Carbonyl­(5-carboxy­pyridine-2-carboxyl­ato-κ2N,O2)chloro­bis­(triphenyl­phosphine-κP)ruthenium(II) 0.345-hydrate benzene sesquisolvate

Sukanya, D.; Natarajan, K.; Dobosh, B.; Zeller, M.

doi:10.1107/S1600536806052251

Buy article online - an online subscription or single-article purchase is required to access this article.

Carbonyl(5-carboxypyridine-2-carboxylato-κ²N,O²)chlorobis(triphenylphosphine-κP)ruthenium(II) 0.345-hydrate benzene sesquisolvate

D. Sukanya, K. Natarajan, B. Dobosh and M. Zeller

The structure of the title compound [Ru(C₇H₄NO₄)Cl(C₁₈H₁₅P)₂(CO)]·1.5C₆H₆·0.345H₂O, exhibits pairs of chains of hydrogen-bonded complex molecules that run parallel to the a axis with two different orientations, A and B, for the isocinchomeranic acid (pyridine-2,5-dicarboxylic acid) ligand as a result of disorder; the minor orientation B may occur in either strand, and is hydrogen bonded via a water molecule to a parallel chain of type A. 69% of the pairs of chains are of type A–B; the rest consist of chains in the combination A–A with no bridging water molecules.

Read article Similar articles

Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806052251/ci2218sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806052251/ci2218Isup2.hkl Contains datablock I

CCDC reference: 633643

checkCIF report

Key indicators

Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.004 Å
Disorder in main residue
R factor = 0.041
wR factor = 0.102
Data-to-parameter ratio = 18.8

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT430_ALERT_2_A Short Inter D...A Contact  O4B    ..  O6      ..       1.87 Ang.

Author Response: The occupancy of both O4B and O6 is 0.345(3) and no real short intermolecular conatcts are present


Alert level B
PLAT220_ALERT_2_B Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       4.16 Ratio
PLAT430_ALERT_2_B Short Inter D...A Contact  O2B    ..  O6      ..       2.80 Ang.

Author Response: The occupancy of both O4B and O6 is 0.345(3) and no real short intermolecular conatcts are present

PLAT430_ALERT_2_B Short Inter D...A Contact  O4B    ..  O6      ..       2.71 Ang.

Author Response: The occupancy of both O4B and O6 is 0.345(3) and no real short intermolecular conatcts are present

PLAT432_ALERT_2_B Short Inter X...Y Contact  O6     ..  C7B     ..       2.88 Ang.

Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       0.50 Ratio
PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms ..          ?
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 =          4
PLAT214_ALERT_2_C Atom O6      (Anion/Solvent) ADP max/min Ratio         4.30 prola
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.12 Ratio
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.32 Ratio
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.07
PLAT301_ALERT_3_C Main Residue  Disorder .........................      18.00 Perc.
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................       5.00 Perc.
PLAT432_ALERT_2_C Short Inter X...Y Contact  C38    ..  O2B     ..       2.98 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          2
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          4
              H1.40 O0.69

Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C53 H43.68 Cl1 N1 O5.345 P2 Ru
            Atom count from the _atom_site data:  C53 H43.7 Cl1 N1 O5.345 P2 Ru1

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

   4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  10 ALERT type 2 Indicator that the structure model may be wrong or deficient
   3 ALERT type 3 Indicator that the structure quality may be low
   4 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Bruker, 2003); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Carbonylchloro(5-carboxypyridine-2-carboxylato- κ²N,O²)bis(triphenylphosphine-κP)ruthenium(II) 0.345-hydrate benzene sesquisolvate top

Crystal data top

[Ru(C₇H₄NO₄)Cl(C₁₈H₁₅P)₂(CO)]·1.5C₆H₆·0.345H₂O	Z = 2
M_r = 978.55	F(000) = 1004.9
Triclinic, P1	D_x = 1.446 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.9570 (7) Å	Cell parameters from 7365 reflections
b = 11.0361 (7) Å	θ = 2.4–30.4°
c = 22.9009 (16) Å	µ = 0.53 mm⁻¹
α = 90.678 (1)°	T = 100 K
β = 96.295 (1)°	Block, colourless
γ = 115.790 (1)°	0.39 × 0.39 × 0.29 mm
V = 2247.2 (3) Å³

Data collection top

Bruker SMART APEX CCD diffractometer	11106 independent reflections
Radiation source: fine-focus sealed tube	10487 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.016
ω scans	θ_max = 28.3°, θ_min = 0.9°
Absorption correction: multi-scan (SADABS in SAINT-Plus; Bruker, 2003)	h = −13→13
T_min = 0.739, T_max = 0.857	k = −14→14
23291 measured reflections	l = −30→30

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.042	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.102	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0402P)² + 4.5218P] where P = (F_o² + 2F_c²)/3
11106 reflections	(Δ/σ)_max = 0.001
592 parameters	Δρ_max = 1.42 e Å⁻³
98 restraints	Δρ_min = −1.31 e Å⁻³

Special details top

Experimental. IR: 3450, 1959, 1721, 1605, 1396, 1479, 1091, 695 cm^-1.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
C1A	0.6756 (5)	0.0903 (4)	0.34682 (18)	0.0206 (8)	0.655 (3)
O1A	0.6668 (4)	0.1418 (3)	0.29778 (16)	0.0180 (6)	0.655 (3)
O2A	0.5766 (3)	0.0533 (3)	0.38034 (12)	0.0257 (6)	0.655 (3)
N1A	0.9250 (5)	0.1299 (6)	0.3278 (2)	0.0236 (7)	0.655 (3)
C2A	0.8120 (5)	0.0716 (6)	0.3635 (2)	0.0252 (9)	0.655 (3)
C3A	0.8306 (4)	−0.0024 (5)	0.40978 (18)	0.0331 (12)	0.655 (3)
H3A	0.7534	−0.0422	0.4342	0.040*	0.655 (3)
C4A	0.9621 (4)	−0.0182 (4)	0.42032 (18)	0.0385 (14)	0.655 (3)
H4A	0.9747	−0.0687	0.4519	0.046*	0.655 (3)
C5A	1.0750 (3)	0.0401 (4)	0.38460 (19)	0.0328 (11)	0.655 (3)
C6A	1.0565 (4)	0.1141 (6)	0.3384 (2)	0.0264 (9)	0.655 (3)
H6A	1.1337	0.1540	0.3139	0.032*	0.655 (3)
C7A	1.2244 (6)	0.0348 (5)	0.3971 (3)	0.0392 (12)	0.655 (3)
O3A	1.3215 (7)	0.0920 (12)	0.3601 (4)	0.0555 (16)	0.655 (3)
H3A1	1.3948	0.0736	0.3674	0.083*	0.655 (3)
O4A	1.2417 (6)	−0.0241 (6)	0.4415 (3)	0.0747 (16)	0.655 (3)
C1B	0.6998 (10)	0.0575 (8)	0.3505 (4)	0.0206 (8)	0.345 (3)
O1B	0.6813 (9)	0.1100 (8)	0.3031 (3)	0.0180 (6)	0.345 (3)
O2B	0.6032 (7)	0.0046 (6)	0.3840 (2)	0.0257 (6)	0.345 (3)
N1B	0.9518 (11)	0.1271 (13)	0.3309 (5)	0.0236 (7)	0.345 (3)
C2B	0.8440 (9)	0.0579 (12)	0.3674 (5)	0.0252 (9)	0.345 (3)
C3B	0.8775 (8)	−0.0090 (10)	0.4136 (4)	0.0331 (12)	0.345 (3)
H3B	0.8038	−0.0563	0.4385	0.040*	0.345 (3)
C4B	1.0189 (8)	−0.0066 (9)	0.4234 (4)	0.0385 (14)	0.345 (3)
H4B	1.0419	−0.0523	0.4550	0.046*	0.345 (3)
C5B	1.1268 (7)	0.0626 (9)	0.3869 (4)	0.0328 (11)	0.345 (3)
C6B	1.0932 (10)	0.1295 (12)	0.3407 (5)	0.0264 (9)	0.345 (3)
H6B	1.1669	0.1768	0.3158	0.032*	0.345 (3)
C7B	1.2789 (11)	0.0616 (12)	0.3957 (6)	0.0392 (12)	0.345 (3)
O3B	1.3620 (19)	0.106 (3)	0.3561 (8)	0.0555 (16)	0.345 (3)
H3B1	1.4397	0.0941	0.3640	0.083*	0.345 (3)
O4B	1.3068 (13)	0.0101 (13)	0.4426 (6)	0.0747 (16)	0.345 (3)
C8	1.0491 (3)	0.2859 (2)	0.22853 (9)	0.0202 (4)
C10	0.7746 (2)	0.1712 (2)	0.10056 (9)	0.0199 (4)
C11	0.8950 (3)	0.1404 (3)	0.09737 (11)	0.0280 (5)
H11	0.9644	0.1536	0.1315	0.034*
C12	0.9146 (3)	0.0905 (3)	0.04451 (11)	0.0327 (6)
H12	0.9979	0.0705	0.0427	0.039*
C13	0.8137 (3)	0.0697 (3)	−0.00542 (11)	0.0283 (5)
H13	0.8265	0.0341	−0.0412	0.034*
C14	0.6947 (3)	0.1009 (3)	−0.00307 (10)	0.0288 (5)
H14	0.6263	0.0885	−0.0375	0.035*
C15	0.6746 (3)	0.1507 (3)	0.04970 (10)	0.0254 (5)
H15	0.5915	0.1711	0.0511	0.030*
C16	0.8288 (2)	0.4294 (2)	0.14323 (10)	0.0208 (4)
C17	0.9368 (3)	0.4720 (3)	0.10410 (10)	0.0253 (5)
H17	0.9662	0.4092	0.0877	0.030*
C18	0.9588 (3)	0.6975 (3)	0.11291 (13)	0.0341 (6)
H18	1.0033	0.7887	0.1027	0.041*
C19	1.0013 (3)	0.6051 (3)	0.08914 (12)	0.0317 (5)
H19	1.0746	0.6330	0.0626	0.038*
C20	0.8516 (3)	0.6569 (3)	0.15144 (12)	0.0308 (5)
H20	0.8222	0.7201	0.1675	0.037*
C21	0.7870 (3)	0.5239 (2)	0.16662 (10)	0.0245 (5)
H21	0.7137	0.4967	0.1931	0.029*
C22	0.5518 (2)	0.1954 (2)	0.16209 (9)	0.0203 (4)
C23	0.4746 (3)	0.2648 (2)	0.13607 (10)	0.0220 (4)
H23	0.5285	0.3482	0.1195	0.026*
C24	0.3193 (3)	0.2125 (2)	0.13432 (10)	0.0236 (4)
H24	0.2676	0.2602	0.1165	0.028*
C25	0.2398 (3)	0.0912 (3)	0.15852 (11)	0.0249 (5)
H25	0.1341	0.0567	0.1582	0.030*
C26	0.3150 (3)	0.0203 (3)	0.18329 (11)	0.0279 (5)
H26	0.2603	−0.0637	0.1993	0.033*
C27	0.4702 (3)	0.0715 (2)	0.18478 (11)	0.0249 (5)
H27	0.5207	0.0218	0.2014	0.030*
C28	0.7848 (3)	0.4793 (3)	0.30593 (10)	0.0293 (5)
C29	0.6323 (3)	0.3918 (4)	0.29441 (11)	0.0391 (7)
H29	0.5998	0.2970	0.2922	0.047*
C30	0.5272 (4)	0.4448 (5)	0.28610 (13)	0.0561 (11)
H30	0.4231	0.3850	0.2783	0.067*
C31	0.5717 (5)	0.5809 (5)	0.28903 (14)	0.0624 (12)
H31	0.4991	0.6152	0.2827	0.075*
C32	0.7215 (5)	0.6679 (4)	0.30111 (14)	0.0549 (10)
H32	0.7525	0.7625	0.3036	0.066*
C33	0.8291 (4)	0.6179 (3)	0.30983 (12)	0.0386 (7)
H33	0.9327	0.6787	0.3184	0.046*
C34	1.0992 (3)	0.5593 (2)	0.30419 (10)	0.0220 (4)
C35	1.1400 (3)	0.5927 (2)	0.24826 (10)	0.0230 (4)
H35	1.0791	0.5360	0.2148	0.028*
C36	1.2690 (3)	0.7079 (3)	0.24093 (12)	0.0284 (5)
H36	1.2958	0.7298	0.2026	0.034*
C37	1.3587 (3)	0.7912 (3)	0.28948 (13)	0.0374 (6)
H37	1.4475	0.8696	0.2845	0.045*
C38	1.3185 (4)	0.7596 (3)	0.34525 (13)	0.0400 (7)
H38	1.3794	0.8169	0.3785	0.048*
C39	1.1901 (3)	0.6450 (2)	0.35279 (11)	0.0309 (5)
H39	1.1633	0.6243	0.3912	0.037*
C40	0.9456 (3)	0.3814 (2)	0.38988 (9)	0.0212 (4)
C41	0.8293 (3)	0.3545 (3)	0.42391 (10)	0.0264 (5)
H41	0.7402	0.3596	0.4076	0.032*
C42	0.8433 (3)	0.3199 (3)	0.48198 (11)	0.0273 (5)
H42	0.7626	0.2995	0.5047	0.033*
C43	0.9745 (3)	0.3153 (2)	0.50663 (10)	0.0256 (5)
H43	0.9840	0.2926	0.5463	0.031*
C44	1.0917 (3)	0.3439 (2)	0.47332 (10)	0.0244 (5)
H44	1.1822	0.3422	0.4903	0.029*
C45	1.0769 (3)	0.3749 (2)	0.41526 (10)	0.0210 (4)
H45	1.1566	0.3919	0.3924	0.025*
C46	0.4935 (3)	0.6875 (3)	0.12708 (13)	0.0387 (6)
H46	0.5257	0.7240	0.1667	0.046*
C47	0.3637 (3)	0.5685 (3)	0.11371 (13)	0.0411 (7)
H47	0.3080	0.5229	0.1443	0.049*
C48	0.3147 (3)	0.5159 (3)	0.05631 (13)	0.0358 (6)
H48	0.2243	0.4354	0.0472	0.043*
C49	0.3975 (3)	0.5808 (3)	0.01204 (12)	0.0347 (6)
H49	0.3645	0.5445	−0.0276	0.042*
C50	0.5292 (3)	0.6991 (3)	0.02552 (12)	0.0343 (6)
H50	0.5870	0.7429	−0.0048	0.041*
C51	0.5762 (3)	0.7533 (3)	0.08294 (12)	0.0331 (5)
H51	0.6649	0.8353	0.0920	0.040*
C52	0.4992 (4)	0.5603 (5)	0.44775 (16)	0.0569 (10)
H52	0.4985	0.6023	0.4118	0.068*
C53	0.4893 (4)	0.4330 (5)	0.44706 (15)	0.0559 (10)
H53	0.4822	0.3869	0.4107	0.067*
C54	0.4897 (4)	0.3712 (5)	0.49908 (17)	0.0560 (9)
H54	0.4825	0.2825	0.4986	0.067*
Cl1	0.78472 (8)	−0.01552 (6)	0.21431 (3)	0.03219 (14)
O5	1.16825 (19)	0.33152 (19)	0.21536 (8)	0.0284 (4)
P1	0.75558 (6)	0.25601 (6)	0.16633 (2)	0.01842 (11)
P2	0.92447 (6)	0.41216 (6)	0.31207 (2)	0.01951 (11)
Ru1	0.865536 (19)	0.212245 (17)	0.255580 (7)	0.01882 (6)
O6	1.5102 (7)	−0.0398 (12)	0.5137 (4)	0.089 (4)	0.345 (3)
H6C	1.4591	−0.0128	0.4891	0.133*	0.35
H6D	1.4755	−0.0259	0.5453	0.133*	0.35

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1A	0.0303 (19)	0.0101 (19)	0.0191 (13)	0.0077 (12)	−0.0008 (12)	−0.0015 (13)
O1A	0.0234 (11)	0.0147 (18)	0.0167 (11)	0.0096 (10)	0.0000 (9)	0.0042 (11)
O2A	0.0366 (13)	0.0159 (14)	0.0199 (10)	0.0069 (10)	0.0047 (9)	0.0025 (10)
N1A	0.034 (2)	0.0174 (9)	0.0149 (11)	0.0094 (14)	−0.0061 (14)	−0.0017 (7)
C2A	0.042 (3)	0.0149 (16)	0.0150 (13)	0.0109 (15)	−0.0073 (16)	−0.0006 (10)
C3A	0.056 (3)	0.0190 (13)	0.0196 (14)	0.015 (2)	−0.006 (2)	0.0025 (10)
C4A	0.063 (4)	0.0218 (16)	0.0242 (15)	0.018 (2)	−0.018 (2)	0.0019 (12)
C5A	0.046 (3)	0.0117 (19)	0.0271 (14)	0.005 (2)	−0.021 (2)	−0.0039 (13)
C6A	0.034 (3)	0.0145 (17)	0.0218 (12)	0.007 (2)	−0.0146 (17)	−0.0045 (12)
C7A	0.041 (3)	0.024 (3)	0.0392 (17)	0.007 (3)	−0.019 (3)	0.0078 (17)
O3A	0.046 (4)	0.037 (3)	0.076 (2)	0.016 (4)	−0.017 (3)	0.0202 (16)
O4A	0.074 (4)	0.050 (3)	0.081 (2)	0.020 (3)	−0.039 (3)	0.024 (2)
C1B	0.0303 (19)	0.0101 (19)	0.0191 (13)	0.0077 (12)	−0.0008 (12)	−0.0015 (13)
O1B	0.0234 (11)	0.0147 (18)	0.0167 (11)	0.0096 (10)	0.0000 (9)	0.0042 (11)
O2B	0.0366 (13)	0.0159 (14)	0.0199 (10)	0.0069 (10)	0.0047 (9)	0.0025 (10)
N1B	0.034 (2)	0.0174 (9)	0.0149 (11)	0.0094 (14)	−0.0061 (14)	−0.0017 (7)
C2B	0.042 (3)	0.0149 (16)	0.0150 (13)	0.0109 (15)	−0.0073 (16)	−0.0006 (10)
C3B	0.056 (3)	0.0190 (13)	0.0196 (14)	0.015 (2)	−0.006 (2)	0.0025 (10)
C4B	0.063 (4)	0.0218 (16)	0.0242 (15)	0.018 (2)	−0.018 (2)	0.0019 (12)
C5B	0.046 (3)	0.0117 (19)	0.0271 (14)	0.005 (2)	−0.021 (2)	−0.0039 (13)
C6B	0.034 (3)	0.0145 (17)	0.0218 (12)	0.007 (2)	−0.0146 (17)	−0.0045 (12)
C7B	0.041 (3)	0.024 (3)	0.0392 (17)	0.007 (3)	−0.019 (3)	0.0078 (17)
O3B	0.046 (4)	0.037 (3)	0.076 (2)	0.016 (4)	−0.017 (3)	0.0202 (16)
O4B	0.074 (4)	0.050 (3)	0.081 (2)	0.020 (3)	−0.039 (3)	0.024 (2)
C8	0.0250 (11)	0.0232 (10)	0.0156 (9)	0.0149 (9)	−0.0023 (8)	−0.0034 (8)
C10	0.0197 (10)	0.0248 (10)	0.0155 (9)	0.0104 (8)	0.0015 (8)	−0.0040 (8)
C11	0.0282 (12)	0.0412 (14)	0.0200 (11)	0.0219 (11)	−0.0032 (9)	−0.0074 (10)
C12	0.0321 (13)	0.0494 (16)	0.0256 (12)	0.0270 (12)	0.0014 (10)	−0.0092 (11)
C13	0.0306 (12)	0.0352 (13)	0.0194 (11)	0.0148 (10)	0.0037 (9)	−0.0071 (9)
C14	0.0260 (12)	0.0406 (14)	0.0172 (10)	0.0135 (11)	−0.0022 (9)	−0.0068 (9)
C15	0.0209 (10)	0.0369 (13)	0.0197 (11)	0.0150 (10)	−0.0012 (8)	−0.0056 (9)
C16	0.0185 (10)	0.0259 (11)	0.0176 (10)	0.0107 (9)	−0.0028 (8)	−0.0036 (8)
C17	0.0219 (11)	0.0306 (12)	0.0230 (11)	0.0117 (9)	0.0008 (8)	−0.0027 (9)
C18	0.0318 (13)	0.0275 (12)	0.0382 (14)	0.0102 (11)	−0.0020 (11)	0.0011 (10)
C19	0.0268 (12)	0.0330 (13)	0.0315 (13)	0.0096 (10)	0.0036 (10)	0.0029 (10)
C20	0.0309 (13)	0.0305 (12)	0.0326 (13)	0.0172 (11)	−0.0049 (10)	−0.0048 (10)
C21	0.0218 (10)	0.0303 (12)	0.0220 (11)	0.0135 (9)	−0.0028 (8)	−0.0057 (9)
C22	0.0171 (9)	0.0281 (11)	0.0159 (9)	0.0108 (9)	−0.0003 (7)	−0.0060 (8)
C23	0.0216 (10)	0.0289 (11)	0.0165 (10)	0.0123 (9)	0.0011 (8)	−0.0024 (8)
C24	0.0213 (10)	0.0317 (12)	0.0208 (10)	0.0151 (9)	0.0002 (8)	−0.0034 (9)
C25	0.0180 (10)	0.0313 (12)	0.0248 (11)	0.0108 (9)	0.0012 (8)	−0.0041 (9)
C26	0.0218 (11)	0.0269 (12)	0.0322 (13)	0.0090 (9)	0.0003 (9)	0.0006 (9)
C27	0.0212 (11)	0.0261 (11)	0.0276 (11)	0.0118 (9)	−0.0018 (9)	−0.0029 (9)
C28	0.0320 (12)	0.0498 (15)	0.0162 (10)	0.0292 (12)	−0.0035 (9)	−0.0087 (10)
C29	0.0315 (13)	0.072 (2)	0.0200 (12)	0.0308 (14)	−0.0030 (10)	−0.0132 (12)
C30	0.0381 (16)	0.122 (4)	0.0246 (14)	0.053 (2)	−0.0044 (12)	−0.0142 (17)
C31	0.079 (3)	0.122 (4)	0.0287 (15)	0.088 (3)	−0.0084 (15)	−0.0151 (18)
C32	0.086 (3)	0.085 (3)	0.0292 (15)	0.073 (2)	−0.0070 (15)	−0.0104 (15)
C33	0.0549 (18)	0.0557 (18)	0.0230 (12)	0.0432 (16)	−0.0059 (11)	−0.0090 (11)
C34	0.0232 (10)	0.0201 (10)	0.0224 (10)	0.0109 (9)	−0.0044 (8)	−0.0039 (8)
C35	0.0212 (10)	0.0240 (11)	0.0237 (11)	0.0114 (9)	−0.0040 (8)	−0.0046 (8)
C36	0.0277 (12)	0.0261 (12)	0.0294 (12)	0.0112 (10)	−0.0024 (9)	0.0016 (9)
C37	0.0366 (14)	0.0233 (12)	0.0377 (15)	0.0034 (11)	−0.0122 (11)	0.0021 (10)
C38	0.0504 (17)	0.0227 (12)	0.0305 (13)	0.0062 (12)	−0.0174 (12)	−0.0033 (10)
C39	0.0434 (15)	0.0216 (11)	0.0234 (11)	0.0132 (11)	−0.0082 (10)	−0.0043 (9)
C40	0.0219 (10)	0.0247 (10)	0.0160 (10)	0.0105 (9)	−0.0023 (8)	−0.0064 (8)
C41	0.0230 (11)	0.0363 (13)	0.0190 (10)	0.0136 (10)	−0.0024 (8)	−0.0081 (9)
C42	0.0270 (12)	0.0306 (12)	0.0208 (11)	0.0095 (10)	0.0035 (9)	−0.0058 (9)
C43	0.0338 (12)	0.0217 (11)	0.0192 (10)	0.0112 (10)	−0.0005 (9)	−0.0022 (8)
C44	0.0269 (11)	0.0213 (10)	0.0247 (11)	0.0119 (9)	−0.0038 (9)	−0.0034 (8)
C45	0.0209 (10)	0.0200 (10)	0.0211 (10)	0.0088 (8)	0.0001 (8)	−0.0047 (8)
C46	0.0336 (14)	0.0504 (17)	0.0285 (13)	0.0156 (13)	0.0023 (11)	−0.0043 (12)
C47	0.0381 (15)	0.0487 (17)	0.0338 (14)	0.0148 (13)	0.0120 (12)	0.0040 (12)
C48	0.0331 (14)	0.0361 (14)	0.0363 (14)	0.0140 (12)	0.0026 (11)	0.0004 (11)
C49	0.0388 (14)	0.0409 (15)	0.0262 (12)	0.0203 (12)	−0.0006 (10)	−0.0001 (11)
C50	0.0327 (13)	0.0436 (15)	0.0293 (13)	0.0189 (12)	0.0039 (10)	0.0060 (11)
C51	0.0267 (12)	0.0386 (14)	0.0324 (13)	0.0138 (11)	−0.0001 (10)	−0.0004 (11)
C52	0.0319 (16)	0.103 (3)	0.0394 (17)	0.0342 (19)	0.0013 (13)	0.0023 (18)
C53	0.0315 (15)	0.103 (3)	0.0372 (17)	0.0348 (19)	−0.0004 (12)	−0.0142 (18)
C54	0.0307 (15)	0.085 (3)	0.058 (2)	0.0313 (17)	0.0011 (14)	−0.0074 (19)
Cl1	0.0461 (4)	0.0222 (3)	0.0219 (3)	0.0120 (3)	−0.0074 (2)	−0.0068 (2)
O5	0.0238 (8)	0.0374 (10)	0.0280 (9)	0.0173 (8)	0.0029 (7)	−0.0035 (7)
P1	0.0163 (2)	0.0242 (3)	0.0155 (2)	0.0103 (2)	−0.00044 (19)	−0.0045 (2)
P2	0.0187 (3)	0.0258 (3)	0.0154 (2)	0.0122 (2)	−0.00188 (19)	−0.0060 (2)
Ru1	0.01962 (9)	0.02068 (9)	0.01352 (9)	0.00713 (7)	−0.00051 (6)	−0.00354 (6)
O6	0.020 (3)	0.164 (10)	0.083 (6)	0.036 (4)	0.014 (3)	0.090 (6)

Geometric parameters (Å, º) top

C1A—O2A	1.245 (5)	C24—C25	1.385 (3)
C1A—O1A	1.277 (5)	C24—H24	0.95
C1A—C2A	1.472 (5)	C25—C26	1.387 (3)
O1A—Ru1	2.134 (4)	C25—H25	0.95
N1A—C2A	1.39	C26—C27	1.392 (3)
N1A—C6A	1.39	C26—H26	0.95
N1A—Ru1	2.050 (3)	C27—H27	0.95
C2A—C3A	1.39	C28—C29	1.392 (4)
C3A—C4A	1.39	C28—C33	1.394 (4)
C3A—H3A	0.95	C28—P2	1.833 (2)
C4A—C5A	1.39	C29—C30	1.402 (4)
C4A—H4A	0.95	C29—H29	0.95
C5A—C6A	1.39	C30—C31	1.368 (6)
C5A—C7A	1.510 (5)	C30—H30	0.95
C6A—H6A	0.95	C31—C32	1.371 (6)
C7A—O4A	1.249 (6)	C31—H31	0.95
C7A—O3A	1.309 (7)	C32—C33	1.401 (4)
O3A—H3A1	0.84	C32—H32	0.95
C1B—O2B	1.241 (9)	C33—H33	0.95
C1B—O1B	1.268 (9)	C34—C35	1.392 (3)
C1B—C2B	1.444 (9)	C34—C39	1.401 (3)
O1B—Ru1	2.119 (8)	C34—P2	1.820 (2)
N1B—C2B	1.39	C35—C36	1.387 (3)
N1B—C6B	1.39	C35—H35	0.95
N1B—Ru1	2.239 (6)	C36—C37	1.387 (4)
C2B—C3B	1.39	C36—H36	0.95
C3B—C4B	1.39	C37—C38	1.383 (4)
C3B—H3B	0.95	C37—H37	0.95
C4B—C5B	1.39	C38—C39	1.382 (4)
C4B—H4B	0.95	C38—H38	0.95
C5B—C6B	1.39	C39—H39	0.95
C5B—C7B	1.511 (9)	C40—C41	1.393 (3)
C6B—H6B	0.95	C40—C45	1.403 (3)
C7B—O3B	1.254 (13)	C40—P2	1.825 (2)
C7B—O4B	1.280 (11)	C41—C42	1.397 (3)
O3B—H3B1	0.84	C41—H41	0.95
C8—O5	1.147 (3)	C42—C43	1.387 (4)
C8—Ru1	1.831 (2)	C42—H42	0.95
C10—C11	1.389 (3)	C43—C44	1.387 (4)
C10—C15	1.394 (3)	C43—H43	0.95
C10—P1	1.835 (2)	C44—C45	1.385 (3)
C11—C12	1.392 (3)	C44—H44	0.95
C11—H11	0.95	C45—H45	0.95
C12—C13	1.382 (4)	C46—C51	1.381 (4)
C12—H12	0.95	C46—C47	1.384 (4)
C13—C14	1.376 (4)	C46—H46	0.95
C13—H13	0.95	C47—C48	1.378 (4)
C14—C15	1.391 (3)	C47—H47	0.95
C14—H14	0.95	C48—C49	1.381 (4)
C15—H15	0.95	C48—H48	0.95
C16—C21	1.400 (3)	C49—C50	1.390 (4)
C16—C17	1.401 (3)	C49—H49	0.95
C16—P1	1.835 (2)	C50—C51	1.382 (4)
C17—C19	1.388 (4)	C50—H50	0.95
C17—H17	0.95	C51—H51	0.95
C18—C20	1.385 (4)	C52—C53	1.364 (6)
C18—C19	1.389 (4)	C52—C54ⁱ	1.394 (5)
C18—H18	0.95	C52—H52	0.95
C19—H19	0.95	C53—C54	1.380 (6)
C20—C21	1.389 (4)	C53—H53	0.95
C20—H20	0.95	C54—C52ⁱ	1.394 (5)
C21—H21	0.95	C54—H54	0.95
C22—C27	1.393 (3)	Cl1—Ru1	2.4241 (6)
C22—C23	1.399 (3)	P1—Ru1	2.3668 (6)
C22—P1	1.830 (2)	P2—Ru1	2.3505 (6)
C23—C24	1.391 (3)	O6—H6C	0.8592
C23—H23	0.95	O6—H6D	0.8733

O2A—C1A—O1A	124.7 (4)	C31—C30—C29	121.2 (3)
O2A—C1A—C2A	118.6 (4)	C31—C30—H30	119.4
O1A—C1A—C2A	116.7 (4)	C29—C30—H30	119.4
C1A—O1A—Ru1	114.9 (3)	C30—C31—C32	119.8 (3)
C2A—N1A—C6A	120.0	C30—C31—H31	120.1
C2A—N1A—Ru1	114.1 (2)	C32—C31—H31	120.1
C6A—N1A—Ru1	125.3 (2)	C31—C32—C33	120.3 (4)
C3A—C2A—N1A	120.0	C31—C32—H32	119.9
C3A—C2A—C1A	124.7 (3)	C33—C32—H32	119.9
N1A—C2A—C1A	115.3 (3)	C28—C33—C32	120.3 (3)
C2A—C3A—C4A	120.0	C28—C33—H33	119.9
C2A—C3A—H3A	120.0	C32—C33—H33	119.9
C4A—C3A—H3A	120.0	C35—C34—C39	118.6 (2)
C5A—C4A—C3A	120.0	C35—C34—P2	119.53 (17)
C5A—C4A—H4A	120.0	C39—C34—P2	121.7 (2)
C3A—C4A—H4A	120.0	C36—C35—C34	120.6 (2)
C4A—C5A—C6A	120.0	C36—C35—H35	119.7
C4A—C5A—C7A	121.9 (3)	C34—C35—H35	119.7
C6A—C5A—C7A	118.0 (3)	C37—C36—C35	120.2 (3)
C5A—C6A—N1A	120.0	C37—C36—H36	119.9
C5A—C6A—H6A	120.0	C35—C36—H36	119.9
N1A—C6A—H6A	120.0	C38—C37—C36	119.7 (3)
O4A—C7A—O3A	127.0 (6)	C38—C37—H37	120.1
O4A—C7A—C5A	116.5 (5)	C36—C37—H37	120.1
O3A—C7A—C5A	116.4 (5)	C39—C38—C37	120.3 (2)
O2B—C1B—O1B	125.4 (8)	C39—C38—H38	119.8
O2B—C1B—C2B	116.3 (8)	C37—C38—H38	119.8
O1B—C1B—C2B	118.3 (8)	C38—C39—C34	120.5 (3)
C1B—O1B—Ru1	120.0 (6)	C38—C39—H39	119.7
C2B—N1B—C6B	120.0	C34—C39—H39	119.7
C2B—N1B—Ru1	113.3 (5)	C41—C40—C45	118.8 (2)
C6B—N1B—Ru1	126.5 (5)	C41—C40—P2	121.28 (17)
C3B—C2B—N1B	120.0	C45—C40—P2	119.76 (17)
C3B—C2B—C1B	125.7 (7)	C40—C41—C42	120.3 (2)
N1B—C2B—C1B	114.2 (7)	C40—C41—H41	119.9
C2B—C3B—C4B	120.0	C42—C41—H41	119.9
C2B—C3B—H3B	120.0	C43—C42—C41	120.2 (2)
C4B—C3B—H3B	120.0	C43—C42—H42	119.9
C5B—C4B—C3B	120.0	C41—C42—H42	119.9
C5B—C4B—H4B	120.0	C44—C43—C42	119.9 (2)
C3B—C4B—H4B	120.0	C44—C43—H43	120.1
C6B—C5B—C4B	120.0	C42—C43—H43	120.1
C6B—C5B—C7B	119.5 (6)	C45—C44—C43	120.1 (2)
C4B—C5B—C7B	120.4 (6)	C45—C44—H44	120.0
C5B—C6B—N1B	120.0	C43—C44—H44	120.0
C5B—C6B—H6B	120.0	C44—C45—C40	120.7 (2)
N1B—C6B—H6B	120.0	C44—C45—H45	119.6
O3B—C7B—O4B	126.7 (13)	C40—C45—H45	119.6
O3B—C7B—C5B	117.6 (11)	C51—C46—C47	120.1 (3)
O4B—C7B—C5B	115.6 (10)	C51—C46—H46	120.0
C7B—O3B—H3B1	109.5	C47—C46—H46	120.0
O5—C8—Ru1	175.34 (19)	C48—C47—C46	120.4 (3)
C11—C10—C15	118.4 (2)	C48—C47—H47	119.8
C11—C10—P1	122.36 (17)	C46—C47—H47	119.8
C15—C10—P1	118.79 (17)	C47—C48—C49	119.8 (3)
C10—C11—C12	120.5 (2)	C47—C48—H48	120.1
C10—C11—H11	119.7	C49—C48—H48	120.1
C12—C11—H11	119.7	C48—C49—C50	119.9 (3)
C13—C12—C11	120.4 (2)	C48—C49—H49	120.1
C13—C12—H12	119.8	C50—C49—H49	120.1
C11—C12—H12	119.8	C51—C50—C49	120.2 (3)
C14—C13—C12	119.8 (2)	C51—C50—H50	119.9
C14—C13—H13	120.1	C49—C50—H50	119.9
C12—C13—H13	120.1	C46—C51—C50	119.6 (3)
C13—C14—C15	120.0 (2)	C46—C51—H51	120.2
C13—C14—H14	120.0	C50—C51—H51	120.2
C15—C14—H14	120.0	C53—C52—C54ⁱ	120.3 (4)
C14—C15—C10	120.9 (2)	C53—C52—H52	119.9
C14—C15—H15	119.6	C54ⁱ—C52—H52	119.9
C10—C15—H15	119.6	C52—C53—C54	120.1 (3)
C21—C16—C17	118.5 (2)	C52—C53—H53	119.9
C21—C16—P1	121.74 (18)	C54—C53—H53	119.9
C17—C16—P1	119.61 (18)	C53—C54—C52ⁱ	119.6 (4)
C19—C17—C16	120.6 (2)	C53—C54—H54	120.2
C19—C17—H17	119.7	C52ⁱ—C54—H54	120.2
C16—C17—H17	119.7	C22—P1—C10	102.55 (10)
C20—C18—C19	120.0 (3)	C22—P1—C16	105.87 (10)
C20—C18—H18	120.0	C10—P1—C16	99.54 (10)
C19—C18—H18	120.0	C22—P1—Ru1	113.44 (8)
C17—C19—C18	120.1 (2)	C10—P1—Ru1	114.21 (7)
C17—C19—H19	120.0	C16—P1—Ru1	119.14 (7)
C18—C19—H19	120.0	C34—P2—C40	103.38 (10)
C18—C20—C21	120.1 (2)	C34—P2—C28	103.26 (12)
C18—C20—H20	120.0	C40—P2—C28	104.01 (11)
C21—C20—H20	120.0	C34—P2—Ru1	118.32 (8)
C20—C21—C16	120.7 (2)	C40—P2—Ru1	108.75 (8)
C20—C21—H21	119.7	C28—P2—Ru1	117.39 (8)
C16—C21—H21	119.7	C8—Ru1—N1A	97.39 (15)
C27—C22—C23	118.9 (2)	C8—Ru1—O1B	165.74 (19)
C27—C22—P1	117.56 (17)	C8—Ru1—O1A	172.39 (13)
C23—C22—P1	123.53 (18)	N1A—Ru1—O1A	78.48 (16)
C24—C23—C22	120.4 (2)	C8—Ru1—N1B	91.8 (3)
C24—C23—H23	119.8	O1B—Ru1—N1B	73.9 (3)
C22—C23—H23	119.8	C8—Ru1—P2	91.50 (7)
C25—C24—C23	120.2 (2)	N1A—Ru1—P2	90.9 (2)
C25—C24—H24	119.9	O1B—Ru1—P2	89.2 (2)
C23—C24—H24	119.9	O1A—Ru1—P2	82.24 (10)
C24—C25—C26	119.8 (2)	N1B—Ru1—P2	92.0 (4)
C24—C25—H25	120.1	C8—Ru1—P1	89.74 (7)
C26—C25—H25	120.1	N1A—Ru1—P1	166.90 (19)
C25—C26—C27	120.3 (2)	O1B—Ru1—P1	104.2 (2)
C25—C26—H26	119.9	O1A—Ru1—P1	95.57 (9)
C27—C26—H26	119.9	N1B—Ru1—P1	167.9 (4)
C26—C27—C22	120.4 (2)	P2—Ru1—P1	99.94 (2)
C26—C27—H27	119.8	C8—Ru1—Cl1	96.73 (7)
C22—C27—H27	119.8	N1A—Ru1—Cl1	80.5 (2)
C29—C28—C33	119.0 (3)	O1B—Ru1—Cl1	80.9 (2)
C29—C28—P2	120.0 (2)	O1A—Ru1—Cl1	88.93 (10)
C33—C28—P2	120.9 (2)	N1B—Ru1—Cl1	80.1 (4)
C28—C29—C30	119.4 (3)	P2—Ru1—Cl1	168.75 (2)
C28—C29—H29	120.3	P1—Ru1—Cl1	87.79 (2)
C30—C29—H29	120.3	H6C—O6—H6D	97.0

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3B—H3B1···O2Bⁱⁱ	0.84	2.25	3.07 (2)	165
O3A—H3A1···O2Aⁱⁱ	0.84	1.91	2.747 (10)	173
O6—H6C···O4B	0.86	1.87	2.706 (11)	165
O6—H6D···O2Bⁱⁱⁱ	0.87	1.93	2.802 (12)	177
O6—H6D···O2Aⁱⁱⁱ	0.87	1.83	2.648 (9)	156

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

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

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

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page

Carbonyl­(5-carboxy­pyridine-2-carboxyl­ato-κ2N,O2)chloro­bis­(triphenyl­phosphine-κP)ruthenium(II) 0.345-hydrate benzene sesquisolvate

Supporting information

Key indicators

checkCIF/PLATON results

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

Buy online

Carbonyl(5-carboxypyridine-2-carboxylato-κ²N,O²)chlorobis(triphenylphosphine-κP)ruthenium(II) 0.345-hydrate benzene sesquisolvate