱⁱ	104.76 (9)	B4—O6—Na2^v	117.1 (2)
O7ⁱⁱ—Na3—O10ⁱⁱ	52.28 (8)	B3—O6—Na2^v	101.9 (2)
O1^vi—Na3—O10ⁱⁱ	67.74 (8)	B4—O6—Na2^xiv	108.2 (2)
O3^vii—Na3—O10ⁱⁱ	153.17 (9)	B3—O6—Na2^xiv	92.4 (2)
B5ⁱⁱ—Na3—O10ⁱⁱ	26.34 (9)	Na2^v—O6—Na2^xiv	107.36 (9)
O5^vii—Na3—B2^vii	26.19 (10)	B5—O7—B3	122.4 (3)
O9—Na3—B2^vii	94.07 (11)	B5—O7—Na3^x	92.7 (2)
O7ⁱⁱ—Na3—B2^vii	126.07 (11)	B3—O7—Na3^x	109.2 (2)
O1^vi—Na3—B2^vii	101.45 (11)	B5—O7—Na1	122.1 (2)
O3^vii—Na3—B2^vii	28.54 (9)	B3—O7—Na1	94.7 (2)
B5ⁱⁱ—Na3—B2^vii	154.88 (13)	Na3^x—O7—Na1	116.90 (9)
O10ⁱⁱ—Na3—B2^vii	160.82 (11)	B4—O8—B5	121.3 (3)
O5^vii—Na3—O2ⁱⁱ	86.75 (9)	B4—O8—Na2	134.1 (2)
O9—Na3—O2ⁱⁱ	68.73 (8)	B5—O8—Na2	76.6 (2)
O7ⁱⁱ—Na3—O2ⁱⁱ	52.31 (8)	B4—O9—Cd1^xiv	117.9 (2)
O1^vi—Na3—O2ⁱⁱ	164.75 (9)	B4—O9—Zn1^xiv	117.9 (2)
O3^vii—Na3—O2ⁱⁱ	108.55 (8)	Cd1^xiv—O9—Zn1^xiv	0.00 (2)
B5ⁱⁱ—Na3—O2ⁱⁱ	70.91 (10)	B4—O9—Na3	117.2 (2)
O10ⁱⁱ—Na3—O2ⁱⁱ	97.01 (8)	Cd1^xiv—O9—Na3	108.72 (10)
B2^vii—Na3—O2ⁱⁱ	93.16 (11)	Zn1^xiv—O9—Na3	108.72 (10)
O5^vii—Na3—Cd1ⁱⁱ	112.99 (8)	B4—O9—Na1^x	102.1 (2)
O9—Na3—Cd1ⁱⁱ	129.54 (8)	Cd1^xiv—O9—Na1^x	108.10 (11)
O7ⁱⁱ—Na3—Cd1ⁱⁱ	76.84 (7)	Zn1^xiv—O9—Na1^x	108.10 (11)
O1^vi—Na3—Cd1ⁱⁱ	37.25 (6)	Na3—O9—Na1^x	100.64 (9)
O3^vii—Na3—Cd1ⁱⁱ	121.39 (7)	B5—O10—Zn1	139.4 (3)
B5ⁱⁱ—Na3—Cd1ⁱⁱ	60.18 (9)	B5—O10—Na2^x	123.5 (2)
O10ⁱⁱ—Na3—Cd1ⁱⁱ	37.07 (5)	Zn1—O10—Na2^x	96.10 (10)
B2^vii—Na3—Cd1ⁱⁱ	125.68 (9)	B5—O10—Na2	83.5 (2)
O2ⁱⁱ—Na3—Cd1ⁱⁱ	128.80 (7)	Zn1—O10—Na2	97.68 (11)
O5^vii—Na3—Zn1ⁱⁱ	112.99 (8)	Na2^x—O10—Na2	102.02 (10)
O9—Na3—Zn1ⁱⁱ	129.54 (8)	B5—O10—Na3^x	76.6 (2)
O7ⁱⁱ—Na3—Zn1ⁱⁱ	76.84 (7)	Zn1—O10—Na3^x	83.12 (10)
O1^vi—Na3—Zn1ⁱⁱ	37.25 (6)	Na2^x—O10—Na3^x	108.52 (12)
O3^vii—Na3—Zn1ⁱⁱ	121.39 (7)	Na2—O10—Na3^x	149.21 (11)
B5ⁱⁱ—Na3—Zn1ⁱⁱ	60.18 (9)

Symmetry codes: (i) x+1/2, −y+1/2, −z; (ii) x+1/2, y, −z+1/2; (iii) −x+3/2, y+1/2, z; (iv) −x+3/2, −y+1, z−1/2; (v) −x+3/2, y−1/2, z; (vi) −x+1, y+1/2, −z+1/2; (vii) x, −y+1/2, z+1/2; (viii) −x+3/2, −y+1, z+1/2; (ix) −x+1/2, y+1/2, z; (x) x−1/2, y, −z+1/2; (xi) −x+1/2, y−1/2, z; (xii) x−1/2, −y+1/2, −z; (xiii) x, −y+1/2, z−1/2; (xiv) −x+1, y−1/2, −z+1/2.

Trisodium zinc magnesium pentaborate (II) top

Crystal data top

Na₃Zn_0.845Mg_0.155B₅O₁₀	D_x = 2.597 Mg m⁻³
M_r = 342.03	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pbca	Cell parameters from 25 reflections
a = 7.8931 (12) Å	θ = 10.2–22.2°
b = 12.2555 (12) Å	µ = 2.60 mm⁻¹
c = 18.0874 (11) Å	T = 293 K
V = 1749.7 (3) Å³	Prism, colorless
Z = 8	0.30 × 0.20 × 0.20 mm
F(000) = 1321.7

Data collection top

Rigaku AFC-7R diffractometer	R_int = 0.053
Radiation source: fine-focus sealed tube	θ_max = 30.0°, θ_min = 2.3°
2θ – ω scans	h = 0→11
Absorption correction: ψ scan (Kopfmann & Huber, 1968)	k = 0→17
T_min = 0.532, T_max = 0.603	l = 0→25
2982 measured reflections	3 standard reflections every 150 reflections
2542 independent reflections	intensity decay: 1.8%
1496 reflections with I > 2σ(I)

Refinement top

Refinement on F²	173 parameters
Least-squares matrix: full	0 restraints
R[F² > 2σ(F²)] = 0.044	w = 1/[σ²(F_o²) + (0.0554P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.113	(Δ/σ)_max < 0.001
S = 0.87	Δρ_max = 1.59 e Å⁻³
2542 reflections	Δρ_min = −0.70 e Å⁻³

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0.8316 (2)	0.41813 (15)	0.07839 (9)	0.0239 (4)
Na2	0.6897 (2)	0.65191 (14)	0.25456 (9)	0.0206 (4)
Na3	0.7931 (2)	0.42713 (14)	0.42996 (9)	0.0200 (4)
Zn1	0.42299 (6)	0.67666 (4)	0.09703 (3)	0.01104 (14)	0.845 (5)
Mg1	0.42299 (6)	0.67666 (4)	0.09703 (3)	0.01104 (14)	0.155 (5)
B1	0.4227 (6)	0.1568 (3)	0.0748 (2)	0.0130 (8)
B2	0.7313 (6)	0.1729 (4)	0.0738 (2)	0.0152 (9)
B3	0.5641 (6)	0.2867 (4)	0.1632 (2)	0.0125 (8)
B4	0.5572 (5)	0.3497 (4)	0.2970 (2)	0.0128 (8)
B5	0.4890 (6)	0.4793 (4)	0.1982 (2)	0.0159 (9)
O1	0.2775 (3)	0.1191 (2)	0.04430 (15)	0.0143 (6)
O2	0.4175 (3)	0.2267 (2)	0.13508 (15)	0.0159 (6)
O3	0.5784 (4)	0.1245 (2)	0.04716 (15)	0.0174 (6)
O4	0.7209 (4)	0.2457 (2)	0.13007 (15)	0.0180 (6)
O5	0.8743 (4)	0.1431 (3)	0.04167 (16)	0.0209 (7)
O6	0.5735 (4)	0.2706 (2)	0.24378 (14)	0.0158 (6)
O7	0.5439 (4)	0.4035 (2)	0.14602 (14)	0.0168 (6)
O8	0.5099 (5)	0.4543 (2)	0.27360 (15)	0.0283 (8)
O9	0.5753 (3)	0.3304 (2)	0.36922 (13)	0.0140 (5)
O10	0.4240 (4)	0.5735 (2)	0.17972 (16)	0.0247 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.0291 (10)	0.0218 (9)	0.0206 (9)	−0.0003 (8)	−0.0034 (7)	0.0017 (7)
Na2	0.0211 (9)	0.0221 (8)	0.0186 (8)	−0.0020 (7)	0.0004 (7)	−0.0022 (7)
Na3	0.0235 (9)	0.0211 (9)	0.0154 (7)	0.0011 (8)	−0.0026 (7)	0.0019 (6)
Zn1	0.0112 (2)	0.0106 (2)	0.0112 (2)	−0.0005 (2)	0.0001 (2)	−0.00064 (19)
Mg1	0.0112 (2)	0.0106 (2)	0.0112 (2)	−0.0005 (2)	0.0001 (2)	−0.00064 (19)
B1	0.0127 (18)	0.015 (2)	0.0114 (17)	0.0013 (18)	0.0066 (17)	−0.0031 (14)
B2	0.019 (2)	0.012 (2)	0.0146 (18)	0.0023 (18)	0.0120 (17)	−0.0025 (17)
B3	0.017 (2)	0.0116 (17)	0.0086 (17)	0.0032 (17)	−0.0014 (17)	0.0005 (14)
B4	0.0098 (19)	0.0127 (19)	0.016 (2)	0.0025 (16)	−0.0006 (16)	−0.0045 (15)
B5	0.024 (2)	0.012 (2)	0.011 (2)	0.0034 (18)	−0.0028 (18)	−0.0025 (16)
O1	0.0121 (13)	0.0150 (14)	0.0159 (13)	−0.0008 (11)	0.0042 (11)	−0.0058 (11)
O2	0.0134 (13)	0.0197 (14)	0.0147 (13)	−0.0020 (12)	−0.0010 (12)	−0.0088 (11)
O3	0.0114 (12)	0.0239 (15)	0.0170 (13)	0.0023 (13)	0.0021 (12)	−0.0112 (11)
O4	0.0150 (14)	0.0187 (14)	0.0204 (14)	−0.0008 (12)	−0.0003 (12)	−0.0088 (12)
O5	0.0128 (13)	0.0301 (16)	0.0197 (15)	0.0046 (12)	0.0005 (12)	−0.0089 (13)
O6	0.0278 (15)	0.0098 (12)	0.0100 (12)	0.0043 (12)	−0.0002 (12)	−0.0011 (10)
O7	0.0285 (17)	0.0107 (13)	0.0112 (12)	0.0022 (11)	−0.0014 (11)	−0.0003 (10)
O8	0.058 (2)	0.0135 (14)	0.0133 (14)	0.0107 (15)	−0.0080 (15)	−0.0036 (12)
O9	0.0204 (13)	0.0116 (13)	0.0101 (12)	−0.0002 (12)	−0.0023 (11)	0.0004 (10)
O10	0.0411 (19)	0.0148 (13)	0.0181 (14)	0.0109 (15)	0.0040 (15)	0.0050 (11)

Geometric parameters (Å, º) top

Na1—O1ⁱ	2.305 (3)	B1—O3	1.384 (5)
Na1—O9ⁱⁱ	2.399 (3)	B1—O2	1.388 (5)
Na1—O4	2.470 (3)	B1—Mg1^xi	2.769 (5)
Na1—O7	2.586 (3)	B1—Na1^xii	3.006 (5)
Na1—O3ⁱⁱⁱ	2.687 (3)	B2—O5	1.321 (5)
Na1—B4ⁱⁱ	2.992 (5)	B2—O4	1.357 (5)
Na1—B1ⁱ	3.006 (5)	B2—O3	1.428 (5)
Na1—B3	3.067 (5)	B2—Mg1^v	2.762 (5)
Na1—B2	3.110 (5)	B2—Na3^xiii	2.916 (4)
Na1—B2ⁱⁱⁱ	3.162 (5)	B2—Na1^v	3.162 (5)
Na1—Na3^iv	3.431 (2)	B3—O2	1.462 (5)
Na1—Zn1^v	3.5530 (18)	B3—O4	1.464 (5)
Na2—O2^vi	2.354 (3)	B3—O6	1.473 (5)
Na2—O6ⁱⁱⁱ	2.377 (3)	B3—O7	1.474 (5)
Na2—O10ⁱⁱ	2.399 (4)	B3—Na2^xiv	2.992 (5)
Na2—O6^vi	2.536 (3)	B3—Na2^v	3.039 (5)
Na2—O4ⁱⁱⁱ	2.625 (3)	B4—O9	1.335 (5)
Na2—O10	2.675 (4)	B4—O6	1.372 (5)
Na2—O8	2.828 (4)	B4—O8	1.400 (5)
Na2—B5	2.832 (5)	B4—Mg1^xiv	2.863 (5)
Na2—B3^vi	2.992 (5)	B4—Na1^x	2.992 (5)
Na2—B3ⁱⁱⁱ	3.039 (5)	B5—O10	1.307 (5)
Na2—Zn1ⁱⁱ	3.2693 (17)	B5—O7	1.393 (5)
Na2—Mg1ⁱⁱ	3.2693 (17)	B5—O8	1.407 (5)
Na3—O5^vii	2.288 (3)	B5—Na3^x	2.859 (5)
Na3—O9	2.360 (3)	O1—Mg1^xi	1.978 (3)
Na3—O7ⁱⁱ	2.427 (3)	O1—Zn1^xi	1.978 (3)
Na3—O1^vi	2.462 (3)	O1—Na1^xii	2.305 (3)
Na3—O3^vii	2.787 (3)	O1—Na3^xiv	2.462 (3)
Na3—B5ⁱⁱ	2.859 (5)	O2—Na2^xiv	2.354 (3)
Na3—O10ⁱⁱ	2.867 (4)	O2—Na3^x	2.895 (3)
Na3—O2ⁱⁱ	2.895 (3)	O3—Na1^v	2.687 (3)
Na3—B2^vii	2.916 (4)	O3—Na3^xiii	2.787 (3)
Na3—Mg1ⁱⁱ	3.2620 (18)	O4—Na2^v	2.625 (3)
Na3—Zn1ⁱⁱ	3.2620 (18)	O5—Mg1^v	1.932 (3)
Na3—Na1^viii	3.431 (2)	O5—Zn1^v	1.932 (3)
Zn1—O5ⁱⁱⁱ	1.932 (3)	O5—Na3^xiii	2.288 (3)
Zn1—O10	1.958 (3)	O6—Na2^v	2.377 (3)
Zn1—O1^ix	1.978 (3)	O6—Na2^xiv	2.536 (3)
Zn1—O9^vi	1.980 (3)	O7—Na3^x	2.427 (3)
Zn1—Na3^x	3.2620 (18)	O9—Mg1^xiv	1.980 (3)
Zn1—Na2^x	3.2692 (17)	O9—Zn1^xiv	1.980 (3)
Zn1—Na3^vi	3.5456 (18)	O9—Na1^x	2.399 (3)
Zn1—Na1ⁱⁱⁱ	3.5530 (19)	O10—Na2^x	2.399 (4)
B1—O1	1.353 (5)	O10—Na3^x	2.867 (4)

O1ⁱ—Na1—O9ⁱⁱ	116.11 (11)	O9—Na3—Na1^viii	115.65 (9)
O1ⁱ—Na1—O4	97.45 (11)	O7ⁱⁱ—Na3—Na1^viii	137.98 (10)
O9ⁱⁱ—Na1—O4	75.55 (10)	O1^vi—Na3—Na1^viii	42.18 (7)
O1ⁱ—Na1—O7	106.21 (11)	O3^vii—Na3—Na1^viii	49.89 (7)
O9ⁱⁱ—Na1—O7	119.10 (11)	B5ⁱⁱ—Na3—Na1^viii	131.76 (11)
O4—Na1—O7	56.72 (10)	O10ⁱⁱ—Na3—Na1^viii	107.39 (8)
O1ⁱ—Na1—O3ⁱⁱⁱ	91.88 (10)	O2ⁱⁱ—Na3—Na1^viii	152.15 (8)
O9ⁱⁱ—Na1—O3ⁱⁱⁱ	107.04 (11)	B2^vii—Na3—Na1^viii	59.09 (10)
O4—Na1—O3ⁱⁱⁱ	168.01 (11)	Mg1ⁱⁱ—Na3—Na1^viii	71.89 (5)
O7—Na1—O3ⁱⁱⁱ	113.37 (11)	Zn1ⁱⁱ—Na3—Na1^viii	71.89 (5)
O1ⁱ—Na1—B4ⁱⁱ	141.23 (13)	O5ⁱⁱⁱ—Zn1—O10	104.78 (13)
O9ⁱⁱ—Na1—B4ⁱⁱ	25.79 (10)	O5ⁱⁱⁱ—Zn1—O1^ix	109.67 (11)
O4—Na1—B4ⁱⁱ	71.67 (11)	O10—Zn1—O1^ix	98.11 (13)
O7—Na1—B4ⁱⁱ	98.45 (11)	O5ⁱⁱⁱ—Zn1—O9^vi	110.90 (12)
O3ⁱⁱⁱ—Na1—B4ⁱⁱ	105.36 (12)	O10—Zn1—O9^vi	112.24 (11)
O1ⁱ—Na1—B1ⁱ	25.40 (11)	O1^ix—Zn1—O9^vi	119.58 (11)
O9ⁱⁱ—Na1—B1ⁱ	92.03 (12)	O5ⁱⁱⁱ—Zn1—Na3^x	89.02 (10)
O4—Na1—B1ⁱ	99.92 (12)	O10—Zn1—Na3^x	60.69 (10)
O7—Na1—B1ⁱ	128.69 (12)	O1^ix—Zn1—Na3^x	48.85 (8)
O3ⁱⁱⁱ—Na1—B1ⁱ	91.74 (11)	O9^vi—Zn1—Na3^x	160.08 (9)
B4ⁱⁱ—Na1—B1ⁱ	117.79 (13)	O5ⁱⁱⁱ—Zn1—Na2^x	150.73 (10)
O1ⁱ—Na1—B3	104.49 (12)	O10—Zn1—Na2^x	46.78 (9)
O9ⁱⁱ—Na1—B3	96.83 (12)	O1^ix—Zn1—Na2^x	84.96 (8)
O4—Na1—B3	28.11 (10)	O9^vi—Zn1—Na2^x	80.74 (8)
O7—Na1—B3	28.65 (10)	Na3^x—Zn1—Na2^x	81.89 (4)
O3ⁱⁱⁱ—Na1—B3	141.40 (12)	O5ⁱⁱⁱ—Zn1—Na3^vi	120.77 (10)
B4ⁱⁱ—Na1—B3	83.44 (12)	O10—Zn1—Na3^vi	131.75 (9)
B1ⁱ—Na1—B3	117.74 (13)	O1^ix—Zn1—Na3^vi	81.81 (8)
O1ⁱ—Na1—B2	74.68 (11)	O9^vi—Zn1—Na3^vi	38.94 (8)
O9ⁱⁱ—Na1—B2	77.38 (12)	Na3^x—Zn1—Na3^vi	129.78 (2)
O4—Na1—B2	24.94 (10)	Na2^x—Zn1—Na3^vi	85.55 (4)
O7—Na1—B2	73.87 (11)	O5ⁱⁱⁱ—Zn1—Na1ⁱⁱⁱ	71.14 (10)
O3ⁱⁱⁱ—Na1—B2	166.29 (12)	O10—Zn1—Na1ⁱⁱⁱ	127.44 (10)
B4ⁱⁱ—Na1—B2	84.31 (13)	O1^ix—Zn1—Na1ⁱⁱⁱ	133.45 (9)
B1ⁱ—Na1—B2	74.99 (12)	O9^vi—Zn1—Na1ⁱⁱⁱ	39.93 (9)
B3—Na1—B2	47.96 (11)	Na3^x—Zn1—Na1ⁱⁱⁱ	159.71 (4)
O1ⁱ—Na1—B2ⁱⁱⁱ	98.09 (11)	Na2^x—Zn1—Na1ⁱⁱⁱ	117.54 (4)
O9ⁱⁱ—Na1—B2ⁱⁱⁱ	125.37 (12)	Na3^vi—Zn1—Na1ⁱⁱⁱ	61.85 (4)
O4—Na1—B2ⁱⁱⁱ	143.05 (13)	O5ⁱⁱⁱ—Zn1—Na2	84.66 (9)
O7—Na1—B2ⁱⁱⁱ	86.73 (12)	O10—Zn1—Na2	47.97 (10)
O3ⁱⁱⁱ—Na1—B2ⁱⁱⁱ	26.71 (10)	O1^ix—Zn1—Na2	146.06 (9)
B4ⁱⁱ—Na1—B2ⁱⁱⁱ	112.96 (12)	O9^vi—Zn1—Na2	80.21 (8)
B1ⁱ—Na1—B2ⁱⁱⁱ	108.33 (13)	Na3^x—Zn1—Na2	103.06 (4)
B3—Na1—B2ⁱⁱⁱ	115.08 (13)	Na2^x—Zn1—Na2	70.585 (14)
B2—Na1—B2ⁱⁱⁱ	156.02 (7)	Na3^vi—Zn1—Na2	117.98 (4)
O1ⁱ—Na1—Na3^iv	45.81 (8)	Na1ⁱⁱⁱ—Zn1—Na2	79.88 (4)
O9ⁱⁱ—Na1—Na3^iv	141.90 (10)	O1—B1—O3	120.5 (3)
O4—Na1—Na3^iv	131.87 (9)	O1—B1—O2	120.4 (4)
O7—Na1—Na3^iv	99.00 (9)	O3—B1—O2	119.1 (4)
O3ⁱⁱⁱ—Na1—Na3^iv	52.49 (7)	O1—B1—Mg1^xi	41.80 (17)
B4ⁱⁱ—Na1—Na3^iv	156.20 (11)	O3—B1—Mg1^xi	162.2 (3)
B1ⁱ—Na1—Na3^iv	61.07 (9)	O2—B1—Mg1^xi	78.6 (2)
B3—Na1—Na3^iv	118.95 (10)	O1—B1—Na1^xii	46.95 (18)
B2—Na1—Na3^iv	116.11 (10)	O3—B1—Na1^xii	78.0 (2)
B2ⁱⁱⁱ—Na1—Na3^iv	52.31 (8)	O2—B1—Na1^xii	154.9 (3)
O1ⁱ—Na1—Zn1^v	91.58 (8)	Mg1^xi—B1—Na1^xii	85.69 (13)
O9ⁱⁱ—Na1—Zn1^v	32.00 (6)	O5—B2—O4	124.3 (4)
O4—Na1—Zn1^v	56.24 (7)	O5—B2—O3	117.3 (4)
O7—Na1—Zn1^v	112.11 (8)	O4—B2—O3	118.4 (3)
O3ⁱⁱⁱ—Na1—Zn1^v	131.28 (9)	O5—B2—Mg1^v	39.4 (2)
B4ⁱⁱ—Na1—Zn1^v	50.99 (9)	O4—B2—Mg1^v	86.2 (3)
B1ⁱ—Na1—Zn1^v	72.70 (9)	O3—B2—Mg1^v	153.3 (3)
B3—Na1—Zn1^v	83.71 (9)	O5—B2—Na3^xiii	49.38 (19)
B2—Na1—Zn1^v	48.41 (9)	O4—B2—Na3^xiii	162.9 (3)
B2ⁱⁱⁱ—Na1—Zn1^v	155.55 (10)	O3—B2—Na3^xiii	70.5 (2)
Na3^iv—Na1—Zn1^v	133.71 (6)	Mg1^v—B2—Na3^xiii	88.71 (12)
O2^vi—Na2—O6ⁱⁱⁱ	96.54 (11)	O5—B2—Na1	93.5 (3)
O2^vi—Na2—O10ⁱⁱ	90.74 (11)	O4—B2—Na1	50.1 (2)
O6ⁱⁱⁱ—Na2—O10ⁱⁱ	71.31 (11)	O3—B2—Na1	128.7 (3)
O2^vi—Na2—O6^vi	58.14 (9)	Mg1^v—B2—Na1	74.21 (12)
O6ⁱⁱⁱ—Na2—O6^vi	107.09 (11)	Na3^xiii—B2—Na1	112.80 (14)
O10ⁱⁱ—Na2—O6^vi	148.77 (12)	O5—B2—Na1^v	82.7 (3)
O2^vi—Na2—O4ⁱⁱⁱ	130.80 (11)	O4—B2—Na1^v	128.3 (3)
O6ⁱⁱⁱ—Na2—O4ⁱⁱⁱ	56.64 (10)	O3—B2—Na1^v	57.7 (2)
O10ⁱⁱ—Na2—O4ⁱⁱⁱ	113.16 (12)	Mg1^v—B2—Na1^v	99.65 (14)
O6^vi—Na2—O4ⁱⁱⁱ	88.79 (10)	Na3^xiii—B2—Na1^v	68.60 (11)
O2^vi—Na2—O10	106.68 (11)	Na1—B2—Na1^v	173.51 (18)
O6ⁱⁱⁱ—Na2—O10	142.66 (11)	O2—B3—O4	110.8 (3)
O10ⁱⁱ—Na2—O10	135.35 (14)	O2—B3—O6	108.5 (3)
O6^vi—Na2—O10	64.51 (10)	O4—B3—O6	108.5 (3)
O4ⁱⁱⁱ—Na2—O10	86.21 (10)	O2—B3—O7	109.2 (3)
O2^vi—Na2—O8	92.86 (10)	O4—B3—O7	109.8 (3)
O6ⁱⁱⁱ—Na2—O8	158.26 (12)	O6—B3—O7	110.1 (3)
O10ⁱⁱ—Na2—O8	89.05 (11)	O2—B3—Na2^xiv	50.63 (17)
O6^vi—Na2—O8	94.52 (10)	O4—B3—Na2^xiv	125.5 (3)
O4ⁱⁱⁱ—Na2—O8	127.91 (10)	O6—B3—Na2^xiv	57.85 (19)
O10—Na2—O8	50.26 (9)	O7—B3—Na2^xiv	124.7 (3)
O2^vi—Na2—B5	113.27 (13)	O2—B3—Na2^v	115.0 (2)
O6ⁱⁱⁱ—Na2—B5	150.17 (13)	O4—B3—Na2^v	59.70 (19)
O10ⁱⁱ—Na2—B5	108.08 (13)	O6—B3—Na2^v	49.99 (18)
O6^vi—Na2—B5	88.55 (12)	O7—B3—Na2^v	135.4 (3)
O4ⁱⁱⁱ—Na2—B5	99.71 (12)	Na2^xiv—B3—Na2^v	81.82 (11)
O10—Na2—B5	27.27 (11)	O2—B3—Na1	129.4 (2)
O8—Na2—B5	28.79 (11)	O4—B3—Na1	52.65 (19)
O2^vi—Na2—B3^vi	28.69 (10)	O6—B3—Na1	122.0 (3)
O6ⁱⁱⁱ—Na2—B3^vi	103.26 (12)	O7—B3—Na1	57.23 (19)
O10ⁱⁱ—Na2—B3^vi	119.39 (12)	Na2^xiv—B3—Na1	178.11 (17)
O6^vi—Na2—B3^vi	29.45 (10)	Na2^v—B3—Na1	96.73 (14)
O4ⁱⁱⁱ—Na2—B3^vi	111.38 (12)	O9—B4—O6	123.5 (4)
O10—Na2—B3^vi	85.69 (12)	O9—B4—O8	119.1 (3)
O8—Na2—B3^vi	94.37 (12)	O6—B4—O8	117.3 (3)
B5—Na2—B3^vi	102.52 (14)	O9—B4—Mg1^xiv	37.62 (17)
O2^vi—Na2—B3ⁱⁱⁱ	118.64 (12)	O6—B4—Mg1^xiv	86.7 (2)
O6ⁱⁱⁱ—Na2—B3ⁱⁱⁱ	28.33 (10)	O8—B4—Mg1^xiv	153.5 (3)
O10ⁱⁱ—Na2—B3ⁱⁱⁱ	89.67 (13)	O9—B4—Na1^x	51.42 (19)
O6^vi—Na2—B3ⁱⁱⁱ	102.61 (12)	O6—B4—Na1^x	141.5 (3)
O4ⁱⁱⁱ—Na2—B3ⁱⁱⁱ	28.79 (10)	O8—B4—Na1^x	79.2 (2)
O10—Na2—B3ⁱⁱⁱ	114.92 (12)	Mg1^xiv—B4—Na1^x	74.69 (11)
O8—Na2—B3ⁱⁱⁱ	148.49 (12)	O10—B5—O7	122.5 (4)
B5—Na2—B3ⁱⁱⁱ	124.60 (13)	O10—B5—O8	119.1 (4)
B3^vi—Na2—B3ⁱⁱⁱ	113.48 (16)	O7—B5—O8	118.3 (3)
O2^vi—Na2—Zn1ⁱⁱ	58.00 (7)	O10—B5—Na2	69.6 (2)
O6ⁱⁱⁱ—Na2—Zn1ⁱⁱ	64.38 (7)	O7—B5—Na2	124.6 (3)
O10ⁱⁱ—Na2—Zn1ⁱⁱ	36.50 (7)	O8—B5—Na2	75.5 (2)
O6^vi—Na2—Zn1ⁱⁱ	113.47 (8)	O10—B5—Na3^x	77.2 (2)
O4ⁱⁱⁱ—Na2—Zn1ⁱⁱ	120.82 (8)	O7—B5—Na3^x	58.0 (2)
O10—Na2—Zn1ⁱⁱ	152.94 (9)	O8—B5—Na3^x	143.1 (3)
O8—Na2—Zn1ⁱⁱ	105.19 (8)	Na2—B5—Na3^x	139.58 (18)
B5—Na2—Zn1ⁱⁱ	132.82 (11)	B1—O1—Mg1^xi	111.1 (2)
B3^vi—Na2—Zn1ⁱⁱ	85.28 (9)	B1—O1—Zn1^xi	111.1 (2)
B3ⁱⁱⁱ—Na2—Zn1ⁱⁱ	92.06 (9)	Mg1^xi—O1—Zn1^xi	0.00 (3)
O2^vi—Na2—Mg1ⁱⁱ	58.00 (7)	B1—O1—Na1^xii	107.6 (2)
O6ⁱⁱⁱ—Na2—Mg1ⁱⁱ	64.38 (7)	Mg1^xi—O1—Na1^xii	133.06 (14)
O10ⁱⁱ—Na2—Mg1ⁱⁱ	36.50 (7)	Zn1^xi—O1—Na1^xii	133.06 (14)
O6^vi—Na2—Mg1ⁱⁱ	113.47 (8)	B1—O1—Na3^xiv	116.2 (2)
O4ⁱⁱⁱ—Na2—Mg1ⁱⁱ	120.82 (8)	Mg1^xi—O1—Na3^xiv	93.93 (11)
O10—Na2—Mg1ⁱⁱ	152.94 (9)	Zn1^xi—O1—Na3^xiv	93.93 (11)
O8—Na2—Mg1ⁱⁱ	105.19 (8)	Na1^xii—O1—Na3^xiv	92.00 (10)
B5—Na2—Mg1ⁱⁱ	132.82 (11)	B1—O2—B3	124.1 (3)
B3^vi—Na2—Mg1ⁱⁱ	85.28 (9)	B1—O2—Na2^xiv	115.9 (2)
B3ⁱⁱⁱ—Na2—Mg1ⁱⁱ	92.06 (9)	B3—O2—Na2^xiv	100.7 (2)
Zn1ⁱⁱ—Na2—Mg1ⁱⁱ	0.000 (19)	B1—O2—Na3^x	102.4 (2)
O5^vii—Na3—O9	115.24 (12)	B3—O2—Na3^x	89.0 (2)
O5^vii—Na3—O7ⁱⁱ	103.12 (12)	Na2^xiv—O2—Na3^x	123.59 (12)
O9—Na3—O7ⁱⁱ	105.71 (11)	B1—O3—B2	120.6 (3)
O5^vii—Na3—O1^vi	104.82 (12)	B1—O3—Na1^v	115.3 (2)
O9—Na3—O1^vi	113.76 (11)	B2—O3—Na1^v	95.6 (2)
O7ⁱⁱ—Na3—O1^vi	113.93 (11)	B1—O3—Na3^xiii	151.6 (2)
O5^vii—Na3—O3^vii	54.07 (9)	B2—O3—Na3^xiii	80.6 (2)
O9—Na3—O3^vii	78.29 (10)	Na1^v—O3—Na3^xiii	77.62 (8)
O7ⁱⁱ—Na3—O3^vii	154.12 (11)	B2—O4—B3	125.7 (3)
O1^vi—Na3—O3^vii	86.29 (10)	B2—O4—Na1	104.9 (3)
O5^vii—Na3—B5ⁱⁱ	130.45 (14)	B3—O4—Na1	99.2 (2)
O9—Na3—B5ⁱⁱ	97.41 (13)	B2—O4—Na2^v	109.9 (3)
O7ⁱⁱ—Na3—B5ⁱⁱ	29.12 (11)	B3—O4—Na2^v	91.5 (2)
O1^vi—Na3—B5ⁱⁱ	93.56 (12)	Na1—O4—Na2^v	127.18 (12)
O3^vii—Na3—B5ⁱⁱ	175.18 (13)	B2—O5—Mg1^v	114.9 (3)
O5^vii—Na3—O10ⁱⁱ	138.21 (12)	B2—O5—Zn1^v	114.9 (3)
O9—Na3—O10ⁱⁱ	104.75 (10)	Mg1^v—O5—Zn1^v	0.00 (3)
O7ⁱⁱ—Na3—O10ⁱⁱ	52.34 (9)	B2—O5—Na3^xiii	104.6 (3)
O1^vi—Na3—O10ⁱⁱ	67.33 (9)	Mg1^v—O5—Na3^xiii	140.35 (15)
O3^vii—Na3—O10ⁱⁱ	152.54 (10)	Zn1^v—O5—Na3^xiii	140.35 (15)
B5ⁱⁱ—Na3—O10ⁱⁱ	26.39 (11)	B4—O6—B3	126.6 (3)
O5^vii—Na3—O2ⁱⁱ	86.84 (11)	B4—O6—Na2^v	116.6 (2)
O9—Na3—O2ⁱⁱ	68.39 (9)	B3—O6—Na2^v	101.7 (2)
O7ⁱⁱ—Na3—O2ⁱⁱ	52.57 (9)	B4—O6—Na2^xiv	108.7 (2)
O1^vi—Na3—O2ⁱⁱ	164.65 (10)	B3—O6—Na2^xiv	92.7 (2)
O3^vii—Na3—O2ⁱⁱ	108.84 (9)	Na2^v—O6—Na2^xiv	106.97 (11)
B5ⁱⁱ—Na3—O2ⁱⁱ	71.15 (11)	B5—O7—B3	122.6 (3)
O10ⁱⁱ—Na3—O2ⁱⁱ	97.33 (9)	B5—O7—Na3^x	92.9 (2)
O5^vii—Na3—B2^vii	26.00 (12)	B3—O7—Na3^x	108.9 (2)
O9—Na3—B2^vii	94.71 (13)	B5—O7—Na1	123.2 (3)
O7ⁱⁱ—Na3—B2^vii	126.27 (13)	B3—O7—Na1	94.1 (2)
O1^vi—Na3—B2^vii	101.24 (12)	Na3^x—O7—Na1	116.11 (12)
O3^vii—Na3—B2^vii	28.88 (11)	B4—O8—B5	121.6 (3)
B5ⁱⁱ—Na3—B2^vii	155.19 (14)	B4—O8—Na2	133.4 (3)
O10ⁱⁱ—Na3—B2^vii	160.11 (13)	B5—O8—Na2	75.8 (2)
O2ⁱⁱ—Na3—B2^vii	93.60 (12)	B4—O9—Mg1^xiv	118.1 (2)
O5^vii—Na3—Mg1ⁱⁱ	113.38 (10)	B4—O9—Zn1^xiv	118.1 (2)
O9—Na3—Mg1ⁱⁱ	129.07 (9)	Mg1^xiv—O9—Zn1^xiv	0.00 (4)
O7ⁱⁱ—Na3—Mg1ⁱⁱ	76.74 (8)	B4—O9—Na3	116.4 (2)
O1^vi—Na3—Mg1ⁱⁱ	37.22 (6)	Mg1^xiv—O9—Na3	109.23 (12)
O3^vii—Na3—Mg1ⁱⁱ	121.18 (8)	Zn1^xiv—O9—Na3	109.23 (12)
B5ⁱⁱ—Na3—Mg1ⁱⁱ	59.94 (10)	B4—O9—Na1^x	102.8 (2)
O10ⁱⁱ—Na3—Mg1ⁱⁱ	36.55 (6)	Mg1^xiv—O9—Na1^x	108.08 (12)
O2ⁱⁱ—Na3—Mg1ⁱⁱ	128.91 (8)	Zn1^xiv—O9—Na1^x	108.08 (12)
B2^vii—Na3—Mg1ⁱⁱ	125.45 (11)	Na3—O9—Na1^x	100.09 (11)
O5^vii—Na3—Zn1ⁱⁱ	113.38 (10)	B5—O10—Zn1	140.1 (3)
O9—Na3—Zn1ⁱⁱ	129.07 (9)	B5—O10—Na2^x	122.0 (3)
O7ⁱⁱ—Na3—Zn1ⁱⁱ	76.74 (8)	Zn1—O10—Na2^x	96.72 (12)
O1^vi—Na3—Zn1ⁱⁱ	37.22 (6)	B5—O10—Na2	83.1 (3)
O3^vii—Na3—Zn1ⁱⁱ	121.18 (8)	Zn1—O10—Na2	99.08 (13)
B5ⁱⁱ—Na3—Zn1ⁱⁱ	59.94 (10)	Na2^x—O10—Na2	102.12 (11)
O10ⁱⁱ—Na3—Zn1ⁱⁱ	36.55 (6)	B5—O10—Na3^x	76.5 (2)
O2ⁱⁱ—Na3—Zn1ⁱⁱ	128.91 (8)	Zn1—O10—Na3^x	82.76 (11)
B2^vii—Na3—Zn1ⁱⁱ	125.45 (11)	Na2^x—O10—Na3^x	108.41 (13)
Mg1ⁱⁱ—Na3—Zn1ⁱⁱ	0.000 (17)	Na2—O10—Na3^x	149.01 (13)
O5^vii—Na3—Na1^viii	66.25 (9)

Funding information

Financial support by the National Natural Science Foundation of China (grant No. 20871012) is gratefully acknowledged.

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Volume 73| Part 11| November 2017| Pages 1774-1778

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