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The title centrosymmetric coordination compound, [Ga2(CH3)4(C2H7N2)2], contains tetrahedral Ga atoms bonded to two N atoms of the hydrazide ligands and two C atoms of the methyl groups. The Ga atoms are bridged by hydrazide moieties, creating a planar four-membered Ga2N2 ring, which may be considered as the main structural feature. The Ga—N bond distances are equal [2.018 (2) and 2.019 (2) Å] within experimental error.
Supporting information
CCDC reference: 251619
Key indicators
- Single-crystal X-ray study
- T = 213 K
- Mean (N-C) = 0.006 Å
- R factor = 0.032
- wR factor = 0.079
- Data-to-parameter ratio = 16.6
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.91
PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 6
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for Ga1
PLAT420_ALERT_2_C D-H Without Acceptor N1 - H11 ... ?
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.29 Ratio
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
5 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
2 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
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS90 (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 and PLATON (Spek, 2001).
Bis(µ-
N,
N-dimethylhydrazido-
κ2N':
N')bis[dimethylgallium(III)]
top
Crystal data top
[Ga2(CH3)4(C2H7N2)2] | Z = 1 |
Mr = 317.77 | F(000) = 164 |
Triclinic, P1 | Dx = 1.367 Mg m−3 |
Hall symbol: -P1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.7439 (1) Å | Cell parameters from 1543 reflections |
b = 8.2016 (1) Å | θ = 2–27° |
c = 8.2846 (2) Å | µ = 3.47 mm−1 |
α = 114.052 (1)° | T = 213 K |
β = 95.798 (1)° | Block, colorless |
γ = 107.406 (1)° | 0.30 × 0.30 × 0.20 mm |
V = 385.99 (1) Å3 | |
Data collection top
Bruker SMART CCD diffractometer | 1543 independent reflections |
Radiation source: fine-focus sealed tube | 1383 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
ω scans | θmax = 27.1°, θmin = 2.8° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −8→8 |
Tmin = 0.388, Tmax = 0.500 | k = −10→9 |
3427 measured reflections | l = −10→10 |
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)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.080 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0491P)2] where P = (Fo2 + 2Fc2)/3 |
1543 reflections | (Δ/σ)max < 0.001 |
93 parameters | Δρmax = 0.84 e Å−3 |
0 restraints | Δρmin = −0.45 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 | |
Ga1 | −0.01554 (4) | 0.29896 (4) | 0.91597 (4) | 0.03848 (14) | |
C1 | 0.2019 (6) | 0.2463 (7) | 0.7824 (5) | 0.0672 (10) | |
H1A | 0.2977 | 0.3649 | 0.7889 | 0.116 (8)* | |
H1B | 0.1311 | 0.1537 | 0.6555 | 0.116 (8)* | |
H1C | 0.2840 | 0.1943 | 0.8370 | 0.116 (8)* | |
C3 | 0.2082 (8) | 0.3946 (8) | 1.3388 (7) | 0.0706 (11) | |
N1 | 0.1471 (4) | 0.5401 (4) | 1.1533 (3) | 0.0378 (5) | |
N2 | 0.1256 (4) | 0.5353 (4) | 1.3241 (3) | 0.0496 (6) | |
C2 | −0.2496 (6) | 0.1117 (6) | 0.9467 (6) | 0.0676 (10) | |
H2A | −0.3327 | 0.1769 | 1.0185 | 0.116 (8)* | |
H2B | −0.1895 | 0.0530 | 1.0092 | 0.116 (8)* | |
H2C | −0.3422 | 0.0128 | 0.8277 | 0.116 (8)* | |
C4 | 0.2546 (8) | 0.7251 (7) | 1.4742 (5) | 0.0709 (11) | |
H3C | 0.370 (7) | 0.424 (6) | 1.328 (6) | 0.075 (13)* | |
H11 | 0.284 (6) | 0.575 (5) | 1.154 (5) | 0.049 (9)* | |
H3B | 0.114 (8) | 0.261 (8) | 1.231 (7) | 0.094 (16)* | |
H3A | 0.209 (6) | 0.396 (6) | 1.460 (6) | 0.063 (11)* | |
H4C | 0.410 (7) | 0.764 (7) | 1.471 (6) | 0.076 (13)* | |
H4B | 0.256 (7) | 0.729 (7) | 1.595 (7) | 0.086 (14)* | |
H4A | 0.201 (7) | 0.828 (7) | 1.466 (6) | 0.075 (13)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ga1 | 0.0405 (2) | 0.0400 (2) | 0.0346 (2) | 0.01489 (14) | 0.01106 (13) | 0.01666 (14) |
C1 | 0.068 (2) | 0.087 (3) | 0.057 (2) | 0.047 (2) | 0.0282 (18) | 0.028 (2) |
C3 | 0.072 (3) | 0.099 (3) | 0.065 (3) | 0.039 (2) | 0.011 (2) | 0.057 (3) |
N1 | 0.0338 (12) | 0.0485 (14) | 0.0305 (12) | 0.0146 (10) | 0.0082 (9) | 0.0183 (10) |
N2 | 0.0501 (14) | 0.0693 (18) | 0.0330 (13) | 0.0213 (13) | 0.0099 (11) | 0.0279 (13) |
C2 | 0.059 (2) | 0.058 (2) | 0.080 (3) | 0.0042 (17) | 0.0081 (19) | 0.040 (2) |
C4 | 0.075 (3) | 0.083 (3) | 0.0303 (17) | 0.021 (2) | 0.0013 (17) | 0.0126 (18) |
Geometric parameters (Å, º) top
Ga1—C2 | 1.966 (4) | C3—H3A | 1.00 (4) |
Ga1—C1 | 1.970 (3) | N1—N2 | 1.452 (3) |
Ga1—N1i | 2.018 (2) | N1—Ga1i | 2.018 (2) |
Ga1—N1 | 2.019 (2) | N1—H11 | 0.88 (4) |
Ga1—Ga1i | 2.9397 (6) | N2—C4 | 1.456 (5) |
C1—H1A | 0.9700 | C2—H2A | 0.9700 |
C1—H1B | 0.9700 | C2—H2B | 0.9700 |
C1—H1C | 0.9700 | C2—H2C | 0.9700 |
C3—N2 | 1.464 (5) | C4—H4C | 1.01 (5) |
C3—H3C | 1.06 (4) | C4—H4B | 0.99 (5) |
C3—H3B | 1.04 (6) | C4—H4A | 1.04 (5) |
| | | |
C2—Ga1—C1 | 126.91 (19) | N2—N1—Ga1i | 117.22 (18) |
C2—Ga1—N1i | 106.44 (14) | N2—N1—Ga1 | 118.71 (19) |
C1—Ga1—N1i | 111.39 (14) | Ga1i—N1—Ga1 | 93.46 (9) |
C2—Ga1—N1 | 112.50 (15) | N2—N1—H11 | 109 (2) |
C1—Ga1—N1 | 105.73 (15) | Ga1i—N1—H11 | 110 (2) |
N1i—Ga1—N1 | 86.54 (10) | Ga1—N1—H11 | 108 (2) |
C2—Ga1—Ga1i | 117.20 (14) | N1—N2—C4 | 108.4 (3) |
C1—Ga1—Ga1i | 115.89 (14) | N1—N2—C3 | 108.8 (3) |
N1i—Ga1—Ga1i | 43.27 (7) | C4—N2—C3 | 108.9 (3) |
N1—Ga1—Ga1i | 43.26 (7) | Ga1—C2—H2A | 109.5 |
Ga1—C1—H1A | 109.5 | Ga1—C2—H2B | 109.5 |
Ga1—C1—H1B | 109.5 | H2A—C2—H2B | 109.5 |
H1A—C1—H1B | 109.5 | Ga1—C2—H2C | 109.5 |
Ga1—C1—H1C | 109.5 | H2A—C2—H2C | 109.5 |
H1A—C1—H1C | 109.5 | H2B—C2—H2C | 109.5 |
H1B—C1—H1C | 109.5 | N2—C4—H4C | 111 (3) |
N2—C3—H3C | 112 (2) | N2—C4—H4B | 113 (3) |
N2—C3—H3B | 108 (3) | H4C—C4—H4B | 105 (4) |
H3C—C3—H3B | 108 (4) | N2—C4—H4A | 110 (3) |
N2—C3—H3A | 111 (2) | H4C—C4—H4A | 107 (4) |
H3C—C3—H3A | 106 (3) | H4B—C4—H4A | 110 (4) |
H3B—C3—H3A | 112 (4) | | |
| | | |
C2—Ga1—N1—N2 | 17.4 (3) | N1i—Ga1—N1—Ga1i | 0.0 |
C1—Ga1—N1—N2 | −125.0 (2) | Ga1i—N1—N2—C4 | −68.2 (3) |
N1i—Ga1—N1—N2 | 123.7 (2) | Ga1—N1—N2—C4 | −179.3 (3) |
Ga1i—Ga1—N1—N2 | 123.7 (2) | Ga1i—N1—N2—C3 | 173.5 (3) |
C2—Ga1—N1—Ga1i | −106.37 (15) | Ga1—N1—N2—C3 | 62.4 (3) |
C1—Ga1—N1—Ga1i | 111.25 (15) | | |
Symmetry code: (i) −x, −y+1, −z+2. |
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