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The title bismuth-iodide compound, [Bi2I6(C12H8N2)2], has been synthesized solvothermally by reacting BiI3, Mn(CH3COO)2·4H2O, and 1,10-phenanthroline in an ethanol/water solvent mixture. The compound contains two bismuth centers that are each coordinated by a phenanthroline ligand and two terminal iodide ligands, and the bismuth centers are bridged via two additional iodide ligands to form a molecular dimer. The asymmetric unit of the compound consists of one half of a single dimer molecule located on a crystallographic inversion center.
Supporting information
CCDC reference: 609278
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.006 Å
- R factor = 0.018
- wR factor = 0.044
- Data-to-parameter ratio = 20.7
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Bi1 - I3 .. 12.63 su
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Bi1 - I3_a .. 17.23 su
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
Tmin and Tmax reported: 0.133 0.200
Tmin and Tmax expected: 0.110 0.197
RR = 1.188
Please check that your absorption correction is appropriate.
PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.18
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Bi1 - I2 .. 8.64 su
0 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 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
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2001); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2000); software used to prepare material for publication: SHELXTL.
Di-µ-iodo-bis[diiodobis(1,10-phenanthroline)bismuth(III)]
top
Crystal data top
[Bi2I6(C12H8N2)2] | F(000) = 1344 |
Mr = 1539.77 | Dx = 3.095 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 5952 reflections |
a = 11.4058 (6) Å | θ = 2.4–26.4° |
b = 11.0804 (6) Å | µ = 16.26 mm−1 |
c = 13.5775 (7) Å | T = 150 K |
β = 105.674 (1)° | Block, yellow–orange |
V = 1652.13 (15) Å3 | 0.16 × 0.12 × 0.10 mm |
Z = 2 | |
Data collection top
Bruker SMART APEX CCD diffractometer | 3370 independent reflections |
Radiation source: fine-focus sealed tube | 3278 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
Detector resolution: 12 pixels mm-1 | θmax = 26.4°, θmin = 2.1° |
ω scans | h = −14→14 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | k = −13→13 |
Tmin = 0.133, Tmax = 0.200 | l = −16→16 |
17846 measured reflections | |
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)] = 0.018 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.044 | H-atom parameters constrained |
S = 1.12 | w = 1/[σ2(Fo2) + (0.0214P)2 + 1.7672P] where P = (Fo2 + 2Fc2)/3 |
3370 reflections | (Δ/σ)max = 0.001 |
163 parameters | Δρmax = 0.73 e Å−3 |
0 restraints | Δρmin = −0.70 e Å−3 |
Special details top
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 | Uiso*/Ueq | |
Bi1 | 0.327118 (12) | 0.463186 (12) | 0.536941 (11) | 0.01801 (5) | |
I1 | 0.22124 (3) | 0.48478 (3) | 0.70626 (2) | 0.03277 (8) | |
I2 | 0.16278 (2) | 0.63222 (2) | 0.39782 (2) | 0.02719 (7) | |
I3 | 0.55575 (2) | 0.62289 (2) | 0.64912 (2) | 0.02577 (7) | |
C1 | 0.5325 (4) | 0.2416 (4) | 0.6558 (3) | 0.0267 (9) | |
H1 | 0.5810 | 0.3100 | 0.6822 | 0.032* | |
C2 | 0.5829 (4) | 0.1272 (4) | 0.6773 (3) | 0.0310 (10) | |
H2 | 0.6644 | 0.1182 | 0.7181 | 0.037* | |
C3 | 0.5143 (4) | 0.0272 (4) | 0.6391 (3) | 0.0289 (9) | |
H3 | 0.5477 | −0.0514 | 0.6539 | 0.035* | |
C4 | 0.3944 (4) | 0.0420 (3) | 0.5781 (3) | 0.0231 (8) | |
C5 | 0.3170 (4) | −0.0582 (4) | 0.5350 (3) | 0.0273 (9) | |
H5 | 0.3474 | −0.1382 | 0.5469 | 0.033* | |
C6 | 0.2024 (4) | −0.0398 (3) | 0.4784 (3) | 0.0289 (9) | |
H6 | 0.1528 | −0.1071 | 0.4504 | 0.035* | |
C7 | 0.1534 (4) | 0.0802 (4) | 0.4592 (3) | 0.0225 (8) | |
C8 | 0.0323 (4) | 0.1016 (4) | 0.4032 (3) | 0.0266 (9) | |
H8 | −0.0197 | 0.0360 | 0.3753 | 0.032* | |
C9 | −0.0104 (4) | 0.2177 (4) | 0.3891 (3) | 0.0271 (9) | |
H9 | −0.0928 | 0.2332 | 0.3533 | 0.033* | |
C10 | 0.0687 (3) | 0.3127 (4) | 0.4279 (3) | 0.0237 (8) | |
H10 | 0.0391 | 0.3931 | 0.4167 | 0.028* | |
C11 | 0.2272 (3) | 0.1803 (3) | 0.4981 (3) | 0.0197 (8) | |
C12 | 0.3500 (4) | 0.1608 (4) | 0.5603 (3) | 0.0214 (8) | |
N1 | 0.4183 (3) | 0.2586 (3) | 0.5994 (2) | 0.0217 (7) | |
N2 | 0.1843 (3) | 0.2947 (3) | 0.4800 (2) | 0.0208 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Bi1 | 0.01593 (8) | 0.01762 (8) | 0.01928 (8) | −0.00117 (5) | 0.00268 (6) | −0.00118 (5) |
I1 | 0.02365 (14) | 0.05331 (19) | 0.02198 (15) | 0.00947 (12) | 0.00728 (11) | 0.00309 (12) |
I2 | 0.03038 (15) | 0.01849 (13) | 0.02799 (15) | 0.00128 (10) | −0.00018 (11) | 0.00075 (10) |
I3 | 0.02165 (13) | 0.03037 (14) | 0.02407 (14) | −0.00512 (10) | 0.00409 (11) | −0.00823 (10) |
C1 | 0.023 (2) | 0.035 (2) | 0.022 (2) | 0.0018 (17) | 0.0048 (16) | 0.0038 (17) |
C2 | 0.025 (2) | 0.043 (3) | 0.024 (2) | 0.0100 (19) | 0.0051 (18) | 0.0074 (19) |
C3 | 0.033 (2) | 0.030 (2) | 0.025 (2) | 0.0127 (18) | 0.0105 (19) | 0.0084 (17) |
C4 | 0.029 (2) | 0.023 (2) | 0.021 (2) | 0.0069 (16) | 0.0132 (17) | 0.0048 (15) |
C5 | 0.036 (3) | 0.0200 (19) | 0.028 (2) | 0.0051 (17) | 0.0120 (19) | 0.0025 (16) |
C6 | 0.038 (2) | 0.018 (2) | 0.033 (2) | −0.0050 (17) | 0.015 (2) | −0.0057 (17) |
C7 | 0.029 (2) | 0.0192 (19) | 0.021 (2) | −0.0013 (16) | 0.0107 (17) | −0.0011 (15) |
C8 | 0.024 (2) | 0.029 (2) | 0.027 (2) | −0.0108 (17) | 0.0074 (17) | −0.0066 (17) |
C9 | 0.0162 (19) | 0.032 (2) | 0.030 (2) | −0.0049 (16) | 0.0004 (16) | 0.0010 (18) |
C10 | 0.0167 (18) | 0.0249 (19) | 0.027 (2) | −0.0013 (15) | 0.0019 (16) | 0.0012 (17) |
C11 | 0.0213 (19) | 0.0223 (19) | 0.0166 (18) | −0.0016 (15) | 0.0072 (15) | −0.0001 (15) |
C12 | 0.0214 (19) | 0.025 (2) | 0.0188 (19) | 0.0029 (15) | 0.0071 (15) | 0.0033 (16) |
N1 | 0.0170 (16) | 0.0263 (17) | 0.0213 (17) | 0.0004 (13) | 0.0043 (13) | 0.0016 (14) |
N2 | 0.0185 (16) | 0.0204 (16) | 0.0220 (17) | −0.0021 (12) | 0.0033 (13) | −0.0017 (13) |
Geometric parameters (Å, º) top
Bi1—N2 | 2.461 (3) | C5—C6 | 1.341 (6) |
Bi1—N1 | 2.543 (3) | C5—H5 | 0.9500 |
Bi1—I1 | 2.8810 (3) | C6—C7 | 1.439 (6) |
Bi1—I2 | 2.9456 (3) | C6—H6 | 0.9500 |
Bi1—I3 | 3.1789 (3) | C7—C8 | 1.405 (6) |
Bi1—I3i | 3.3015 (3) | C7—C11 | 1.406 (5) |
I3—Bi1i | 3.3015 (3) | C8—C9 | 1.371 (6) |
C1—N1 | 1.333 (5) | C8—H8 | 0.9500 |
C1—C2 | 1.390 (6) | C9—C10 | 1.393 (5) |
C1—H1 | 0.9500 | C9—H9 | 0.9500 |
C2—C3 | 1.375 (7) | C10—N2 | 1.333 (5) |
C2—H2 | 0.9500 | C10—H10 | 0.9500 |
C3—C4 | 1.403 (6) | C11—N2 | 1.357 (5) |
C3—H3 | 0.9500 | C11—C12 | 1.443 (5) |
C4—C12 | 1.408 (5) | C12—N1 | 1.356 (5) |
C4—C5 | 1.441 (6) | | |
| | | |
N2—Bi1—N1 | 66.72 (10) | C6—C5—H5 | 119.6 |
N2—Bi1—I1 | 85.92 (7) | C4—C5—H5 | 119.6 |
N1—Bi1—I1 | 91.70 (7) | C5—C6—C7 | 121.0 (4) |
N2—Bi1—I2 | 91.63 (8) | C5—C6—H6 | 119.5 |
N1—Bi1—I2 | 155.93 (7) | C7—C6—H6 | 119.5 |
I1—Bi1—I2 | 97.331 (9) | C8—C7—C11 | 118.1 (4) |
N2—Bi1—I3 | 163.84 (8) | C8—C7—C6 | 122.1 (4) |
N1—Bi1—I3 | 97.34 (7) | C11—C7—C6 | 119.8 (4) |
I1—Bi1—I3 | 92.172 (9) | C9—C8—C7 | 119.6 (4) |
I2—Bi1—I3 | 104.527 (9) | C9—C8—H8 | 120.2 |
N2—Bi1—I3i | 84.89 (7) | C7—C8—H8 | 120.2 |
N1—Bi1—I3i | 77.53 (7) | C8—C9—C10 | 119.2 (4) |
I1—Bi1—I3i | 167.973 (10) | C8—C9—H9 | 120.4 |
I2—Bi1—I3i | 90.684 (9) | C10—C9—H9 | 120.4 |
I3—Bi1—I3i | 94.487 (8) | N2—C10—C9 | 122.3 (4) |
Bi1—I3—Bi1i | 85.512 (8) | N2—C10—H10 | 118.9 |
N1—C1—C2 | 122.3 (4) | C9—C10—H10 | 118.9 |
N1—C1—H1 | 118.9 | N2—C11—C7 | 121.3 (3) |
C2—C1—H1 | 118.9 | N2—C11—C12 | 119.4 (3) |
C3—C2—C1 | 119.6 (4) | C7—C11—C12 | 119.3 (3) |
C3—C2—H2 | 120.2 | N1—C12—C4 | 122.5 (4) |
C1—C2—H2 | 120.2 | N1—C12—C11 | 118.3 (3) |
C2—C3—C4 | 119.5 (4) | C4—C12—C11 | 119.2 (4) |
C2—C3—H3 | 120.2 | C1—N1—C12 | 118.7 (4) |
C4—C3—H3 | 120.2 | C1—N1—Bi1 | 124.4 (3) |
C3—C4—C12 | 117.3 (4) | C12—N1—Bi1 | 116.2 (2) |
C3—C4—C5 | 122.8 (4) | C10—N2—C11 | 119.5 (3) |
C12—C4—C5 | 119.9 (4) | C10—N2—Bi1 | 121.9 (3) |
C6—C5—C4 | 120.8 (4) | C11—N2—Bi1 | 118.4 (2) |
| | | |
N2—Bi1—I3—Bi1i | 87.1 (3) | C2—C1—N1—Bi1 | −171.7 (3) |
N1—Bi1—I3—Bi1i | 77.98 (7) | C4—C12—N1—C1 | 0.9 (6) |
I1—Bi1—I3—Bi1i | 169.977 (9) | C11—C12—N1—C1 | −179.1 (3) |
I2—Bi1—I3—Bi1i | −91.875 (9) | C4—C12—N1—Bi1 | 172.2 (3) |
I3i—Bi1—I3—Bi1i | 0.0 | C11—C12—N1—Bi1 | −7.8 (4) |
N1—C1—C2—C3 | 0.4 (7) | N2—Bi1—N1—C1 | 178.8 (3) |
C1—C2—C3—C4 | 0.6 (6) | I1—Bi1—N1—C1 | −96.4 (3) |
C2—C3—C4—C12 | −0.9 (6) | I2—Bi1—N1—C1 | 151.3 (2) |
C2—C3—C4—C5 | 179.7 (4) | I3—Bi1—N1—C1 | −4.0 (3) |
C3—C4—C5—C6 | 179.0 (4) | I3i—Bi1—N1—C1 | 89.0 (3) |
C12—C4—C5—C6 | −0.3 (6) | N2—Bi1—N1—C12 | 8.0 (3) |
C4—C5—C6—C7 | −0.2 (6) | I1—Bi1—N1—C12 | 92.9 (3) |
C5—C6—C7—C8 | −177.6 (4) | I2—Bi1—N1—C12 | −19.4 (4) |
C5—C6—C7—C11 | 1.6 (6) | I3—Bi1—N1—C12 | −174.7 (3) |
C11—C7—C8—C9 | −0.6 (6) | I3i—Bi1—N1—C12 | −81.7 (3) |
C6—C7—C8—C9 | 178.6 (4) | C9—C10—N2—C11 | −1.2 (6) |
C7—C8—C9—C10 | 2.1 (6) | C9—C10—N2—Bi1 | 175.3 (3) |
C8—C9—C10—N2 | −1.2 (6) | C7—C11—N2—C10 | 2.7 (5) |
C8—C7—C11—N2 | −1.8 (5) | C12—C11—N2—C10 | −175.9 (3) |
C6—C7—C11—N2 | 178.9 (4) | C7—C11—N2—Bi1 | −173.9 (3) |
C8—C7—C11—C12 | 176.8 (3) | C12—C11—N2—Bi1 | 7.5 (4) |
C6—C7—C11—C12 | −2.5 (5) | N1—Bi1—N2—C10 | 175.6 (3) |
C3—C4—C12—N1 | 0.1 (6) | I1—Bi1—N2—C10 | 81.9 (3) |
C5—C4—C12—N1 | 179.6 (4) | I2—Bi1—N2—C10 | −15.3 (3) |
C3—C4—C12—C11 | −179.9 (4) | I3—Bi1—N2—C10 | 165.7 (2) |
C5—C4—C12—C11 | −0.5 (6) | I3i—Bi1—N2—C10 | −105.8 (3) |
N2—C11—C12—N1 | 0.5 (5) | N1—Bi1—N2—C11 | −7.9 (3) |
C7—C11—C12—N1 | −178.2 (3) | I1—Bi1—N2—C11 | −101.5 (3) |
N2—C11—C12—C4 | −179.4 (3) | I2—Bi1—N2—C11 | 161.2 (3) |
C7—C11—C12—C4 | 1.9 (5) | I3—Bi1—N2—C11 | −17.8 (5) |
C2—C1—N1—C12 | −1.2 (6) | I3i—Bi1—N2—C11 | 70.7 (3) |
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 |
C6—H6···I2ii | 0.95 | 2.98 | 3.787 (3) | 143 |
Symmetry code: (ii) x, y−1, z. |
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