Bis(2,3-dimethyl­anilinium) diaqua­bis[dihydrogendiphosphato(2-)]cobaltate(II)

In the title compound, (C₈H₁₂N)₂[Co(H₂P₂O₇)₂(H₂O)₂], the Co atom is located on an inversion center and is surrounded by two dihydrogendiphosphate ligands and two water mol­ecules in an octa­hedral coordination. The packing is organized in layers containing the cobaltate anions with organic cations arranged in the inter­layer spaces and connected through hydrogen bonds to the anions.

Key indicators

• Single-crystal X-ray study
• T = 296 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.027
• wR factor = 0.076
• Data-to-parameter ratio = 26.3

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Co1    -   O2      ..       5.18 su

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

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

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Computing details

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Bis(2,3-dimethylanilinium) diaquabis[dihydrogendiphosphato(2-)]cobalt(II)

Crystal data

2C8H12N^+·CoH8O16P4^2^−	Z = 1
Mr = 691.25	F(000) = 357
Triclinic, P1	Dx = 1.648 Mg m^−3
Hall symbol: -P 1	Ag Kα radiation, λ = 0.56080 Å
a = 7.420 (4) Å	Cell parameters from 25 reflections
b = 7.502 (5) Å	θ = 8–10°
c = 13.265 (4) Å	µ = 0.48 mm^−1
α = 90.14 (6)°	T = 296 K
β = 102.73 (4)°	Prism, pink
γ = 104.27 (5)°	0.19 × 0.15 × 0.12 mm
V = 696.8 (7) Å^3

Data collection

Enraf–Nonius CAD-4 diffractometer	Rint = 0.008
Radiation source: fine-focus sealed tube	θmax = 25.0°, θmin = 2.2°
Graphite monochromator	h = −11→10
Non–profiled ω scans	k = −11→11
5154 measured reflections	l = 0→19
4968 independent reflections	2 standard reflections every 120 reflections
4360 reflections with I > 2σ(I)	intensity decay: 0.03%

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) = 0.076	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0422P)^2 + 0.1924P] where P = (Fo^2 + 2Fc^2)/3
4968 reflections	(Δ/σ)max = 0.001
189 parameters	Δρmax = 0.45 e Å^−3
3 restraints	Δρmin = −0.27 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
Co1	0.5000	0.5000	0.5000	0.01841 (5)
P1	0.71130 (4)	0.25756 (4)	0.38369 (2)	0.01997 (6)
P2	0.80307 (4)	0.26539 (4)	0.60886 (2)	0.01981 (6)
N1	0.34015 (16)	0.25550 (15)	0.72360 (8)	0.02616 (19)
H1A	0.3992	0.3451	0.6895	0.039*
H1B	0.2198	0.2611	0.7176	0.039*
H1C	0.3415	0.1468	0.6972	0.039*
O1	0.85612 (14)	0.30641 (13)	0.31356 (8)	0.03062 (19)
H1	0.9105	0.4164	0.3227	0.046*
O2	0.59716 (13)	0.39590 (12)	0.38331 (7)	0.02485 (16)
O3	0.60207 (14)	0.06129 (12)	0.35823 (9)	0.0316 (2)
O4	0.85272 (12)	0.27167 (14)	0.49651 (7)	0.02775 (18)
O5	0.73908 (14)	0.05674 (12)	0.62658 (9)	0.0328 (2)
H51	0.6275	0.0304	0.6315	0.049*
O6	0.64505 (12)	0.35655 (12)	0.60623 (7)	0.02449 (16)
O7	0.98964 (12)	0.34924 (13)	0.68190 (7)	0.02851 (18)
O8	0.25487 (13)	0.26937 (13)	0.48436 (9)	0.0321 (2)
H81	0.1442 (17)	0.286 (3)	0.4712 (16)	0.048*
H82	0.254 (3)	0.174 (2)	0.4498 (15)	0.048*
C1	0.43859 (18)	0.27762 (18)	0.83304 (10)	0.0273 (2)
C2	0.3460 (2)	0.1880 (2)	0.90581 (11)	0.0319 (3)
C3	0.4452 (3)	0.2135 (2)	1.01001 (12)	0.0415 (3)
C4	0.6298 (3)	0.3253 (3)	1.03492 (14)	0.0519 (4)
H4	0.6963	0.3420	1.1038	0.062*
C5	0.7175 (3)	0.4120 (3)	0.96093 (16)	0.0532 (5)
H5	0.8415	0.4863	0.9802	0.064*
C6	0.6221 (2)	0.3891 (2)	0.85808 (13)	0.0399 (3)
H6	0.6798	0.4472	0.8072	0.048*
C7	0.1465 (3)	0.0686 (3)	0.87421 (14)	0.0476 (4)
H7A	0.0575	0.1435	0.8696	0.071*
H7B	0.1253	−0.0209	0.9247	0.071*
H7C	0.1289	0.0066	0.8080	0.071*
C8	0.3536 (4)	0.1271 (3)	1.09442 (14)	0.0609 (5)
H8A	0.4473	0.1468	1.1588	0.091*
H8B	0.3027	−0.0028	1.0778	0.091*
H8C	0.2522	0.1820	1.1006	0.091*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.01761 (9)	0.01647 (9)	0.02390 (10)	0.00761 (7)	0.00672 (7)	0.00373 (7)
P1	0.01793 (12)	0.01585 (12)	0.02738 (14)	0.00415 (9)	0.00790 (10)	−0.00022 (9)
P2	0.01544 (11)	0.01650 (12)	0.02777 (14)	0.00539 (9)	0.00396 (10)	0.00373 (10)
N1	0.0291 (5)	0.0262 (5)	0.0256 (5)	0.0093 (4)	0.0087 (4)	0.0041 (4)
O1	0.0317 (5)	0.0249 (4)	0.0392 (5)	0.0037 (3)	0.0204 (4)	−0.0011 (4)
O2	0.0278 (4)	0.0241 (4)	0.0274 (4)	0.0134 (3)	0.0087 (3)	0.0029 (3)
O3	0.0271 (4)	0.0180 (4)	0.0495 (6)	0.0009 (3)	0.0135 (4)	−0.0034 (4)
O4	0.0201 (4)	0.0362 (5)	0.0296 (4)	0.0115 (3)	0.0063 (3)	0.0019 (3)
O5	0.0254 (4)	0.0178 (4)	0.0573 (6)	0.0063 (3)	0.0131 (4)	0.0081 (4)
O6	0.0245 (4)	0.0264 (4)	0.0280 (4)	0.0142 (3)	0.0088 (3)	0.0073 (3)
O7	0.0211 (4)	0.0257 (4)	0.0340 (5)	0.0034 (3)	−0.0005 (3)	0.0050 (3)
O8	0.0205 (4)	0.0224 (4)	0.0530 (6)	0.0048 (3)	0.0086 (4)	−0.0024 (4)
C1	0.0285 (5)	0.0289 (6)	0.0270 (5)	0.0125 (4)	0.0058 (4)	0.0025 (4)
C2	0.0353 (6)	0.0357 (6)	0.0291 (6)	0.0157 (5)	0.0088 (5)	0.0075 (5)
C3	0.0521 (9)	0.0485 (9)	0.0296 (6)	0.0260 (7)	0.0062 (6)	0.0062 (6)
C4	0.0524 (10)	0.0653 (12)	0.0360 (8)	0.0266 (9)	−0.0073 (7)	−0.0043 (8)
C5	0.0325 (8)	0.0643 (12)	0.0547 (10)	0.0109 (8)	−0.0054 (7)	−0.0117 (9)
C6	0.0307 (7)	0.0436 (8)	0.0442 (8)	0.0073 (6)	0.0084 (6)	−0.0015 (6)
C7	0.0415 (8)	0.0533 (10)	0.0460 (9)	0.0054 (7)	0.0127 (7)	0.0188 (7)
C8	0.0862 (16)	0.0726 (14)	0.0347 (8)	0.0339 (12)	0.0206 (9)	0.0188 (8)

Geometric parameters (Å, º)

Co1—O6^i	2.0524 (15)	O8—H81	0.840 (9)
Co1—O6	2.0524 (14)	O8—H82	0.847 (9)
Co1—O2^i	2.0710 (12)	C1—C6	1.379 (2)
Co1—O2	2.0710 (12)	C1—C2	1.387 (2)
Co1—O8^i	2.1506 (18)	C2—C3	1.403 (2)
Co1—O8	2.1506 (18)	C2—C7	1.497 (3)
P1—O2	1.4919 (12)	C3—C4	1.386 (3)
P1—O3	1.4925 (15)	C3—C8	1.503 (3)
P1—O1	1.5500 (12)	C4—C5	1.373 (3)
P1—O4	1.6139 (13)	C4—H4	0.9300
P2—O6	1.4903 (11)	C5—C6	1.380 (3)
P2—O7	1.4925 (14)	C5—H5	0.9300
P2—O5	1.5542 (14)	C6—H6	0.9300
P2—O4	1.6102 (11)	C7—H7A	0.9600
N1—C1	1.4631 (18)	C7—H7B	0.9600
N1—H1A	0.8900	C7—H7C	0.9600
N1—H1B	0.8900	C8—H8A	0.9600
N1—H1C	0.8900	C8—H8B	0.9600
O1—H1	0.8200	C8—H8C	0.9600
O5—H51	0.8200
O6^i—Co1—O6	180.0	P2—O5—H51	109.5
O6^i—Co1—O2^i	90.33 (5)	P2—O6—Co1	135.18 (6)
O6—Co1—O2^i	89.67 (5)	Co1—O8—H81	120.4 (14)
O6^i—Co1—O2	89.67 (5)	Co1—O8—H82	117.4 (14)
O6—Co1—O2	90.33 (5)	H81—O8—H82	108.7 (17)
O2^i—Co1—O2	180.00 (3)	C6—C1—C2	123.32 (14)
O6^i—Co1—O8^i	87.30 (7)	C6—C1—N1	117.03 (13)
O6—Co1—O8^i	92.70 (7)	C2—C1—N1	119.65 (13)
O2^i—Co1—O8^i	93.55 (7)	C1—C2—C3	117.84 (15)
O2—Co1—O8^i	86.45 (7)	C1—C2—C7	121.04 (14)
O6^i—Co1—O8	92.70 (7)	C3—C2—C7	121.13 (15)
O6—Co1—O8	87.30 (7)	C4—C3—C2	118.72 (16)
O2^i—Co1—O8	86.45 (7)	C4—C3—C8	119.82 (17)
O2—Co1—O8	93.55 (7)	C2—C3—C8	121.44 (18)
O8^i—Co1—O8	180.0	C5—C4—C3	122.00 (16)
O2—P1—O3	116.78 (7)	C5—C4—H4	119.0
O2—P1—O1	112.73 (7)	C3—C4—H4	119.0
O3—P1—O1	108.19 (7)	C4—C5—C6	120.13 (18)
O2—P1—O4	108.30 (7)	C4—C5—H5	119.9
O3—P1—O4	108.36 (9)	C6—C5—H5	119.9
O1—P1—O4	101.27 (7)	C1—C6—C5	117.98 (17)
O6—P2—O7	117.27 (7)	C1—C6—H6	121.0
O6—P2—O5	111.20 (7)	C5—C6—H6	121.0
O7—P2—O5	109.48 (8)	C2—C7—H7A	109.5
O6—P2—O4	108.87 (6)	C2—C7—H7B	109.5
O7—P2—O4	104.44 (7)	H7A—C7—H7B	109.5
O5—P2—O4	104.63 (8)	C2—C7—H7C	109.5
C1—N1—H1A	109.5	H7A—C7—H7C	109.5
C1—N1—H1B	109.5	H7B—C7—H7C	109.5
H1A—N1—H1B	109.5	C3—C8—H8A	109.5
C1—N1—H1C	109.5	C3—C8—H8B	109.5
H1A—N1—H1C	109.5	H8A—C8—H8B	109.5
H1B—N1—H1C	109.5	C3—C8—H8C	109.5
P1—O1—H1	109.5	H8A—C8—H8C	109.5
P1—O2—Co1	131.44 (6)	H8B—C8—H8C	109.5
P2—O4—P1	129.06 (6)

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
N1—H1A···O2^i	0.89	2.17	2.962 (2)	148
N1—H1A···O6	0.89	2.32	2.971 (2)	130
N1—H1B···O7^ii	0.89	1.94	2.799 (2)	161
N1—H1C···O3^iii	0.89	1.90	2.776 (2)	168
O5—H51···O3^iii	0.82	1.71	2.521 (2)	171
O8—H82···O5^iii	0.85 (1)	2.02 (1)	2.867 (2)	177 (2)
O8—H81···O4^ii	0.84 (1)	2.24 (1)	3.028 (2)	157 (2)
O1—H1···O7^iv	0.82	1.74	2.549 (2)	170

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