Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
Colourless crystals of the title compound, catena-poly[hemi­(piperazine-1,4-diium) [boron-di-μ-hydrogenphosphato-κ4O:O′]], [C4H12N22+·B2(HPO4)4]n or [C4H12N22+·H8B4O32P8]n, were prepared under solvothermal conditions. The structure contains infinite borophosphate double chains, which are inter­connected by piperazinium cations via a complex hydrogen-bond network to form a three-dimensional supra­molecular network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680701029X/cf2088sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680701029X/cf2088Isup2.hkl
Contains datablock I

CCDC reference: 642938

Key indicators

  • Single-crystal X-ray study
  • T = 291 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.032
  • wR factor = 0.084
  • Data-to-parameter ratio = 11.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 200 Deg. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.20 Ratio
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2000); software used to prepare material for publication: SHELXTL.

catena-poly[hemi(piperazine-1,4-diium) [boron-di-µ-hydrogenphosphato- κ4O:O']] top
Crystal data top
C4H12N22+·H4B2O16P42Z = 2
Mr = 493.69F(000) = 504
Triclinic, P1Dx = 2.107 Mg m3
a = 7.3433 (10) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.1179 (13) ÅCell parameters from 2443 reflections
c = 10.5228 (14) Åθ = 2.8–28.2°
α = 89.510 (2)°µ = 0.58 mm1
β = 84.514 (2)°T = 291 K
γ = 88.697 (2)°Block, colourless
V = 778.03 (18) Å30.25 × 0.09 × 0.08 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
2876 independent reflections
Radiation source: fine-focus sealed tube2424 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
φ and ω scansθmax = 25.5°, θmin = 2.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
h = 88
Tmin = 0.870, Tmax = 0.957k = 1212
5963 measured reflectionsl = 1212
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.084H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0406P)2 + 0.712P]
where P = (Fo2 + 2Fc2)/3
2876 reflections(Δ/σ)max < 0.001
257 parametersΔρmax = 0.35 e Å3
0 restraintsΔρmin = 0.43 e Å3
Special details top

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 (Å2) top
xyzUiso*/Ueq
P10.42963 (8)0.50205 (6)0.67864 (6)0.01232 (16)
P20.06302 (8)0.30552 (6)0.44962 (6)0.01184 (16)
P30.56363 (9)0.81378 (6)0.97631 (6)0.01386 (17)
P40.98552 (8)1.06796 (6)0.81318 (6)0.01277 (16)
B10.2375 (4)0.5449 (3)0.4661 (3)0.0131 (6)
B20.7594 (4)1.0311 (3)1.0326 (3)0.0134 (6)
O10.4829 (3)0.64730 (17)0.69034 (18)0.0203 (4)
H10.52790.65750.75790.030*
O20.3670 (2)0.43791 (18)0.80281 (17)0.0206 (4)
O30.2685 (2)0.50034 (17)0.59469 (16)0.0174 (4)
O40.4075 (2)0.57938 (16)0.38951 (17)0.0166 (4)
O50.1243 (2)0.66728 (17)0.47089 (16)0.0160 (4)
O60.1416 (2)0.44118 (16)0.40246 (16)0.0139 (4)
O70.1839 (2)0.22481 (17)0.52817 (17)0.0176 (4)
O80.0244 (3)0.23977 (18)0.32408 (17)0.0227 (4)
H80.05360.16120.32630.034*
O90.6164 (3)0.69944 (18)0.89065 (19)0.0262 (5)
O100.4918 (3)0.7706 (2)1.11273 (19)0.0269 (5)
H100.54820.70401.13290.040*
O110.7342 (2)0.89789 (17)0.98443 (18)0.0189 (4)
O120.8617 (2)1.02598 (17)1.14493 (16)0.0172 (4)
O130.5861 (2)1.09856 (17)1.07686 (16)0.0156 (4)
O140.8575 (2)1.10984 (17)0.93127 (16)0.0164 (4)
O151.0700 (3)1.20272 (18)0.76941 (17)0.0231 (4)
H151.10071.20080.69240.035*
O160.8975 (2)1.00171 (18)0.70898 (17)0.0209 (4)
N10.9916 (3)0.5199 (2)0.8664 (2)0.0238 (5)
H1A0.93910.55720.80060.029*
H1B1.08720.46950.83390.029*
N20.5450 (3)0.1303 (2)0.5369 (2)0.0291 (6)
H2A0.44710.17740.51520.035*
H2B0.62080.18620.57050.035*
C10.8561 (4)0.4342 (3)0.9410 (3)0.0215 (6)
H1C0.81860.36480.88670.026*
H1D0.74840.48660.97080.026*
C20.9407 (4)0.3738 (3)1.0533 (3)0.0243 (6)
H2C0.85050.32211.10410.029*
H2D1.04170.31521.02320.029*
C30.6406 (4)0.0681 (3)0.4210 (3)0.0251 (6)
H3A0.75080.02210.44290.030*
H3B0.67600.13590.35820.030*
C40.4840 (4)0.0283 (3)0.6347 (3)0.0279 (7)
H4A0.41950.07120.70850.034*
H4B0.58980.01880.66240.034*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
P10.0116 (3)0.0133 (3)0.0119 (3)0.0009 (2)0.0004 (2)0.0001 (2)
P20.0115 (3)0.0104 (3)0.0134 (3)0.0002 (2)0.0003 (2)0.0006 (2)
P30.0127 (3)0.0124 (3)0.0166 (3)0.0003 (3)0.0021 (3)0.0001 (3)
P40.0126 (3)0.0131 (3)0.0128 (3)0.0006 (2)0.0026 (2)0.0007 (2)
B10.0111 (13)0.0119 (14)0.0160 (14)0.0008 (11)0.0002 (11)0.0002 (11)
B20.0104 (13)0.0137 (14)0.0163 (14)0.0002 (11)0.0023 (11)0.0033 (11)
O10.0251 (10)0.0147 (9)0.0217 (10)0.0005 (8)0.0061 (8)0.0032 (8)
O20.0218 (10)0.0227 (10)0.0163 (9)0.0029 (8)0.0022 (8)0.0053 (8)
O30.0150 (9)0.0213 (10)0.0165 (9)0.0027 (7)0.0039 (7)0.0017 (7)
O40.0131 (9)0.0128 (9)0.0228 (10)0.0011 (7)0.0045 (7)0.0006 (7)
O50.0119 (9)0.0133 (9)0.0220 (10)0.0014 (7)0.0024 (7)0.0014 (7)
O60.0143 (9)0.0133 (9)0.0144 (9)0.0024 (7)0.0020 (7)0.0011 (7)
O70.0161 (9)0.0166 (9)0.0193 (9)0.0032 (7)0.0008 (7)0.0028 (7)
O80.0311 (11)0.0158 (10)0.0222 (10)0.0009 (8)0.0072 (8)0.0051 (8)
O90.0249 (10)0.0201 (10)0.0353 (12)0.0061 (8)0.0124 (9)0.0106 (9)
O100.0236 (11)0.0284 (12)0.0268 (11)0.0069 (9)0.0040 (8)0.0124 (9)
O110.0121 (9)0.0151 (9)0.0299 (11)0.0004 (7)0.0038 (8)0.0039 (8)
O120.0145 (9)0.0205 (10)0.0173 (9)0.0043 (7)0.0052 (7)0.0036 (7)
O130.0122 (9)0.0187 (9)0.0158 (9)0.0030 (7)0.0021 (7)0.0015 (7)
O140.0160 (9)0.0139 (9)0.0185 (9)0.0002 (7)0.0025 (7)0.0001 (7)
O150.0325 (11)0.0195 (10)0.0163 (10)0.0044 (8)0.0034 (8)0.0030 (8)
O160.0219 (10)0.0225 (10)0.0202 (10)0.0024 (8)0.0108 (8)0.0056 (8)
N10.0232 (12)0.0299 (13)0.0181 (12)0.0032 (10)0.0018 (10)0.0030 (10)
N20.0218 (13)0.0199 (13)0.0455 (16)0.0042 (10)0.0009 (11)0.0080 (11)
C10.0169 (13)0.0203 (14)0.0272 (15)0.0016 (11)0.0016 (11)0.0029 (12)
C20.0214 (14)0.0184 (14)0.0326 (16)0.0020 (11)0.0001 (12)0.0038 (12)
C30.0190 (14)0.0226 (15)0.0321 (16)0.0009 (11)0.0056 (12)0.0057 (12)
C40.0246 (15)0.0402 (18)0.0189 (14)0.0020 (13)0.0026 (12)0.0013 (13)
Geometric parameters (Å, º) top
P1—O21.4914 (18)O5—P2ii1.5603 (17)
P1—O11.5383 (18)O8—H80.820
P1—O31.5431 (18)O10—H100.820
P1—O4i1.5573 (18)O12—P4iv1.5475 (17)
P2—O71.4947 (18)O13—P3iii1.5405 (17)
P2—O81.5374 (18)O15—H150.820
P2—O61.5597 (17)N1—C11.495 (3)
P2—O5ii1.5603 (17)N1—C2v1.496 (3)
P3—O91.4939 (19)N1—H1A0.900
P3—O111.5398 (18)N1—H1B0.900
P3—O13iii1.5405 (17)N2—C31.486 (4)
P3—O101.544 (2)N2—C41.497 (4)
P4—O161.4955 (18)N2—H2A0.900
P4—O141.5411 (18)N2—H2B0.900
P4—O12iv1.5475 (17)C1—C21.506 (4)
P4—O151.5585 (19)C1—H1C0.970
B1—O31.460 (3)C1—H1D0.970
B1—O41.467 (3)C2—N1v1.497 (3)
B1—O51.474 (3)C2—H2C0.970
B1—O61.477 (3)C2—H2D0.970
B2—O121.460 (3)C3—C4vi1.512 (4)
B2—O111.465 (3)C3—H3A0.970
B2—O131.468 (3)C3—H3B0.970
B2—O141.468 (3)C4—C3vi1.512 (4)
O1—H10.820C4—H4A0.970
O4—P1i1.5572 (18)C4—H4B0.970
O2—P1—O1114.04 (11)P3—O10—H10109.5
O2—P1—O3107.33 (10)B2—O11—P3132.70 (16)
O1—P1—O3107.01 (10)B2—O12—P4iv133.11 (16)
O2—P1—O4i109.78 (10)B2—O13—P3iii139.54 (17)
O1—P1—O4i110.05 (10)B2—O14—P4131.14 (16)
O3—P1—O4i108.42 (10)P4—O15—H15109.5
O7—P2—O8114.12 (11)C1—N1—C2v112.1 (2)
O7—P2—O6115.00 (10)C1—N1—H1A109.2
O8—P2—O6102.30 (10)C2v—N1—H1A109.2
O7—P2—O5ii109.16 (10)C1—N1—H1B109.2
O8—P2—O5ii107.85 (10)C2v—N1—H1B109.2
O6—P2—O5ii107.95 (9)H1A—N1—H1B107.9
O9—P3—O11108.07 (11)C3—N2—C4111.2 (2)
O9—P3—O13iii111.37 (10)C3—N2—H2A109.4
O11—P3—O13iii108.33 (10)C4—N2—H2A109.4
O9—P3—O10112.84 (12)C3—N2—H2B109.4
O11—P3—O10108.50 (11)C4—N2—H2B109.4
O13iii—P3—O10107.62 (10)H2A—N2—H2B108.0
O16—P4—O14116.28 (10)N1—C1—C2109.8 (2)
O16—P4—O12iv107.93 (10)N1—C1—H1C109.7
O14—P4—O12iv109.42 (10)C2—C1—H1C109.7
O16—P4—O15112.34 (11)N1—C1—H1D109.7
O14—P4—O15101.35 (10)C2—C1—H1D109.7
O12iv—P4—O15109.28 (11)H1C—C1—H1D108.2
O3—B1—O4112.6 (2)N1v—C2—C1110.0 (2)
O3—B1—O5110.6 (2)N1v—C2—H2C109.7
O4—B1—O5104.90 (19)C1—C2—H2C109.7
O3—B1—O6109.1 (2)N1v—C2—H2D109.7
O4—B1—O6110.6 (2)C1—C2—H2D109.7
O5—B1—O6108.9 (2)H2C—C2—H2D108.2
O12—B2—O11110.9 (2)N2—C3—C4vi109.9 (2)
O12—B2—O13104.4 (2)N2—C3—H3A109.7
O11—B2—O13113.0 (2)C4vi—C3—H3A109.7
O12—B2—O14110.0 (2)N2—C3—H3B109.7
O11—B2—O14109.0 (2)C4vi—C3—H3B109.7
O13—B2—O14109.6 (2)H3A—C3—H3B108.2
P1—O1—H1109.5N2—C4—C3vi110.1 (2)
B1—O3—P1135.78 (16)N2—C4—H4A109.6
B1—O4—P1i134.29 (16)C3vi—C4—H4A109.6
B1—O5—P2ii128.08 (16)N2—C4—H4B109.6
B1—O6—P2132.53 (16)C3vi—C4—H4B109.6
P2—O8—H8109.5H4A—C4—H4B108.2
O4—B1—O3—P112.7 (3)O14—B2—O11—P3124.9 (2)
O5—B1—O3—P1104.3 (2)O9—P3—O11—B2166.8 (2)
O6—B1—O3—P1135.9 (2)O13iii—P3—O11—B246.0 (2)
O2—P1—O3—B1179.7 (2)O10—P3—O11—B270.6 (2)
O1—P1—O3—B157.5 (3)O11—B2—O12—P4iv32.2 (3)
O4i—P1—O3—B161.2 (3)O13—B2—O12—P4iv154.16 (17)
O3—B1—O4—P1i74.6 (3)O14—B2—O12—P4iv88.4 (3)
O5—B1—O4—P1i165.11 (17)O12—B2—O13—P3iii151.9 (2)
O6—B1—O4—P1i47.8 (3)O11—B2—O13—P3iii87.5 (3)
O3—B1—O5—P2ii51.5 (3)O14—B2—O13—P3iii34.2 (3)
O4—B1—O5—P2ii173.21 (15)O12—B2—O14—P498.3 (2)
O6—B1—O5—P2ii68.4 (3)O11—B2—O14—P423.5 (3)
O3—B1—O6—P24.1 (3)O13—B2—O14—P4147.55 (17)
O4—B1—O6—P2128.56 (19)O16—P4—O14—B270.1 (2)
O5—B1—O6—P2116.7 (2)O12iv—P4—O14—B252.4 (2)
O7—P2—O6—B143.1 (2)O15—P4—O14—B2167.8 (2)
O8—P2—O6—B1167.4 (2)C2v—N1—C1—C257.4 (3)
O5ii—P2—O6—B179.0 (2)N1—C1—C2—N1v56.2 (3)
O12—B2—O11—P3113.9 (2)C4—N2—C3—C4vi57.8 (3)
O13—B2—O11—P32.8 (3)C3—N2—C4—C3vi57.9 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1; (iii) x+1, y+2, z+2; (iv) x+2, y+2, z+2; (v) x+2, y+1, z+2; (vi) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···O90.821.662.474 (3)173
O8—H8···O16i0.821.712.516 (3)165
O10—H10···O2vii0.821.712.522 (3)169
O15—H15···O7viii0.821.792.605 (3)170
N1—H1B···O2ix0.902.072.878 (3)149
N1—H1A···O6i0.902.273.100 (3)153
N1—H1A···O8i0.902.433.145 (3)136
N2—H2A···O70.901.972.807 (3)154
N2—H2B···O4i0.902.413.080 (3)131
N2—H2B···O5i0.902.423.207 (3)146
Symmetry codes: (i) x+1, y+1, z+1; (vii) x+1, y+1, z+2; (viii) x+1, y+1, z; (ix) x+1, y, z.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds