2,2′-Bipyrimidinium hexa­chloro­rhenate(IV) dihydrate

In the title compound, (C₈H₈N₄)[ReCl₆]·2H₂O, the Re atom occupies an inversion centre and is octahedrally coordinated by chloride anions. The cation also has an inversion centre. Various N—H...O, O—H...Cl and C—H...Cl interactions help to stabilize the crystal packing.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.028
• wR factor = 0.057
• Data-to-parameter ratio = 35.0

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.95

Alert level C
ABSTY02_ALERT_1_C  An _exptl_absorpt_correction_type has been given without
            a literature citation. This should be contained in the
            _exptl_absorpt_process_details field.
            Absorption correction given as numerical
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?

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

   3 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
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: KM4CCD software (Oxford Diffraction, 2004); cell refinement: KM4CCD; data reduction: KM4CCD; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

2,2'-Bipyrimidinium hexachlororhenate(IV) dihydrate

Crystal data

(C8H8N4)[ReCl6]·2H2O	F(000) = 562
Mr = 595.13	Dx = 2.361 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2760 reflections
a = 7.941 (2) Å	θ = 3.2–36.5°
b = 12.199 (2) Å	µ = 8.22 mm^−1
c = 9.804 (2) Å	T = 100 K
β = 118.18 (3)°	Plate, yellow
V = 837.2 (3) Å^3	0.12 × 0.10 × 0.05 mm
Z = 2

Data collection

KM4/CCD diffractometer	3711 independent reflections
Radiation source: fine-focus sealed tube	2860 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.049
ω scans	θmax = 36.5°, θmin = 3.2°
Absorption correction: numerical	h = −13→12
Tmin = 0.567, Tmax = 0.897	k = −20→16
14616 measured reflections	l = −14→16

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)] = 0.028	Hydrogen site location: difmap (O-H and N-H) and geom (C-H)
wR(F^2) = 0.057	H atoms treated by a mixture of independent and constrained refinement
S = 1.07	w = 1/[σ^2(Fo^2) + (0.0255P)^2] where P = (Fo^2 + 2Fc^2)/3
3711 reflections	(Δ/σ)max < 0.001
106 parameters	Δρmax = 1.75 e Å^−3
0 restraints	Δρmin = −2.24 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
Re	0.0000	0.0000	0.0000	0.00865 (4)
Cl1	0.31200 (9)	0.03698 (6)	0.03806 (8)	0.01349 (12)
Cl2	0.05830 (9)	0.11702 (6)	0.20879 (8)	0.01580 (13)
Cl3	−0.11358 (9)	0.15207 (6)	−0.16823 (8)	0.01603 (13)
O	0.5775 (3)	0.2861 (2)	0.4616 (3)	0.0229 (5)
N1	0.4278 (3)	0.1280 (2)	0.5515 (3)	0.0131 (4)
N2	0.3475 (3)	−0.0543 (2)	0.5735 (3)	0.0135 (4)
C1	0.4397 (4)	0.0194 (2)	0.5343 (3)	0.0128 (5)
C2	0.3161 (4)	0.1673 (3)	0.6083 (3)	0.0158 (5)
H2	0.3056	0.2425	0.6179	0.019*
C3	0.2168 (3)	0.09521 (19)	0.6524 (2)	0.0169 (5)
H3	0.1384	0.1199	0.6926	0.020*
C4	0.2389 (3)	−0.01476 (19)	0.6343 (2)	0.0178 (6)
H4	0.1754	−0.0646	0.6657	0.021*
H1	0.488 (5)	0.169 (4)	0.524 (4)	0.023 (11)*
H1W	0.581 (6)	0.351 (4)	0.487 (5)	0.035 (12)*
H2W	0.680 (7)	0.268 (4)	0.466 (6)	0.054 (15)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Re	0.00822 (6)	0.00970 (6)	0.00911 (6)	−0.00007 (6)	0.00500 (4)	0.00034 (6)
Cl1	0.0099 (3)	0.0138 (3)	0.0187 (3)	−0.0011 (2)	0.0083 (2)	−0.0002 (2)
Cl2	0.0172 (3)	0.0187 (3)	0.0141 (3)	−0.0035 (2)	0.0095 (2)	−0.0057 (2)
Cl3	0.0155 (3)	0.0160 (3)	0.0175 (3)	0.0030 (2)	0.0085 (2)	0.0073 (3)
O	0.0241 (12)	0.0110 (11)	0.0408 (14)	0.0000 (9)	0.0214 (11)	0.0023 (10)
N1	0.0121 (10)	0.0149 (12)	0.0119 (10)	−0.0018 (8)	0.0053 (8)	−0.0001 (9)
N2	0.0150 (11)	0.0134 (12)	0.0146 (10)	−0.0009 (8)	0.0089 (9)	0.0010 (8)
C1	0.0111 (11)	0.0181 (16)	0.0088 (10)	−0.0003 (8)	0.0045 (8)	0.0013 (9)
C2	0.0168 (13)	0.0158 (14)	0.0150 (12)	0.0035 (10)	0.0075 (10)	−0.0002 (10)
C3	0.0172 (13)	0.0201 (15)	0.0150 (12)	0.0033 (10)	0.0090 (10)	−0.0009 (11)
C4	0.0153 (12)	0.0255 (18)	0.0159 (11)	−0.0001 (10)	0.0101 (10)	0.0032 (11)

Geometric parameters (Å, º)

Re—Cl1	2.3681 (9)	N1—H1	0.82 (4)
Re—Cl2	2.3553 (8)	N2—C1	1.326 (4)
Re—Cl3	2.3601 (8)	N2—C4	1.348 (3)
Re—Cl2^i	2.3553 (8)	C1—C1^ii	1.483 (5)
Re—Cl3^i	2.3601 (8)	C2—C3	1.380 (4)
Re—Cl1^i	2.3681 (9)	C2—H2	0.9300
O—H1W	0.83 (5)	C3—C4	1.375 (3)
O—H2W	0.82 (5)	C3—H3	0.9300
N1—C2	1.339 (4)	C4—H4	0.9300
N1—C1	1.345 (4)
Cl2—Re—Cl2^i	180.0	C2—N1—C1	120.3 (3)
Cl2—Re—Cl3^i	90.90 (3)	C2—N1—H1	121 (3)
Cl2^i—Re—Cl3^i	89.10 (3)	C1—N1—H1	118 (3)
Cl2—Re—Cl3	89.10 (3)	C1—N2—C4	116.3 (2)
Cl2^i—Re—Cl3	90.90 (3)	N2—C1—N1	123.4 (3)
Cl3^i—Re—Cl3	180.0	N2—C1—C1^ii	118.6 (3)
Cl2—Re—Cl1	89.20 (3)	N1—C1—C1^ii	118.0 (3)
Cl2^i—Re—Cl1	90.80 (3)	N1—C2—C3	119.4 (3)
Cl3^i—Re—Cl1	90.77 (3)	N1—C2—H2	120.3
Cl3—Re—Cl1	89.23 (3)	C3—C2—H2	120.3
Cl2—Re—Cl1^i	90.80 (3)	C4—C3—C2	117.02 (15)
Cl2^i—Re—Cl1^i	89.20 (3)	C4—C3—H3	121.5
Cl3^i—Re—Cl1^i	89.23 (3)	C2—C3—H3	121.5
Cl3—Re—Cl1^i	90.77 (3)	N2—C4—C3	123.61 (15)
Cl1—Re—Cl1^i	180.0	N2—C4—H4	118.2
H1W—O—H2W	111 (5)	C3—C4—H4	118.2

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···O	0.82 (5)	1.83 (5)	2.627 (4)	165 (5)
N1—H1···N2^ii	0.82 (5)	2.40 (4)	2.749 (4)	107 (4)
O—H1W···Cl1^iii	0.83 (5)	2.48 (5)	3.183 (3)	144 (4)
O—H1W···Cl1^iv	0.83 (5)	2.77 (5)	3.340 (3)	127 (4)
O—H2W···Cl3^v	0.82 (6)	2.72 (6)	3.340 (3)	133 (4)
C2—H2···Cl1^iv	0.93	2.81	3.670 (4)	154
C4—H4···Cl2^vi	0.93	2.74	3.595 (4)	153

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