Di-μ-hypophosphito-bis­[(2,2′-bi­pyridine)copper(II)] nitrate

The structure of blue [Cu₂(O₂PH₂)₂(C₁₀H₈N₂)₂](NO₃)₂ consists of dimeric [Cu(O₂PH₂)(bipy)] subunits (bipy = 2,2′-bi­pyridine) joined by two hypophosphite bridging ligands, with each metal center in a distorted planar arrangement. These joined subunits exist as a discrete cation with the equivalent of two nitrates as counter-ions. The subunits have a four-coordinated distorted square-planar arrangement of N and O atoms from the 2,2′-bi­pyridine and hypophosphite ligands, with the fifth and sixth positions of the copper coordination occupied by neighboring O atoms of the nitrate counter-ions.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.024
• wR factor = 0.070
• Data-to-parameter ratio = 11.6

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



PLAT_420  Alert C D-H Without Acceptor       P      -   H(40A)            ?


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 1 Alert Level C = Please check

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Computing details

Data collection: CAD-4 Manual (Schagen et al., 1989); cell refinement: CAD-4 Manual; data reduction: MolEN (Fair, 1990); program(s) used to solve structure: SHELXTL/PC (Siemens , 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL/PC; software used to prepare material for publication: SHELXTL/PC.

(I)

Crystal data

[Cu2(H2PO2)2(C10H8N2)2](NO3)2	F(000) = 700
Mr = 346.73	Dx = 1.851 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 25 reflections
a = 6.727 (3) Å	θ = 20.0–24.9°
b = 12.8420 (13) Å	µ = 1.91 mm^−1
c = 15.209 (7) Å	T = 295 K
β = 108.72 (2)°	Prism, blue
V = 1244.4 (8) Å^3	0.50 × 0.30 × 0.20 mm
Z = 4

Data collection

Enraf-Nonius CAD-4 diffractometer	Rint = 0.010
θ/2θ scans	θmax = 25.0°
Absorption correction: ψ scan MolEN (Fair, 1990)	h = −7→7
Tmin = 0.513, Tmax = 0.683	k = 0→15
2251 measured reflections	l = 0→17
2165 independent reflections	1 standard reflections every 167 min
2090 reflections with I > 2σ(I)	intensity decay: 1.1%

Refinement

Refinement on F^2	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.024	w = 1/[σ^2(Fo^2) + (0.0366P)^2 + 0.9392P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.070	(Δ/σ)max = 0.001
S = 1.16	Δρmax = 0.32 e Å^−3
2165 reflections	Δρmin = −0.28 e Å^−3
187 parameters

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

	x	y	z	Uiso*/Ueq
Cu	0.01098 (4)	0.197063 (18)	0.472137 (17)	0.02809 (11)
P	−0.25122 (8)	−0.00012 (4)	0.42439 (4)	0.02823 (15)
H40A	−0.437 (6)	−0.025 (3)	0.366 (2)	0.080*
H40B	−0.287 (6)	0.013 (3)	0.500 (2)	0.080*
O1	−0.1809 (2)	0.09920 (11)	0.38931 (10)	0.0301 (3)
O2	−0.1068 (3)	−0.09195 (11)	0.43206 (10)	0.0315 (3)
O4	−0.5309 (3)	0.29020 (15)	0.37638 (15)	0.0544 (5)
C5	0.0805 (3)	0.39498 (16)	0.40663 (15)	0.0272 (4)
C6	0.1957 (3)	0.39698 (16)	0.50766 (15)	0.0273 (4)
N1	−0.0215 (3)	0.30531 (13)	0.37583 (13)	0.0277 (4)
N2	0.1783 (3)	0.30844 (13)	0.55231 (13)	0.0295 (4)
C2	−0.1333 (4)	0.3722 (2)	0.22166 (17)	0.0423 (6)
H2B	−0.2072	0.3620	0.1568	0.080*
N3	−0.4810 (3)	0.23597 (16)	0.44684 (17)	0.0415 (5)
C9	0.3963 (4)	0.3807 (2)	0.69422 (17)	0.0402 (6)
H9A	0.4661	0.3733	0.7597	0.080*
O3	−0.3143 (3)	0.25649 (18)	0.51158 (14)	0.0591 (5)
C10	0.2767 (4)	0.30077 (17)	0.64395 (17)	0.0367 (5)
H10A	0.2634	0.2376	0.6754	0.080*
C3	−0.0318 (4)	0.4646 (2)	0.25298 (18)	0.0432 (6)
H3A	−0.0366	0.5202	0.2102	0.080*
C7	0.3123 (4)	0.48054 (18)	0.55445 (17)	0.0339 (5)
H7A	0.3225	0.5434	0.5220	0.080*
C8	0.4144 (4)	0.47157 (19)	0.64934 (18)	0.0384 (5)
H8A	0.4970	0.5283	0.6833	0.080*
C4	0.0774 (4)	0.47713 (19)	0.34653 (17)	0.0369 (5)
H4A	0.1494	0.5411	0.3694	0.080*
C1	−0.1269 (4)	0.29448 (18)	0.28496 (16)	0.0349 (5)
H1A	−0.2001	0.2305	0.2634	0.080*
O5	0.4075 (4)	0.16036 (16)	0.45229 (19)	0.0697 (7)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cu	0.03652 (18)	0.01912 (16)	0.02482 (17)	−0.00294 (10)	0.00453 (12)	0.00234 (9)
P	0.0270 (3)	0.0225 (3)	0.0307 (3)	−0.0022 (2)	0.0030 (2)	0.0040 (2)
O1	0.0361 (8)	0.0222 (7)	0.0275 (8)	−0.0024 (6)	0.0038 (6)	0.0025 (6)
O2	0.0429 (9)	0.0228 (7)	0.0268 (8)	0.0020 (6)	0.0087 (7)	0.0035 (6)
O4	0.0537 (12)	0.0443 (11)	0.0634 (13)	0.0053 (9)	0.0165 (10)	0.0147 (10)
C5	0.0256 (10)	0.0250 (10)	0.0345 (11)	0.0037 (8)	0.0144 (9)	0.0048 (8)
C6	0.0241 (10)	0.0230 (10)	0.0371 (12)	0.0015 (8)	0.0132 (9)	0.0007 (9)
N1	0.0289 (9)	0.0260 (9)	0.0291 (9)	0.0011 (7)	0.0104 (8)	0.0041 (7)
N2	0.0304 (10)	0.0239 (9)	0.0309 (10)	0.0007 (7)	0.0052 (8)	0.0006 (7)
C2	0.0503 (15)	0.0488 (15)	0.0299 (12)	0.0080 (12)	0.0160 (11)	0.0098 (11)
N3	0.0413 (12)	0.0302 (11)	0.0617 (14)	0.0072 (9)	0.0289 (11)	0.0035 (10)
C9	0.0383 (13)	0.0375 (13)	0.0371 (13)	0.0013 (10)	0.0014 (10)	−0.0069 (10)
O3	0.0619 (13)	0.0656 (14)	0.0485 (12)	0.0083 (11)	0.0160 (10)	−0.0037 (10)
C10	0.0418 (13)	0.0300 (12)	0.0324 (12)	0.0009 (9)	0.0036 (10)	0.0004 (9)
C3	0.0548 (15)	0.0410 (13)	0.0421 (14)	0.0078 (12)	0.0272 (12)	0.0164 (11)
C7	0.0309 (11)	0.0261 (11)	0.0484 (13)	−0.0026 (9)	0.0179 (10)	−0.0038 (10)
C8	0.0298 (11)	0.0349 (12)	0.0488 (14)	−0.0055 (10)	0.0102 (10)	−0.0123 (11)
C4	0.0389 (13)	0.0312 (12)	0.0472 (14)	0.0021 (10)	0.0231 (11)	0.0090 (10)
C1	0.0385 (13)	0.0348 (12)	0.0308 (12)	0.0010 (10)	0.0104 (10)	0.0024 (9)
O5	0.0637 (14)	0.0386 (11)	0.125 (2)	0.0017 (10)	0.0562 (14)	0.0160 (12)

Geometric parameters (Å, º)

Cu—O2^i	1.9385 (15)	N2—C10	1.341 (3)
Cu—O1	1.9466 (15)	C2—C3	1.376 (4)
Cu—N2	1.9794 (19)	C2—C1	1.378 (3)
Cu—N1	1.9799 (18)	C2—H2B	0.96
Cu—O3	2.564 (2)	N3—O5^ii	1.246 (3)
Cu—O5	2.819 (2)	N3—O3	1.260 (3)
P—O2	1.5085 (16)	C9—C10	1.375 (3)
P—O1	1.5155 (15)	C9—C8	1.377 (4)
P—H40A	1.32 (4)	C9—H9A	0.96
P—H40B	1.27 (3)	C10—H10A	0.96
O4—N3	1.231 (3)	C3—C4	1.385 (4)
C5—N1	1.345 (3)	C3—H3A	0.96
C5—C4	1.392 (3)	C7—C8	1.390 (4)
C5—C6	1.482 (3)	C7—H7A	0.96
C6—N2	1.349 (3)	C8—H8A	0.96
C6—C7	1.384 (3)	C4—H4A	0.96
N1—C1	1.343 (3)	C1—H1A	0.96
O2^i—Cu—O1	91.62 (7)	C10—N2—C6	119.44 (19)
O2^i—Cu—N2	93.10 (7)	C10—N2—Cu	125.50 (15)
O1—Cu—N2	173.22 (7)	C6—N2—Cu	115.03 (15)
O2^i—Cu—N1	167.45 (7)	C3—C2—C1	118.8 (2)
O1—Cu—N1	94.69 (7)	C3—C2—H2B	120.6
N2—Cu—N1	81.62 (8)	C1—C2—H2B	120.6
O2^i—Cu—O3	97.72 (7)	O4—N3—O5^ii	119.8 (3)
O1—Cu—O3	84.54 (7)	O4—N3—O3	119.2 (2)
N2—Cu—O3	90.00 (8)	O5^ii—N3—O3	121.0 (2)
N1—Cu—O3	93.67 (8)	C10—C9—C8	119.1 (2)
O2^i—Cu—O5	82.31 (7)	C10—C9—H9A	120.5
O1—Cu—O5	106.06 (8)	C8—C9—H9A	120.5
N2—Cu—O5	79.42 (8)	N3—O3—Cu	111.55 (15)
N1—Cu—O5	85.52 (7)	N2—C10—C9	121.9 (2)
O3—Cu—O5	169.39 (7)	N2—C10—H10A	119.0
O2—P—O1	114.79 (9)	C9—C10—H10A	119.0
O2—P—H40A	107.9 (16)	C2—C3—C4	119.8 (2)
O1—P—H40A	107.8 (16)	C2—C3—H3A	120.1
O2—P—H40B	109.9 (17)	C4—C3—H3A	120.1
O1—P—H40B	112.5 (16)	C6—C7—C8	118.6 (2)
H40A—P—H40B	103 (2)	C6—C7—H7A	120.7
P—O1—Cu	122.18 (9)	C8—C7—H7A	120.7
P—O2—Cu^i	130.77 (10)	C9—C8—C7	119.5 (2)
N1—C5—C4	121.4 (2)	C9—C8—H8A	120.3
N1—C5—C6	114.46 (18)	C7—C8—H8A	120.3
C4—C5—C6	124.1 (2)	C3—C4—C5	118.5 (2)
N2—C6—C7	121.4 (2)	C3—C4—H4A	120.7
N2—C6—C5	113.98 (18)	C5—C4—H4A	120.7
C7—C6—C5	124.6 (2)	N1—C1—C2	122.1 (2)
C1—N1—C5	119.26 (19)	N1—C1—H1A	118.9
C1—N1—Cu	125.82 (15)	C2—C1—H1A	118.9
C5—N1—Cu	114.87 (15)	N3^iii—O5—Cu	119.16 (16)

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