Di-μ-hydro­xo-bis­[aqua(1,10-phenanthroline-κ²N,N′)copper(II)] dinitrate hexahydrate

The title compound, [Cu₂(OH)₂(C₁₂H₈N₂)₂(H₂O)₂](NO₃)₂·6H₂O, consists of a hydro­xo-bridged dinuclear complex dication, two nitrate anions and six water mol­ecules arranged around an inversion center. The Cu...Cu distance is 2.902 (1) Å. The packing is governed by an intricate O—H...O hydrogen-bond network and also by π–π interactions.

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.045
• wR factor = 0.115
• Data-to-parameter ratio = 11.0

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT430_ALERT_2_B Short Inter D...A Contact  O3     ..  O4      ..       2.59 Ang.

Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.98
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          2
              N O3
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          4
              H2 O

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

   0 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
   1 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; 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) and CAMERON (Watkin et al., 1993); software used to prepare material for publication: SHELXTL/PC.

Di-µ-hydroxo-bis[aqua(1,10-phenanthroline-κ²N,N')copper(II)] dinitrate hexahydrate

Crystal data

[Cu2(OH)2(C12H8N2)2(H2O)2](NO3)2·6H2O	Z = 1
Mr = 789.65	F(000) = 406
Triclinic, P1	Dx = 1.684 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.078 (2) Å	Cell parameters from 1793 reflections
b = 9.604 (2) Å	θ = 2.6–26.8°
c = 10.480 (3) Å	µ = 1.45 mm^−1
α = 81.145 (3)°	T = 173 K
β = 88.341 (4)°	Block, blue
γ = 75.731 (3)°	0.25 × 0.20 × 0.20 mm
V = 778.4 (3) Å^3

Data collection

Bruker SMART 1K CCD area-detector diffractometer	2687 independent reflections
Radiation source: fine-focus sealed tube	2359 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.020
φ and ω scans	θmax = 25.0°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 2000)	h = −9→8
Tmin = 0.699, Tmax = 0.745	k = −11→11
3804 measured reflections	l = −11→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)] = 0.045	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.115	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	w = 1/[σ^2(Fo^2) + (0.0703P)^2] where P = (Fo^2 + 2Fc^2)/3
2687 reflections	(Δ/σ)max = 0.001
244 parameters	Δρmax = 0.80 e Å^−3
13 restraints	Δρmin = −0.61 e Å^−3

Special details

Experimental. CHN were analysed in a Perkin-Elmer 240 C Elemental Analyzer.?

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
Cu1	0.58181 (5)	0.86055 (4)	0.96171 (4)	0.01861 (17)
N1	0.7245 (4)	0.6677 (3)	1.0486 (3)	0.0199 (7)
N2	0.5391 (4)	0.7353 (3)	0.8334 (3)	0.0189 (7)
O1	0.4013 (3)	1.0311 (3)	0.9001 (2)	0.0200 (6)
H1A	0.423 (5)	1.076 (4)	0.834 (3)	0.024*
O2	0.7832 (4)	0.9338 (3)	0.8371 (3)	0.0329 (7)
H2C	0.768 (5)	0.957 (5)	0.7609 (19)	0.040*
H2B	0.870 (4)	0.944 (5)	0.865 (4)	0.040*
C1	0.8201 (5)	0.6376 (4)	1.1541 (3)	0.0229 (8)
H1	0.8268	0.7132	1.1979	0.027*
C2	0.9111 (5)	0.4975 (4)	1.2023 (4)	0.0256 (9)
H2A	0.9776	0.4807	1.2767	0.031*
C3	0.9025 (5)	0.3846 (4)	1.1400 (4)	0.0261 (9)
H3	0.9625	0.2905	1.1720	0.031*
C4	0.8022 (5)	0.4117 (4)	1.0271 (4)	0.0226 (8)
C5	0.7170 (4)	0.5555 (4)	0.9849 (3)	0.0197 (8)
C6	0.6167 (5)	0.5927 (4)	0.8690 (3)	0.0210 (8)
C7	0.7871 (5)	0.3019 (4)	0.9529 (4)	0.0281 (9)
H7	0.8437	0.2055	0.9804	0.034*
C8	0.6912 (5)	0.3368 (4)	0.8430 (4)	0.0271 (9)
H8	0.6828	0.2638	0.7966	0.033*
C9	0.6029 (5)	0.4837 (4)	0.7973 (4)	0.0235 (8)
C10	0.5036 (5)	0.5284 (4)	0.6842 (4)	0.0266 (9)
H10	0.4902	0.4602	0.6337	0.032*
C11	0.4267 (5)	0.6713 (4)	0.6481 (4)	0.0278 (9)
H11	0.3608	0.7014	0.5730	0.033*
C12	0.4474 (5)	0.7731 (4)	0.7250 (4)	0.0238 (8)
H12	0.3949	0.8708	0.6992	0.029*
N3	0.0219 (5)	1.2914 (4)	0.5455 (3)	0.0443 (10)
O3	0.1462 (3)	1.3469 (3)	0.5175 (3)	0.0329 (7)
O4	−0.1362 (3)	1.3799 (3)	0.5443 (3)	0.0290 (6)
O5	0.0327 (4)	1.1573 (3)	0.5776 (3)	0.0304 (7)
O6	0.7643 (4)	1.0316 (3)	0.5700 (3)	0.0316 (7)
H6A	0.801 (5)	0.971 (4)	0.524 (4)	0.038*
H6B	0.835 (4)	1.080 (4)	0.577 (4)	0.038*
O7	0.4406 (4)	1.1663 (4)	0.6498 (3)	0.0417 (8)
H7B	0.363 (4)	1.205 (5)	0.599 (3)	0.050*
H7A	0.528 (3)	1.121 (5)	0.621 (4)	0.050*
O8	0.0816 (4)	1.0159 (4)	0.8339 (3)	0.0406 (8)
H8A	0.072 (5)	1.058 (5)	0.760 (2)	0.049*
H8B	0.173 (4)	1.010 (5)	0.867 (4)	0.049*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cu1	0.0208 (3)	0.0131 (3)	0.0213 (3)	−0.00258 (18)	−0.00257 (18)	−0.00258 (18)
N1	0.0209 (16)	0.0182 (16)	0.0209 (16)	−0.0054 (13)	0.0010 (13)	−0.0029 (13)
N2	0.0203 (16)	0.0129 (16)	0.0226 (16)	−0.0033 (12)	0.0001 (13)	−0.0011 (13)
O1	0.0234 (14)	0.0153 (13)	0.0199 (14)	−0.0029 (11)	−0.0020 (11)	−0.0012 (11)
O2	0.0277 (16)	0.0438 (18)	0.0290 (16)	−0.0172 (14)	−0.0019 (13)	0.0034 (14)
C1	0.022 (2)	0.022 (2)	0.024 (2)	−0.0038 (16)	0.0018 (16)	−0.0042 (16)
C2	0.023 (2)	0.028 (2)	0.022 (2)	−0.0018 (17)	−0.0004 (16)	−0.0002 (17)
C3	0.029 (2)	0.018 (2)	0.026 (2)	0.0009 (16)	0.0027 (17)	0.0033 (16)
C4	0.0226 (19)	0.020 (2)	0.025 (2)	−0.0061 (16)	0.0076 (16)	−0.0015 (16)
C5	0.0167 (18)	0.0168 (19)	0.025 (2)	−0.0046 (15)	0.0045 (15)	−0.0022 (15)
C6	0.024 (2)	0.018 (2)	0.0216 (19)	−0.0053 (15)	0.0054 (15)	−0.0041 (15)
C7	0.034 (2)	0.015 (2)	0.032 (2)	−0.0038 (17)	0.0064 (18)	−0.0005 (17)
C8	0.036 (2)	0.018 (2)	0.029 (2)	−0.0082 (17)	0.0047 (18)	−0.0068 (17)
C9	0.025 (2)	0.020 (2)	0.027 (2)	−0.0075 (16)	0.0073 (16)	−0.0062 (16)
C10	0.033 (2)	0.027 (2)	0.025 (2)	−0.0126 (18)	0.0032 (17)	−0.0110 (17)
C11	0.030 (2)	0.032 (2)	0.023 (2)	−0.0099 (18)	−0.0004 (16)	−0.0029 (17)
C12	0.023 (2)	0.019 (2)	0.028 (2)	−0.0038 (16)	−0.0001 (16)	−0.0020 (16)
N3	0.053 (3)	0.052 (3)	0.029 (2)	−0.013 (2)	−0.0040 (18)	−0.0087 (19)
O3	0.0214 (15)	0.0235 (15)	0.0528 (19)	−0.0082 (12)	0.0015 (13)	0.0013 (13)
O4	0.0216 (14)	0.0260 (15)	0.0378 (16)	−0.0036 (12)	0.0009 (12)	−0.0040 (13)
O5	0.0398 (17)	0.0128 (14)	0.0388 (17)	−0.0087 (12)	0.0024 (13)	−0.0010 (12)
O6	0.0289 (16)	0.0300 (17)	0.0362 (17)	−0.0074 (13)	0.0021 (13)	−0.0059 (13)
O7	0.0296 (17)	0.054 (2)	0.0305 (17)	0.0047 (15)	0.0011 (13)	0.0037 (15)
O8	0.0285 (16)	0.052 (2)	0.0407 (19)	−0.0211 (15)	−0.0117 (14)	0.0135 (16)

Geometric parameters (Å, º)

Cu1—O1^i	1.935 (2)	C5—C6	1.428 (5)
Cu1—O1	1.944 (2)	C6—C9	1.406 (5)
Cu1—N1	2.019 (3)	C7—C8	1.358 (5)
Cu1—N2	2.025 (3)	C7—H7	0.9300
Cu1—O2	2.237 (3)	C8—C9	1.430 (5)
Cu1—Cu1^i	2.9018 (9)	C8—H8	0.9300
N1—C1	1.320 (5)	C9—C10	1.400 (5)
N1—C5	1.366 (5)	C10—C11	1.359 (5)
N2—C12	1.327 (5)	C10—H10	0.9300
N2—C6	1.357 (4)	C11—C12	1.402 (5)
O1—Cu1^i	1.935 (2)	C11—H11	0.9300
O1—H1A	0.80 (4)	C12—H12	0.9300
O2—H2C	0.80 (4)	N3—O3	1.256 (5)
O2—H2B	0.80 (4)	N3—O5	1.261 (5)
C1—C2	1.390 (5)	N3—O4	1.348 (4)
C1—H1	0.9300	O6—H6A	0.80 (4)
C2—C3	1.365 (5)	O6—H6B	0.83 (3)
C2—H2A	0.9300	O7—H7B	0.81 (4)
C3—C4	1.408 (5)	O7—H7A	0.81 (4)
C3—H3	0.9300	O8—H8A	0.81 (4)
C4—C5	1.391 (5)	O8—H8B	0.81 (3)
C4—C7	1.432 (5)
O1^i—Cu1—O1	83.14 (10)	C4—C3—H3	120.2
O1^i—Cu1—N1	96.36 (11)	C5—C4—C3	116.8 (3)
O1—Cu1—N1	166.59 (11)	C5—C4—C7	119.1 (3)
O1^i—Cu1—N2	171.68 (12)	C3—C4—C7	124.1 (3)
O1—Cu1—N2	96.75 (11)	N1—C5—C4	123.3 (3)
N1—Cu1—N2	81.81 (11)	N1—C5—C6	116.4 (3)
O1^i—Cu1—O2	96.44 (11)	C4—C5—C6	120.3 (3)
O1—Cu1—O2	94.59 (11)	N2—C6—C9	123.2 (3)
N1—Cu1—O2	98.77 (12)	N2—C6—C5	116.8 (3)
N2—Cu1—O2	91.86 (12)	C9—C6—C5	120.0 (3)
O1^i—Cu1—Cu1^i	41.69 (7)	C8—C7—C4	120.7 (3)
O1—Cu1—Cu1^i	41.45 (7)	C8—C7—H7	119.6
N1—Cu1—Cu1^i	136.51 (9)	C4—C7—H7	119.6
N2—Cu1—Cu1^i	137.60 (8)	C7—C8—C9	121.3 (4)
O2—Cu1—Cu1^i	97.38 (9)	C7—C8—H8	119.3
C1—N1—C5	117.9 (3)	C9—C8—H8	119.3
C1—N1—Cu1	129.6 (3)	C10—C9—C6	116.8 (3)
C5—N1—Cu1	112.5 (2)	C10—C9—C8	124.6 (3)
C12—N2—C6	118.0 (3)	C6—C9—C8	118.5 (3)
C12—N2—Cu1	129.5 (2)	C11—C10—C9	120.1 (3)
C6—N2—Cu1	112.4 (2)	C11—C10—H10	120.0
Cu1^i—O1—Cu1	96.86 (10)	C9—C10—H10	120.0
Cu1^i—O1—H1A	108 (3)	C10—C11—C12	119.5 (4)
Cu1—O1—H1A	114 (3)	C10—C11—H11	120.3
Cu1—O2—H2C	120 (3)	C12—C11—H11	120.3
Cu1—O2—H2B	124 (3)	N2—C12—C11	122.4 (3)
H2C—O2—H2B	116 (3)	N2—C12—H12	118.8
N1—C1—C2	122.7 (4)	C11—C12—H12	118.8
N1—C1—H1	118.7	O3—N3—O5	125.1 (4)
C2—C1—H1	118.7	O3—N3—O4	118.7 (4)
C3—C2—C1	119.7 (4)	O5—N3—O4	116.3 (4)
C3—C2—H2A	120.2	H6A—O6—H6B	110 (3)
C1—C2—H2A	120.2	H7B—O7—H7A	117 (3)
C2—C3—C4	119.6 (3)	H8A—O8—H8B	114 (3)
C2—C3—H3	120.2

Symmetry code: (i) −x+1, −y+2, −z+2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···O7	0.80 (4)	2.01 (2)	2.789 (4)	166 (4)
O2—H2C···O6	0.80 (4)	2.02 (2)	2.809 (4)	170 (4)
O2—H2B···O8^ii	0.80 (4)	2.00 (3)	2.713 (4)	149 (4)
O6—H6A···O5^iii	0.80 (4)	1.99 (2)	2.761 (4)	160 (4)
O6—H6B···O5^ii	0.83 (3)	1.92 (2)	2.738 (4)	168 (4)
O7—H7B···O3	0.81 (4)	2.05 (2)	2.829 (4)	160 (4)
O7—H7A···O6	0.81 (4)	1.99 (2)	2.784 (4)	169 (5)
O8—H8A···O5	0.81 (4)	2.00 (2)	2.809 (4)	176 (4)
O8—H8B···O1	0.81 (4)	1.95 (2)	2.737 (4)	164 (4)

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