Download citation
Download citation
link to html
The title compound, [Cu(C10H9N3)2(CH3OH)2](SiF6), was obtained in low yield in the reaction of dipyridylamine with Cu(BF4)2 using thermal conditions in a sealed pressure tube. The Cu-based cation lies at the centre of the triclinic unit cell, the hexa­fluoro­silicate anions lying at the corners. Cations and anions, which are centrosymmetric, are held together by hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805014777/bd6002sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805014777/bd6002Isup2.hkl
Contains datablock I

CCDC reference: 255651

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.032
  • wR factor = 0.074
  • Data-to-parameter ratio = 14.8

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
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 0 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: KappaCCD (Nonius, 1998); cell refinement: DENZO–SMN (Otwinowski & Minor, 1997); data reduction: DENZO–SMN; program(s) used to solve structure: SIR92 (Giacovazzo, 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Bis(2,2'-dipyridylamine)dimethanolcopper(II) hexafluorosilicate top
Crystal data top
[Cu(C10H9N3)2(CH4O)2](SiF6)Z = 1
Mr = 612.12F(000) = 313
Triclinic, P1Dx = 1.671 Mg m3
a = 8.0593 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 8.4334 (3) ÅCell parameters from 2188 reflections
c = 9.8099 (4) Åθ = 2.6–27.5°
α = 111.688 (2)°µ = 1.03 mm1
β = 91.079 (2)°T = 150 K
γ = 99.634 (2)°Prism, yellow
V = 608.44 (4) Å30.25 × 0.20 × 0.10 mm
Data collection top
Nonius KappaCCD
diffractometer
2684 independent reflections
Radiation source: fine-focus sealed tube2327 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
Detector resolution: 0.055 pixels mm-1θmax = 27.5°, θmin = 2.6°
ω scansh = 1010
Absorption correction: multi-scan
(SCALEPACK; Otwinowski & Minor, 1997)
k = 1010
Tmin = 0.783, Tmax = 0.904l = 1212
4671 measured reflections
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)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.074H atoms treated by a mixture of independent and constrained refinement
S = 1.06 w = 1/[σ2(Fo2) + 0.7099P]
where P = (Fo2 + 2Fc2)/3
2684 reflections(Δ/σ)max = 0.0001
181 parametersΔρmax = 0.31 e Å3
0 restraintsΔρmin = 0.47 e Å3
Special details top

Experimental. 211 frames in 7 sets of ω scans at fixed χ = 55°. Rotation/frame = 2.0 °. Crystal-detector distance = 35 mm. Measuring time = 180 s/°.

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
Cu10.50000.50000.50000.01646 (11)
Si11.00000.00000.00000.01540 (17)
F11.07772 (16)0.19673 (15)0.13482 (14)0.0234 (3)
F20.97542 (16)0.09647 (16)0.11862 (14)0.0257 (3)
F30.80195 (15)0.01991 (16)0.04965 (14)0.0233 (3)
O10.3525 (2)0.21426 (19)0.31992 (18)0.0280 (4)
H10.27050.21180.26460.042*
N10.7033 (2)0.4058 (2)0.53269 (18)0.0162 (3)
N20.6219 (2)0.5532 (2)0.33988 (19)0.0168 (4)
N30.7374 (2)0.2998 (2)0.2789 (2)0.0184 (4)
C100.7486 (3)0.4462 (3)0.1110 (2)0.0216 (5)
H100.79210.35480.04020.026*
C110.6992 (3)0.4344 (3)0.2444 (2)0.0170 (4)
C120.6660 (3)0.7238 (3)0.1901 (2)0.0230 (5)
H120.65870.82820.17640.028*
C130.8748 (3)0.3353 (3)0.6966 (2)0.0225 (5)
H130.90900.34990.79440.027*
C140.8942 (3)0.2085 (3)0.4370 (3)0.0230 (5)
H140.93960.13340.35430.028*
C150.7773 (3)0.3065 (3)0.4185 (2)0.0172 (4)
C160.7327 (3)0.5923 (3)0.0853 (2)0.0237 (5)
H160.76680.60420.00320.028*
C170.6116 (3)0.6983 (3)0.3126 (2)0.0205 (4)
H170.56400.78670.38260.025*
C180.7583 (3)0.4240 (3)0.6702 (2)0.0186 (4)
H180.71390.50180.75200.022*
C190.9417 (3)0.2234 (3)0.5770 (3)0.0243 (5)
H191.01990.15750.59210.029*
C200.3972 (3)0.0469 (3)0.2723 (3)0.0348 (6)
H20A0.44110.01990.17530.052*
H20B0.29720.04040.26550.052*
H20C0.48420.04620.34310.052*
H30.772 (3)0.223 (3)0.212 (3)0.022 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.01969 (19)0.01904 (18)0.01522 (19)0.00916 (14)0.00585 (14)0.00912 (14)
Si10.0182 (4)0.0138 (4)0.0133 (4)0.0041 (3)0.0038 (3)0.0035 (3)
F10.0259 (7)0.0167 (6)0.0215 (6)0.0034 (5)0.0024 (5)0.0006 (5)
F20.0293 (7)0.0272 (7)0.0251 (7)0.0028 (6)0.0001 (5)0.0161 (6)
F30.0198 (6)0.0239 (6)0.0235 (7)0.0062 (5)0.0064 (5)0.0047 (5)
O10.0279 (9)0.0216 (8)0.0301 (9)0.0080 (7)0.0050 (7)0.0037 (7)
N10.0186 (9)0.0164 (8)0.0153 (8)0.0057 (7)0.0030 (7)0.0067 (7)
N20.0184 (9)0.0181 (8)0.0165 (9)0.0056 (7)0.0044 (7)0.0085 (7)
N30.0243 (10)0.0180 (8)0.0147 (9)0.0107 (7)0.0073 (7)0.0049 (7)
C100.0239 (11)0.0249 (11)0.0157 (10)0.0049 (9)0.0046 (8)0.0071 (9)
C110.0168 (10)0.0183 (10)0.0149 (10)0.0029 (8)0.0022 (8)0.0052 (8)
C120.0253 (12)0.0225 (11)0.0259 (12)0.0040 (9)0.0011 (9)0.0148 (9)
C130.0233 (11)0.0259 (11)0.0195 (11)0.0036 (9)0.0019 (8)0.0107 (9)
C140.0242 (11)0.0227 (11)0.0256 (12)0.0120 (9)0.0082 (9)0.0097 (9)
C150.0179 (10)0.0164 (9)0.0186 (10)0.0040 (8)0.0040 (8)0.0075 (8)
C160.0258 (12)0.0302 (11)0.0168 (11)0.0010 (9)0.0016 (9)0.0128 (9)
C170.0215 (11)0.0187 (10)0.0236 (11)0.0059 (8)0.0032 (9)0.0099 (9)
C180.0214 (11)0.0185 (10)0.0151 (10)0.0031 (8)0.0012 (8)0.0058 (8)
C190.0218 (11)0.0265 (11)0.0298 (12)0.0101 (9)0.0009 (9)0.0143 (10)
C200.0346 (14)0.0200 (11)0.0460 (16)0.0046 (10)0.0100 (12)0.0091 (11)
Geometric parameters (Å, º) top
Cu1—N1i2.0061 (17)C10—C161.371 (3)
Cu1—N12.0061 (17)C10—C111.408 (3)
Cu1—N2i2.0165 (17)C10—H100.9500
Cu1—N22.0165 (17)C12—C171.364 (3)
Si1—F2ii1.6734 (12)C12—C161.398 (3)
Si1—F21.6734 (12)C12—H120.9500
Si1—F31.6946 (12)C13—C181.370 (3)
Si1—F3ii1.6946 (12)C13—C191.391 (3)
Si1—F11.7010 (12)C13—H130.9500
Si1—F1ii1.7010 (12)C14—C191.373 (3)
O1—C201.424 (3)C14—C151.402 (3)
O1—H10.8400C14—H140.9500
N1—C151.345 (3)C16—H160.9500
N1—C181.357 (3)C17—H170.9500
N2—C111.344 (3)C18—H180.9500
N2—C171.361 (3)C19—H190.9500
N3—C111.376 (3)C20—H20A0.9800
N3—C151.380 (3)C20—H20B0.9800
N3—H30.82 (3)C20—H20C0.9800
N1i—Cu1—N1180.000 (1)N2—C11—N3119.65 (18)
N1i—Cu1—N2i85.95 (7)N2—C11—C10121.99 (19)
N1—Cu1—N2i94.05 (7)N3—C11—C10118.32 (18)
N1i—Cu1—N294.05 (7)C17—C12—C16118.4 (2)
N1—Cu1—N285.95 (7)C17—C12—H12120.8
N2i—Cu1—N2180.0C16—C12—H12120.8
F2ii—Si1—F2180.00 (6)C18—C13—C19118.4 (2)
F2ii—Si1—F390.03 (6)C18—C13—H13120.8
F2—Si1—F389.97 (6)C19—C13—H13120.8
F2ii—Si1—F3ii89.97 (6)C19—C14—C15118.7 (2)
F2—Si1—F3ii90.03 (6)C19—C14—H14120.7
F3—Si1—F3ii180.0C15—C14—H14120.7
F2ii—Si1—F189.81 (6)N1—C15—N3119.40 (18)
F2—Si1—F190.19 (6)N1—C15—C14121.90 (19)
F3—Si1—F189.96 (6)N3—C15—C14118.70 (18)
F3ii—Si1—F190.04 (6)C10—C16—C12119.6 (2)
F2ii—Si1—F1ii90.19 (6)C10—C16—H16120.2
F2—Si1—F1ii89.81 (6)C12—C16—H16120.2
F3—Si1—F1ii90.04 (6)N2—C17—C12123.6 (2)
F3ii—Si1—F1ii89.96 (6)N2—C17—H17118.2
F1—Si1—F1ii180.00 (12)C12—C17—H17118.2
C20—O1—H1109.5N1—C18—C13123.06 (19)
C15—N1—C18117.87 (18)N1—C18—H18118.5
C15—N1—Cu1121.09 (14)C13—C18—H18118.5
C18—N1—Cu1120.63 (13)C14—C19—C13119.7 (2)
C11—N2—C17117.42 (18)C14—C19—H19120.1
C11—N2—Cu1120.15 (14)C13—C19—H19120.1
C17—N2—Cu1121.92 (14)O1—C20—H20A109.5
C11—N3—C15125.96 (18)O1—C20—H20B109.5
C11—N3—H3115.7 (17)H20A—C20—H20B109.5
C15—N3—H3114.7 (17)O1—C20—H20C109.5
C16—C10—C11118.6 (2)H20A—C20—H20C109.5
C16—C10—H10120.7H20B—C20—H20C109.5
C11—C10—H10120.7
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+2, y, z.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds