Poly[propane-1,3-diammonium hydroxy­deca-μ₂-oxo-penta­borate]

The title compound, {C₃H₁₂N₂²⁺·B₅O₈(OH)²⁻}_n, has been synthesized under mild solvothermal conditions in the presence of 1,3-diamino­propane acting as a template. The structure consists of two-dimensional polymeric sheets constructed from [B₅O₈(OH)]²⁻ penta­borate anions. Adjacent borate sheets are linked by O—H...O hydrogen bonds to form a three-dimensional framework with channels running along one direction. The propane-1,3-diammonium cations lie within the channels, inter­acting with the framework through N—H...O hydrogen bonds.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](O-B) = 0.002 Å
• Disorder in main residue
• R factor = 0.033
• wR factor = 0.093
• Data-to-parameter ratio = 11.7

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical .          ?
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         N2
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.15
PLAT301_ALERT_3_C Main Residue  Disorder .........................       4.00 Perc.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          6

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   6 ALERT level C = Check and explain
   2 ALERT level G = General alerts; check

   4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.

Poly[propane-1,3-diammonium hydroxydeca-µ₂-oxo-pentaboron]

Crystal data

C3H12N2^2+·HB5O9^2^−	F(000) = 568
Mr = 275.20	Dx = 1.694 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 2237 reflections
a = 6.7156 (2) Å	θ = 2.3–26.5°
b = 14.8400 (5) Å	µ = 0.15 mm^−1
c = 10.8345 (3) Å	T = 293 K
β = 92.102 (4)°	Prism, colourless
V = 1079.03 (6) Å^3	0.40 × 0.20 × 0.10 mm
Z = 4

Data collection

Siemens SMART CCD diffractometer	2237 independent reflections
Radiation source: fine-focus sealed tube	2010 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.018
φ and ω scans	θmax = 26.5°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −8→8
Tmin = 0.964, Tmax = 0.985	k = −18→12
7427 measured reflections	l = −13→12

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.033	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.093	H-atom parameters constrained
S = 1.06	w = 1/[σ^2(Fo^2) + (0.051P)^2 + 0.4012P] where P = (Fo^2 + 2Fc^2)/3
2237 reflections	(Δ/σ)max < 0.001
191 parameters	Δρmax = 0.22 e Å^−3
6 restraints	Δρmin = −0.29 e Å^−3

Special details

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.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
B1	0.1068 (2)	0.76516 (10)	0.35304 (13)	0.0155 (3)
B2	0.3369 (2)	0.81123 (10)	0.19673 (13)	0.0158 (3)
B3	0.4638 (2)	0.79988 (10)	0.41755 (13)	0.0148 (3)
B4	0.8002 (2)	0.74388 (10)	0.48478 (13)	0.0143 (3)
B5	0.6911 (2)	0.89806 (10)	0.54346 (14)	0.0189 (3)
O1	−0.08109 (14)	0.73765 (7)	0.37134 (8)	0.0189 (2)
O2	0.14807 (14)	0.78488 (8)	0.23107 (9)	0.0256 (3)
O3	0.37762 (13)	0.82227 (7)	0.07624 (8)	0.0187 (2)
O4	0.25421 (13)	0.77310 (7)	0.44157 (8)	0.0167 (2)
O5	0.48060 (14)	0.82559 (7)	0.28509 (8)	0.0214 (2)
O6	0.59465 (13)	0.72856 (6)	0.45188 (8)	0.0162 (2)
O7	0.50417 (14)	0.88338 (6)	0.49191 (9)	0.0199 (2)
O8	0.83695 (13)	0.83542 (7)	0.54017 (9)	0.0205 (2)
O9	0.73653 (17)	0.97780 (8)	0.60137 (12)	0.0365 (3)
H9	0.6450	1.0237	0.5844	0.055*
N1	0.3084 (2)	0.37271 (9)	0.81988 (12)	0.0282 (3)
H1A	0.2081	0.3852	0.8686	0.042*
H1B	0.4130	0.3538	0.8656	0.042*
H1C	0.2711	0.3298	0.7665	0.042*
N2	0.29447 (17)	0.64352 (8)	0.62671 (11)	0.0207 (3)
H2A	0.2104	0.6504	0.6876	0.031*
H2B	0.2711	0.6858	0.5697	0.031*
H2C	0.4191	0.6486	0.6567	0.031*
C1	0.3633 (6)	0.4564 (2)	0.7491 (3)	0.0292 (7)	0.50
H1D	0.4814	0.4450	0.7026	0.035*	0.50
H1E	0.3921	0.5055	0.8061	0.035*	0.50
C2	0.1910 (4)	0.4817 (2)	0.6621 (3)	0.0263 (6)	0.50
H2D	0.0821	0.5058	0.7083	0.032*	0.50
H2E	0.1433	0.4289	0.6171	0.032*	0.50
C3	0.2661 (3)	0.55358 (11)	0.57072 (15)	0.0387 (4)	0.50
H3A	0.3917	0.5335	0.5388	0.046*	0.50
H3B	0.1709	0.5584	0.5015	0.046*	0.50
C1'	0.2575 (7)	0.4648 (2)	0.7689 (3)	0.0363 (9)	0.50
H1D'	0.1164	0.4679	0.7466	0.044*	0.50
H1E'	0.2872	0.5104	0.8310	0.044*	0.50
C2'	0.3780 (5)	0.4816 (2)	0.6568 (3)	0.0318 (7)	0.50
H2D'	0.3947	0.4258	0.6118	0.038*	0.50
H2E'	0.5090	0.5040	0.6819	0.038*	0.50
C3'	0.2661 (3)	0.55358 (11)	0.57072 (15)	0.0387 (4)	0.50
H3A'	0.3199	0.5526	0.4889	0.046*	0.50
H3B'	0.1252	0.5394	0.5632	0.046*	0.50

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
B1	0.0148 (7)	0.0181 (7)	0.0136 (7)	0.0018 (5)	0.0012 (5)	−0.0007 (5)
B2	0.0146 (7)	0.0186 (7)	0.0141 (7)	−0.0007 (5)	0.0012 (5)	−0.0006 (5)
B3	0.0125 (6)	0.0196 (7)	0.0122 (7)	−0.0016 (5)	−0.0002 (5)	0.0004 (5)
B4	0.0123 (6)	0.0181 (7)	0.0125 (6)	0.0005 (5)	0.0005 (5)	−0.0002 (5)
B5	0.0190 (7)	0.0193 (7)	0.0182 (7)	0.0000 (6)	−0.0023 (6)	−0.0002 (6)
O1	0.0138 (4)	0.0298 (5)	0.0132 (5)	−0.0027 (4)	0.0009 (4)	−0.0013 (4)
O2	0.0145 (5)	0.0496 (7)	0.0125 (5)	−0.0060 (4)	−0.0001 (4)	0.0028 (4)
O3	0.0188 (5)	0.0245 (5)	0.0127 (5)	−0.0070 (4)	0.0007 (4)	−0.0003 (4)
O4	0.0123 (4)	0.0253 (5)	0.0124 (4)	−0.0004 (4)	0.0001 (3)	0.0022 (4)
O5	0.0165 (5)	0.0343 (6)	0.0133 (5)	−0.0075 (4)	−0.0010 (4)	0.0056 (4)
O6	0.0125 (4)	0.0170 (5)	0.0189 (5)	−0.0006 (3)	−0.0003 (4)	−0.0008 (4)
O7	0.0176 (5)	0.0182 (5)	0.0233 (5)	0.0034 (4)	−0.0047 (4)	−0.0029 (4)
O8	0.0146 (4)	0.0209 (5)	0.0258 (5)	−0.0005 (4)	−0.0030 (4)	−0.0052 (4)
O9	0.0302 (6)	0.0222 (6)	0.0556 (8)	0.0053 (5)	−0.0178 (5)	−0.0139 (5)
N1	0.0336 (7)	0.0258 (7)	0.0248 (6)	0.0011 (5)	−0.0040 (5)	0.0059 (5)
N2	0.0180 (5)	0.0228 (6)	0.0215 (6)	0.0015 (5)	0.0004 (4)	0.0041 (5)
C1	0.0262 (18)	0.0315 (18)	0.0296 (19)	−0.0019 (16)	−0.0031 (15)	0.0077 (15)
C2	0.0312 (16)	0.0182 (13)	0.0289 (15)	0.0025 (12)	−0.0066 (12)	0.0011 (12)
C3	0.0734 (13)	0.0227 (8)	0.0200 (7)	0.0082 (8)	0.0026 (8)	−0.0007 (6)
C1'	0.047 (2)	0.0258 (18)	0.037 (2)	0.0124 (18)	0.0127 (19)	0.0077 (14)
C2'	0.0457 (19)	0.0218 (15)	0.0286 (17)	0.0090 (14)	0.0089 (14)	0.0023 (13)
C3'	0.0734 (13)	0.0227 (8)	0.0200 (7)	0.0082 (8)	0.0026 (8)	−0.0007 (6)

Geometric parameters (Å, º)

B1—O1	1.3476 (17)	N1—C1	1.512 (3)
B1—O4	1.3582 (17)	N1—H1A	0.890
B1—O2	1.3913 (17)	N1—H1B	0.890
B2—O5	1.3510 (18)	N1—H1C	0.890
B2—O3	1.3535 (17)	N2—C3	1.476 (2)
B2—O2	1.3909 (17)	N2—H2A	0.890
B3—O6	1.4167 (17)	N2—H2B	0.890
B3—O5	1.4932 (16)	N2—H2C	0.890
B3—O4	1.4945 (16)	C1—C2	1.513 (4)
B3—O7	1.4974 (17)	C1—H1D	0.970
B4—O6	1.4312 (17)	C1—H1E	0.970
B4—O3^i	1.4759 (17)	C2—C3	1.552 (3)
B4—O1^ii	1.4922 (16)	C2—H2D	0.970
B4—O8	1.5018 (17)	C2—H2E	0.970
B5—O8	1.3516 (18)	C3—H3A	0.970
B5—O9	1.3685 (19)	C3—H3B	0.970
B5—O7	1.3728 (18)	C1'—C2'	1.505 (5)
O1—B4^iii	1.4922 (16)	C1'—H1D'	0.970
O3—B4^iv	1.4758 (17)	C1'—H1E'	0.970
O9—H9	0.931	C2'—H2D'	0.970
N1—C1'	1.508 (4)	C2'—H2E'	0.970
O1—B1—O4	125.77 (12)	H1B—N1—H1C	109.5
O1—B1—O2	115.07 (12)	C3—N2—H2A	109.4
O4—B1—O2	119.14 (12)	C3—N2—H2B	109.6
O5—B2—O3	120.01 (12)	H2A—N2—H2B	109.5
O5—B2—O2	119.30 (12)	C3—N2—H2C	109.4
O3—B2—O2	120.69 (12)	H2A—N2—H2C	109.5
O6—B3—O5	112.04 (11)	H2B—N2—H2C	109.5
O6—B3—O4	109.55 (11)	N1—C1—C2	108.9 (3)
O5—B3—O4	109.89 (10)	N1—C1—H1D	109.9
O6—B3—O7	112.25 (10)	C2—C1—H1D	109.9
O5—B3—O7	106.68 (11)	N1—C1—H1E	109.9
O4—B3—O7	106.23 (10)	C2—C1—H1E	109.9
O6—B4—O3^i	111.98 (11)	H1D—C1—H1E	108.3
O6—B4—O1^ii	108.94 (10)	C1—C2—C3	108.0 (2)
O3^i—B4—O1^ii	109.03 (10)	C1—C2—H2D	110.1
O6—B4—O8	112.71 (10)	C3—C2—H2D	110.1
O3^i—B4—O8	106.54 (10)	C1—C2—H2E	110.1
O1^ii—B4—O8	107.47 (10)	C3—C2—H2E	110.1
O8—B5—O9	117.22 (12)	H2D—C2—H2E	108.4
O8—B5—O7	122.20 (13)	N2—C3—C2	113.57 (16)
O9—B5—O7	120.58 (13)	N2—C3—H3A	108.9
B1—O1—B4^iii	129.33 (11)	C2—C3—H3A	108.9
B2—O2—B1	121.92 (11)	N2—C3—H3B	108.9
B2—O3—B4^iv	119.24 (10)	C2—C3—H3B	108.9
B1—O4—B3	124.53 (10)	H3A—C3—H3B	107.7
B2—O5—B3	124.30 (10)	C2'—C1'—N1	108.9 (3)
B3—O6—B4	122.01 (11)	C2'—C1'—H1D'	109.9
B5—O7—B3	119.68 (11)	N1—C1'—H1D'	109.9
B5—O8—B4	121.60 (11)	C2'—C1'—H1E'	109.9
B5—O9—H9	114.0	N1—C1'—H1E'	109.9
C1—N1—H1A	109.5	H1D'—C1'—H1E'	108.3
C1—N1—H1B	109.8	C1'—C2'—H2D'	109.8
H1A—N1—H1B	109.5	C1'—C2'—H2E'	109.8
C1—N1—H1C	109.1	H2D'—C2'—H2E'	108.3
H1A—N1—H1C	109.5
O4—B1—O1—B4^iii	26.9 (2)	O7—B3—O5—B2	−125.60 (13)
O2—B1—O1—B4^iii	−154.40 (12)	O5—B3—O6—B4	82.22 (14)
O5—B2—O2—B1	−5.7 (2)	O4—B3—O6—B4	−155.55 (10)
O3—B2—O2—B1	174.10 (13)	O7—B3—O6—B4	−37.80 (16)
O1—B1—O2—B2	−177.84 (12)	O3^i—B4—O6—B3	149.10 (11)
O4—B1—O2—B2	1.0 (2)	O1^ii—B4—O6—B3	−90.21 (13)
O5—B2—O3—B4^iv	137.98 (13)	O8—B4—O6—B3	28.99 (16)
O2—B2—O3—B4^iv	−41.86 (18)	O8—B5—O7—B3	−6.8 (2)
O1—B1—O4—B3	177.13 (13)	O9—B5—O7—B3	173.56 (13)
O2—B1—O4—B3	−1.6 (2)	O6—B3—O7—B5	25.62 (16)
O6—B3—O4—B1	−117.64 (13)	O5—B3—O7—B5	−97.46 (13)
O5—B3—O4—B1	5.86 (18)	O4—B3—O7—B5	145.33 (11)
O7—B3—O4—B1	120.90 (13)	O9—B5—O8—B4	176.80 (12)
O3—B2—O5—B3	−168.55 (12)	O7—B5—O8—B4	−2.9 (2)
O2—B2—O5—B3	11.3 (2)	O6—B4—O8—B5	−7.12 (17)
O6—B3—O5—B2	111.18 (14)	O3^i—B4—O8—B5	−130.32 (12)
O4—B3—O5—B2	−10.85 (18)	O1^ii—B4—O8—B5	112.93 (13)

Symmetry codes: (i) x+1/2, −y+3/2, z+1/2; (ii) x+1, y, z; (iii) x−1, y, z; (iv) x−1/2, −y+3/2, z−1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O9—H9···O7^v	0.93	1.88	2.7853 (15)	164
N1—H1C···O1^vi	0.89	2.17	3.0120 (16)	157
N1—H1A···O7^vii	0.89	2.12	2.9837 (16)	165
N1—H1B···O8^viii	0.89	1.95	2.8309 (16)	169
N2—H2C···O2^i	0.89	1.97	2.8017 (16)	154
N2—H2B···O4	0.89	1.90	2.7847 (15)	173
N2—H2A···O5^ix	0.89	1.93	2.8041 (15)	165

Symmetry codes: (i) x+1/2, −y+3/2, z+1/2; (v) −x+1, −y+2, −z+1; (vi) −x, −y+1, −z+1; (vii) −x+1/2, y−1/2, −z+3/2; (viii) −x+3/2, y−1/2, −z+3/2; (ix) x−1/2, −y+3/2, z+1/2.