The title compound, Rb3CoCl4NO3, is isostructural with K3ZnCl4NO3. It is built up from Rb+ cations, NO3- anions and [CoCl4]2- complex ions which form a layer-like arrangement: one layer contains only rubidium cations while the other contains a mixture of rubidium, nitrate and tetrachlorocobaltate ions. Both rubidium cations are ninefold coordinated by three O atoms and six Cl ions. One Rb atom, the Co atom, two Cl atoms, the N atom and one O atom lie on a crystallographic mirror plane.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (O-N) = 0.003 Å
- R factor = 0.020
- wR factor = 0.043
- Data-to-parameter ratio = 27.6
checkCIF/PLATON results
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Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
1 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
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97.
Trirubidium cobalt tetrachloride nitrate(V), Rb
3CoCl
4NO
3 top
Crystal data top
Rb3CoCl4NO3 | F(000) = 948 |
Mr = 519.15 | Dx = 2.953 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 16196 reflections |
a = 9.3183 (7) Å | θ = 3.8–32.3° |
b = 10.0730 (9) Å | µ = 14.78 mm−1 |
c = 12.4423 (9) Å | T = 173 K |
V = 1167.87 (16) Å3 | Block, blue |
Z = 4 | 0.12 × 0.11 × 0.07 mm |
Data collection top
Stoe IPDS-II two-circle diffractometer | 1793 independent reflections |
Radiation source: fine-focus sealed tube | 1596 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.061 |
ω scans | θmax = 30.0°, θmin = 3.9° |
Absorption correction: multi-scan (MULABS; Spek, 1990; Blessing, 1995) | h = −13→13 |
Tmin = 0.189, Tmax = 0.361 | k = −14→14 |
18011 measured reflections | l = −17→17 |
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)] = 0.020 | w = 1/[σ2(Fo2) + (0.0233P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.043 | (Δ/σ)max = 0.001 |
S = 1.02 | Δρmax = 0.42 e Å−3 |
1793 reflections | Δρmin = −0.49 e Å−3 |
65 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0031 (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 | |
Rb1 | 0.58800 (3) | 0.7500 | 0.46770 (2) | 0.03377 (7) | |
Rb2 | 0.11752 (2) | 0.49488 (2) | 0.320448 (16) | 0.03718 (6) | |
Co1 | 0.17994 (4) | 0.7500 | 0.59052 (3) | 0.03156 (8) | |
Cl1 | 0.62423 (8) | 0.7500 | 0.73074 (6) | 0.03910 (15) | |
Cl2 | 0.30329 (6) | 0.56233 (5) | 0.55412 (4) | 0.04036 (11) | |
Cl3 | 0.97074 (8) | 0.7500 | 0.49510 (6) | 0.04051 (15) | |
N1 | 0.3405 (3) | 0.7500 | 0.27463 (18) | 0.0329 (4) | |
O1 | 0.40210 (16) | 0.64210 (17) | 0.29311 (13) | 0.0401 (3) | |
O2 | 0.2141 (2) | 0.7500 | 0.23954 (19) | 0.0402 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rb1 | 0.03532 (13) | 0.03422 (13) | 0.03177 (11) | 0.000 | −0.00098 (9) | 0.000 |
Rb2 | 0.03975 (10) | 0.03417 (11) | 0.03763 (10) | −0.00110 (6) | −0.00170 (7) | 0.00247 (7) |
Co1 | 0.03301 (17) | 0.03051 (17) | 0.03117 (17) | 0.000 | 0.00100 (12) | 0.000 |
Cl1 | 0.0440 (4) | 0.0423 (4) | 0.0310 (3) | 0.000 | −0.0034 (2) | 0.000 |
Cl2 | 0.0477 (3) | 0.0330 (2) | 0.0405 (2) | 0.00555 (17) | −0.00051 (19) | −0.00259 (18) |
Cl3 | 0.0369 (3) | 0.0459 (4) | 0.0387 (3) | 0.000 | −0.0043 (2) | 0.000 |
N1 | 0.0326 (11) | 0.0356 (12) | 0.0305 (10) | 0.000 | 0.0020 (8) | 0.000 |
O1 | 0.0377 (7) | 0.0367 (8) | 0.0460 (8) | 0.0055 (6) | −0.0019 (6) | 0.0008 (6) |
O2 | 0.0336 (10) | 0.0410 (11) | 0.0459 (11) | 0.000 | −0.0081 (8) | 0.000 |
Geometric parameters (Å, º) top
Rb1—O2i | 2.834 (2) | Co1—Cl3vii | 2.2825 (8) |
Rb1—O1ii | 2.9835 (16) | Co1—Cl1viii | 2.2837 (8) |
Rb1—O1 | 2.9835 (17) | Cl1—Co1ix | 2.2837 (8) |
Rb1—Cl1 | 3.2903 (8) | Cl1—Rb2iv | 3.5045 (6) |
Rb1—Cl2iii | 3.3163 (6) | Cl1—Rb2iii | 3.5045 (6) |
Rb1—Cl2iv | 3.3163 (6) | Cl1—Rb2x | 3.5221 (6) |
Rb1—Cl2 | 3.4305 (6) | Cl1—Rb2xi | 3.5221 (6) |
Rb1—Cl2ii | 3.4305 (6) | Cl2—Rb1iii | 3.3163 (6) |
Rb1—Cl3 | 3.5827 (8) | Cl2—Rb2xi | 3.4434 (6) |
Rb2—O1v | 2.8679 (16) | Cl3—Co1xii | 2.2824 (8) |
Rb2—O2 | 2.9031 (12) | Cl3—Rb2iv | 3.4681 (6) |
Rb2—O1 | 3.0572 (17) | Cl3—Rb2iii | 3.4681 (6) |
Rb2—Cl2vi | 3.4434 (6) | Cl3—Rb2xiii | 3.6328 (6) |
Rb2—Cl2 | 3.4513 (6) | Cl3—Rb2xii | 3.6328 (6) |
Rb2—Cl3iii | 3.4681 (6) | N1—O1 | 1.250 (2) |
Rb2—Cl1iii | 3.5044 (6) | N1—O1ii | 1.250 (2) |
Rb2—Cl1vi | 3.5221 (6) | N1—O2 | 1.256 (3) |
Rb2—Cl3vii | 3.6328 (6) | O1—Rb2i | 2.8679 (16) |
Co1—Cl2 | 2.2583 (6) | O2—Rb1v | 2.834 (2) |
Co1—Cl2ii | 2.2583 (6) | O2—Rb2ii | 2.9030 (12) |
| | | |
O2i—Rb1—O1ii | 65.06 (5) | Cl1iii—Rb2—Cl1vi | 83.606 (8) |
O2i—Rb1—O1 | 65.06 (5) | O1v—Rb2—Cl3vii | 70.45 (4) |
O1ii—Rb1—O1 | 42.73 (6) | O2—Rb2—Cl3vii | 72.42 (4) |
O2i—Rb1—Cl1 | 149.61 (5) | O1—Rb2—Cl3vii | 92.87 (3) |
O1ii—Rb1—Cl1 | 141.61 (4) | N1—Rb2—Cl3vii | 78.05 (3) |
O1—Rb1—Cl1 | 141.61 (4) | Cl2vi—Rb2—Cl3vii | 140.779 (14) |
O2i—Rb1—Cl2iii | 78.395 (16) | Cl2—Rb2—Cl3vii | 62.977 (15) |
O1ii—Rb1—Cl2iii | 117.60 (3) | Cl3iii—Rb2—Cl3vii | 91.032 (8) |
O1—Rb1—Cl2iii | 76.83 (3) | Cl1iii—Rb2—Cl3vii | 149.904 (17) |
Cl1—Rb1—Cl2iii | 92.871 (11) | Cl1vi—Rb2—Cl3vii | 116.370 (16) |
O2i—Rb1—Cl2iv | 78.395 (16) | Cl2—Co1—Cl2ii | 113.67 (3) |
O1ii—Rb1—Cl2iv | 76.83 (3) | Cl2—Co1—Cl3vii | 109.29 (2) |
O1—Rb1—Cl2iv | 117.60 (3) | Cl2ii—Co1—Cl3vii | 109.29 (2) |
Cl1—Rb1—Cl2iv | 92.871 (11) | Cl2—Co1—Cl1viii | 108.12 (2) |
Cl2iii—Rb1—Cl2iv | 143.13 (2) | Cl2ii—Co1—Cl1viii | 108.12 (2) |
O2i—Rb1—Cl2 | 127.30 (4) | Cl3vii—Co1—Cl1viii | 108.20 (3) |
O1ii—Rb1—Cl2 | 88.85 (3) | Co1ix—Cl1—Rb1 | 172.75 (3) |
O1—Rb1—Cl2 | 65.07 (3) | Co1ix—Cl1—Rb2iv | 91.198 (19) |
Cl1—Rb1—Cl2 | 76.557 (15) | Rb1—Cl1—Rb2iv | 83.665 (15) |
Cl2iii—Rb1—Cl2 | 74.876 (15) | Co1ix—Cl1—Rb2iii | 91.197 (19) |
Cl2iv—Rb1—Cl2 | 141.687 (13) | Rb1—Cl1—Rb2iii | 83.665 (15) |
N1—Rb1—Cl2 | 71.97 (3) | Rb2iv—Cl1—Rb2iii | 89.477 (19) |
O2i—Rb1—Cl2ii | 127.30 (4) | Co1ix—Cl1—Rb2x | 80.607 (18) |
O1ii—Rb1—Cl2ii | 65.07 (3) | Rb1—Cl1—Rb2x | 104.455 (16) |
O1—Rb1—Cl2ii | 88.85 (3) | Rb2iv—Cl1—Rb2x | 90.220 (8) |
Cl1—Rb1—Cl2ii | 76.558 (15) | Rb2iii—Cl1—Rb2x | 171.79 (2) |
Cl2iii—Rb1—Cl2ii | 141.688 (13) | Co1ix—Cl1—Rb2xi | 80.607 (18) |
Cl2iv—Rb1—Cl2ii | 74.876 (15) | Rb1—Cl1—Rb2xi | 104.454 (16) |
N1—Rb1—Cl2ii | 71.97 (3) | Rb2iv—Cl1—Rb2xi | 171.79 (2) |
Cl2—Rb1—Cl2ii | 66.878 (19) | Rb2iii—Cl1—Rb2xi | 90.220 (8) |
O2i—Rb1—Cl3 | 70.96 (5) | Rb2x—Cl1—Rb2xi | 88.910 (19) |
O1ii—Rb1—Cl3 | 130.34 (3) | Co1—Cl2—Rb1iii | 165.02 (3) |
O1—Rb1—Cl3 | 130.34 (3) | Co1—Cl2—Rb1 | 89.73 (2) |
Cl1—Rb1—Cl3 | 78.649 (18) | Rb1iii—Cl2—Rb1 | 105.124 (15) |
Cl2iii—Rb1—Cl3 | 72.767 (11) | Co1—Cl2—Rb2xi | 93.222 (19) |
Cl2iv—Rb1—Cl3 | 72.768 (11) | Rb1iii—Cl2—Rb2xi | 81.636 (13) |
N1—Rb1—Cl3 | 139.29 (4) | Rb1—Cl2—Rb2xi | 103.190 (16) |
Cl2—Rb1—Cl3 | 137.732 (13) | Co1—Cl2—Rb2 | 94.50 (2) |
Cl2ii—Rb1—Cl3 | 137.732 (13) | Rb1iii—Cl2—Rb2 | 84.115 (13) |
O1v—Rb2—O2 | 65.70 (5) | Rb1—Cl2—Rb2 | 103.433 (16) |
O1v—Rb2—O1 | 107.55 (5) | Rb2xi—Cl2—Rb2 | 152.277 (18) |
O2—Rb2—O1 | 42.53 (5) | Co1xii—Cl3—Rb2iv | 81.858 (18) |
O1v—Rb2—Cl2vi | 76.26 (3) | Co1xii—Cl3—Rb2iii | 81.858 (18) |
O2—Rb2—Cl2vi | 75.40 (5) | Rb2iv—Cl3—Rb2iii | 90.67 (2) |
O1—Rb2—Cl2vi | 77.77 (3) | Co1xii—Cl3—Rb1 | 154.12 (3) |
N1—Rb2—Cl2vi | 80.32 (4) | Rb2iv—Cl3—Rb1 | 80.033 (14) |
O1v—Rb2—Cl2 | 131.63 (4) | Rb2iii—Cl3—Rb1 | 80.033 (14) |
O2—Rb2—Cl2 | 87.84 (4) | Co1xii—Cl3—Rb2xiii | 89.402 (19) |
O1—Rb2—Cl2 | 64.10 (3) | Rb2iv—Cl3—Rb2xiii | 88.968 (8) |
N1—Rb2—Cl2 | 71.43 (4) | Rb2iii—Cl3—Rb2xiii | 171.21 (2) |
Cl2vi—Rb2—Cl2 | 137.405 (8) | Rb1—Cl3—Rb2xiii | 108.533 (15) |
O1v—Rb2—Cl3iii | 121.86 (4) | Co1xii—Cl3—Rb2xii | 89.402 (19) |
O2—Rb2—Cl3iii | 158.84 (5) | Rb2iv—Cl3—Rb2xii | 171.21 (2) |
O1—Rb2—Cl3iii | 128.63 (3) | Rb2iii—Cl3—Rb2xii | 88.968 (8) |
N1—Rb2—Cl3iii | 143.56 (4) | Rb1—Cl3—Rb2xii | 108.533 (15) |
Cl2vi—Rb2—Cl3iii | 124.652 (15) | Rb2xiii—Cl3—Rb2xii | 90.047 (19) |
Cl2—Rb2—Cl3iii | 72.633 (15) | O1—N1—O1ii | 120.7 (2) |
O1v—Rb2—Cl1iii | 139.03 (4) | O1—N1—O2 | 119.62 (12) |
O2—Rb2—Cl1iii | 110.31 (4) | O1ii—N1—O2 | 119.62 (12) |
O1—Rb2—Cl1iii | 74.07 (3) | N1—O1—Rb2i | 132.85 (15) |
N1—Rb2—Cl1iii | 94.76 (3) | N1—O1—Rb1 | 94.80 (13) |
Cl2vi—Rb2—Cl1iii | 63.906 (14) | Rb2i—O1—Rb1 | 98.09 (5) |
Cl2—Rb2—Cl1iii | 86.978 (15) | N1—O1—Rb2 | 92.52 (12) |
Cl3iii—Rb2—Cl1iii | 77.437 (16) | Rb2i—O1—Rb2 | 114.28 (6) |
O1v—Rb2—Cl1vi | 76.01 (4) | Rb1—O1—Rb2 | 126.82 (6) |
O2—Rb2—Cl1vi | 135.11 (4) | N1—O2—Rb1v | 134.84 (18) |
O1—Rb2—Cl1vi | 149.23 (3) | N1—O2—Rb2ii | 99.80 (8) |
N1—Rb2—Cl1vi | 151.53 (4) | Rb1v—O2—Rb2ii | 100.77 (5) |
Cl2vi—Rb2—Cl1vi | 73.434 (16) | N1—O2—Rb2 | 99.80 (8) |
Cl2—Rb2—Cl1vi | 136.522 (15) | Rb1v—O2—Rb2 | 100.77 (5) |
Cl3iii—Rb2—Cl1vi | 63.890 (16) | Rb2ii—O2—Rb2 | 124.56 (8) |
Symmetry codes: (i) x+1/2, y, −z+1/2; (ii) x, −y+3/2, z; (iii) −x+1, −y+1, −z+1; (iv) −x+1, y+1/2, −z+1; (v) x−1/2, y, −z+1/2; (vi) −x+1/2, −y+1, z−1/2; (vii) x−1, y, z; (viii) x−1/2, y, −z+3/2; (ix) x+1/2, y, −z+3/2; (x) −x+1/2, y+1/2, z+1/2; (xi) −x+1/2, −y+1, z+1/2; (xii) x+1, y, z; (xiii) x+1, −y+3/2, z. |