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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680402080X/bt6502sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680402080X/bt6502Isup2.hkl
Contains datablock I

CCDC reference: 251619

Key indicators

  • Single-crystal X-ray study
  • T = 213 K
  • Mean [sigma](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

Computing details top

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 = 317.77F(000) = 164
Triclinic, P1Dx = 1.367 Mg m3
Hall symbol: -P1Mo Kα radiation, λ = 0.71073 Å
a = 6.7439 (1) ÅCell parameters from 1543 reflections
b = 8.2016 (1) Åθ = 2–27°
c = 8.2846 (2) ŵ = 3.47 mm1
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 tube1383 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
ω scansθmax = 27.1°, θmin = 2.8°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
h = 88
Tmin = 0.388, Tmax = 0.500k = 109
3427 measured reflectionsl = 1010
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.080H 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 parametersΔρmax = 0.84 e Å3
0 restraintsΔρmin = 0.45 e Å3
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
xyzUiso*/Ueq
Ga10.01554 (4)0.29896 (4)0.91597 (4)0.03848 (14)
C10.2019 (6)0.2463 (7)0.7824 (5)0.0672 (10)
H1A0.29770.36490.78890.116 (8)*
H1B0.13110.15370.65550.116 (8)*
H1C0.28400.19430.83700.116 (8)*
C30.2082 (8)0.3946 (8)1.3388 (7)0.0706 (11)
N10.1471 (4)0.5401 (4)1.1533 (3)0.0378 (5)
N20.1256 (4)0.5353 (4)1.3241 (3)0.0496 (6)
C20.2496 (6)0.1117 (6)0.9467 (6)0.0676 (10)
H2A0.33270.17691.01850.116 (8)*
H2B0.18950.05301.00920.116 (8)*
H2C0.34220.01280.82770.116 (8)*
C40.2546 (8)0.7251 (7)1.4742 (5)0.0709 (11)
H3C0.370 (7)0.424 (6)1.328 (6)0.075 (13)*
H110.284 (6)0.575 (5)1.154 (5)0.049 (9)*
H3B0.114 (8)0.261 (8)1.231 (7)0.094 (16)*
H3A0.209 (6)0.396 (6)1.460 (6)0.063 (11)*
H4C0.410 (7)0.764 (7)1.471 (6)0.076 (13)*
H4B0.256 (7)0.729 (7)1.595 (7)0.086 (14)*
H4A0.201 (7)0.828 (7)1.466 (6)0.075 (13)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ga10.0405 (2)0.0400 (2)0.0346 (2)0.01489 (14)0.01106 (13)0.01666 (14)
C10.068 (2)0.087 (3)0.057 (2)0.047 (2)0.0282 (18)0.028 (2)
C30.072 (3)0.099 (3)0.065 (3)0.039 (2)0.011 (2)0.057 (3)
N10.0338 (12)0.0485 (14)0.0305 (12)0.0146 (10)0.0082 (9)0.0183 (10)
N20.0501 (14)0.0693 (18)0.0330 (13)0.0213 (13)0.0099 (11)0.0279 (13)
C20.059 (2)0.058 (2)0.080 (3)0.0042 (17)0.0081 (19)0.040 (2)
C40.075 (3)0.083 (3)0.0303 (17)0.021 (2)0.0013 (17)0.0126 (18)
Geometric parameters (Å, º) top
Ga1—C21.966 (4)C3—H3A1.00 (4)
Ga1—C11.970 (3)N1—N21.452 (3)
Ga1—N1i2.018 (2)N1—Ga1i2.018 (2)
Ga1—N12.019 (2)N1—H110.88 (4)
Ga1—Ga1i2.9397 (6)N2—C41.456 (5)
C1—H1A0.9700C2—H2A0.9700
C1—H1B0.9700C2—H2B0.9700
C1—H1C0.9700C2—H2C0.9700
C3—N21.464 (5)C4—H4C1.01 (5)
C3—H3C1.06 (4)C4—H4B0.99 (5)
C3—H3B1.04 (6)C4—H4A1.04 (5)
C2—Ga1—C1126.91 (19)N2—N1—Ga1i117.22 (18)
C2—Ga1—N1i106.44 (14)N2—N1—Ga1118.71 (19)
C1—Ga1—N1i111.39 (14)Ga1i—N1—Ga193.46 (9)
C2—Ga1—N1112.50 (15)N2—N1—H11109 (2)
C1—Ga1—N1105.73 (15)Ga1i—N1—H11110 (2)
N1i—Ga1—N186.54 (10)Ga1—N1—H11108 (2)
C2—Ga1—Ga1i117.20 (14)N1—N2—C4108.4 (3)
C1—Ga1—Ga1i115.89 (14)N1—N2—C3108.8 (3)
N1i—Ga1—Ga1i43.27 (7)C4—N2—C3108.9 (3)
N1—Ga1—Ga1i43.26 (7)Ga1—C2—H2A109.5
Ga1—C1—H1A109.5Ga1—C2—H2B109.5
Ga1—C1—H1B109.5H2A—C2—H2B109.5
H1A—C1—H1B109.5Ga1—C2—H2C109.5
Ga1—C1—H1C109.5H2A—C2—H2C109.5
H1A—C1—H1C109.5H2B—C2—H2C109.5
H1B—C1—H1C109.5N2—C4—H4C111 (3)
N2—C3—H3C112 (2)N2—C4—H4B113 (3)
N2—C3—H3B108 (3)H4C—C4—H4B105 (4)
H3C—C3—H3B108 (4)N2—C4—H4A110 (3)
N2—C3—H3A111 (2)H4C—C4—H4A107 (4)
H3C—C3—H3A106 (3)H4B—C4—H4A110 (4)
H3B—C3—H3A112 (4)
C2—Ga1—N1—N217.4 (3)N1i—Ga1—N1—Ga1i0.0
C1—Ga1—N1—N2125.0 (2)Ga1i—N1—N2—C468.2 (3)
N1i—Ga1—N1—N2123.7 (2)Ga1—N1—N2—C4179.3 (3)
Ga1i—Ga1—N1—N2123.7 (2)Ga1i—N1—N2—C3173.5 (3)
C2—Ga1—N1—Ga1i106.37 (15)Ga1—N1—N2—C362.4 (3)
C1—Ga1—N1—Ga1i111.25 (15)
Symmetry code: (i) x, y+1, z+2.
 

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