Redetermination of CaB8O11(OH)4 at low temperature

Wiggin, S.B.; Weller, M.T.

doi:10.1107/S1600536805029296

inorganic compounds

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ISSN: 2056-9890

Volume 61| Part 11| November 2005| Pages i243-i245

https://doi.org/10.1107/S1600536805029296

Redetermination of CaB₈O₁₁(OH)₄ at low temperature

Seth B. Wiggin ^a and Mark T. Weller ^a ^*

^aSchool of Chemistry, University of Southampton, Southampton SO17 1BJ, England
^*Correspondence e-mail: mtw@soton.ac.uk

(Received 31 August 2005; accepted 15 September 2005; online 27 October 2005)

The structure of CaB₈O₁₁(OH)₄ (calcium octaborate tetrahydroxide) [Zayakina & Brovkin (1978 ). Kristallografiya, 23, 1167–1170] has been redetermined at 120 (2) K with improved precision. The O—H⋯O hydrogen-bonding arrangement has been established, based on freely refined H-atom positions.

Comment

During the investigation of templated boroarsenate frameworks, single crystals of the known (Zayakina & Brovkin, 1978) title compound, (I) (Fig. 1), were obtained from a molten salt reaction of CaCl₂, H₃BO₃ and NH₄(H₂AsO₄). This redetermination at 120 (2) K offers a significantly better structural model and the H-atom positions and hydrogen-bonding scheme have been established. There is also an isostructural strontium material, strontioborite, reported by Brovkin et al. (1975 ).

The structure of (I) can be described in terms of linked triple six-rings of stoichiometry B₆O₁₂H with a pendant H₃B₂O₅ group, as shown in Fig. 2. The three-coordinate O8 species (Table 1) is a distinctive feature of these units. Each of these triple-six-ring units have six O atoms that do not contribute to the ring formation. One of these forms a hydroxide grouping, four link to further similar units to form a sheet in the bc plane and the last bridges to an H₃B₂O₅ unit that is located outside the plane. The triple six-ring unit has two of the rings in the bc plane, while the third is below this plane. The out-of-plane ring has the hydroxide group attached, forming, along with the pendant H₃B₂O₅ unit, an extensive hydrogen-bonding network between the borate sheets (Table 2). There are six distinct hydrogen bonds per unit, with O⋯O distances ranging from 2.585 (3) to 2.917 (4) Å. This network connects four adjacent B₈O₁₁(OH)₄ units to a central unit, as shown in Fig. 2.

The calcium ion sits in the centre of an 18-atom ring formed by four of the triple six-ring units (Fig. 3). Nine O atoms coordinate to the calcium cation, with Ca—O distances ranging from 2.482 (2) to 2.634 (2) Å (Table 1). Six of these Ca—O bonds arise from the 18-atom ring, and two H₃B₂O₅ units that occur above and below the plane complete the Ca nine-coordination.

Figure 1
The asymmetric unit of (I), showing 50% probability displacement ellipsoids and arbitrary spheres for the H atoms. The mixture of trigonal (B1, B2, B4, B6 and B8) and tetrahedral (B3, B5 and B7) B atoms and the three-coordinate O8 species are evident.

Figure 2
View of the borate unit in (I). Colour key: B blue, O red, and H white. Dotted lines signify hydrogen bonds.

Figure 3
Detail of (I), showing the Ca²⁺ ion within its 18-atom ring. The H₃B₂O₅ units above and below the plane have been removed for clarity. Colour key: Ca green, other atom colours as in Fig. 2

Experimental

Compound (I) was prepared using a molten salt technique. A typical reaction involved grinding H₃BO₃ (0.4637 g, 7.5 mmol), NH₄(H₂AsO₄) (1.1923 g, 7.5 mmol) and CaCl₂ (0.5549 g, 5 mmol) in a pestle and mortar before placing the powder in a 23 ml Parr Teflon-lined steel autoclave and heating to 513 K for 120 h. The product was washed with hot water to dissolve any remaining borate flux, leaving a white powder containing many colourless crystals of (I) in moderate yield (34% based on Ca). The material appears completely air- and water-stable.

Crystal data

CaB₈O₁₁(OH)₄
M_r = 370.59
Monoclinic, P 2₁
a = 7.481 (6) Å
b = 8.2693 (12) Å
c = 9.859 (3) Å
β = 108.76 (6)°
V = 577.5 (5) Å³
Z = 2
D_x = 2.131 Mg m⁻³
Mo Kα radiation
Cell parameters from 2430 reflections
θ = 2.9–27.5°
μ = 0.64 mm⁻¹
T = 120 (2) K
Plate, colourless
0.06 × 0.06 × 0.01 mm

Data collection

Bruker–Nonius KappaCCD area-detector diffractometer
φ and ω scans
Absorption correction: multi-scan(SADABS; Sheldrick, 2003 )T_min = 0.732, T_max = 0.994
13192 measured reflections
2611 independent reflections
2430 reflections with I > 2σ(I)
R_int = 0.059
θ_max = 27.5°
h = −9 → 9
k = −10 → 10
l = −12 → 12

Refinement

Refinement on F²
R[F² > 2σ(F²)] = 0.034
wR(F²) = 0.075
S = 1.05
2611 reflections
233 parameters
All H-atom parameters refined
w = 1/[σ²(F_o²) + (0.0314P)² + 0.2076P] where P = (F_o² + 2F_c²)/3
(Δ/σ)_max < 0.001
Δρ_max = 0.32 e Å⁻³
Δρ_min = −0.40 e Å⁻³
Absolute structure: Flack (1983 ), 1196 Friedel pairs
Flack parameter: 0.03 (3)

Table 1
Selected geometric parameters (Å, °)

Ca1—O1	2.619 (3)
Ca1—O13	2.5329 (18)
Ca1—O15	2.634 (2)
Ca1—O9ⁱ	2.4806 (18)
Ca1—O4ⁱⁱ	2.528 (3)
Ca1—O7ⁱⁱⁱ	2.5610 (19)
Ca1—O10^iv	2.621 (2)
Ca1—O2ⁱⁱ	2.626 (3)
Ca1—O6ⁱ	2.6320 (18)

B5—O8—B7	116.33 (19)
B5—O8—B3	122.88 (18)
B7—O8—B3	120.73 (18)
Symmetry codes: (i) $[-x+1, y+{\script{1\over 2}}, -z+1]$ ; (ii) x+1, y, z; (iii) x, y, z-1; (iv) $[-x+1, y-{\script{1\over 2}}, -z+1]$ .

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O14—H14⋯O5ⁱⁱ	0.98 (4)	1.93 (4)	2.900 (3)	173 (3)
O1—H1⋯O14^v	0.86 (3)	1.95 (3)	2.817 (3)	177 (3)
O2—H2⋯O11^v	0.87 (4)	1.72 (4)	2.585 (3)	172 (4)
O2—H2⋯O7^v	0.87 (4)	2.50 (4)	2.917 (4)	110 (3)
O4—H4⋯O12^vi	0.90 (4)	1.81 (4)	2.695 (3)	171 (4)
O4—H4⋯O13^vi	0.90 (4)	2.27 (4)	2.751 (3)	113 (3)
Symmetry codes: (ii) x+1, y, z; (v) x-1, y, z-1; (vi) x-1, y, z.

The H atoms were found in a difference map and their positions and U_iso values were freely refined.

Data collection: COLLECT (Hooft, 1998 ); cell refinement: DENZO (Otwinowski & Minor, 1997 ) and COLLECT; data reduction: DENZO and COLLECT; method used to solve structure: coordinates taken from Zayakina & Brovkin (1978); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ); molecular graphics: DIAMOND (Brandenburg, 1999 ); software used to prepare material for publication: WinGX (Farrugia, 1999 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536805029296/hb6258sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536805029296/hb6258Isup2.hkl

Computing details top

Data collection: COLLECT (Hooft, 1998); cell refinement: DENZO (Otwinowski & Minor, 1997) and COLLECT; data reduction: DENZO and COLLECT; program(s) used to solve structure: Please specify; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: Please specify.

calcium octaborate tetrahydroxide top

Crystal data top

CaB₈O₁₁(OH)₄	F(000) = 368
M_r = 370.59	D_x = 2.131 Mg m⁻³
Monoclinic, P2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2yb	Cell parameters from 2430 reflections
a = 7.481 (6) Å	θ = 2.9–27.5°
b = 8.2693 (12) Å	µ = 0.64 mm⁻¹
c = 9.859 (3) Å	T = 120 K
β = 108.76 (6)°	Plate, colourless
V = 577.5 (5) Å³	0.06 × 0.06 × 0.01 mm
Z = 2

Data collection top

Bruker–Nonius KappaCCD area-detector diffractometer	2611 independent reflections
Radiation source: Bruker-Nonius FR591 rotating anode	2430 reflections with I > 2σ(I)
10cm confocal mirrors monochromator	R_int = 0.059
Detector resolution: 9.091 pixels mm^-1	θ_max = 27.5°, θ_min = 3°
φ and ω scans	h = −9→9
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	k = −10→10
T_min = 0.732, T_max = 0.994	l = −12→12
13192 measured reflections

Refinement top

Refinement on F²	All H-atom parameters refined
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0314P)² + 0.2076P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.034	(Δ/σ)_max < 0.001
wR(F²) = 0.075	Δρ_max = 0.32 e Å⁻³
S = 1.05	Δρ_min = −0.40 e Å⁻³
2611 reflections	Absolute structure: Flack (1983), 1196 Friedel pairs
233 parameters	Absolute structure parameter: 0.03 (3)
1 restraint

Special details top

Experimental. SADABS was used to perform the Absorption correction Parameter refinement on 11680 reflections reduced R(int) from 0.1212 to 0.0551 Ratio of minimum to maximum apparent transmission: 0.736941 The given Tmin and Tmax were generated using the SHELX SIZE command

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

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

	x	y	z	U_iso*/U_eq
B1	0.1035 (4)	0.2765 (4)	0.2720 (3)	0.0113 (5)
B2	0.0908 (4)	0.2695 (4)	0.5216 (3)	0.0114 (6)
B3	0.3787 (4)	0.1696 (3)	0.7189 (3)	0.0086 (6)
B4	0.4671 (4)	0.1318 (3)	0.9806 (3)	0.0095 (6)
B5	0.5905 (4)	0.3827 (3)	0.9050 (3)	0.0092 (6)
B6	0.8931 (4)	0.3814 (4)	0.8517 (3)	0.0121 (6)
B7	0.5944 (4)	0.3830 (3)	0.6449 (3)	0.0087 (5)
B8	0.4913 (4)	0.1220 (3)	0.5148 (3)	0.0099 (6)
O1	0.2331 (2)	0.3060 (2)	0.20108 (18)	0.0141 (4)
O2	−0.0882 (2)	0.2699 (3)	0.2085 (2)	0.0166 (4)
O3	0.1776 (2)	0.2518 (2)	0.41723 (18)	0.0137 (4)
O4	−0.0921 (3)	0.3203 (3)	0.48254 (19)	0.0202 (5)
O5	0.1892 (2)	0.2394 (2)	0.66179 (18)	0.0116 (4)
O6	0.3931 (2)	0.0722 (2)	0.84528 (18)	0.0105 (4)
O7	0.5296 (2)	0.2872 (2)	1.00614 (16)	0.0102 (3)
O8	0.5214 (2)	0.3078 (2)	0.75752 (16)	0.0092 (3)
O9	0.4256 (2)	0.0600 (2)	0.61924 (18)	0.0094 (4)
O10	0.5179 (2)	0.5466 (2)	0.89685 (18)	0.0108 (4)
O11	0.7977 (2)	0.3809 (2)	0.94971 (17)	0.0124 (4)
O12	0.8015 (2)	0.4038 (2)	0.70949 (18)	0.0117 (4)
O13	0.5652 (2)	0.2750 (2)	0.52450 (17)	0.0101 (4)
O14	1.0848 (3)	0.3566 (3)	0.9032 (2)	0.0190 (4)
O15	0.4999 (2)	0.0372 (2)	0.39748 (18)	0.0107 (4)
Ca1	0.60200 (6)	0.29083 (6)	0.27828 (5)	0.01030 (12)
H1	0.191 (5)	0.320 (4)	0.109 (3)	0.029 (9)*
H2	−0.120 (5)	0.300 (5)	0.119 (4)	0.047 (11)*
H4	−0.127 (6)	0.337 (5)	0.560 (4)	0.061 (14)*
H14	1.130 (6)	0.314 (5)	0.827 (4)	0.054 (12)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
B1	0.0134 (12)	0.0077 (14)	0.0125 (13)	0.0017 (11)	0.0038 (10)	−0.0002 (11)
B2	0.0106 (12)	0.0130 (14)	0.0108 (13)	0.0025 (12)	0.0037 (10)	0.0016 (11)
B3	0.0082 (13)	0.0079 (14)	0.0096 (13)	−0.0014 (10)	0.0028 (11)	−0.0012 (10)
B4	0.0081 (13)	0.0114 (13)	0.0081 (14)	0.0012 (11)	0.0015 (11)	0.0006 (11)
B5	0.0096 (13)	0.0100 (13)	0.0077 (13)	−0.0015 (11)	0.0025 (11)	−0.0010 (11)
B6	0.0111 (14)	0.0117 (14)	0.0125 (14)	−0.0002 (11)	0.0024 (11)	−0.0006 (11)
B7	0.0104 (14)	0.0091 (13)	0.0061 (13)	−0.0001 (11)	0.0017 (11)	−0.0018 (11)
B8	0.0073 (13)	0.0107 (13)	0.0105 (14)	0.0027 (10)	0.0010 (10)	0.0022 (11)
O1	0.0138 (8)	0.0197 (10)	0.0082 (8)	0.0015 (8)	0.0025 (7)	0.0029 (8)
O2	0.0120 (8)	0.0257 (12)	0.0108 (9)	0.0016 (8)	0.0021 (7)	0.0009 (8)
O3	0.0088 (8)	0.0214 (10)	0.0105 (9)	0.0030 (7)	0.0027 (7)	0.0016 (7)
O4	0.0140 (9)	0.0376 (13)	0.0091 (9)	0.0075 (9)	0.0039 (7)	0.0012 (8)
O5	0.0101 (9)	0.0132 (9)	0.0120 (9)	0.0016 (6)	0.0039 (7)	0.0000 (6)
O6	0.0125 (9)	0.0101 (9)	0.0089 (9)	−0.0027 (7)	0.0035 (7)	−0.0001 (7)
O7	0.0130 (8)	0.0085 (7)	0.0094 (7)	0.0003 (9)	0.0040 (6)	−0.0004 (8)
O8	0.0136 (8)	0.0068 (8)	0.0076 (8)	−0.0032 (8)	0.0037 (6)	−0.0010 (7)
O9	0.0113 (9)	0.0088 (9)	0.0086 (8)	−0.0010 (7)	0.0038 (7)	−0.0001 (7)
O10	0.0139 (9)	0.0093 (8)	0.0087 (9)	0.0015 (7)	0.0029 (7)	0.0003 (7)
O11	0.0119 (9)	0.0159 (9)	0.0089 (9)	0.0013 (8)	0.0026 (7)	0.0003 (7)
O12	0.0114 (9)	0.0120 (9)	0.0115 (9)	0.0001 (7)	0.0035 (7)	0.0013 (7)
O13	0.0112 (8)	0.0093 (9)	0.0099 (8)	−0.0012 (8)	0.0038 (6)	−0.0022 (7)
O14	0.0095 (9)	0.0366 (12)	0.0108 (9)	0.0043 (8)	0.0030 (7)	0.0018 (8)
O15	0.0123 (9)	0.0107 (8)	0.0082 (8)	−0.0013 (7)	0.0017 (7)	−0.0013 (7)
Ca1	0.0114 (2)	0.0098 (2)	0.0096 (2)	0.0003 (2)	0.00327 (17)	−0.0004 (2)

Geometric parameters (Å, º) top

B1—O2	1.370 (3)	B8—O15	1.372 (3)
B1—O3	1.374 (3)	B8—O13	1.372 (3)
B1—O1	1.387 (3)	B8—O9	1.375 (3)
B2—O4	1.363 (3)	O1—H1	0.86 (3)
B2—O5	1.364 (3)	O2—H2	0.87 (4)
B2—O3	1.390 (3)	O4—H4	0.90 (4)
B3—O6	1.458 (3)	O14—H14	0.98 (4)
B3—O9	1.460 (3)	O2—Ca1ⁱⁱⁱ	2.626 (3)
B3—O5	1.465 (3)	O4—Ca1ⁱⁱⁱ	2.528 (3)
B3—O8	1.526 (3)	O6—Ca1^iv	2.6320 (18)
B4—O6	1.361 (3)	O7—Ca1^v	2.5610 (19)
B4—O7	1.363 (4)	O9—Ca1^iv	2.4806 (18)
B4—O10ⁱ	1.372 (3)	O10—B4^vi	1.372 (3)
B5—O10	1.452 (3)	O10—Ca1ⁱⁱ	2.621 (2)
B5—O7	1.455 (3)	O15—B7^iv	1.453 (3)
B5—O11	1.469 (3)	Ca1—O1	2.619 (3)
B5—O8	1.511 (3)	Ca1—O13	2.5329 (18)
B6—O12	1.361 (3)	Ca1—O15	2.634 (2)
B6—O11	1.374 (3)	Ca1—O9ⁱⁱ	2.4806 (18)
B6—O14	1.374 (4)	Ca1—O4^vii	2.528 (3)
B7—O13	1.444 (3)	Ca1—O7^viii	2.5610 (19)
B7—O15ⁱⁱ	1.453 (3)	Ca1—O10^iv	2.621 (2)
B7—O12	1.483 (3)	Ca1—O2^vii	2.626 (3)
B7—O8	1.519 (3)	Ca1—O6ⁱⁱ	2.6320 (18)

O2—B1—O3	118.8 (2)	O9ⁱⁱ—Ca1—O4^vii	76.20 (7)
O2—B1—O1	125.2 (2)	O9ⁱⁱ—Ca1—O13	66.86 (6)
O3—B1—O1	116.0 (2)	O4^vii—Ca1—O13	65.85 (8)
O4—B2—O5	120.6 (2)	O9ⁱⁱ—Ca1—O7^viii	114.83 (6)
O4—B2—O3	119.2 (2)	O4^vii—Ca1—O7^viii	131.92 (7)
O5—B2—O3	120.2 (2)	O13—Ca1—O7^viii	162.18 (6)
O6—B3—O9	105.4 (2)	O9ⁱⁱ—Ca1—O1	81.81 (7)
O6—B3—O5	110.0 (2)	O4^vii—Ca1—O1	145.73 (7)
O9—B3—O5	113.5 (2)	O13—Ca1—O1	81.49 (8)
O6—B3—O8	110.3 (2)	O7^viii—Ca1—O1	81.26 (8)
O9—B3—O8	109.42 (19)	O9ⁱⁱ—Ca1—O10^iv	154.72 (6)
O5—B3—O8	108.3 (2)	O4^vii—Ca1—O10^iv	129.02 (7)
O6—B4—O7	122.0 (2)	O13—Ca1—O10^iv	118.17 (6)
O6—B4—O10ⁱ	124.7 (2)	O7^viii—Ca1—O10^iv	52.31 (6)
O7—B4—O10ⁱ	113.3 (2)	O1—Ca1—O10^iv	74.93 (7)
O10—B5—O7	110.5 (2)	O9ⁱⁱ—Ca1—O2^vii	111.21 (6)
O10—B5—O11	111.5 (2)	O4^vii—Ca1—O2^vii	64.27 (8)
O7—B5—O11	108.7 (2)	O13—Ca1—O2^vii	128.64 (8)
O10—B5—O8	108.9 (2)	O7^viii—Ca1—O2^vii	68.41 (8)
O7—B5—O8	110.6 (2)	O1—Ca1—O2^vii	149.66 (6)
O11—B5—O8	106.6 (2)	O10^iv—Ca1—O2^vii	85.45 (7)
O12—B6—O11	121.5 (2)	O9ⁱⁱ—Ca1—O6ⁱⁱ	53.88 (6)
O12—B6—O14	121.4 (2)	O4^vii—Ca1—O6ⁱⁱ	98.03 (7)
O11—B6—O14	117.1 (2)	O13—Ca1—O6ⁱⁱ	120.74 (6)
O13—B7—O15ⁱⁱ	112.0 (2)	O7^viii—Ca1—O6ⁱⁱ	63.58 (6)
O13—B7—O12	106.6 (2)	O1—Ca1—O6ⁱⁱ	89.61 (7)
O15ⁱⁱ—B7—O12	111.4 (2)	O10^iv—Ca1—O6ⁱⁱ	115.40 (6)
O13—B7—O8	110.7 (2)	O2^vii—Ca1—O6ⁱⁱ	78.02 (7)
O15ⁱⁱ—B7—O8	108.32 (19)	O9ⁱⁱ—Ca1—O15	117.30 (6)
O12—B7—O8	107.76 (19)	O4^vii—Ca1—O15	92.26 (7)
O15—B8—O13	113.8 (2)	O13—Ca1—O15	52.77 (6)
O15—B8—O9	124.5 (2)	O7^viii—Ca1—O15	117.66 (7)
O13—B8—O9	121.7 (2)	O1—Ca1—O15	74.82 (7)
B1—O1—H1	118 (2)	O10^iv—Ca1—O15	66.02 (6)
Ca1—O1—H1	108 (2)	O2^vii—Ca1—O15	118.11 (7)
B1—O2—Ca1ⁱⁱⁱ	139.51 (16)	O6ⁱⁱ—Ca1—O15	163.61 (6)
B1—O2—H2	111 (3)	O9ⁱⁱ—Ca1—B8	91.19 (7)
Ca1ⁱⁱⁱ—O2—H2	105 (3)	O4^vii—Ca1—B8	80.44 (8)
B1—O3—B2	128.9 (2)	O13—Ca1—B8	26.40 (7)
B2—O4—Ca1ⁱⁱⁱ	139.90 (17)	O7^viii—Ca1—B8	141.02 (7)
B2—O4—H4	110 (3)	O1—Ca1—B8	74.02 (9)
Ca1ⁱⁱⁱ—O4—H4	105 (3)	O10^iv—Ca1—B8	91.80 (7)
B2—O5—B3	127.0 (2)	O2^vii—Ca1—B8	130.46 (8)
B4—O6—B3	122.2 (2)	O6ⁱⁱ—Ca1—B8	143.67 (7)
B4—O6—Ca1^iv	135.38 (16)	O15—Ca1—B8	26.64 (7)
B3—O6—Ca1^iv	95.79 (13)	O9ⁱⁱ—Ca1—B4^viii	136.70 (7)
B4—O7—B5	123.3 (2)	O4^vii—Ca1—B4^viii	137.46 (8)
B4—O7—Ca1^v	98.58 (15)	O13—Ca1—B4^viii	142.12 (7)
B5—O7—Ca1^v	134.77 (15)	O7^viii—Ca1—B4^viii	26.00 (7)
B5—O8—B7	116.33 (19)	O1—Ca1—B4^viii	75.61 (9)
B5—O8—B3	122.88 (18)	O10^iv—Ca1—B4^viii	26.36 (7)
B7—O8—B3	120.73 (18)	O2^vii—Ca1—B4^viii	76.60 (9)
B8—O9—B3	119.6 (2)	O6ⁱⁱ—Ca1—B4^viii	89.16 (7)
B8—O9—Ca1^iv	137.40 (16)	O15—Ca1—B4^viii	91.85 (7)
B3—O9—Ca1^iv	102.32 (14)	B8—Ca1—B4^viii	116.57 (8)
B4^vi—O10—B5	120.5 (2)	O9ⁱⁱ—Ca1—B3ⁱⁱ	27.05 (6)
B4^vi—O10—Ca1ⁱⁱ	95.64 (15)	O4^vii—Ca1—B3ⁱⁱ	82.49 (7)
B5—O10—Ca1ⁱⁱ	142.95 (15)	O13—Ca1—B3ⁱⁱ	93.55 (7)
B6—O11—B5	121.7 (2)	O7^viii—Ca1—B3ⁱⁱ	90.83 (7)
B6—O12—B7	122.5 (2)	O1—Ca1—B3ⁱⁱ	89.77 (7)
B8—O13—B7	125.3 (2)	O10^iv—Ca1—B3ⁱⁱ	141.33 (7)
B8—O13—Ca1	98.42 (15)	O2^vii—Ca1—B3ⁱⁱ	91.50 (7)
B7—O13—Ca1	136.19 (15)	O6ⁱⁱ—Ca1—B3ⁱⁱ	27.57 (6)
B6—O14—H14	110 (2)	O15—Ca1—B3ⁱⁱ	144.13 (7)
B8—O15—B7^iv	122.8 (2)	B8—Ca1—B3ⁱⁱ	118.24 (8)
B8—O15—Ca1	93.93 (15)	B4^viii—Ca1—B3ⁱⁱ	115.83 (8)
B7^iv—O15—Ca1	138.97 (15)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O14—H14···O5^vii	0.98 (4)	1.93 (4)	2.900 (3)	173 (3)
O1—H1···O14^ix	0.86 (3)	1.95 (3)	2.817 (3)	177 (3)
O2—H2···O11^ix	0.87 (4)	1.72 (4)	2.585 (3)	172 (4)
O2—H2···O7^ix	0.87 (4)	2.50 (4)	2.917 (4)	110 (3)
O4—H4···O12ⁱⁱⁱ	0.90 (4)	1.81 (4)	2.695 (3)	171 (4)
O4—H4···O13ⁱⁱⁱ	0.90 (4)	2.27 (4)	2.751 (3)	113 (3)

Symmetry codes: (iii) x−1, y, z; (vii) x+1, y, z; (ix) x−1, y, z−1.

References

Brandenburg, K. (1999). DIAMOND. Release 2.1a. Crystal Impact GbR, Bonn, Germany. Google Scholar
Brovkin, A. A., Zayakina, N. V. & Brovkina, V. S. (1975). Kristallografiya, 20, 911–916. CAS Google Scholar
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838. CrossRef CAS IUCr Journals Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Hooft, R. W. W. (1998). COLLECT. Nonius BV, Delft, The Netherlands. Google Scholar
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307–326. New York: Academic Press. Google Scholar
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2003). SADABS. Version 2.10. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Zayakina, N. V. & Brovkin, A. A. (1978). Kristallografiya, 23, 1167–1170. CAS Google Scholar

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Volume 61| Part 11| November 2005| Pages i243-i245

https://doi.org/10.1107/S1600536805029296

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