Bis[N-methyl­piperidinium(2+)] di-μ-chloro-bis­[tetra­chloro­bismuthate(III)] dihydrate

In the title compound, (C₅H₁₄N₂)₂[Bi₂Cl₁₀]·2H₂O, each Bi^III atom of the centrosymmetric anion is six-coordinate in a distorted octa­hedral geometry. The salt adopts a three-dimensional network arising from the hydrogen bonds between the cations, anions and water mol­ecules.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.027
• wR factor = 0.064
• Data-to-parameter ratio = 25.1

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X)  Bi1    -   Cl1_a   ..      16.40 su
PLAT420_ALERT_2_B D-H Without Acceptor       O1W    -   H1W1   ...          ?

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
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.90
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Bi1    -   Cl1     ..       9.53 su
PLAT480_ALERT_4_C Long H...A H-Bond Reported H1W1   ..  CL3     ..       3.00 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          4

Alert level G
ABSTM02_ALERT_3_G  When printed, the submitted absorption T values will be
            replaced by the scaled T values. Since the ratio of scaled T's
            is identical to the ratio of reported T values, the scaling
            does not imply a change to the absorption corrections used in
            the study.
            Ratio of Tmax expected/reported      0.897
            Tmax scaled      0.452 Tmin scaled      0.164

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

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 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
   3 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Bis[N-methylpiperidinium(2+)] di-µ-chloro-bis[tetrachlorobismuthate(III)] dihydrate

Crystal data

(C5H14N2)2[Bi2Cl10]·2H2O	F(000) = 944
Mr = 1012.86	Dx = 2.351 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 3612 reflections
a = 7.7443 (6) Å	θ = 2.2–28.2°
b = 18.550 (2) Å	µ = 13.23 mm^−1
c = 9.9726 (8) Å	T = 295 K
β = 92.925 (1)°	Block, colorless
V = 1430.8 (2) Å^3	0.31 × 0.09 × 0.06 mm
Z = 2

Data collection

Bruker APEX area-detector diffractometer	3219 independent reflections
Radiation source: fine-focus sealed tube	2724 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.030
φ and ω scans	θmax = 27.5°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −10→7
Tmin = 0.183, Tmax = 0.504	k = −21→23
9046 measured reflections	l = −12→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)] = 0.027	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.064	H-atom parameters constrained
S = 1.01	w = 1/[σ^2(Fo^2) + (0.0326P)^2] where P = (Fo^2 + 2Fc^2)/3
3219 reflections	(Δ/σ)max = 0.001
128 parameters	Δρmax = 1.78 e Å^−3
0 restraints	Δρmin = −0.93 e Å^−3

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

	x	y	z	Uiso*/Ueq
Bi1	0.52096 (2)	0.40831 (1)	0.62536 (2)	0.03328 (7)
Cl1	0.2510 (2)	0.49955 (7)	0.5175 (1)	0.0427 (3)
Cl2	0.7876 (2)	0.32776 (7)	0.6832 (1)	0.0511 (3)
Cl3	0.3186 (2)	0.33389 (7)	0.7741 (1)	0.0490 (3)
Cl4	0.5779 (2)	0.49496 (8)	0.8297 (1)	0.0573 (4)
Cl5	0.4211 (2)	0.31313 (7)	0.4240 (1)	0.0435 (3)
O1w	0.0223 (5)	0.4698 (2)	0.7953 (4)	0.061 (1)
N1	−0.1117 (6)	0.6074 (2)	0.7515 (4)	0.043 (1)
N2	0.1893 (5)	0.6761 (2)	0.8749 (4)	0.037 (1)
C1	0.1881 (7)	0.6476 (3)	0.7356 (5)	0.042 (1)
C2	0.0099 (7)	0.6477 (3)	0.6702 (5)	0.044 (1)
C3	−0.1149 (7)	0.6366 (3)	0.8901 (5)	0.046 (1)
C4	0.0664 (7)	0.6358 (3)	0.9562 (5)	0.043 (1)
C5	0.3669 (7)	0.6762 (3)	0.9409 (6)	0.059 (2)
H1w1	0.1206	0.4674	0.8375	0.073*
H1w2	−0.0493	0.4367	0.8208	0.073*
H1n1	−0.0803	0.5607	0.7551	0.052*
H1n2	−0.2186	0.6099	0.7119	0.052*
H2n	0.1529	0.7222	0.8701	0.045*
H1a	0.2328	0.5987	0.7374	0.050*
H1b	0.2635	0.6768	0.6831	0.050*
H2a	−0.0299	0.6971	0.6591	0.053*
H2b	0.0127	0.6260	0.5818	0.053*
H3a	−0.1913	0.6076	0.9422	0.056*
H3b	−0.1588	0.6856	0.8872	0.056*
H4a	0.0642	0.6572	1.0448	0.051*
H4b	0.1054	0.5863	0.9667	0.051*
H5a	0.3619	0.6934	1.0314	0.088*
H5b	0.4404	0.7073	0.8919	0.088*
H5c	0.4127	0.6281	0.9417	0.088*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Bi1	0.0371 (1)	0.0265 (1)	0.0363 (1)	−0.0009 (1)	0.0027 (1)	0.0003 (1)
Cl1	0.0396 (6)	0.0416 (6)	0.0472 (7)	0.0032 (5)	0.0060 (5)	0.0009 (5)
Cl2	0.0499 (8)	0.0421 (7)	0.0603 (8)	0.0113 (6)	−0.0078 (6)	0.0005 (6)
Cl3	0.0564 (8)	0.0386 (6)	0.0533 (7)	−0.0054 (5)	0.0164 (6)	0.0013 (5)
Cl4	0.0765 (10)	0.0484 (7)	0.0483 (7)	−0.0170 (7)	0.0150 (7)	−0.0151 (6)
Cl5	0.0455 (7)	0.0406 (6)	0.0442 (6)	−0.0034 (5)	0.0002 (6)	−0.0073 (5)
O1w	0.063 (3)	0.042 (2)	0.078 (3)	−0.002 (2)	0.015 (2)	0.000 (2)
N1	0.040 (2)	0.042 (2)	0.047 (2)	−0.008 (2)	−0.005 (2)	−0.002 (2)
N2	0.040 (2)	0.027 (2)	0.044 (2)	0.002 (2)	0.001 (2)	−0.004 (2)
C1	0.042 (3)	0.041 (3)	0.043 (3)	0.001 (2)	0.011 (2)	−0.001 (2)
C2	0.054 (3)	0.043 (3)	0.036 (3)	−0.006 (2)	0.001 (2)	0.002 (2)
C3	0.049 (3)	0.043 (3)	0.048 (3)	−0.004 (2)	0.012 (3)	−0.004 (2)
C4	0.055 (3)	0.034 (3)	0.040 (3)	−0.004 (2)	0.003 (2)	−0.001 (2)
C5	0.041 (3)	0.056 (3)	0.077 (4)	0.004 (3)	−0.014 (3)	−0.009 (3)

Geometric parameters (Å, º)

Bi1—Cl1	2.857 (1)	N1—H1n1	0.90
Bi1—Cl1^i	2.885 (1)	N1—H1n2	0.90
Bi1—Cl2	2.590 (1)	N2—H2n	0.900
Bi1—Cl3	2.608 (1)	C1—H1a	0.97
Bi1—Cl4	2.615 (1)	C1—H1b	0.97
Bi1—Cl5	2.755 (1)	C2—H2a	0.97
N1—C2	1.477 (6)	C2—H2b	0.97
N1—C3	1.486 (6)	C3—H3a	0.97
N2—C4	1.484 (6)	C3—H3b	0.97
N2—C1	1.486 (6)	C4—H4a	0.97
N2—C5	1.494 (6)	C4—H4b	0.97
C1—C2	1.496 (7)	C5—H5a	0.96
C3—C4	1.521 (7)	C5—H5b	0.96
O1w—H1w1	0.85	C5—H5c	0.96
O1w—H1w2	0.87
Cl1—Bi1—Cl1^i	85.28 (4)	C4—N2—H2n	107.5
Cl1—Bi1—Cl2	170.19 (4)	C1—N2—H2n	107.5
Cl1—Bi1—Cl3	94.49 (4)	C5—N2—H2n	107.5
Cl1—Bi1—Cl4	91.17 (5)	N2—C1—H1a	109.3
Cl1—Bi1—Cl5	86.12 (4)	C2—C1—H1a	109.3
Cl1^i—Bi1—Cl2	87.17 (4)	N2—C1—H1b	109.3
Cl1^i—Bi1—Cl3	174.37 (4)	C2—C1—H1b	109.3
Cl1^i—Bi1—Cl4	86.42 (4)	H1a—C1—H1b	108.0
Cl1^i—Bi1—Cl5	100.13 (4)	N1—C2—H2a	109.4
Cl2—Bi1—Cl3	93.64 (5)	C1—C2—H2a	109.4
Cl2—Bi1—Cl4	94.60 (5)	N1—C2—H2b	109.4
Cl2—Bi1—Cl5	89.05 (4)	C1—C2—H2b	109.4
Cl3—Bi1—Cl4	87.97 (4)	H2a—C2—H2b	108.0
Cl3—Bi1—Cl5	85.46 (4)	N1—C3—H3a	109.7
Cl4—Bi1—Cl5	172.67 (4)	C4—C3—H3a	109.7
Bi1—Cl1—Bi1^i	94.72 (4)	N1—C3—H3b	109.7
C2—N1—C3	111.6 (4)	C4—C3—H3b	109.7
C4—N2—C1	110.9 (4)	H3a—C3—H3b	108.2
C4—N2—C5	111.2 (4)	N2—C4—H4a	109.4
C1—N2—C5	111.9 (4)	C3—C4—H4a	109.4
N2—C1—C2	111.6 (4)	N2—C4—H4b	109.4
N1—C2—C1	111.1 (4)	C3—C4—H4b	109.4
N1—C3—C4	109.9 (4)	H4a—C4—H4b	108.0
N2—C4—C3	111.2 (4)	N2—C5—H5a	109.5
H1w1—O1w—H1w2	112.6	N2—C5—H5b	109.5
C2—N1—H1n1	109.3	H5a—C5—H5b	109.5
C3—N1—H1n1	109.3	N2—C5—H5c	109.5
C2—N1—H1n2	109.3	H5a—C5—H5c	109.5
C3—N1—H1n2	109.3	H5b—C5—H5c	109.5
H1n1—N1—H1n2	108.0
Cl3—Bi1—Cl1—Bi1^i	174.36 (4)	C3—N1—C2—C1	56.6 (5)
Cl4—Bi1—Cl1—Bi1^i	86.31 (4)	N2—C1—C2—N1	−55.5 (5)
Cl5—Bi1—Cl1—Bi1^i	−100.51 (4)	C2—N1—C3—C4	−56.5 (5)
Cl1^i—Bi1—Cl1—Bi1^i	0.0	C1—N2—C4—C3	−55.6 (5)
C4—N2—C1—C2	55.2 (5)	C5—N2—C4—C3	179.2 (4)
C5—N2—C1—C2	−179.9 (4)	N1—C3—C4—N2	56.1 (5)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H1w2···Cl2^ii	0.87	2.72	3.360 (4)	131
O1w—H1w1···Cl3	0.85	3.00	3.423 (4)	113
N1—H1n1···O1w	0.90	1.90	2.781 (6)	167
N1—H1n2···Cl5^iii	0.90	2.47	3.248 (5)	145
N2—H2n···Cl3^iv	0.90	2.54	3.281 (4)	140

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