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The asymmetric unit of the title compound, [Ru(OH)(NH3)4(NO)][Pd(NO2)4]·H2O, consists of one complex [Ru(NO)(NH3)4OH]2+ cation, two half [Pd(NO2)4]2- complex anions, each anion located on an inversion centre, and a water mol­ecule of crystallization. The crystal structure exhibits an extensive hydrogen-bonding network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805016673/ac6171sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805016673/ac6171Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](O-N) = 0.003 Å
  • R factor = 0.018
  • wR factor = 0.045
  • Data-to-parameter ratio = 12.8

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.99 PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.48 PLAT230_ALERT_2_C Hirshfeld Test Diff for O61 - N6 .. 5.34 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru1 - N .. 5.76 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pd1 - N6 .. 7.49 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pd2 - N8 .. 5.50 su PLAT420_ALERT_2_C D-H Without Acceptor N3 - H3A ... ?
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 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 6 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2004); program(s) used to refine structure: SHELXTL; molecular graphics: Ball & Stick (BS) (Ozawa & Kang, 2004); software used to prepare material for publication: SHELXTL.

Tetraamminehydroxonitrosylruthenium(III) tetranitropalladate(II) monohydrate top
Crystal data top
[Ru(OH)(NH3)4(NO)][Pd(NO2)4]·H2OZ = 2
Mr = 524.68F(000) = 512
Triclinic, P1Dx = 2.349 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.0710 (3) ÅCell parameters from 4128 reflections
b = 10.0861 (5) Åθ = 2.4–32.5°
c = 10.1864 (3) ŵ = 2.30 mm1
α = 100.147 (1)°T = 150 K
β = 115.390 (1)°Prism, light yellow
γ = 108.728 (1)°0.21 × 0.19 × 0.12 mm
V = 741.78 (5) Å3
Data collection top
Bruker–Nonius X8APEX CCD area-detector
diffractometer
2756 independent reflections
Radiation source: fine-focus sealed tube2535 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.013
Detector resolution: 25 pixels mm-1θmax = 25.7°, θmin = 2.3°
φ scansh = 1110
Absorption correction: multi-scan
(SADABS; Blessing, 1995)
k = 129
Tmin = 0.643, Tmax = 0.770l = 1212
4633 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)] = 0.018Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.045H atoms treated by a mixture of independent and constrained refinement
S = 1.07 w = 1/[σ2(Fo2) + (0.0239P)2 + 0.2798P]
where P = (Fo2 + 2Fc2)/3
2756 reflections(Δ/σ)max = 0.001
215 parametersΔρmax = 1.16 e Å3
0 restraintsΔρmin = 0.47 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
Ru10.00142 (2)0.822966 (19)0.28190 (2)0.01188 (6)
Pd10.50000.50000.50000.01480 (7)
Pd20.50000.00000.00000.01464 (7)
O10.1482 (2)0.91272 (18)0.32070 (18)0.0155 (3)
H10.25500.86980.24290.019*
N10.2342 (3)0.6131 (2)0.1541 (2)0.0181 (4)
H1A0.27170.58710.05090.027*
H1B0.32490.61940.16760.027*
H1C0.20650.54200.18850.027*
N20.0799 (3)0.8803 (2)0.0824 (2)0.0161 (4)
H2A0.01720.86350.03690.024*
H2B0.05480.97930.11030.024*
H2C0.20160.82300.01360.024*
N30.2128 (3)1.0431 (2)0.4139 (2)0.0184 (4)
H3A0.31731.04370.42300.028*
H3B0.22891.07410.51060.028*
H3C0.18451.10630.36500.028*
N40.0561 (3)0.7846 (2)0.4916 (2)0.0164 (4)
H4A0.04240.70500.47430.025*
H4B0.08160.86800.56520.025*
H4C0.15390.76420.52560.025*
N0.1227 (3)0.7424 (2)0.2373 (2)0.0192 (4)
O0.1878 (3)0.6816 (2)0.1895 (2)0.0365 (5)
N50.4345 (3)0.5241 (2)0.2926 (2)0.0182 (4)
N60.6647 (3)0.4096 (2)0.4783 (2)0.0207 (4)
O510.2904 (2)0.42761 (19)0.1719 (2)0.0252 (4)
O520.5378 (3)0.6320 (2)0.2849 (2)0.0312 (4)
O610.6177 (3)0.2754 (2)0.4635 (3)0.0369 (5)
O620.7966 (3)0.4812 (3)0.4807 (3)0.0560 (7)
N70.4323 (3)0.0112 (2)0.1660 (2)0.0180 (4)
N80.5986 (3)0.2263 (2)0.0803 (2)0.0194 (4)
O710.5217 (3)0.0422 (2)0.2758 (2)0.0344 (5)
O720.3036 (2)0.0107 (2)0.1525 (2)0.0300 (4)
O810.4924 (2)0.2824 (2)0.0455 (3)0.0339 (5)
O820.7650 (2)0.3096 (2)0.1623 (2)0.0301 (4)
O1W0.0408 (3)0.2095 (2)0.2116 (2)0.0252 (4)
H20.031 (5)0.232 (4)0.196 (4)0.035 (10)*
H30.124 (5)0.286 (4)0.219 (4)0.048 (11)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.01227 (10)0.01102 (10)0.01379 (10)0.00542 (8)0.00773 (8)0.00467 (7)
Pd10.01389 (13)0.01419 (13)0.01600 (13)0.00612 (10)0.00853 (11)0.00315 (10)
Pd20.01320 (13)0.01103 (13)0.02025 (14)0.00484 (10)0.00944 (11)0.00601 (10)
O10.0133 (8)0.0156 (8)0.0160 (8)0.0070 (7)0.0068 (7)0.0039 (7)
N10.0197 (10)0.0137 (10)0.0193 (10)0.0060 (8)0.0107 (9)0.0039 (8)
N20.0172 (10)0.0145 (10)0.0170 (10)0.0062 (8)0.0097 (9)0.0061 (8)
N30.0159 (10)0.0180 (10)0.0160 (10)0.0036 (8)0.0080 (8)0.0036 (8)
N40.0185 (10)0.0168 (10)0.0187 (10)0.0096 (8)0.0115 (9)0.0083 (8)
N0.0204 (11)0.0184 (10)0.0222 (11)0.0102 (9)0.0124 (9)0.0088 (9)
O0.0456 (13)0.0401 (12)0.0497 (13)0.0319 (11)0.0352 (11)0.0189 (10)
N50.0195 (10)0.0173 (10)0.0214 (11)0.0099 (9)0.0128 (9)0.0055 (9)
N60.0264 (12)0.0183 (11)0.0156 (10)0.0116 (10)0.0095 (9)0.0033 (9)
O510.0275 (10)0.0225 (9)0.0184 (9)0.0075 (8)0.0099 (8)0.0046 (8)
O520.0335 (11)0.0263 (10)0.0368 (11)0.0067 (9)0.0251 (9)0.0125 (9)
O610.0361 (12)0.0305 (11)0.0538 (14)0.0213 (10)0.0265 (11)0.0159 (10)
O620.0426 (14)0.0364 (12)0.104 (2)0.0208 (11)0.0501 (15)0.0191 (13)
N70.0153 (10)0.0163 (10)0.0195 (11)0.0059 (8)0.0077 (9)0.0064 (8)
N80.0161 (10)0.0164 (10)0.0252 (11)0.0064 (9)0.0112 (9)0.0069 (9)
O710.0304 (11)0.0460 (12)0.0339 (11)0.0213 (10)0.0156 (9)0.0243 (10)
O720.0254 (10)0.0443 (12)0.0291 (10)0.0195 (9)0.0171 (9)0.0167 (9)
O810.0183 (9)0.0177 (9)0.0591 (14)0.0091 (8)0.0144 (9)0.0133 (9)
O820.0153 (9)0.0177 (9)0.0453 (12)0.0058 (8)0.0094 (9)0.0063 (8)
O1W0.0241 (10)0.0198 (10)0.0353 (11)0.0117 (9)0.0167 (9)0.0104 (8)
Geometric parameters (Å, º) top
Ru1—N1.742 (2)Pd1—N5i2.018 (2)
N—O1.155 (3)Pd1—N6i2.049 (2)
Ru1—O11.9618 (15)Pd2—N7ii2.040 (2)
Ru1—N12.1062 (19)Pd2—N8ii2.020 (2)
Ru1—N22.0995 (18)O1—H10.8400
Ru1—N32.1095 (19)N1—H1A0.9100
Ru1—N42.1091 (19)N1—H1B0.9100
Pd1—N52.018 (2)N1—H1C0.9100
Pd1—N62.049 (2)N2—H2A0.9100
N5—O511.245 (3)N2—H2B0.9100
N5—O521.228 (3)N2—H2C0.9100
N6—O611.241 (3)N3—H3A0.9100
N6—O621.170 (3)N3—H3B0.9100
Pd2—N72.040 (2)N3—H3C0.9100
Pd2—N82.020 (2)N4—H4A0.9100
N7—O711.231 (3)N4—H4B0.9100
N7—O721.212 (3)N4—H4C0.9100
N8—O811.226 (3)O1W—H20.72 (3)
N8—O821.241 (3)O1W—H30.85 (4)
Ru1—N—O171.8 (2)Ru1—N1—H1A109.5
N—Ru1—O1176.99 (8)Ru1—N1—H1B109.5
O1—Ru1—N189.19 (7)H1A—N1—H1B109.5
O1—Ru1—N284.90 (7)Ru1—N1—H1C109.5
O1—Ru1—N384.35 (7)H1A—N1—H1C109.5
O1—Ru1—N485.85 (7)H1B—N1—H1C109.5
N—Ru1—N189.84 (9)Ru1—N2—H2A109.5
N—Ru1—N292.27 (9)Ru1—N2—H2B109.5
N—Ru1—N396.62 (9)H2A—N2—H2B109.5
N—Ru1—N497.00 (8)Ru1—N2—H2C109.5
N1—Ru1—N290.39 (8)H2A—N2—H2C109.5
N1—Ru1—N490.49 (8)H2B—N2—H2C109.5
N2—Ru1—N389.00 (8)Ru1—N3—H3A109.5
N3—Ru1—N489.08 (8)Ru1—N3—H3B109.5
N5—Pd1—N689.53 (8)H3A—N3—H3B109.5
N7—Pd2—N890.52 (8)Ru1—N3—H3C109.5
O51—N5—O52120.1 (2)H3A—N3—H3C109.5
O61—N6—O62121.9 (2)H3B—N3—H3C109.5
O71—N7—O72121.9 (2)Ru1—N4—H4A109.5
O81—N8—O82119.35 (19)Ru1—N4—H4B109.5
N2—Ru1—N4170.69 (7)H4A—N4—H4B109.5
N1—Ru1—N3173.54 (8)Ru1—N4—H4C109.5
N5i—Pd1—N5180.0H4A—N4—H4C109.5
N5i—Pd1—N690.47 (8)H4B—N4—H4C109.5
N5i—Pd1—N6i89.53 (8)O52—N5—Pd1120.15 (16)
N5—Pd1—N6i90.47 (8)O51—N5—Pd1119.78 (15)
N6—Pd1—N6i180.000 (1)O62—N6—Pd1121.64 (17)
N8ii—Pd2—N8180.00 (14)O61—N6—Pd1116.50 (17)
N8ii—Pd2—N7ii90.52 (8)O72—N7—Pd2119.12 (16)
N8—Pd2—N7ii89.48 (8)O71—N7—Pd2119.01 (16)
N8ii—Pd2—N789.48 (8)O81—N8—Pd2119.49 (15)
N7ii—Pd2—N7180.00 (19)O82—N8—Pd2121.15 (15)
Ru1—O1—H1109.5H2—O1W—H3103 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···O81iii0.842.553.319 (3)153
O1—H1···O71iv0.842.583.025 (2)115
N1—H1A···O51iii0.912.183.064 (3)165
N1—H1B···O52v0.912.082.936 (3)157
N1—H1C···O82v0.912.233.075 (3)154
N2—H2A···O72vi0.912.392.990 (3)123
N2—H2B···O1Wvi0.912.072.974 (3)170
N2—H2B···O1Wvi0.912.072.974 (3)170
N2—H2C···O81iii0.912.253.085 (3)152
N2—H2C···O51iii0.912.513.020 (3)116
N3—H3B···O1vii0.912.142.992 (3)156
N3—H3B···O71i0.912.543.048 (3)116
N3—H3C···O1Wvi0.912.223.105 (3)165
N4—H4A···O62v0.912.293.154 (3)158
N4—H4B···O1vii0.912.062.934 (3)161
N4—H4C···O61i0.912.193.069 (3)161
O1W—H2···O82v0.72 (3)2.15 (4)2.873 (3)177 (4)
O1W—H3···O510.85 (4)2.00 (4)2.833 (3)164 (3)
Symmetry codes: (i) x+1, y+1, z+1; (iii) x, y+1, z; (iv) x1, y+1, z; (v) x1, y, z; (vi) x, y+1, z; (vii) x, y+2, z+1.
 

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