Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The structure of the title compound, [RuCl(C23H21N5)]ClO4·CH4O, has been determined at 113 K, revealing a mononuclear six-coordinate structure with a 0.263 (2) Å displacement of the RuII atom from the N4 equatorial plane.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804032209/sj6039sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804032209/sj6039Isup2.hkl
Contains datablock I

CCDC reference: 263526

Key indicators

  • Single-crystal X-ray study
  • T = 113 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.044
  • wR factor = 0.119
  • Data-to-parameter ratio = 17.2

checkCIF/PLATON results

No syntax errors found



Alert level B ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 Tmin and Tmax reported: 0.444 0.841 Tmin' and Tmax expected: 0.652 0.841 RR' = 0.681 Please check that your absorption correction is appropriate. PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.67
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl2
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 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 2 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: PROCESS-AUTO (Rigaku Corporation, 1998); cell refinement: PROCESS-AUTO; data reduction: TEXSAN Version 1.11 (Molecular Structure Corporation & Rigaku Corporation, 2000); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: TEXSAN Version 1.10 (Molecular Structure Corporation, 1985–1999); molecular graphics: TEXSAN Version 1.11; software used to prepare material for publication: TEXSAN Version 1.11.

(I) top
Crystal data top
[RuCl(C23H21N5)]ClO4·CH4OF(000) = 1288.00
Mr = 635.47Dx = 1.650 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
a = 14.768 (2) ÅCell parameters from 31496 reflections
b = 13.048 (2) Åθ = 2.2–27.5°
c = 15.084 (2) ŵ = 0.87 mm1
β = 118.349 (3)°T = 113 K
V = 2558.0 (5) Å3Block, orange
Z = 40.48 × 0.45 × 0.20 mm
Data collection top
Rigaku R-AXIS RAPID imaging-plate
diffractometer
4780 reflections with F2 > 2σ(F2)
Detector resolution: 10.00 pixels mm-1Rint = 0.042
ω scansθmax = 27.5°
Absorption correction: multi-scan
(Higashi, 1995)
h = 1919
Tmin = 0.444, Tmax = 0.841k = 1616
17293 measured reflectionsl = 1919
5745 independent reflections
Refinement top
Refinement on F2H-atom parameters not refined
R[F2 > 2σ(F2)] = 0.044 w = 1/{σ2(Fo2) + [0.06(max(Fo2,0) + 2Fc2)/3]2}
wR(F2) = 0.120(Δ/σ)max = 0.0003
S = 1.32Δρmax = 1.18 e Å3
5743 reflectionsΔρmin = 1.24 e Å3
334 parameters
Special details top

Refinement. Refinement using reflections with F2 > -10.0 σ(F2). The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ru10.70547 (2)0.22301 (2)1.00203 (2)0.02233 (7)
Cl10.59649 (6)0.09344 (6)1.01679 (7)0.0329 (2)
Cl20.85078 (8)0.64572 (8)0.91484 (8)0.0463 (3)
O10.9151 (3)0.7323 (2)0.9355 (3)0.059 (1)
O20.8308 (4)0.6020 (3)0.8228 (3)0.096 (1)
O30.7648 (3)0.6672 (3)0.9264 (5)0.112 (2)
O40.9089 (3)0.5672 (2)0.9878 (2)0.0594 (9)
O50.5929 (2)0.7398 (2)0.5370 (2)0.0497 (8)
N10.7957 (2)0.3330 (2)0.9881 (2)0.0260 (7)
N20.8360 (2)0.1917 (2)1.1354 (2)0.0268 (7)
N30.7716 (2)0.1308 (2)0.9374 (2)0.0273 (7)
N40.5980 (2)0.2829 (2)0.8662 (2)0.0252 (7)
N50.6634 (2)0.3426 (2)1.0624 (2)0.0232 (6)
C10.8845 (2)0.3534 (3)1.0891 (3)0.0305 (8)
C20.9129 (3)0.2585 (3)1.1544 (3)0.0304 (9)
C31.0116 (3)0.2428 (3)1.2317 (3)0.0369 (10)
C41.0305 (3)0.1578 (3)1.2949 (3)0.042 (1)
C50.9514 (3)0.0915 (3)1.2767 (3)0.041 (1)
C60.8545 (3)0.1095 (3)1.1954 (3)0.0327 (9)
C70.8292 (3)0.2987 (3)0.9134 (3)0.0309 (9)
C80.8344 (3)0.1830 (3)0.9104 (2)0.0317 (9)
C90.8963 (3)0.1334 (3)0.8793 (3)0.041 (1)
C100.8935 (3)0.0265 (3)0.8736 (3)0.047 (1)
C110.8302 (3)0.0269 (3)0.9006 (3)0.044 (1)
C120.7710 (3)0.0268 (3)0.9330 (3)0.0339 (9)
C130.7163 (2)0.4189 (2)0.9492 (2)0.0270 (8)
C140.6264 (2)0.3789 (3)0.8555 (2)0.0276 (8)
C150.5758 (3)0.4337 (3)0.7665 (3)0.0331 (9)
C160.4900 (3)0.3893 (3)0.6869 (3)0.0377 (10)
C170.4572 (3)0.2945 (3)0.6995 (3)0.0377 (10)
C180.5126 (3)0.2427 (3)0.7894 (3)0.0302 (9)
C190.6787 (2)0.4335 (2)1.0266 (2)0.0273 (8)
C200.6577 (3)0.5271 (3)1.0549 (3)0.0324 (9)
C210.6212 (3)0.5289 (3)1.1253 (3)0.0355 (9)
C220.6062 (3)0.4376 (3)1.1619 (3)0.0337 (9)
C230.6270 (3)0.3458 (3)1.1296 (2)0.0294 (8)
C240.6815 (4)0.6902 (4)0.6023 (4)0.071 (1)
H10.94190.37411.08120.0366*
H20.86670.40671.12090.0366*
H31.06550.28881.24180.0443*
H41.09720.14621.34970.0500*
H50.96270.03391.31920.0486*
H60.80020.06271.18200.0393*
H70.89540.32620.93200.0371*
H80.78140.32310.84850.0371*
H90.94050.17120.86180.0491*
H100.93510.00900.85120.0569*
H110.82740.09960.89710.0529*
H120.72830.01030.95300.0406*
H130.74330.48030.93730.0323*
H140.59900.49980.76000.0397*
H150.45440.42430.62440.0453*
H160.39690.26480.64680.0452*
H170.48990.17680.79730.0362*
H180.66780.58891.02740.0389*
H190.60700.59221.14740.0427*
H200.58140.43771.20960.0405*
H210.61550.28341.15520.0353*
H220.66540.62280.61420.0858*
H230.71400.72670.66420.0858*
H240.72660.68670.57380.0858*
H250.53380.70060.51810.0436*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.0229 (2)0.0187 (1)0.0281 (2)0.00078 (9)0.0144 (1)0.00029 (9)
Cl10.0337 (4)0.0228 (4)0.0492 (5)0.0042 (3)0.0255 (4)0.0005 (3)
Cl20.0426 (5)0.0462 (5)0.0536 (6)0.0102 (4)0.0256 (5)0.0003 (4)
O10.049 (2)0.032 (2)0.112 (3)0.010 (1)0.050 (2)0.006 (2)
O20.137 (4)0.080 (3)0.047 (2)0.022 (3)0.023 (2)0.016 (2)
O30.074 (3)0.057 (2)0.255 (6)0.029 (2)0.118 (4)0.046 (3)
O40.058 (2)0.047 (2)0.058 (2)0.002 (1)0.015 (2)0.011 (1)
O50.044 (2)0.037 (1)0.052 (2)0.012 (1)0.009 (1)0.005 (1)
N10.028 (1)0.024 (1)0.030 (1)0.001 (1)0.017 (1)0.001 (1)
N20.027 (1)0.027 (1)0.030 (1)0.004 (1)0.016 (1)0.001 (1)
N30.028 (1)0.026 (1)0.028 (1)0.002 (1)0.014 (1)0.000 (1)
N40.025 (1)0.026 (1)0.028 (1)0.001 (1)0.016 (1)0.001 (1)
N50.021 (1)0.022 (1)0.028 (1)0.001 (1)0.012 (1)0.000 (1)
C10.024 (2)0.031 (2)0.035 (2)0.002 (1)0.013 (1)0.001 (1)
C20.030 (2)0.032 (2)0.033 (2)0.001 (1)0.018 (2)0.002 (1)
C30.026 (2)0.045 (2)0.037 (2)0.002 (2)0.013 (2)0.000 (2)
C40.033 (2)0.054 (2)0.034 (2)0.011 (2)0.013 (2)0.006 (2)
C50.045 (2)0.041 (2)0.037 (2)0.017 (2)0.021 (2)0.009 (2)
C60.042 (2)0.027 (2)0.035 (2)0.007 (1)0.023 (2)0.002 (1)
C70.029 (2)0.034 (2)0.035 (2)0.003 (1)0.020 (2)0.003 (1)
C80.031 (2)0.036 (2)0.029 (2)0.001 (1)0.016 (1)0.001 (1)
C90.038 (2)0.049 (2)0.043 (2)0.006 (2)0.026 (2)0.001 (2)
C100.051 (2)0.050 (2)0.050 (2)0.014 (2)0.031 (2)0.007 (2)
C110.046 (2)0.033 (2)0.051 (2)0.008 (2)0.021 (2)0.008 (2)
C120.038 (2)0.028 (2)0.036 (2)0.004 (1)0.018 (2)0.003 (1)
C130.027 (2)0.022 (1)0.035 (2)0.003 (1)0.017 (1)0.000 (1)
C140.028 (2)0.029 (2)0.031 (2)0.003 (1)0.018 (1)0.001 (1)
C150.039 (2)0.033 (2)0.034 (2)0.009 (2)0.023 (2)0.005 (1)
C160.035 (2)0.048 (2)0.033 (2)0.014 (2)0.019 (2)0.005 (2)
C170.028 (2)0.052 (2)0.033 (2)0.005 (2)0.014 (2)0.006 (2)
C180.028 (2)0.034 (2)0.032 (2)0.002 (1)0.017 (1)0.006 (1)
C190.025 (2)0.024 (1)0.034 (2)0.002 (1)0.015 (1)0.002 (1)
C200.033 (2)0.022 (2)0.041 (2)0.002 (1)0.016 (2)0.002 (1)
C210.040 (2)0.029 (2)0.039 (2)0.005 (2)0.019 (2)0.006 (1)
C220.033 (2)0.037 (2)0.036 (2)0.002 (2)0.020 (2)0.003 (1)
C230.029 (2)0.026 (2)0.036 (2)0.001 (1)0.018 (1)0.000 (1)
C240.051 (3)0.040 (2)0.089 (4)0.007 (2)0.004 (3)0.010 (3)
Geometric parameters (Å, º) top
Ru1—Cl12.4162 (8)C14—C151.384 (4)
Ru1—N12.036 (3)C15—C161.392 (5)
Ru1—N22.060 (3)C16—C171.375 (6)
Ru1—N32.062 (3)C17—C181.383 (5)
Ru1—N42.059 (3)C19—C201.377 (4)
Ru1—N52.047 (3)C20—C211.401 (5)
Cl2—O11.413 (3)C21—C221.374 (5)
Cl2—O21.396 (4)C22—C231.382 (5)
Cl2—O31.390 (3)O5—H250.931
Cl2—O41.449 (3)C1—H10.950
O5—C241.371 (6)C1—H20.950
N1—C11.488 (4)C3—H30.950
N1—C71.497 (4)C4—H40.950
N1—C131.524 (4)C5—H50.950
N2—C21.350 (4)C6—H60.950
N2—C61.344 (4)C7—H70.950
N3—C81.360 (4)C7—H80.950
N3—C121.359 (4)C9—H90.950
N4—C141.356 (4)C10—H100.950
N4—C181.349 (4)C11—H110.950
N5—C191.364 (4)C12—H120.950
N5—C231.355 (4)C13—H130.950
C1—C21.513 (5)C15—H140.950
C2—C31.383 (5)C16—H150.950
C3—C41.402 (6)C17—H160.950
C4—C51.371 (6)C18—H170.950
C5—C61.394 (5)C20—H180.950
C7—C81.513 (5)C21—H190.950
C8—C91.373 (5)C22—H200.950
C9—C101.396 (6)C23—H210.950
C10—C111.373 (6)C24—H220.950
C11—C121.378 (5)C24—H230.950
C13—C141.500 (4)C24—H240.950
C13—C191.525 (4)
CL1···O5i3.158 (3)O3···C17vii3.346 (6)
CL1···C16ii3.598 (4)O3···C133.371 (5)
CL1···CL1iii3.599 (2)O3···C203.536 (5)
O1···C3iv3.199 (5)O4···O4iv3.084 (7)
O1···C11v3.330 (5)O4···C5viii3.164 (5)
O1···C1iv3.345 (5)O4···C4viii3.186 (5)
O1···C9iv3.354 (5)O4···C133.257 (4)
O1···C7iv3.384 (5)O4···C13.282 (5)
O1···C2iv3.403 (5)O4···N13.485 (4)
O1···C8iv3.486 (5)O5···C20ix3.161 (4)
O2···C243.207 (7)O5···C21ix3.244 (5)
O2···C5vi3.349 (7)O5···C17x3.312 (5)
O2···C3iv3.466 (6)O5···C23vii3.320 (4)
O2···C6vi3.476 (6)O5···C16x3.438 (5)
Cl1—Ru1—N1179.28 (8)C15—C16—C17119.5 (3)
Cl1—Ru1—N297.27 (8)C16—C17—C18119.5 (3)
Cl1—Ru1—N396.94 (8)N4—C18—C17121.9 (3)
Cl1—Ru1—N497.16 (8)N5—C19—C13112.5 (3)
Cl1—Ru1—N597.85 (7)N5—C19—C20123.0 (3)
N1—Ru1—N283.4 (1)C13—C19—C20124.4 (3)
N1—Ru1—N383.2 (1)C19—C20—C21118.2 (3)
N1—Ru1—N482.1 (1)C20—C21—C22118.9 (3)
N1—Ru1—N582.0 (1)C21—C22—C23120.3 (3)
N2—Ru1—N385.0 (1)N5—C23—C22121.6 (3)
N2—Ru1—N4165.6 (1)C24—O5—H25113.3
N2—Ru1—N593.3 (1)N1—C1—H1109.1
N3—Ru1—N493.7 (1)N1—C1—H2109.1
N3—Ru1—N5165.2 (1)C2—C1—H1109.1
N4—Ru1—N584.25 (10)C2—C1—H2109.1
O1—Cl2—O2110.4 (3)H1—C1—H2109.5
O1—Cl2—O3111.7 (2)C2—C3—H3120.7
O1—Cl2—O4107.7 (2)C4—C3—H3120.7
O2—Cl2—O3115.6 (4)C3—C4—H4120.4
O2—Cl2—O4103.6 (2)C5—C4—H4120.4
O3—Cl2—O4107.1 (3)C4—C5—H5120.3
Ru1—N1—C1108.8 (2)C6—C5—H5120.3
Ru1—N1—C7109.5 (2)N2—C6—H6119.2
Ru1—N1—C1397.8 (2)C5—C6—H6119.3
C1—N1—C7112.2 (2)N1—C7—H7109.1
C1—N1—C13113.9 (2)N1—C7—H8109.1
C7—N1—C13113.5 (2)C8—C7—H7109.1
Ru1—N2—C2112.5 (2)C8—C7—H8109.1
Ru1—N2—C6127.7 (2)H7—C7—H8109.5
C2—N2—C6119.3 (3)C8—C9—H9120.4
Ru1—N3—C8113.1 (2)C10—C9—H9120.4
Ru1—N3—C12127.8 (2)C9—C10—H10120.3
C8—N3—C12118.3 (3)C11—C10—H10120.3
Ru1—N4—C14109.5 (2)C10—C11—H11120.5
Ru1—N4—C18132.2 (2)C12—C11—H11120.5
C14—N4—C18118.3 (3)N3—C12—H12118.8
Ru1—N5—C19110.2 (2)C11—C12—H12118.8
Ru1—N5—C23131.9 (2)N1—C13—H13112.2
C19—N5—C23117.9 (3)C14—C13—H13112.2
N1—C1—C2110.9 (3)C19—C13—H13112.2
N2—C2—C1116.4 (3)C14—C15—H14120.9
N2—C2—C3121.9 (3)C16—C15—H14120.9
C1—C2—C3121.7 (3)C15—C16—H15120.3
C2—C3—C4118.7 (4)C17—C16—H15120.3
C3—C4—C5119.2 (3)C16—C17—H16120.3
C4—C5—C6119.4 (3)C18—C17—H16120.3
N2—C6—C5121.5 (3)N4—C18—H17119.1
N1—C7—C8111.1 (3)C17—C18—H17119.1
N3—C8—C7116.0 (3)C19—C20—H18120.9
N3—C8—C9121.8 (3)C21—C20—H18120.9
C7—C8—C9122.2 (3)C20—C21—H19120.5
C8—C9—C10119.1 (4)C22—C21—H19120.5
C9—C10—C11119.5 (3)C21—C22—H20119.9
C10—C11—C12118.9 (4)C23—C22—H20119.9
N3—C12—C11122.3 (3)N5—C23—H21119.2
N1—C13—C14106.4 (2)C22—C23—H21119.2
N1—C13—C19106.9 (2)O5—C24—H22109.5
C14—C13—C19106.5 (3)O5—C24—H23109.5
N4—C14—C13113.2 (3)O5—C24—H24109.5
N4—C14—C15122.5 (3)H22—C24—H23109.5
C13—C14—C15124.3 (3)H22—C24—H24109.5
C14—C15—C16118.2 (3)H23—C24—H24109.5
Symmetry codes: (i) x+1, y1/2, z+3/2; (ii) x, y+1/2, z+1/2; (iii) x+1, y, z+2; (iv) x+2, y+1, z+2; (v) x, y+1, z; (vi) x, y+1/2, z1/2; (vii) x+1, y+1/2, z+3/2; (viii) x+2, y+1/2, z+5/2; (ix) x, y+3/2, z1/2; (x) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H25···Cl1vii0.932.233.158 (3)174
Symmetry code: (vii) x+1, y+1/2, z+3/2.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

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