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In the title compound, [Cu(SO4)(C12H8N2)(H2O)3]·H2O, the CuII centre exhibits a slightly distorted cis-CuN2O4 octa­hedral coordination defined by two N atoms from a 1,10-phenanthroline mol­ecule, one O atom from a sulfato dianion and three O atoms from coordinated water mol­ecules.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807000591/hb2258sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807000591/hb2258Isup2.hkl
Contains datablock I

CCDC reference: 1175333

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.030
  • wR factor = 0.090
  • Data-to-parameter ratio = 11.4

checkCIF/PLATON results

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Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.99 PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 100 Deg. PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 3 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 8
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 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 0 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 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Triaqua(1,10-phenanthroline)sulfatocopper(II) monohydrate top
Crystal data top
[Cu(SO4)(C12H8N2)(H2O)3]·H2OZ = 2
Mr = 411.87F(000) = 422
Triclinic, P1Dx = 1.779 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.9908 (7) ÅCell parameters from 3806 reflections
b = 8.5918 (7) Åθ = 2.6–25.3°
c = 11.5799 (9) ŵ = 1.60 mm1
α = 91.934 (1)°T = 295 K
β = 92.149 (1)°Prism, blue
γ = 104.319 (1)°0.36 × 0.28 × 0.16 mm
V = 769.02 (11) Å3
Data collection top
Bruker SMART CCD
diffractometer
2754 independent reflections
Radiation source: fine-focus sealed tube2681 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.010
ω scansθmax = 25.3°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 99
Tmin = 0.596, Tmax = 0.784k = 810
3923 measured reflectionsl = 1311
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)] = 0.030Hydrogen site location: difmap and geom
wR(F2) = 0.090H atoms treated by a mixture of independent and constrained refinement
S = 1.12 w = 1/[σ2(Fo2) + (0.0488P)2 + 0.9465P]
where P = (Fo2 + 2Fc2)/3
2754 reflections(Δ/σ)max < 0.001
241 parametersΔρmax = 0.36 e Å3
12 restraintsΔρmin = 0.75 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
Cu10.30191 (4)0.73753 (3)0.80384 (2)0.01995 (12)
S10.71978 (7)0.94251 (7)0.84582 (5)0.01918 (16)
O1W0.3754 (2)0.7171 (2)0.97358 (15)0.0247 (4)
H1W10.4795 (17)0.771 (3)0.976 (3)0.037*
H1W20.318 (3)0.758 (3)1.020 (2)0.037*
O2W0.1984 (2)0.9298 (2)0.84087 (17)0.0253 (4)
H2W10.0893 (14)0.913 (4)0.833 (3)0.038*
H2W20.235 (3)0.993 (3)0.899 (2)0.038*
O3W0.0624 (2)0.5833 (2)0.84191 (16)0.0247 (4)
H3W10.081 (4)0.500 (2)0.870 (2)0.037*
H3W20.012 (4)0.630 (3)0.890 (2)0.037*
O4W0.0720 (3)0.3069 (2)0.9586 (2)0.0336 (5)
H4W10.154 (3)0.266 (4)0.976 (3)0.050*
H4W20.013 (3)0.237 (3)0.928 (3)0.050*
O10.5511 (2)0.8914 (2)0.78070 (16)0.0266 (4)
O20.8542 (3)0.8910 (3)0.78394 (18)0.0349 (5)
O30.7034 (2)0.8709 (2)0.96266 (16)0.0268 (4)
O40.7670 (3)1.1196 (2)0.86395 (17)0.0288 (4)
N10.3684 (3)0.5310 (3)0.74336 (18)0.0198 (4)
N20.2322 (3)0.7403 (3)0.63026 (18)0.0198 (4)
C10.1727 (3)0.8502 (3)0.5741 (2)0.0270 (6)
H10.15970.94090.61530.032*
C20.1290 (4)0.8336 (4)0.4552 (3)0.0338 (7)
H20.09210.91440.41820.041*
C30.1409 (4)0.6982 (4)0.3936 (2)0.0326 (7)
H30.10990.68540.31500.039*
C40.2006 (3)0.5783 (3)0.4506 (2)0.0250 (6)
C50.2203 (4)0.4327 (4)0.3937 (2)0.0312 (6)
H50.18540.41100.31600.037*
C60.2886 (4)0.3273 (3)0.4511 (2)0.0295 (6)
H60.30220.23520.41200.035*
C70.3405 (3)0.3545 (3)0.5712 (2)0.0245 (6)
C80.4160 (4)0.2511 (3)0.6356 (3)0.0295 (6)
H80.43300.15750.60060.035*
C90.4641 (4)0.2883 (3)0.7491 (3)0.0322 (6)
H90.51340.22010.79220.039*
C100.4390 (4)0.4300 (3)0.8006 (2)0.0276 (6)
H100.47310.45440.87810.033*
C110.3200 (3)0.4938 (3)0.6302 (2)0.0189 (5)
C120.2481 (3)0.6075 (3)0.5688 (2)0.0193 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.01938 (19)0.02302 (19)0.01799 (19)0.00717 (13)0.00208 (12)0.00219 (12)
S10.0144 (3)0.0237 (3)0.0197 (3)0.0068 (2)0.0033 (2)0.0056 (2)
O1W0.0235 (9)0.0328 (10)0.0178 (9)0.0076 (8)0.0018 (7)0.0029 (7)
O2W0.0221 (9)0.0262 (10)0.0291 (10)0.0110 (8)0.0045 (8)0.0084 (8)
O3W0.0237 (9)0.0236 (9)0.0266 (10)0.0056 (8)0.0008 (7)0.0009 (7)
O4W0.0264 (10)0.0248 (10)0.0500 (13)0.0078 (8)0.0026 (9)0.0030 (9)
O10.0163 (9)0.0366 (11)0.0232 (9)0.0007 (8)0.0065 (7)0.0022 (8)
O20.0234 (10)0.0483 (13)0.0358 (11)0.0168 (9)0.0009 (8)0.0171 (9)
O30.0250 (9)0.0314 (10)0.0240 (10)0.0085 (8)0.0083 (8)0.0003 (8)
O40.0304 (10)0.0231 (10)0.0316 (10)0.0055 (8)0.0016 (8)0.0045 (8)
N10.0202 (10)0.0233 (11)0.0171 (10)0.0076 (8)0.0001 (8)0.0001 (8)
N20.0162 (10)0.0232 (11)0.0196 (10)0.0044 (8)0.0015 (8)0.0014 (8)
C10.0252 (13)0.0286 (14)0.0285 (14)0.0091 (11)0.0020 (11)0.0053 (11)
C20.0302 (15)0.0436 (17)0.0300 (15)0.0129 (13)0.0029 (12)0.0149 (13)
C30.0263 (14)0.0517 (18)0.0179 (13)0.0064 (13)0.0037 (11)0.0067 (12)
C40.0165 (12)0.0366 (15)0.0187 (13)0.0007 (11)0.0001 (10)0.0002 (11)
C50.0273 (14)0.0418 (16)0.0183 (13)0.0017 (12)0.0008 (11)0.0094 (12)
C60.0280 (14)0.0298 (14)0.0263 (14)0.0000 (12)0.0029 (11)0.0125 (11)
C70.0199 (12)0.0236 (13)0.0274 (14)0.0008 (10)0.0032 (10)0.0056 (11)
C80.0277 (14)0.0214 (13)0.0401 (16)0.0074 (11)0.0069 (12)0.0044 (11)
C90.0352 (16)0.0287 (15)0.0379 (16)0.0172 (12)0.0024 (13)0.0065 (12)
C100.0320 (14)0.0314 (14)0.0228 (13)0.0148 (12)0.0011 (11)0.0017 (11)
C110.0145 (11)0.0222 (12)0.0190 (12)0.0024 (9)0.0020 (9)0.0012 (10)
C120.0135 (11)0.0252 (13)0.0174 (12)0.0018 (10)0.0006 (9)0.0001 (10)
Geometric parameters (Å, º) top
Cu1—O1W2.0559 (18)N2—C121.360 (3)
Cu1—O2W2.0619 (18)C1—C21.401 (4)
Cu1—N22.068 (2)C1—H10.9300
Cu1—N12.081 (2)C2—C31.369 (5)
Cu1—O3W2.1122 (19)C2—H20.9300
Cu1—O12.1323 (18)C3—C41.410 (4)
S1—O21.4608 (19)C3—H30.9300
S1—O11.4787 (18)C4—C121.404 (4)
S1—O41.4796 (19)C4—C51.441 (4)
S1—O31.502 (2)C5—C61.348 (4)
O1W—H1W10.845 (10)C5—H50.9300
O1W—H1W20.843 (10)C6—C71.431 (4)
O2W—H2W10.848 (10)C6—H60.9300
O2W—H2W20.844 (10)C7—C111.406 (4)
O3W—H3W10.844 (10)C7—C81.410 (4)
O3W—H3W20.85 (3)C8—C91.360 (4)
O4W—H4W10.84 (3)C8—H80.9300
O4W—H4W20.85 (3)C9—C101.400 (4)
N1—C101.328 (3)C9—H90.9300
N1—C111.357 (3)C10—H100.9300
N2—C11.334 (3)C11—C121.443 (3)
O1W—Cu1—O2W93.57 (8)C12—N2—Cu1112.84 (16)
O1W—Cu1—N2175.38 (8)N2—C1—C2122.3 (3)
O2W—Cu1—N290.96 (8)N2—C1—H1118.9
O1W—Cu1—N195.12 (8)C2—C1—H1118.9
O2W—Cu1—N1169.29 (8)C3—C2—C1119.9 (3)
N2—Cu1—N180.27 (8)C3—C2—H2120.1
O1W—Cu1—O3W85.94 (8)C1—C2—H2120.1
O2W—Cu1—O3W88.26 (8)C2—C3—C4119.3 (3)
N2—Cu1—O3W93.27 (8)C2—C3—H3120.3
N1—Cu1—O3W86.13 (8)C4—C3—H3120.3
O1W—Cu1—O189.02 (7)C12—C4—C3117.1 (3)
O2W—Cu1—O192.16 (8)C12—C4—C5119.1 (3)
N2—Cu1—O191.74 (8)C3—C4—C5123.8 (3)
N1—Cu1—O194.23 (8)C6—C5—C4121.1 (2)
O3W—Cu1—O1174.97 (7)C6—C5—H5119.5
O2—S1—O1110.91 (12)C4—C5—H5119.5
O2—S1—O4110.00 (12)C5—C6—C7121.2 (3)
O1—S1—O4109.34 (12)C5—C6—H6119.4
O2—S1—O3109.75 (12)C7—C6—H6119.4
O1—S1—O3109.02 (11)C11—C7—C8116.6 (2)
O4—S1—O3107.76 (11)C11—C7—C6119.3 (3)
Cu1—O1W—H1W1102 (2)C8—C7—C6124.0 (2)
Cu1—O1W—H1W2112 (2)C9—C8—C7119.9 (2)
H1W1—O1W—H1W2110.1 (16)C9—C8—H8120.0
Cu1—O2W—H2W1117 (2)C7—C8—H8120.0
Cu1—O2W—H2W2121 (2)C8—C9—C10119.5 (3)
H2W1—O2W—H2W2109.7 (16)C8—C9—H9120.3
Cu1—O3W—H3W1108 (2)C10—C9—H9120.3
Cu1—O3W—H3W2110 (2)N1—C10—C9122.7 (3)
H3W1—O3W—H3W2110.1 (16)N1—C10—H10118.6
H4W1—O4W—H4W2110.8 (17)C9—C10—H10118.6
S1—O1—Cu1137.73 (12)N1—C11—C7123.4 (2)
C10—N1—C11117.9 (2)N1—C11—C12116.9 (2)
C10—N1—Cu1129.48 (18)C7—C11—C12119.6 (2)
C11—N1—Cu1112.51 (16)N2—C12—C4123.3 (2)
C1—N2—C12118.0 (2)N2—C12—C11117.0 (2)
C1—N2—Cu1129.16 (19)C4—C12—C11119.7 (2)
O2—S1—O1—Cu1116.80 (19)C3—C4—C5—C6175.6 (3)
O4—S1—O1—Cu1121.73 (18)C4—C5—C6—C71.3 (4)
O3—S1—O1—Cu14.2 (2)C5—C6—C7—C110.1 (4)
O1W—Cu1—O1—S110.21 (19)C5—C6—C7—C8178.6 (3)
O2W—Cu1—O1—S1103.76 (19)C11—C7—C8—C90.3 (4)
N2—Cu1—O1—S1165.22 (19)C6—C7—C8—C9178.8 (3)
O1W—Cu1—N1—C101.9 (2)C7—C8—C9—C100.4 (4)
O2W—Cu1—N1—C10146.0 (4)C11—N1—C10—C90.3 (4)
N2—Cu1—N1—C10178.6 (2)Cu1—N1—C10—C9175.0 (2)
O3W—Cu1—N1—C1087.4 (2)C8—C9—C10—N10.4 (5)
O1—Cu1—N1—C1087.5 (2)C10—N1—C11—C70.2 (4)
O1W—Cu1—N1—C11173.59 (16)Cu1—N1—C11—C7175.86 (19)
O2W—Cu1—N1—C1129.4 (5)C10—N1—C11—C12178.3 (2)
N2—Cu1—N1—C115.97 (16)Cu1—N1—C11—C125.7 (3)
O3W—Cu1—N1—C1188.02 (17)C8—C7—C11—N10.2 (4)
O1—Cu1—N1—C1197.02 (17)C6—C7—C11—N1178.8 (2)
O2W—Cu1—N2—C110.0 (2)C8—C7—C11—C12178.3 (2)
N1—Cu1—N2—C1176.2 (2)C6—C7—C11—C120.4 (4)
O3W—Cu1—N2—C198.3 (2)C1—N2—C12—C41.8 (4)
O1—Cu1—N2—C182.2 (2)Cu1—N2—C12—C4176.81 (19)
O2W—Cu1—N2—C12168.44 (17)C1—N2—C12—C11177.3 (2)
N1—Cu1—N2—C125.38 (16)Cu1—N2—C12—C114.0 (3)
O3W—Cu1—N2—C1280.13 (17)C3—C4—C12—N22.9 (4)
O1—Cu1—N2—C1299.37 (17)C5—C4—C12—N2179.2 (2)
C12—N2—C1—C20.9 (4)C3—C4—C12—C11176.3 (2)
Cu1—N2—C1—C2179.3 (2)C5—C4—C12—C111.7 (4)
N2—C1—C2—C32.5 (4)N1—C11—C12—N21.2 (3)
C1—C2—C3—C41.3 (4)C7—C11—C12—N2179.7 (2)
C2—C3—C4—C121.2 (4)N1—C11—C12—C4178.0 (2)
C2—C3—C4—C5179.1 (3)C7—C11—C12—C40.5 (4)
C12—C4—C5—C62.2 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O30.85 (1)1.80 (1)2.637 (3)172 (3)
O1W—H1W2···O4i0.84 (1)1.92 (1)2.753 (3)168 (3)
O2W—H2W1···O2ii0.85 (1)1.91 (1)2.740 (3)168 (3)
O2W—H2W2···O3i0.84 (1)1.93 (1)2.768 (3)174 (3)
O3W—H3W1···O4W0.84 (1)1.96 (1)2.787 (3)165 (3)
O3W—H3W2···O4Wiii0.85 (3)2.01 (2)2.814 (3)160 (3)
O4W—H4W1···O3iv0.84 (3)1.96 (2)2.777 (3)165 (4)
O4W—H4W2···O4v0.85 (3)1.91 (3)2.734 (3)166 (3)
Symmetry codes: (i) x+1, y+2, z+2; (ii) x1, y, z; (iii) x, y+1, z+2; (iv) x+1, y+1, z+2; (v) x1, y1, z.
 

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