Crystals of the title compound, [Ga(NH3)5Cl]Cl2, were prepared from 1-butyl-3-methylimidazolium chloride and GaCl3. The crystal structure is isotypic with [Al(NH3)5Cl]Cl2 and other members of the series [M(NH3)5Cl]Cl2, with M = Cr, Co, Rh, Ir, Ru or Os. It consists of discrete cationic [Ga(NH3)5Cl]2+ octahedra and Cl- anions arranged in motifs related to the K2PtCl6 structure type. In the cation, the Ga atom, one Cl atom and three N atoms are located on a mirror plane.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (a-N) = 0.003 Å
- R factor = 0.022
- wR factor = 0.053
- Data-to-parameter ratio = 14.1
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT352_ALERT_3_C Short N-H Bond (0.87A) N2 - H4 ... 0.74 Ang.
PLAT352_ALERT_3_C Short N-H Bond (0.87A) N2 - H4_a ... 0.74 Ang.
PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1 ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N2 - H3 ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N3 - H5 ... ?
PLAT480_ALERT_4_C Long H...A H-Bond Reported H1 .. CL2 .. 3.10 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H3 .. CL2 .. 3.20 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H5 .. CL2 .. 3.04 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H9 .. CL2 .. 2.86 Ang.
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
10 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 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
4 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: PROCESS-AUTO (Rigaku/MSC, 2005); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2005); program(s) used to solve structure: coordinates taken from an isotypic structure (Jacobs & Schröder, 2002); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 2005); software used to prepare material for publication: SHELXL97.
pentaamminechlorogallium(III) dichloride
top
Crystal data top
ClGaH15N52+·2Cl− | F(000) = 528 |
Mr = 261.24 | Dx = 1.817 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 7848 reflections |
a = 13.448 (6) Å | θ = 3.0–27.5° |
b = 10.518 (5) Å | µ = 3.66 mm−1 |
c = 6.750 (4) Å | T = 295 K |
V = 954.8 (8) Å3 | Block, colourless |
Z = 4 | 0.18 × 0.17 × 0.10 mm |
Data collection top
Rigaku R-AXIS RAPID CCD area-detector diffractometer | 1157 independent reflections |
Radiation source: fine-focus sealed tube | 1041 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.047 |
Detector resolution: 10.00 pixels mm-1 | θmax = 27.5°, θmin = 3.0° |
ω scans | h = −17→17 |
Absorption correction: numerical (NUMABS; Higashi, 1999) | k = −13→13 |
Tmin = 0.476, Tmax = 0.577 | l = −8→8 |
8938 measured reflections | |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | All H-atom parameters refined |
R[F2 > 2σ(F2)] = 0.022 | w = 1/[σ2(Fo2) + (0.0282P)2 + 0.3606P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.053 | (Δ/σ)max < 0.001 |
S = 1.07 | Δρmax = 0.31 e Å−3 |
1157 reflections | Δρmin = −0.28 e Å−3 |
82 parameters | |
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 | |
Cl1 | −0.02810 (5) | 0.2500 | −0.05178 (10) | 0.02976 (15) | |
Cl2 | 0.35244 (3) | 0.00215 (5) | 0.16337 (7) | 0.03187 (13) | |
Ga1 | 0.104663 (19) | 0.2500 | 0.18229 (4) | 0.02031 (10) | |
N1 | 0.2066 (2) | 0.2500 | −0.0481 (4) | 0.0354 (6) | |
N2 | 0.0042 (2) | 0.2500 | 0.4150 (4) | 0.0326 (5) | |
N3 | 0.2209 (2) | 0.2500 | 0.3846 (4) | 0.0314 (5) | |
N4 | 0.10274 (15) | 0.05470 (17) | 0.1783 (3) | 0.0319 (4) | |
H1 | 0.262 (5) | 0.2500 | −0.006 (11) | 0.12 (2)* | |
H2 | 0.198 (3) | 0.194 (3) | −0.121 (5) | 0.098 (14)* | |
H3 | 0.033 (4) | 0.2500 | 0.528 (9) | 0.11 (2)* | |
H4 | −0.027 (2) | 0.192 (3) | 0.407 (4) | 0.067 (10)* | |
H5 | 0.277 (4) | 0.2500 | 0.342 (7) | 0.089 (19)* | |
H6 | 0.215 (3) | 0.189 (3) | 0.466 (6) | 0.107 (14)* | |
H7 | 0.047 (3) | 0.024 (3) | 0.207 (5) | 0.071 (10)* | |
H8 | 0.113 (2) | 0.027 (3) | 0.074 (6) | 0.069 (11)* | |
H9 | 0.145 (3) | 0.022 (4) | 0.249 (7) | 0.113 (15)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cl1 | 0.0294 (3) | 0.0296 (3) | 0.0303 (3) | 0.000 | −0.0078 (3) | 0.000 |
Cl2 | 0.0335 (2) | 0.0295 (2) | 0.0326 (3) | −0.00100 (19) | −0.00102 (18) | −0.00154 (18) |
Ga1 | 0.02220 (15) | 0.01730 (14) | 0.02142 (15) | 0.000 | −0.00078 (9) | 0.000 |
N1 | 0.0349 (14) | 0.0393 (14) | 0.0319 (14) | 0.000 | 0.0061 (11) | 0.000 |
N2 | 0.0347 (13) | 0.0330 (13) | 0.0299 (15) | 0.000 | 0.0050 (11) | 0.000 |
N3 | 0.0289 (12) | 0.0299 (12) | 0.0354 (13) | 0.000 | −0.0109 (10) | 0.000 |
N4 | 0.0363 (9) | 0.0216 (8) | 0.0378 (10) | −0.0013 (7) | −0.0046 (8) | −0.0014 (7) |
Geometric parameters (Å, º) top
Cl1—Ga1 | 2.3840 (11) | N2—H3 | 0.85 (6) |
Ga1—N4 | 2.055 (2) | N2—H4 | 0.74 (3) |
Ga1—N2 | 2.072 (3) | N3—H5 | 0.81 (6) |
Ga1—N1 | 2.073 (3) | N3—H6 | 0.85 (4) |
Ga1—N3 | 2.076 (3) | N4—H7 | 0.83 (4) |
N1—H1 | 0.79 (6) | N4—H8 | 0.77 (4) |
N1—H2 | 0.77 (4) | N4—H9 | 0.81 (5) |
| | | |
N1—Ga1—N3 | 89.73 (13) | H4i—N2—H4 | 110 (5) |
N1—Ga1—Cl1 | 89.89 (10) | H5—N3—H6 | 109 (3) |
N2—Ga1—N3 | 89.57 (13) | H6i—N3—H6 | 98 (5) |
N2—Ga1—N1 | 179.30 (13) | H7—N4—H8 | 103 (3) |
N2—Ga1—Cl1 | 90.80 (10) | H7—N4—H9 | 109 (4) |
N3—Ga1—Cl1 | 179.63 (9) | H8—N4—H9 | 105 (4) |
N4—Ga1—N4i | 177.91 (12) | Ga1—N1—H2 | 112 (3) |
N4—Ga1—N2 | 90.10 (6) | Ga1—N1—H1 | 111 (5) |
N4i—Ga1—N2 | 90.10 (6) | Ga1—N2—H3 | 113 (4) |
N4—Ga1—N1 | 89.91 (6) | Ga1—N2—H4 | 109 (2) |
N4i—Ga1—N1 | 89.91 (6) | Ga1—N3—H5 | 118 (4) |
N4—Ga1—N3 | 91.04 (6) | Ga1—N3—H6 | 111 (3) |
N4i—Ga1—N3 | 91.04 (6) | Ga1—N4—H7 | 113 (2) |
N4—Ga1—Cl1 | 88.96 (6) | Ga1—N4—H8 | 112 (3) |
N4i—Ga1—Cl1 | 88.96 (6) | Ga1—N4—H9 | 114 (3) |
H1—N1—H2 | 111 (4) | H2i—N1—Ga1 | 112 (3) |
H2i—N1—H2 | 99 (5) | H4i—N2—Ga1 | 109 (2) |
H3—N2—H4 | 109 (3) | H6i—N3—Ga1 | 111 (3) |
Symmetry code: (i) x, −y+1/2, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···Cl2 | 0.79 (6) | 3.10 (4) | 3.561 (3) | 120 (2) |
N1—H2···Cl2ii | 0.77 (4) | 2.62 (4) | 3.385 (2) | 172 (4) |
N2—H3···Cl2iii | 0.85 (6) | 3.20 (3) | 3.683 (3) | 118 (2) |
N2—H4···Cl2iv | 0.74 (3) | 2.61 (3) | 3.353 (2) | 172 (3) |
N3—H5···Cl2 | 0.81 (6) | 3.04 (3) | 3.486 (2) | 117 (2) |
N3—H6···Cl2iii | 0.85 (4) | 2.58 (4) | 3.398 (2) | 164 (3) |
N4—H7···Cl2iv | 0.83 (4) | 2.77 (4) | 3.575 (3) | 162 (3) |
N4—H8···Cl2ii | 0.77 (4) | 2.83 (4) | 3.578 (3) | 164 (3) |
N4—H9···Cl2iii | 0.81 (5) | 2.81 (5) | 3.383 (3) | 129 (4) |
N4—H9···Cl2 | 0.81 (5) | 2.86 (4) | 3.405 (3) | 126 (4) |
Symmetry codes: (ii) −x+1/2, −y, z−1/2; (iii) −x+1/2, −y, z+1/2; (iv) x−1/2, y, −z+1/2. |