fac-Aqua­(2,2'-bipyrazine)tricarbonyl­rhenium(I) hexafluorophosphate dihydrate

The crystal structure of the title compound, [Re(C₈H₆N₄)(CO)₃(H₂O)]PF₆·2H₂O, shows the Re center to be in a distorted octa­hedral geometry with a facial distribution of the carbonyl ligands. Two other water mol­ecules are hydrogen bonded to the coordinated water mol­ecule. The cation lies on a crystallographic mirror plane, across which the anion is disordered.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.004 Å
• Disorder in solvent or counterion
• R factor = 0.016
• wR factor = 0.037
• Data-to-parameter ratio = 11.6

checkCIF/PLATON results

No syntax errors found



Alert level A
DIFF019_ALERT_1_A  _diffrn_standards_number is missing
            Number of standards used in measurement.
DIFF020_ALERT_1_A  _diffrn_standards_interval_count and
            _diffrn_standards_interval_time are missing. Number of measurements
            between standards or time (min) between standards.
DIFF022_ALERT_1_A  _diffrn_standards_decay_% is missing
            Percentage decrease in standards intensity.

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for         F3
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for         F4
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for         F6
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for         P2
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.22
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      33.00 Perc.
PLAT431_ALERT_2_C Short Inter HL..A Contact  F6     ..  O1      ..       2.98 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H102   ..  O1      ..       2.62 Ang.
PLAT751_ALERT_4_C Bond    Calc     0.97000, Rep  0.9713(16) ......  Senseless su
              O3   -H103    1.555   1.555
PLAT751_ALERT_4_C Bond    Calc     0.91000, Rep    0.910(2) ......  Senseless su
              O101 -H101    1.555   1.555
PLAT751_ALERT_4_C Bond    Calc     0.93000, Rep    0.932(3) ......  Senseless su
              O101 -H102    1.555   1.555
PLAT752_ALERT_4_C Angle   Calc      117.00, Rep  117.07(15) ......  Senseless su
              RE1  -O3   -H103    1.555   1.555   1.555
PLAT752_ALERT_4_C Angle   Calc       97.00, Rep     97.2(2) ......  Senseless su
              H101 -O101 -H102    1.555   1.555   1.555
PLAT755_ALERT_4_C D-H     Calc     0.91000, Rep    0.910(2) ......  Senseless su
              O101 -H101    1.555   1.555
PLAT755_ALERT_4_C D-H     Calc     0.93000, Rep    0.933(3) ......  Senseless su
              O101 -H102    1.555   1.555
PLAT755_ALERT_4_C D-H     Calc     0.93000, Rep    0.933(3) ......  Senseless su
              O101 -H102    1.555   1.555
PLAT755_ALERT_4_C D-H     Calc     0.93000, Rep    0.933(3) ......  Senseless su
              O101 -H102    1.555   1.555
PLAT755_ALERT_4_C D-H     Calc     0.97000, Rep  0.9710(17) ......  Senseless su
              O3   -H103    1.555   1.555
PLAT756_ALERT_4_C H...A   Calc     1.99000, Rep    1.994(3) ......  Senseless su
              H101 -N2      1.555   2.655
PLAT756_ALERT_4_C H...A   Calc     2.62000, Rep    2.622(2) ......  Senseless su
              H102 -O1      1.555   2.654
PLAT756_ALERT_4_C H...A   Calc     1.67000, Rep    1.670(2) ......  Senseless su
              H103 -O101    1.555   6.657

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K

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

   5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 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
  20 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

---

Computing details

Data collection: APEX2 (Bruker, 2006); cell refinement: APEX2; data reduction: SAINT (Bruker, 2006); program(s) used to solve structure: SHELXTL (Bruker, 2006); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

fac-Aqua(bipyrazine)tricarbonylrhenium(I) hexafluorophosphate dihydrate

Crystal data

[Re(C8H6N4)(CO)3(H2O)]PF6·2H2O	Dx = 2.258 Mg m^−3
Mr = 627.42	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pnma	Cell parameters from 8341 reflections
a = 15.5869 (6) Å	θ = 3.0–43.0°
b = 13.1068 (5) Å	µ = 6.77 mm^−1
c = 9.0349 (4) Å	T = 293 K
V = 1845.78 (13) Å^3	Block, orange
Z = 4	0.42 × 0.24 × 0.20 mm
F(000) = 1192

Data collection

Bruker Kappa-APEXII diffractometer	1892 independent reflections
Radiation source: fine-focus sealed tube	1880 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.034
φ and ω scans	θmax = 26.0°, θmin = 3.5°
Absorption correction: numerical (SADABS; Bruker, 2006)	h = −19→19
Tmin = 0.158, Tmax = 0.450	k = −16→16
49927 measured reflections	l = −11→11

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.016	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.037	H-atom parameters constrained
S = 1.17	w = 1/[σ^2(Fo^2) + (0.0071P)^2 + 4.7736P] where P = (Fo^2 + 2Fc^2)/3
1892 reflections	(Δ/σ)max = 0.001
163 parameters	Δρmax = 0.68 e Å^−3
0 restraints	Δρmin = −0.67 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.82905 (17)	0.1471 (2)	0.9631 (3)	0.0246 (6)
C2	0.7097 (3)	0.2500	0.8145 (5)	0.0273 (9)
C3	0.84846 (19)	0.0471 (2)	0.6279 (3)	0.0265 (6)
H3	0.8291	0.0141	0.7126	0.032*
C4	0.8740 (2)	−0.0096 (2)	0.5074 (4)	0.0310 (7)
H4	0.8714	−0.0803	0.5131	0.037*
C5	0.9042 (2)	0.1350 (2)	0.3794 (3)	0.0294 (6)
H5	0.9235	0.1674	0.2941	0.035*
C6	0.87832 (17)	0.1940 (2)	0.4986 (3)	0.0228 (6)
O1	0.82694 (15)	0.08427 (18)	1.0518 (3)	0.0374 (5)
O2	0.6365 (2)	0.2500	0.8250 (4)	0.0411 (8)
O3	0.96933 (17)	0.2500	0.7918 (3)	0.0238 (6)
O101	0.52257 (16)	0.06874 (17)	0.6314 (3)	0.0370 (5)
N1	0.85100 (14)	0.14918 (18)	0.6248 (3)	0.0207 (5)
N2	0.90248 (18)	0.0332 (2)	0.3828 (3)	0.0324 (6)
P2	0.63555 (8)	0.2500	0.32697 (12)	0.0302 (2)
F1	0.6022 (3)	0.2500	0.1613 (4)	0.0858 (14)
F2	0.6640 (3)	0.2500	0.4909 (4)	0.108 (2)
F3	0.5475 (4)	0.2138 (7)	0.3846 (7)	0.110 (5)	0.50
F4	0.6768 (9)	0.1465 (6)	0.3355 (10)	0.126 (4)	0.50
F5	0.5921 (6)	0.1392 (5)	0.3165 (7)	0.0808 (19)	0.50
F6	0.7203 (4)	0.2023 (8)	0.2657 (9)	0.120 (5)	0.50
Re1	0.832360 (9)	0.2500	0.812157 (16)	0.01747 (6)
H101	0.5541	0.0337	0.6992	0.072 (15)*
H102	0.5625	0.0665	0.5546	0.12 (2)*
H103	0.9995	0.1897	0.8264	0.048 (11)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0204 (13)	0.0302 (15)	0.0231 (14)	0.0001 (11)	−0.0008 (11)	−0.0023 (12)
C2	0.025 (2)	0.032 (2)	0.025 (2)	0.000	−0.0035 (17)	0.000
C3	0.0326 (15)	0.0201 (14)	0.0268 (14)	−0.0033 (12)	−0.0013 (12)	0.0007 (12)
C4	0.0394 (17)	0.0204 (14)	0.0333 (16)	−0.0014 (13)	−0.0031 (14)	−0.0039 (12)
C5	0.0386 (16)	0.0277 (15)	0.0220 (14)	0.0007 (13)	0.0012 (13)	−0.0016 (12)
C6	0.0253 (13)	0.0216 (14)	0.0214 (13)	−0.0020 (11)	−0.0023 (11)	−0.0001 (11)
O1	0.0425 (13)	0.0387 (13)	0.0309 (12)	0.0003 (10)	0.0033 (10)	0.0149 (11)
O2	0.0200 (16)	0.061 (2)	0.0424 (19)	0.000	−0.0024 (14)	0.000
O3	0.0198 (13)	0.0218 (14)	0.0298 (15)	0.000	0.0012 (11)	0.000
O101	0.0499 (14)	0.0261 (11)	0.0351 (12)	0.0097 (10)	−0.0081 (11)	0.0008 (10)
N1	0.0211 (11)	0.0192 (11)	0.0218 (11)	−0.0011 (9)	−0.0028 (9)	0.0003 (9)
N2	0.0434 (15)	0.0254 (13)	0.0284 (13)	0.0031 (12)	−0.0010 (12)	−0.0084 (11)
P2	0.0395 (6)	0.0285 (6)	0.0225 (5)	0.000	0.0007 (5)	0.000
F1	0.100 (3)	0.127 (4)	0.0311 (18)	0.000	−0.0110 (19)	0.000
F2	0.086 (3)	0.206 (6)	0.033 (2)	0.000	−0.021 (2)	0.000
F3	0.071 (3)	0.194 (14)	0.066 (3)	−0.068 (5)	0.000 (3)	0.062 (5)
F4	0.215 (12)	0.053 (4)	0.109 (7)	0.079 (6)	−0.035 (7)	−0.031 (4)
F5	0.113 (6)	0.049 (3)	0.080 (4)	−0.023 (4)	−0.019 (4)	−0.015 (3)
F6	0.057 (3)	0.220 (15)	0.082 (5)	0.059 (5)	0.007 (3)	−0.025 (6)
Re1	0.01705 (8)	0.01873 (8)	0.01662 (8)	0.000	−0.00096 (5)	0.000

Geometric parameters (Å, º)

C1—O1	1.150 (4)	O101—H101	0.910 (2)
C1—Re1	1.918 (3)	O101—H102	0.932 (3)
C2—O2	1.145 (5)	N1—Re1	2.167 (2)
C2—Re1	1.912 (4)	P2—F4^i	1.503 (6)
C3—N1	1.338 (4)	P2—F4	1.503 (6)
C3—C4	1.377 (4)	P2—F3^i	1.543 (5)
C3—H3	0.930	P2—F3	1.543 (5)
C4—N2	1.334 (4)	P2—F2	1.546 (4)
C4—H4	0.930	P2—F6	1.563 (6)
C5—N2	1.334 (4)	P2—F6^i	1.563 (6)
C5—C6	1.386 (4)	P2—F1	1.585 (4)
C5—H5	0.930	P2—F5	1.606 (6)
C6—N1	1.351 (4)	P2—F5^i	1.606 (6)
C6—C6^i	1.468 (5)	Re1—C1^i	1.918 (3)
O3—Re1	2.143 (3)	Re1—N1^i	2.167 (2)
O3—H103	0.9713 (16)
O1—C1—Re1	178.9 (3)	F3—P2—F6^i	174.1 (5)
O2—C2—Re1	175.9 (4)	F2—P2—F6^i	95.6 (3)
N1—C3—C4	121.0 (3)	F3^i—P2—F1	91.5 (3)
N1—C3—H3	119.5	F3—P2—F1	91.5 (3)
C4—C3—H3	119.5	F2—P2—F1	177.5 (3)
N2—C4—C3	122.4 (3)	F6—P2—F1	86.7 (3)
N2—C4—H4	118.8	F6^i—P2—F1	86.7 (3)
C3—C4—H4	118.8	F4^i—P2—F5	179.4 (7)
N2—C5—C6	122.3 (3)	F3^i—P2—F5	85.6 (5)
N2—C5—H5	118.9	F6—P2—F5	88.5 (5)
C6—C5—H5	118.9	F4—P2—F5^i	179.4 (7)
N1—C6—C5	120.3 (3)	F3—P2—F5^i	85.6 (5)
N1—C6—C6^i	115.78 (15)	F6^i—P2—F5^i	88.5 (5)
C5—C6—C6^i	123.92 (17)	C2—Re1—C1^i	88.01 (12)
Re1—O3—H103	117.07 (15)	C2—Re1—C1	88.01 (12)
H101—O101—H102	97.2 (2)	C1^i—Re1—C1	89.30 (17)
C3—N1—C6	117.5 (3)	C2—Re1—O3	175.71 (15)
C3—N1—Re1	126.1 (2)	C1^i—Re1—O3	95.03 (10)
C6—N1—Re1	115.85 (18)	C1—Re1—O3	95.03 (10)
C4—N2—C5	116.5 (3)	C2—Re1—N1	98.20 (12)
F4^i—P2—F3^i	94.9 (6)	C1^i—Re1—N1	170.92 (10)
F4—P2—F3	94.9 (6)	C1—Re1—N1	97.49 (11)
F3^i—P2—F2	86.1 (3)	O3—Re1—N1	78.43 (8)
F3—P2—F2	86.1 (3)	C2—Re1—N1^i	98.20 (12)
F4^i—P2—F6	91.0 (8)	C1^i—Re1—N1^i	97.49 (11)
F3^i—P2—F6	174.1 (5)	C1—Re1—N1^i	170.92 (10)
F2—P2—F6	95.6 (3)	O3—Re1—N1^i	78.43 (8)
F4—P2—F6^i	91.0 (8)	N1—Re1—N1^i	75.14 (12)

Symmetry code: (i) x, −y+1/2, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O101—H101···N2^ii	0.910 (2)	1.994 (3)	2.882 (4)	164.83 (18)
O101—H102···F5	0.933 (3)	2.395 (7)	3.180 (8)	141.7 (3)
O101—H102···F3	0.933 (3)	2.475 (7)	2.955 (7)	112.1 (2)
O101—H102···O1^iii	0.933 (3)	2.622 (2)	3.168 (3)	117.99 (15)
O3—H103···O101^iv	0.9710 (17)	1.670 (2)	2.611 (3)	161.87 (17)

Symmetry codes: (ii) −x+3/2, −y, z+1/2; (iii) −x+3/2, −y, z−1/2; (iv) x+1/2, y, −z+3/2.