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The crystal structure of metachloro-nitrobenzene, C 6 H 4 C1 (1)  (NO 2 ) (3)  was redetermined at  T  = 298 K: Space group  Pna 2 1 ,  Z  = 4,  a  = 2114.90(40) pm,  b  = 593.20(10) pm,  c  = 529.00(10) pm,  R w  ( F ) = 0.038. The molecule is almost planar, with a small out of plane bending of the NO 2  group. Measurements of Zeeman-split  35 Cl NQR spectra give a nuclear quadrupole coupling constant  e  2  ϕ zz Qh  −1  = (69.745 ± 0.002) MHz at  T  = 298 K and (70.608 ± 0.002) MHz at  T  = 129 K. The asymmetry parameter is 0.1091 ± 0.0015 at 298 K (0.1066 ± 0.0040 at 129 K).  ϕ zz   is within 0.45° parallel to the bond direction C (1)  – Cl (1) ;  ϕ yy   and  ϕ xx   are almost in the C (1 … 6) -plane and perpendicular to it, respectively. The temperature dependence  v  ( 35 Cl) =  f ( T ) was studied from 77 K up to the melting point. Structure and electric field gradient orientation are discussed.

Structure and C–Cl bond in 1-Cl-3-NO 2 C 6 H 4: A 35 Cl–NQR and X-ray single crystal study