Bis(tetra­phenyl­arsonium) hexa­bromo­rhenate(IV)

The title compound, (C₂₄H₂₀As)₂[ReBr₆], consists of tetra­phenyl­arsonium cations and [ReBr₆]²⁻ dianions, the latter lying on inversion centres. A possible C—H...Br inter­action stabilizes the crystal packing.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C) = 0.010 Å
• R factor = 0.034
• wR factor = 0.069
• Data-to-parameter ratio = 15.6

checkCIF/PLATON results

No syntax errors found



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
CELLV02_ALERT_1_C  The supplied cell volume s.u. differs from that
            calculated from the cell parameter s.u.'s by > 2
            Calculated cell volume su =      19.54
            Cell volume su given      =      16.00
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) .         90 Ang.
PLAT213_ALERT_2_C Atom C7      has ADP max/min Ratio .............       3.30 prola
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         10

   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

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

---

Computing details

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

Bis(tetraphenylarsonium) hexabromorhenate(IV)

Crystal data

(C24H20As)2[ReBr6]	Z = 1
Mr = 1432.25	F(000) = 679
Triclinic, P1	Dx = 2.072 Mg m^−3
a = 10.4085 (9) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.4157 (9) Å	Cell parameters from 2876 reflections
c = 12.1694 (9) Å	θ = 3.0–25°
α = 92.565 (7)°	µ = 9.33 mm^−1
β = 99.915 (7)°	T = 100 K
γ = 116.880 (9)°	Prism, orange
V = 1147.85 (16) Å^3	0.13 × 0.10 × 0.07 mm

Data collection

Kuma KM-4-CCD diffractometer	4040 independent reflections
Radiation source: fine-focus sealed tube	2979 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.060
ω scans	θmax = 25.0°, θmin = 3.0°
Absorption correction: numerical (CrysAlis RED; Oxford Diffraction, 2004)	h = −11→12
Tmin = 0.318, Tmax = 0.598	k = −12→11
9761 measured reflections	l = −14→14

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)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.069	H-atom parameters constrained
S = 0.93	w = 1/[σ^2(Fo^2) + (0.0254P)^2] where P = (Fo^2 + 2Fc^2)/3
4040 reflections	(Δ/σ)max < 0.001
259 parameters	Δρmax = 0.98 e Å^−3
0 restraints	Δρmin = −1.16 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
As1	0.32040 (7)	0.38983 (7)	0.18172 (5)	0.01200 (17)
C1	0.3148 (7)	0.2496 (7)	0.0703 (5)	0.0123 (14)
C2	0.4456 (7)	0.2440 (7)	0.0635 (5)	0.0145 (15)
H2	0.5339	0.3050	0.1136	0.017*
C3	0.4397 (7)	0.1451 (8)	−0.0199 (6)	0.0205 (16)
H3	0.5252	0.1398	−0.0257	0.025*
C4	0.3097 (7)	0.0551 (7)	−0.0939 (6)	0.0194 (16)
H4	0.3085	−0.0079	−0.1510	0.023*
C5	0.1797 (7)	0.0573 (7)	−0.0842 (6)	0.0200 (17)
H5	0.0911	−0.0071	−0.1326	0.024*
C6	0.1829 (7)	0.1561 (7)	−0.0019 (6)	0.0191 (16)
H6	0.0966	0.1592	0.0045	0.023*
C7	0.1753 (6)	0.2831 (7)	0.2665 (5)	0.0117 (15)
C8	0.1737 (7)	0.1609 (8)	0.3060 (5)	0.0175 (16)
H8	0.2465	0.1356	0.2967	0.021*
C9	0.0636 (7)	0.0756 (8)	0.3597 (5)	0.0177 (16)
H9	0.0638	−0.0060	0.3876	0.021*
C10	−0.0475 (7)	0.1114 (8)	0.3720 (5)	0.0155 (16)
H10	−0.1230	0.0527	0.4061	0.019*
C11	−0.0439 (7)	0.2363 (8)	0.3325 (5)	0.0208 (17)
H11	−0.1167	0.2620	0.3411	0.025*
C12	0.0679 (7)	0.3220 (7)	0.2807 (5)	0.0146 (15)
H12	0.0708	0.4060	0.2553	0.018*
C13	0.2637 (6)	0.5190 (7)	0.1055 (5)	0.0146 (15)
C14	0.2138 (6)	0.4939 (7)	−0.0097 (5)	0.0153 (16)
H14	0.2136	0.4169	−0.0516	0.018*
C15	0.1639 (7)	0.5827 (7)	−0.0636 (6)	0.0180 (16)
H15	0.1293	0.5652	−0.1413	0.022*
C16	0.1666 (7)	0.6983 (8)	0.0005 (6)	0.0224 (17)
H16	0.1322	0.7576	−0.0349	0.027*
C17	0.2193 (7)	0.7266 (7)	0.1153 (6)	0.0185 (16)
H17	0.2206	0.8046	0.1568	0.022*
C18	0.2703 (7)	0.6388 (7)	0.1690 (6)	0.0173 (16)
H18	0.3085	0.6589	0.2463	0.021*
C19	0.5169 (7)	0.4923 (7)	0.2704 (5)	0.0143 (15)
C20	0.5544 (7)	0.4442 (7)	0.3698 (5)	0.0166 (15)
H20	0.4820	0.3714	0.3987	0.020*
C21	0.7013 (7)	0.5064 (8)	0.4251 (6)	0.0247 (18)
H21	0.7282	0.4736	0.4906	0.030*
C22	0.8081 (8)	0.6172 (8)	0.3830 (6)	0.0254 (18)
H22	0.9067	0.6585	0.4200	0.031*
C23	0.7681 (7)	0.6657 (8)	0.2867 (6)	0.0200 (16)
H23	0.8396	0.7418	0.2597	0.024*
C24	0.6218 (7)	0.6023 (7)	0.2293 (6)	0.0174 (16)
H24	0.5955	0.6346	0.1633	0.021*
Re1	0.5000	0.0000	0.5000	0.01204 (12)
Br1	0.41777 (7)	0.17716 (7)	0.56344 (5)	0.01620 (17)
Br2	0.23487 (7)	−0.18757 (7)	0.42280 (6)	0.01797 (17)
Br3	0.51341 (7)	0.08706 (7)	0.31040 (5)	0.01729 (17)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
As1	0.0094 (3)	0.0134 (4)	0.0127 (4)	0.0049 (3)	0.0028 (3)	0.0004 (3)
C1	0.020 (4)	0.015 (4)	0.007 (3)	0.011 (3)	0.004 (3)	0.004 (3)
C2	0.007 (3)	0.020 (4)	0.015 (4)	0.005 (3)	0.003 (3)	0.003 (3)
C3	0.017 (4)	0.020 (4)	0.025 (4)	0.008 (3)	0.007 (3)	0.004 (3)
C4	0.029 (4)	0.012 (4)	0.019 (4)	0.009 (3)	0.011 (3)	0.001 (3)
C5	0.015 (4)	0.011 (4)	0.025 (4)	0.001 (3)	−0.003 (3)	−0.001 (3)
C6	0.011 (3)	0.020 (4)	0.030 (4)	0.010 (3)	0.006 (3)	0.004 (3)
C7	0.011 (3)	0.013 (4)	0.006 (3)	0.000 (3)	0.004 (3)	0.005 (3)
C8	0.008 (3)	0.024 (4)	0.022 (4)	0.009 (3)	0.002 (3)	−0.002 (3)
C9	0.018 (4)	0.016 (4)	0.014 (4)	0.004 (3)	0.002 (3)	0.007 (3)
C10	0.007 (3)	0.027 (5)	0.011 (4)	0.006 (3)	0.001 (3)	0.004 (3)
C11	0.014 (4)	0.031 (5)	0.014 (4)	0.009 (3)	0.003 (3)	−0.004 (3)
C12	0.014 (3)	0.010 (4)	0.017 (4)	0.005 (3)	−0.001 (3)	−0.001 (3)
C13	0.006 (3)	0.019 (4)	0.017 (4)	0.005 (3)	0.000 (3)	0.005 (3)
C14	0.009 (3)	0.018 (4)	0.019 (4)	0.005 (3)	0.007 (3)	0.003 (3)
C15	0.012 (3)	0.014 (4)	0.023 (4)	0.003 (3)	0.001 (3)	0.001 (3)
C16	0.015 (4)	0.018 (4)	0.032 (5)	0.005 (3)	0.004 (3)	0.015 (3)
C17	0.018 (4)	0.012 (4)	0.028 (4)	0.007 (3)	0.010 (3)	0.003 (3)
C18	0.014 (3)	0.014 (4)	0.023 (4)	0.006 (3)	0.004 (3)	0.003 (3)
C19	0.014 (3)	0.015 (4)	0.014 (4)	0.007 (3)	0.002 (3)	−0.007 (3)
C20	0.015 (3)	0.010 (4)	0.019 (4)	0.001 (3)	0.003 (3)	0.000 (3)
C21	0.023 (4)	0.022 (5)	0.024 (4)	0.011 (4)	−0.005 (3)	−0.001 (3)
C22	0.020 (4)	0.020 (5)	0.029 (4)	0.009 (4)	−0.006 (3)	−0.005 (4)
C23	0.008 (3)	0.017 (4)	0.028 (4)	0.000 (3)	0.007 (3)	0.000 (3)
C24	0.016 (4)	0.019 (4)	0.016 (4)	0.009 (3)	−0.001 (3)	0.001 (3)
Re1	0.0109 (2)	0.0122 (3)	0.0135 (2)	0.00532 (18)	0.00478 (16)	0.00020 (17)
Br1	0.0168 (3)	0.0161 (4)	0.0180 (4)	0.0092 (3)	0.0056 (3)	0.0004 (3)
Br2	0.0116 (3)	0.0186 (4)	0.0213 (4)	0.0047 (3)	0.0057 (3)	−0.0018 (3)
Br3	0.0192 (4)	0.0194 (4)	0.0168 (4)	0.0108 (3)	0.0071 (3)	0.0037 (3)

Geometric parameters (Å, º)

As1—C19	1.910 (6)	C13—C18	1.406 (9)
As1—C13	1.914 (6)	C14—C15	1.388 (9)
As1—C1	1.922 (6)	C14—H14	0.9300
As1—C7	1.924 (6)	C15—C16	1.392 (9)
C1—C6	1.380 (9)	C15—H15	0.9300
C1—C2	1.405 (8)	C16—C17	1.375 (9)
C2—C3	1.386 (9)	C16—H16	0.9300
C2—H2	0.9300	C17—C18	1.385 (9)
C3—C4	1.371 (9)	C17—H17	0.9300
C3—H3	0.9300	C18—H18	0.9300
C4—C5	1.387 (9)	C19—C24	1.365 (9)
C4—H4	0.9300	C19—C20	1.391 (9)
C5—C6	1.389 (9)	C20—C21	1.386 (9)
C5—H5	0.9300	C20—H20	0.9300
C6—H6	0.9300	C21—C22	1.385 (10)
C7—C8	1.375 (9)	C21—H21	0.9300
C7—C12	1.383 (9)	C22—C23	1.370 (10)
C8—C9	1.386 (9)	C22—H22	0.9300
C8—H8	0.9300	C23—C24	1.388 (9)
C9—C10	1.394 (9)	C23—H23	0.9300
C9—H9	0.9300	C24—H24	0.9300
C10—C11	1.393 (9)	Re1—Br1	2.5023 (7)
C10—H10	0.9300	Re1—Br1^i	2.5023 (7)
C11—C12	1.383 (9)	Re1—Br3^i	2.5197 (7)
C11—H11	0.9300	Re1—Br3	2.5197 (7)
C12—H12	0.9300	Re1—Br2^i	2.5264 (7)
C13—C14	1.376 (9)	Re1—Br2	2.5264 (7)
C19—As1—C13	111.1 (3)	C15—C14—H14	119.8
C19—As1—C1	108.0 (3)	C14—C15—C16	118.9 (6)
C13—As1—C1	108.3 (3)	C14—C15—H15	120.6
C19—As1—C7	113.8 (3)	C16—C15—H15	120.6
C13—As1—C7	108.7 (3)	C17—C16—C15	121.2 (6)
C1—As1—C7	106.6 (3)	C17—C16—H16	119.4
C6—C1—C2	120.9 (6)	C15—C16—H16	119.4
C6—C1—As1	119.7 (5)	C16—C17—C18	119.9 (6)
C2—C1—As1	119.4 (5)	C16—C17—H17	120.1
C3—C2—C1	118.3 (6)	C18—C17—H17	120.1
C3—C2—H2	120.8	C17—C18—C13	119.3 (6)
C1—C2—H2	120.8	C17—C18—H18	120.3
C4—C3—C2	120.9 (6)	C13—C18—H18	120.3
C4—C3—H3	119.6	C24—C19—C20	120.9 (6)
C2—C3—H3	119.6	C24—C19—As1	119.2 (5)
C3—C4—C5	120.6 (6)	C20—C19—As1	119.6 (5)
C3—C4—H4	119.7	C21—C20—C19	119.0 (7)
C5—C4—H4	119.7	C21—C20—H20	120.5
C4—C5—C6	119.5 (6)	C19—C20—H20	120.5
C4—C5—H5	120.2	C22—C21—C20	120.2 (7)
C6—C5—H5	120.2	C22—C21—H21	119.9
C1—C6—C5	119.7 (6)	C20—C21—H21	119.9
C1—C6—H6	120.2	C23—C22—C21	119.8 (7)
C5—C6—H6	120.2	C23—C22—H22	120.1
C8—C7—C12	120.4 (6)	C21—C22—H22	120.1
C8—C7—As1	118.6 (5)	C22—C23—C24	120.6 (7)
C12—C7—As1	120.8 (5)	C22—C23—H23	119.7
C7—C8—C9	120.0 (6)	C24—C23—H23	119.7
C7—C8—H8	120.0	C19—C24—C23	119.5 (6)
C9—C8—H8	120.0	C19—C24—H24	120.3
C8—C9—C10	120.3 (6)	C23—C24—H24	120.3
C8—C9—H9	119.9	Br1—Re1—Br1^i	180.0
C10—C9—H9	119.9	Br1—Re1—Br3^i	88.25 (2)
C11—C10—C9	119.2 (6)	Br1^i—Re1—Br3^i	91.75 (2)
C11—C10—H10	120.4	Br1—Re1—Br3	91.75 (2)
C9—C10—H10	120.4	Br1^i—Re1—Br3	88.25 (2)
C12—C11—C10	120.1 (6)	Br3^i—Re1—Br3	180.0
C12—C11—H11	120.0	Br1—Re1—Br2^i	89.56 (2)
C10—C11—H11	120.0	Br1^i—Re1—Br2^i	90.44 (2)
C11—C12—C7	120.1 (7)	Br3^i—Re1—Br2^i	89.75 (2)
C11—C12—H12	119.9	Br3—Re1—Br2^i	90.25 (2)
C7—C12—H12	119.9	Br1—Re1—Br2	90.44 (2)
C14—C13—C18	120.2 (6)	Br1^i—Re1—Br2	89.56 (2)
C14—C13—As1	120.8 (5)	Br3^i—Re1—Br2	90.25 (2)
C18—C13—As1	119.1 (5)	Br3—Re1—Br2	89.74 (2)
C13—C14—C15	120.4 (6)	Br2^i—Re1—Br2	180.0
C13—C14—H14	119.8
C19—As1—C1—C6	177.1 (5)	C19—As1—C13—C14	124.9 (5)
C13—As1—C1—C6	−62.5 (6)	C1—As1—C13—C14	6.4 (6)
C7—As1—C1—C6	54.4 (6)	C7—As1—C13—C14	−109.1 (5)
C19—As1—C1—C2	−3.0 (6)	C19—As1—C13—C18	−56.6 (6)
C13—As1—C1—C2	117.4 (5)	C1—As1—C13—C18	−175.1 (5)
C7—As1—C1—C2	−125.7 (5)	C7—As1—C13—C18	69.5 (5)
C6—C1—C2—C3	2.0 (10)	C18—C13—C14—C15	−2.7 (9)
As1—C1—C2—C3	−177.9 (5)	As1—C13—C14—C15	175.9 (5)
C1—C2—C3—C4	0.0 (10)	C13—C14—C15—C16	0.7 (9)
C2—C3—C4—C5	−2.4 (11)	C14—C15—C16—C17	0.8 (10)
C3—C4—C5—C6	2.9 (10)	C15—C16—C17—C18	−0.2 (10)
C2—C1—C6—C5	−1.5 (10)	C16—C17—C18—C13	−1.8 (10)
As1—C1—C6—C5	178.4 (5)	C14—C13—C18—C17	3.2 (9)
C4—C5—C6—C1	−0.9 (10)	As1—C13—C18—C17	−175.3 (5)
C19—As1—C7—C8	−70.8 (5)	C13—As1—C19—C24	−38.6 (6)
C13—As1—C7—C8	164.7 (5)	C1—As1—C19—C24	80.1 (6)
C1—As1—C7—C8	48.2 (5)	C7—As1—C19—C24	−161.7 (5)
C19—As1—C7—C12	113.8 (5)	C13—As1—C19—C20	148.1 (5)
C13—As1—C7—C12	−10.6 (6)	C1—As1—C19—C20	−93.3 (5)
C1—As1—C7—C12	−127.2 (5)	C7—As1—C19—C20	24.9 (6)
C12—C7—C8—C9	0.4 (9)	C24—C19—C20—C21	−2.2 (10)
As1—C7—C8—C9	−175.0 (5)	As1—C19—C20—C21	171.1 (5)
C7—C8—C9—C10	1.2 (10)	C19—C20—C21—C22	1.6 (10)
C8—C9—C10—C11	−1.8 (9)	C20—C21—C22—C23	0.3 (11)
C9—C10—C11—C12	0.8 (9)	C21—C22—C23—C24	−1.7 (11)
C10—C11—C12—C7	0.8 (9)	C20—C19—C24—C23	0.8 (10)
C8—C7—C12—C11	−1.4 (9)	As1—C19—C24—C23	−172.4 (5)
As1—C7—C12—C11	173.9 (5)

Symmetry code: (i) −x+1, −y, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C20—H20···Br1	0.93	2.86	3.671 (6)	147