The crystal structure of the title compound, dimethylammonium tetrachlorocobaltate(II), has been determined at four temperatures between 297 and 366 K, in order to investigate possible phase transitions at 313 and 353 K [Kapustianik, Polovinko & Kaluza et al. (1996). Phys. Status Solidi A, 153, 117-122]. We found that there is no significant change either in the hydrogen-bonding network or in the cell parameters, apart from a linear dilatation with temperature. This study reveals that the anomalous variation in electric conductivity and some of the other physical properties of the compound cannot be explained by structural changes.
Supporting information
| Crystallographic Information File (CIF) Contains datablocks 297, 320, 343, 366, global |
| Structure factor file (CIF format) Contains datablock co |
| Structure factor file (CIF format) Contains datablock co |
| Structure factor file (CIF format) Contains datablock co |
| Structure factor file (CIF format) Contains datablock Co-93 |
CCDC references: 136453; 136454; 136455; 136456
For all compounds, data collection: Siemens SMART; cell refinement: Siemens SAINT; data reduction: Siemens SAINT & SADABS; program(s) used to solve structure: SHELXTL (Bruker AXS, 1997); program(s) used to refine structure: SHELXTL (Bruker AXS, 1997); molecular graphics: SHELXTL.
(297) Dimethylammonium tetrachlorocobaltate(II)
top
Crystal data top
2(C2H8N)·CoCl4 | F(000) = 596 |
Mr = 292.92 | Dx = 1.498 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 3419 reflections |
a = 8.5313 (2) Å | θ = 1–25° |
b = 11.4382 (2) Å | µ = 2.10 mm−1 |
c = 13.3070 (1) Å | T = 297 K |
β = 90.038 (1)° | Plate, dark-blue |
V = 1298.53 (4) Å3 | 0.50 × 0.35 × 0.06 mm |
Z = 4 | |
Data collection top
Siemens SMART CCD diffractometer | 2372 independent reflections |
Radiation source: fine-focus sealed tube | 1794 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.036 |
Detector resolution: no pixels mm-1 | θmax = 25.4°, θmin = 2.4° |
ω scans | h = −9→10 |
Absorption correction: multi-scan (blessing, 1995; Sheldrick, 1996) Blessing, Acta Cryst. (1995), A51, 33-38. | k = −13→13 |
Tmin = 0.420, Tmax = 0.884 | l = −16→15 |
6987 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.034 | See experimental |
wR(F2) = 0.082 | w = 1/[σ2(Fo2) + (0.0419P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.001 |
2372 reflections | Δρmax = 0.30 e Å−3 |
121 parameters | Δρmin = −0.56 e Å−3 |
0 restraints | Extinction correction: SHELXTL (Bruker AXS, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0066 (8) |
Crystal data top
2(C2H8N)·CoCl4 | V = 1298.53 (4) Å3 |
Mr = 292.92 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 8.5313 (2) Å | µ = 2.10 mm−1 |
b = 11.4382 (2) Å | T = 297 K |
c = 13.3070 (1) Å | 0.50 × 0.35 × 0.06 mm |
β = 90.038 (1)° | |
Data collection top
Siemens SMART CCD diffractometer | 2372 independent reflections |
Absorption correction: multi-scan (blessing, 1995; Sheldrick, 1996) Blessing, Acta Cryst. (1995), A51, 33-38. | 1794 reflections with I > 2σ(I) |
Tmin = 0.420, Tmax = 0.884 | Rint = 0.036 |
6987 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.034 | 0 restraints |
wR(F2) = 0.082 | See experimental |
S = 1.00 | Δρmax = 0.30 e Å−3 |
2372 reflections | Δρmin = −0.56 e Å−3 |
121 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 | |
Co1 | 0.83030 (4) | 0.79927 (3) | 0.58124 (3) | 0.04144 (16) | |
Cl1 | 1.07371 (10) | 0.73758 (7) | 0.63113 (6) | 0.0562 (2) | |
Cl2 | 0.80783 (11) | 0.73567 (7) | 0.41972 (6) | 0.0568 (2) | |
Cl3 | 0.81891 (10) | 0.99667 (7) | 0.59011 (6) | 0.0575 (2) | |
Cl4 | 0.64014 (11) | 0.72083 (8) | 0.67735 (7) | 0.0669 (3) | |
N1 | 0.7900 (3) | 0.9975 (3) | 0.3351 (2) | 0.0565 (7) | |
H1A | 0.8422 | 1.0551 | 0.3668 | 0.112 (16)* | |
H1B | 0.8115 | 0.9301 | 0.3672 | 0.121 (17)* | |
N2 | 0.7068 (3) | 0.8097 (2) | 0.9034 (2) | 0.0591 (7) | |
H2A | 0.6733 | 0.7726 | 0.8478 | 0.077 (13)* | |
H2B | 0.6509 | 0.7822 | 0.9557 | 0.099 (15)* | |
C11 | 0.8467 (4) | 0.9893 (3) | 0.2315 (3) | 0.0638 (9) | |
H11A | 0.9583 | 0.9784 | 0.2317 | 0.090 (13)* | |
H11B | 0.8213 | 1.0600 | 0.1961 | 0.096 (14)* | |
H11C | 0.7976 | 0.9241 | 0.1987 | 0.129 (18)* | |
C21 | 0.6747 (6) | 0.9348 (4) | 0.8925 (4) | 0.0868 (13) | |
H21A | 0.7114 | 0.9756 | 0.9510 | 0.127 (19)* | |
H21B | 0.5639 | 0.9468 | 0.8851 | 0.122 (18)* | |
H21C | 0.7278 | 0.9641 | 0.8341 | 0.118 (18)* | |
C22 | 0.8730 (5) | 0.7810 (4) | 0.9196 (4) | 0.0874 (14) | |
H22A | 0.8845 | 0.6979 | 0.9263 | 0.14 (2)* | |
H22B | 0.9094 | 0.8185 | 0.9798 | 0.14 (2)* | |
H22C | 0.9335 | 0.8078 | 0.8634 | 0.128 (19)* | |
C12 | 0.6201 (4) | 1.0207 (4) | 0.3421 (4) | 0.0838 (12) | |
H12A | 0.5897 | 1.0239 | 0.4115 | 0.115 (16)* | |
H12B | 0.5635 | 0.9593 | 0.3089 | 0.105 (16)* | |
H12C | 0.5968 | 1.0941 | 0.3104 | 0.13 (2)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0409 (3) | 0.0424 (3) | 0.0411 (2) | 0.00027 (18) | 0.00110 (17) | 0.00023 (17) |
Cl1 | 0.0498 (5) | 0.0593 (5) | 0.0596 (5) | 0.0104 (4) | −0.0100 (4) | 0.0019 (4) |
Cl2 | 0.0665 (6) | 0.0573 (5) | 0.0466 (4) | −0.0024 (4) | −0.0060 (4) | −0.0097 (4) |
Cl3 | 0.0636 (5) | 0.0429 (4) | 0.0661 (5) | 0.0035 (4) | −0.0032 (4) | −0.0062 (4) |
Cl4 | 0.0657 (6) | 0.0672 (6) | 0.0680 (6) | −0.0106 (4) | 0.0204 (5) | 0.0069 (4) |
N1 | 0.0505 (18) | 0.0633 (19) | 0.0556 (17) | −0.0004 (14) | −0.0072 (14) | 0.0058 (14) |
N2 | 0.0552 (19) | 0.0605 (18) | 0.0615 (18) | −0.0144 (14) | 0.0084 (15) | 0.0033 (14) |
C11 | 0.062 (3) | 0.070 (2) | 0.060 (2) | 0.001 (2) | 0.0008 (18) | −0.0036 (19) |
C21 | 0.096 (4) | 0.065 (3) | 0.099 (4) | −0.001 (2) | 0.003 (3) | 0.008 (2) |
C22 | 0.055 (3) | 0.086 (3) | 0.121 (4) | −0.007 (2) | 0.004 (3) | 0.008 (3) |
C12 | 0.052 (2) | 0.112 (4) | 0.087 (3) | 0.014 (2) | 0.001 (2) | −0.005 (3) |
Geometric parameters (Å, º) top
Co1—Cl4 | 2.2529 (9) | C11—H11A | 0.96 |
Co1—Cl3 | 2.2631 (9) | C11—H11B | 0.96 |
Co1—Cl2 | 2.2770 (9) | C11—H11C | 0.96 |
Co1—Cl1 | 2.2911 (9) | C21—H21A | 0.96 |
N1—C11 | 1.464 (4) | C21—H21B | 0.96 |
N1—C12 | 1.476 (4) | C21—H21C | 0.96 |
N1—H1A | 0.90 | C22—H22A | 0.96 |
N1—H1B | 0.90 | C22—H22B | 0.96 |
N2—C21 | 1.464 (5) | C22—H22C | 0.96 |
N2—C22 | 1.472 (5) | C12—H12A | 0.96 |
N2—H2A | 0.90 | C12—H12B | 0.96 |
N2—H2B | 0.90 | C12—H12C | 0.96 |
| | | |
Cl4—Co1—Cl3 | 109.68 (4) | N1—C11—H11C | 109.5 |
Cl4—Co1—Cl2 | 110.39 (4) | H11A—C11—H11C | 109.5 |
Cl3—Co1—Cl2 | 111.37 (3) | H11B—C11—H11C | 109.5 |
Cl4—Co1—Cl1 | 111.45 (4) | N2—C21—H21A | 109.5 |
Cl3—Co1—Cl1 | 109.34 (3) | N2—C21—H21B | 109.5 |
Cl2—Co1—Cl1 | 104.53 (3) | H21A—C21—H21B | 109.5 |
C11—N1—C12 | 113.3 (3) | N2—C21—H21C | 109.5 |
C11—N1—H1A | 108.9 | H21A—C21—H21C | 109.5 |
C12—N1—H1A | 108.9 | H21B—C21—H21C | 109.5 |
C11—N1—H1B | 108.9 | N2—C22—H22A | 109.5 |
C12—N1—H1B | 108.9 | N2—C22—H22B | 109.5 |
H1A—N1—H1B | 107.7 | H22A—C22—H22B | 109.5 |
C21—N2—C22 | 114.4 (3) | N2—C22—H22C | 109.5 |
C21—N2—H2A | 108.7 | H22A—C22—H22C | 109.5 |
C22—N2—H2A | 108.7 | H22B—C22—H22C | 109.5 |
C21—N2—H2B | 108.7 | N1—C12—H12A | 109.5 |
C22—N2—H2B | 108.7 | N1—C12—H12B | 109.5 |
H2A—N2—H2B | 107.6 | H12A—C12—H12B | 109.5 |
N1—C11—H11A | 109.5 | N1—C12—H12C | 109.5 |
N1—C11—H11B | 109.5 | H12A—C12—H12C | 109.5 |
H11A—C11—H11B | 109.5 | H12B—C12—H12C | 109.5 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1B···Cl2 | 0.90 | 2.33 | 3.203 (3) | 163 |
N1—H1A···Cl1i | 0.90 | 2.48 | 3.277 (3) | 148 |
N2—H2B···Cl1ii | 0.90 | 2.44 | 3.281 (3) | 156 |
N2—H2A···Cl4 | 0.90 | 2.36 | 3.226 (3) | 161 |
C11—H11B···Cl2iii | 0.96 | 2.76 | 3.705 (4) | 167 |
C11—H11C···Cl1iv | 0.96 | 2.81 | 3.733 (4) | 163 |
C11—H11A···Cl4v | 0.96 | 2.85 | 3.545 (4) | 130 |
C22—H22A···Cl3vi | 0.96 | 2.89 | 3.643 (5) | 136 |
Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) x−1/2, −y+3/2, z+1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) x−1/2, −y+3/2, z−1/2; (v) x+1/2, −y+3/2, z−1/2; (vi) −x+3/2, y−1/2, −z+3/2. |
(320) Dimethylammonium tetrachlorocobaltate(II)
top
Crystal data top
2(C2H8N)·CoCl4 | F(000) = 596 |
Mr = 292.92 | Dx = 1.490 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 2719 reflections |
a = 8.5513 (5) Å | θ = 1–25° |
b = 11.4527 (7) Å | µ = 2.09 mm−1 |
c = 13.3364 (8) Å | T = 320 K |
β = 90.010 (1)° | Plate, dark-blue |
V = 1306.11 (14) Å3 | 0.50 × 0.35 × 0.06 mm |
Z = 4 | |
Data collection top
Siemens SMART CCD diffractometer | 2397 independent reflections |
Radiation source: fine-focus sealed tube | 1688 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.036 |
Detector resolution: no pixels mm-1 | θmax = 25.4°, θmin = 2.3° |
ω scans | h = −9→10 |
Absorption correction: multi-scan (blessing, 1995; Sheldrick, 1996) Blessing, Acta Cryst. (1995), A51, 33-38. | k = −13→13 |
Tmin = 0.422, Tmax = 0.885 | l = −16→10 |
6082 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.034 | See experimental |
wR(F2) = 0.084 | w = 1/[σ2(Fo2) + (0.0398P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.99 | (Δ/σ)max = 0.001 |
2397 reflections | Δρmax = 0.28 e Å−3 |
121 parameters | Δρmin = −0.34 e Å−3 |
0 restraints | Extinction correction: SHELXTL (Bruker AXS, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0072 (8) |
Crystal data top
2(C2H8N)·CoCl4 | V = 1306.11 (14) Å3 |
Mr = 292.92 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 8.5513 (5) Å | µ = 2.09 mm−1 |
b = 11.4527 (7) Å | T = 320 K |
c = 13.3364 (8) Å | 0.50 × 0.35 × 0.06 mm |
β = 90.010 (1)° | |
Data collection top
Siemens SMART CCD diffractometer | 2397 independent reflections |
Absorption correction: multi-scan (blessing, 1995; Sheldrick, 1996) Blessing, Acta Cryst. (1995), A51, 33-38. | 1688 reflections with I > 2σ(I) |
Tmin = 0.422, Tmax = 0.885 | Rint = 0.036 |
6082 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.034 | 0 restraints |
wR(F2) = 0.084 | See experimental |
S = 0.99 | Δρmax = 0.28 e Å−3 |
2397 reflections | Δρmin = −0.34 e Å−3 |
121 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 | |
Co1 | 0.83017 (5) | 0.79888 (3) | 0.58100 (3) | 0.04526 (17) | |
Cl1 | 1.07291 (11) | 0.73707 (8) | 0.63069 (7) | 0.0617 (3) | |
Cl2 | 0.80759 (11) | 0.73592 (8) | 0.41975 (7) | 0.0622 (3) | |
Cl3 | 0.81906 (11) | 0.99600 (7) | 0.59014 (7) | 0.0633 (3) | |
Cl4 | 0.64042 (13) | 0.72056 (8) | 0.67701 (8) | 0.0738 (3) | |
N1 | 0.7898 (3) | 0.9979 (3) | 0.3350 (2) | 0.0618 (8) | |
H1A | 0.8114 | 0.9308 | 0.3673 | 0.14 (2)* | |
H1B | 0.8418 | 1.0557 | 0.3663 | 0.113 (17)* | |
N2 | 0.7067 (4) | 0.8094 (3) | 0.9032 (3) | 0.0661 (8) | |
H2A | 0.6728 | 0.7726 | 0.8476 | 0.094 (16)* | |
H2B | 0.6514 | 0.7817 | 0.9554 | 0.112 (17)* | |
C11 | 0.8463 (5) | 0.9891 (4) | 0.2317 (3) | 0.0696 (10) | |
H11A | 0.9578 | 0.9792 | 0.2320 | 0.108 (16)* | |
H11B | 0.8200 | 1.0591 | 0.1959 | 0.101 (15)* | |
H11C | 0.7983 | 0.9233 | 0.1996 | 0.118 (17)* | |
C21 | 0.6746 (6) | 0.9345 (4) | 0.8928 (4) | 0.0971 (15) | |
H21A | 0.7092 | 0.9747 | 0.9519 | 0.14 (2)* | |
H21B | 0.5643 | 0.9464 | 0.8841 | 0.14 (2)* | |
H21C | 0.7294 | 0.9645 | 0.8354 | 0.124 (19)* | |
C22 | 0.8724 (5) | 0.7806 (5) | 0.9185 (5) | 0.0962 (16) | |
H22A | 0.8835 | 0.6977 | 0.9263 | 0.17 (3)* | |
H22B | 0.9099 | 0.8192 | 0.9777 | 0.15 (3)* | |
H22C | 0.9319 | 0.8060 | 0.8616 | 0.14 (2)* | |
C12 | 0.6215 (5) | 1.0208 (5) | 0.3418 (4) | 0.0900 (13) | |
H12A | 0.5904 | 1.0219 | 0.4109 | 0.103 (16)* | |
H12B | 0.5652 | 0.9606 | 0.3071 | 0.17 (3)* | |
H12C | 0.5985 | 1.0951 | 0.3117 | 0.13 (2)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0445 (3) | 0.0460 (3) | 0.0453 (3) | 0.0004 (2) | 0.00140 (19) | 0.00013 (19) |
Cl1 | 0.0537 (5) | 0.0640 (5) | 0.0675 (6) | 0.0115 (4) | −0.0114 (4) | 0.0015 (4) |
Cl2 | 0.0724 (6) | 0.0621 (5) | 0.0520 (5) | −0.0018 (4) | −0.0079 (4) | −0.0106 (4) |
Cl3 | 0.0698 (6) | 0.0469 (5) | 0.0732 (6) | 0.0039 (4) | −0.0042 (5) | −0.0067 (4) |
Cl4 | 0.0718 (7) | 0.0734 (6) | 0.0761 (7) | −0.0123 (5) | 0.0236 (5) | 0.0064 (5) |
N1 | 0.0526 (19) | 0.067 (2) | 0.066 (2) | −0.0017 (16) | −0.0090 (16) | 0.0053 (17) |
N2 | 0.062 (2) | 0.066 (2) | 0.070 (2) | −0.0159 (16) | 0.0087 (17) | 0.0029 (17) |
C11 | 0.070 (3) | 0.074 (3) | 0.065 (3) | −0.001 (2) | −0.001 (2) | −0.006 (2) |
C21 | 0.104 (4) | 0.076 (3) | 0.111 (4) | 0.002 (3) | 0.007 (3) | 0.015 (3) |
C22 | 0.059 (3) | 0.100 (4) | 0.129 (5) | −0.007 (3) | 0.003 (3) | 0.015 (3) |
C12 | 0.058 (3) | 0.119 (4) | 0.093 (4) | 0.018 (3) | 0.001 (2) | 0.001 (3) |
Geometric parameters (Å, º) top
Co1—Cl4 | 2.2533 (10) | C11—H11A | 0.96 |
Co1—Cl3 | 2.2628 (9) | C11—H11B | 0.96 |
Co1—Cl2 | 2.2763 (10) | C11—H11C | 0.96 |
Co1—Cl1 | 2.2910 (10) | C21—H21A | 0.96 |
N1—C12 | 1.466 (5) | C21—H21B | 0.96 |
N1—C11 | 1.463 (4) | C21—H21C | 0.96 |
N1—H1A | 0.90 | C22—H22A | 0.96 |
N1—H1B | 0.90 | C22—H22B | 0.96 |
N2—C21 | 1.465 (5) | C22—H22C | 0.96 |
N2—C22 | 1.469 (5) | C12—H12A | 0.96 |
N2—H2A | 0.90 | C12—H12B | 0.96 |
N2—H2B | 0.90 | C12—H12C | 0.96 |
| | | |
Cl4—Co1—Cl3 | 109.65 (4) | N1—C11—H11C | 109.5 |
Cl4—Co1—Cl2 | 110.48 (4) | H11A—C11—H11C | 109.5 |
Cl3—Co1—Cl2 | 111.30 (4) | H11B—C11—H11C | 109.5 |
Cl4—Co1—Cl1 | 111.42 (4) | N2—C21—H21A | 109.5 |
Cl3—Co1—Cl1 | 109.31 (4) | N2—C21—H21B | 109.5 |
Cl2—Co1—Cl1 | 104.60 (4) | H21A—C21—H21B | 109.5 |
C12—N1—C11 | 113.3 (3) | N2—C21—H21C | 109.5 |
C12—N1—H1A | 108.9 | H21A—C21—H21C | 109.5 |
C11—N1—H1A | 108.9 | H21B—C21—H21C | 109.5 |
C12—N1—H1B | 108.9 | N2—C22—H22A | 109.5 |
C11—N1—H1B | 108.9 | N2—C22—H22B | 109.5 |
H1A—N1—H1B | 107.7 | H22A—C22—H22B | 109.5 |
C21—N2—C22 | 114.4 (4) | N2—C22—H22C | 109.5 |
C21—N2—H2A | 108.6 | H22A—C22—H22C | 109.5 |
C22—N2—H2A | 108.6 | H22B—C22—H22C | 109.5 |
C21—N2—H2B | 108.6 | N1—C12—H12A | 109.5 |
C22—N2—H2B | 108.6 | N1—C12—H12B | 109.5 |
H2A—N2—H2B | 107.6 | H12A—C12—H12B | 109.5 |
N1—C11—H11A | 109.5 | N1—C12—H12C | 109.5 |
N1—C11—H11B | 109.5 | H12A—C12—H12C | 109.5 |
H11A—C11—H11B | 109.5 | H12B—C12—H12C | 109.5 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···Cl2 | 0.90 | 2.34 | 3.210 (3) | 163 |
N1—H1B···Cl1i | 0.90 | 2.48 | 3.286 (3) | 149 |
N2—H2B···Cl1ii | 0.90 | 2.44 | 3.287 (3) | 156 |
N2—H2A···Cl4 | 0.90 | 2.37 | 3.233 (4) | 161 |
C11—H11B···Cl2iii | 0.96 | 2.77 | 3.715 (4) | 169 |
C11—H11C···Cl1iv | 0.96 | 2.82 | 3.741 (4) | 162 |
C11—H11A···Cl4v | 0.96 | 2.87 | 3.553 (4) | 129 |
C22—H22A···Cl3vi | 0.96 | 2.90 | 3.649 (5) | 136 |
Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) x−1/2, −y+3/2, z+1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) x−1/2, −y+3/2, z−1/2; (v) x+1/2, −y+3/2, z−1/2; (vi) −x+3/2, y−1/2, −z+3/2. |
(343) Dimethylammonium tetrachlorocobaltate(II)
top
Crystal data top
2(C2H8N)·CoCl4 | F(000) = 596 |
Mr = 292.92 | Dx = 1.484 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 2563 reflections |
a = 8.5640 (2) Å | θ = 1–25° |
b = 11.4573 (3) Å | µ = 2.08 mm−1 |
c = 13.3590 (3) Å | T = 343 K |
β = 90.037 (1)° | Plate, dark-blue |
V = 1310.79 (5) Å3 | 0.50 × 0.35 × 0.06 mm |
Z = 4 | |
Data collection top
Siemens SMART CCD diffractometer | 2399 independent reflections |
Radiation source: fine-focus sealed tube | 1639 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
Detector resolution: no pixels mm-1 | θmax = 25.3°, θmin = 2.3° |
ω scans | h = −10→9 |
Absorption correction: multi-scan (blessing, 1995; Sheldrick, 1996) Blessing, Acta Cryst. (1995), A51, 33-38. | k = −13→13 |
Tmin = 0.423, Tmax = 0.885 | l = −10→16 |
6097 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.036 | See experimental |
wR(F2) = 0.085 | w = 1/[σ2(Fo2) + (0.0365P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.001 |
2399 reflections | Δρmax = 0.31 e Å−3 |
121 parameters | Δρmin = −0.33 e Å−3 |
0 restraints | Extinction correction: SHELXTL (Bruker AXS, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0119 (9) |
Crystal data top
2(C2H8N)·CoCl4 | V = 1310.79 (5) Å3 |
Mr = 292.92 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 8.5640 (2) Å | µ = 2.08 mm−1 |
b = 11.4573 (3) Å | T = 343 K |
c = 13.3590 (3) Å | 0.50 × 0.35 × 0.06 mm |
β = 90.037 (1)° | |
Data collection top
Siemens SMART CCD diffractometer | 2399 independent reflections |
Absorption correction: multi-scan (blessing, 1995; Sheldrick, 1996) Blessing, Acta Cryst. (1995), A51, 33-38. | 1639 reflections with I > 2σ(I) |
Tmin = 0.423, Tmax = 0.885 | Rint = 0.039 |
6097 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.036 | 0 restraints |
wR(F2) = 0.085 | See experimental |
S = 1.00 | Δρmax = 0.31 e Å−3 |
2399 reflections | Δρmin = −0.33 e Å−3 |
121 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 | |
Co1 | 0.83009 (5) | 0.79838 (4) | 0.58077 (3) | 0.04963 (18) | |
Cl1 | 1.07231 (12) | 0.73664 (8) | 0.63023 (8) | 0.0682 (3) | |
Cl2 | 0.80728 (12) | 0.73594 (8) | 0.41986 (7) | 0.0684 (3) | |
Cl3 | 0.81917 (11) | 0.99526 (8) | 0.59017 (8) | 0.0695 (3) | |
Cl4 | 0.64056 (13) | 0.72035 (9) | 0.67655 (8) | 0.0815 (3) | |
N1 | 0.7899 (3) | 0.9989 (3) | 0.3355 (2) | 0.0675 (8) | |
H1A | 0.8118 | 0.9323 | 0.3683 | 0.128 (19)* | |
H1B | 0.8417 | 1.0573 | 0.3661 | 0.19 (3)* | |
N2 | 0.7066 (4) | 0.8092 (3) | 0.9022 (3) | 0.0718 (9) | |
H2A | 0.6740 | 0.7727 | 0.8463 | 0.13 (2)* | |
H2B | 0.6504 | 0.7812 | 0.9538 | 0.116 (18)* | |
C11 | 0.8459 (5) | 0.9889 (4) | 0.2317 (3) | 0.0781 (11) | |
H11A | 0.9572 | 0.9795 | 0.2317 | 0.113 (17)* | |
H11B | 0.8187 | 1.0583 | 0.1953 | 0.13 (2)* | |
H11C | 0.7981 | 0.9224 | 0.2004 | 0.16 (2)* | |
C21 | 0.6749 (7) | 0.9344 (4) | 0.8920 (5) | 0.1046 (16) | |
H21A | 0.5649 | 0.9463 | 0.8826 | 0.13 (2)* | |
H21B | 0.7306 | 0.9646 | 0.8353 | 0.18 (3)* | |
H21C | 0.7083 | 0.9742 | 0.9515 | 0.15 (2)* | |
C22 | 0.8717 (6) | 0.7807 (5) | 0.9188 (5) | 0.1062 (17) | |
H22A | 0.8822 | 0.6984 | 0.9303 | 0.19 (3)* | |
H22B | 0.9095 | 0.8227 | 0.9761 | 0.18 (3)* | |
H22C | 0.9313 | 0.8024 | 0.8609 | 0.16 (3)* | |
C12 | 0.6214 (5) | 1.0216 (6) | 0.3421 (4) | 0.1019 (15) | |
H12A | 0.5903 | 1.0223 | 0.4111 | 0.115 (18)* | |
H12B | 0.5655 | 0.9614 | 0.3073 | 0.17 (3)* | |
H12C | 0.5984 | 1.0959 | 0.3123 | 0.15 (2)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0490 (3) | 0.0506 (3) | 0.0493 (3) | 0.0003 (2) | 0.0011 (2) | 0.0003 (2) |
Cl1 | 0.0597 (6) | 0.0704 (6) | 0.0746 (6) | 0.0123 (5) | −0.0128 (5) | 0.0015 (5) |
Cl2 | 0.0804 (7) | 0.0684 (6) | 0.0565 (6) | −0.0017 (5) | −0.0083 (5) | −0.0111 (4) |
Cl3 | 0.0778 (7) | 0.0508 (5) | 0.0799 (7) | 0.0040 (5) | −0.0037 (5) | −0.0075 (4) |
Cl4 | 0.0795 (7) | 0.0813 (7) | 0.0836 (7) | −0.0128 (5) | 0.0264 (6) | 0.0085 (5) |
N1 | 0.061 (2) | 0.071 (2) | 0.071 (2) | −0.0011 (17) | −0.0101 (17) | 0.0094 (18) |
N2 | 0.065 (2) | 0.073 (2) | 0.077 (2) | −0.0156 (18) | 0.0092 (19) | 0.0055 (19) |
C11 | 0.075 (3) | 0.089 (3) | 0.071 (3) | −0.002 (3) | 0.003 (2) | −0.009 (2) |
C21 | 0.115 (5) | 0.079 (3) | 0.120 (5) | −0.001 (3) | 0.001 (4) | 0.010 (3) |
C22 | 0.066 (3) | 0.111 (4) | 0.142 (5) | −0.007 (3) | 0.004 (4) | 0.014 (4) |
C12 | 0.060 (3) | 0.140 (5) | 0.105 (4) | 0.022 (3) | 0.002 (3) | −0.001 (4) |
Geometric parameters (Å, º) top
Co1—Cl4 | 2.2525 (10) | C11—H11A | 0.96 |
Co1—Cl3 | 2.2611 (10) | C11—H11B | 0.96 |
Co1—Cl2 | 2.2738 (10) | C11—H11C | 0.96 |
Co1—Cl1 | 2.2887 (10) | C21—H21A | 0.96 |
N1—C12 | 1.469 (5) | C21—H21B | 0.96 |
N1—C11 | 1.471 (5) | C21—H21C | 0.96 |
N1—H1A | 0.90 | C22—H22A | 0.96 |
N1—H1B | 0.90 | C22—H22B | 0.96 |
N2—C21 | 1.466 (5) | C22—H22C | 0.96 |
N2—C22 | 1.467 (6) | C12—H12A | 0.96 |
N2—H2A | 0.90 | C12—H12B | 0.96 |
N2—H2B | 0.90 | C12—H12C | 0.96 |
| | | |
Cl4—Co1—Cl3 | 109.54 (4) | N1—C11—H11C | 109.5 |
Cl4—Co1—Cl2 | 110.53 (4) | H11A—C11—H11C | 109.5 |
Cl3—Co1—Cl2 | 111.28 (4) | H11B—C11—H11C | 109.5 |
Cl4—Co1—Cl1 | 111.51 (4) | N2—C21—H21A | 109.5 |
Cl3—Co1—Cl1 | 109.26 (4) | N2—C21—H21B | 109.5 |
Cl2—Co1—Cl1 | 104.65 (4) | H21A—C21—H21B | 109.5 |
C12—N1—C11 | 113.1 (4) | N2—C21—H21C | 109.5 |
C12—N1—H1A | 109.0 | H21A—C21—H21C | 109.5 |
C11—N1—H1A | 109.0 | H21B—C21—H21C | 109.5 |
C12—N1—H1B | 109.0 | N2—C22—H22A | 109.5 |
C11—N1—H1B | 109.0 | N2—C22—H22B | 109.5 |
H1A—N1—H1B | 107.8 | H22A—C22—H22B | 109.5 |
C21—N2—C22 | 114.2 (4) | N2—C22—H22C | 109.5 |
C21—N2—H2A | 108.7 | H22A—C22—H22C | 109.5 |
C22—N2—H2A | 108.7 | H22B—C22—H22C | 109.5 |
C21—N2—H2B | 108.7 | N1—C12—H12A | 109.5 |
C22—N2—H2B | 108.7 | N1—C12—H12B | 109.5 |
H2A—N2—H2B | 107.6 | H12A—C12—H12B | 109.5 |
N1—C11—H11A | 109.5 | N1—C12—H12C | 109.5 |
N1—C11—H11B | 109.5 | H12A—C12—H12C | 109.5 |
H11A—C11—H11B | 109.5 | H12B—C12—H12C | 109.5 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···Cl2 | 0.90 | 2.35 | 3.221 (3) | 162 |
N1—H1B···Cl1i | 0.90 | 2.47 | 3.283 (4) | 150 |
N2—H2B···Cl1ii | 0.90 | 2.46 | 3.299 (4) | 155 |
N2—H2A···Cl4 | 0.90 | 2.36 | 3.231 (4) | 162 |
C11—H11B···Cl2iii | 0.96 | 2.77 | 3.718 (5) | 170 |
C11—H11C···Cl1iv | 0.96 | 2.82 | 3.742 (5) | 162 |
C11—H11A···Cl4v | 0.96 | 2.87 | 3.559 (5) | 129 |
C22—H22A···Cl3vi | 0.96 | 2.91 | 3.658 (6) | 136 |
Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) x−1/2, −y+3/2, z+1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) x−1/2, −y+3/2, z−1/2; (v) x+1/2, −y+3/2, z−1/2; (vi) −x+3/2, y−1/2, −z+3/2. |
(366) Dimethylammonium Tetrachlorocobaltate(II)
top
Crystal data top
2(C2H8N)·CoCl4 | F(000) = 596 |
Mr = 292.92 | Dx = 1.478 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 2910 reflections |
a = 8.5775 (5) Å | θ = 1–25° |
b = 11.4679 (6) Å | µ = 2.07 mm−1 |
c = 13.3855 (6) Å | T = 366 K |
β = 90.021 (1)° | Plate, dark-blue |
V = 1316.68 (12) Å3 | 0.50 × 0.35 × 0.06 mm |
Z = 4 | |
Data collection top
Siemens SMART CCD diffractometer | 2412 independent reflections |
Radiation source: fine-focus sealed tube | 1666 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.038 |
Detector resolution: no pixels mm-1 | θmax = 25.4°, θmin = 2.3° |
ω scans | h = −9→10 |
Absorption correction: multi-scan (blessing, 1995; Sheldrick, 1996) Blessing, Acta Cryst. (1995), A51, 33-38. | k = −13→13 |
Tmin = 0.424, Tmax = 0.886 | l = −16→15 |
7139 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.037 | See experimental |
wR(F2) = 0.092 | w = 1/[σ2(Fo2) + (0.0457P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max = 0.001 |
2412 reflections | Δρmax = 0.33 e Å−3 |
121 parameters | Δρmin = −0.31 e Å−3 |
0 restraints | Extinction correction: SHELXTL (Bruker AXS, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0153 (11) |
Crystal data top
2(C2H8N)·CoCl4 | V = 1316.68 (12) Å3 |
Mr = 292.92 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 8.5775 (5) Å | µ = 2.07 mm−1 |
b = 11.4679 (6) Å | T = 366 K |
c = 13.3855 (6) Å | 0.50 × 0.35 × 0.06 mm |
β = 90.021 (1)° | |
Data collection top
Siemens SMART CCD diffractometer | 2412 independent reflections |
Absorption correction: multi-scan (blessing, 1995; Sheldrick, 1996) Blessing, Acta Cryst. (1995), A51, 33-38. | 1666 reflections with I > 2σ(I) |
Tmin = 0.424, Tmax = 0.886 | Rint = 0.038 |
7139 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.037 | 0 restraints |
wR(F2) = 0.092 | See experimental |
S = 1.01 | Δρmax = 0.33 e Å−3 |
2412 reflections | Δρmin = −0.31 e Å−3 |
121 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 | |
Co1 | 0.82990 (5) | 0.79809 (4) | 0.58059 (3) | 0.0542 (2) | |
Cl1 | 1.07183 (12) | 0.73627 (9) | 0.62985 (8) | 0.0747 (3) | |
Cl2 | 0.80737 (13) | 0.73574 (9) | 0.41987 (7) | 0.0753 (3) | |
Cl3 | 0.81945 (11) | 0.99470 (8) | 0.59026 (8) | 0.0763 (3) | |
Cl4 | 0.64044 (14) | 0.72026 (9) | 0.67605 (9) | 0.0891 (4) | |
N1 | 0.7898 (4) | 0.9986 (3) | 0.3355 (2) | 0.0742 (9) | |
H1A | 0.8426 | 1.0561 | 0.3664 | 0.15 (2)* | |
H1B | 0.8101 | 0.9317 | 0.3682 | 0.21 (3)* | |
N2 | 0.7066 (4) | 0.8099 (3) | 0.9019 (3) | 0.0810 (10) | |
H2A | 0.6741 | 0.7738 | 0.8459 | 0.15 (3)* | |
H2B | 0.6502 | 0.7815 | 0.9531 | 0.14 (2)* | |
C11 | 0.8459 (5) | 0.9883 (4) | 0.2327 (3) | 0.0839 (12) | |
H11A | 0.9573 | 0.9800 | 0.2329 | 0.16 (2)* | |
H11B | 0.8177 | 1.0570 | 0.1959 | 0.130 (19)* | |
H11C | 0.7995 | 0.9212 | 0.2018 | 0.19 (3)* | |
C21 | 0.6742 (7) | 0.9339 (5) | 0.8924 (5) | 0.1145 (17) | |
H21A | 0.5642 | 0.9454 | 0.8836 | 0.14 (2)* | |
H21B | 0.7290 | 0.9645 | 0.8356 | 0.17 (3)* | |
H21C | 0.7081 | 0.9735 | 0.9517 | 0.19 (3)* | |
C22 | 0.8708 (6) | 0.7803 (5) | 0.9185 (6) | 0.1146 (19) | |
H22A | 0.8804 | 0.6978 | 0.9291 | 0.21 (3)* | |
H22B | 0.9086 | 0.8211 | 0.9762 | 0.17 (3)* | |
H22C | 0.9309 | 0.8025 | 0.8611 | 0.13 (2)* | |
C12 | 0.6220 (5) | 1.0232 (6) | 0.3421 (5) | 0.1111 (17) | |
H12A | 0.6005 | 1.0975 | 0.3122 | 0.24 (4)* | |
H12B | 0.5909 | 1.0246 | 0.4110 | 0.13 (2)* | |
H12C | 0.5650 | 0.9636 | 0.3075 | 0.16 (2)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0525 (3) | 0.0545 (3) | 0.0554 (3) | 0.0004 (2) | 0.0035 (2) | 0.0004 (2) |
Cl1 | 0.0645 (6) | 0.0769 (6) | 0.0829 (6) | 0.0135 (5) | −0.0119 (5) | 0.0017 (5) |
Cl2 | 0.0886 (7) | 0.0738 (6) | 0.0636 (6) | −0.0014 (5) | −0.0082 (5) | −0.0120 (5) |
Cl3 | 0.0839 (7) | 0.0546 (5) | 0.0905 (7) | 0.0045 (5) | −0.0021 (5) | −0.0087 (5) |
Cl4 | 0.0862 (8) | 0.0879 (8) | 0.0931 (8) | −0.0149 (6) | 0.0297 (6) | 0.0088 (6) |
N1 | 0.064 (2) | 0.086 (2) | 0.073 (2) | −0.0030 (18) | −0.0093 (17) | 0.0066 (18) |
N2 | 0.076 (2) | 0.081 (2) | 0.087 (2) | −0.0153 (19) | 0.013 (2) | 0.004 (2) |
C11 | 0.082 (3) | 0.088 (3) | 0.081 (3) | −0.001 (3) | 0.002 (2) | 0.000 (2) |
C21 | 0.121 (5) | 0.083 (4) | 0.140 (5) | 0.004 (3) | 0.006 (4) | 0.014 (4) |
C22 | 0.073 (3) | 0.113 (5) | 0.158 (6) | −0.006 (3) | 0.010 (4) | 0.019 (4) |
C12 | 0.064 (3) | 0.154 (5) | 0.115 (4) | 0.017 (3) | 0.005 (3) | −0.005 (4) |
Geometric parameters (Å, º) top
Co1—Cl4 | 2.2520 (11) | C11—H11A | 0.96 |
Co1—Cl3 | 2.2602 (10) | C11—H11B | 0.96 |
Co1—Cl2 | 2.2752 (10) | C11—H11C | 0.96 |
Co1—Cl1 | 2.2897 (10) | C21—H21A | 0.96 |
N1—C11 | 1.463 (5) | C21—H21B | 0.96 |
N1—C12 | 1.469 (5) | C21—H21C | 0.96 |
N1—H1A | 0.90 | C22—H22A | 0.96 |
N1—H1B | 0.90 | C22—H22B | 0.96 |
N2—C21 | 1.455 (6) | C22—H22C | 0.96 |
N2—C22 | 1.466 (6) | C12—H12A | 0.96 |
N2—H2A | 0.90 | C12—H12B | 0.96 |
N2—H2B | 0.90 | C12—H12C | 0.96 |
| | | |
Cl4—Co1—Cl3 | 109.52 (4) | N1—C11—H11C | 109.5 |
Cl4—Co1—Cl2 | 110.54 (5) | H11A—C11—H11C | 109.5 |
Cl3—Co1—Cl2 | 111.36 (4) | H11B—C11—H11C | 109.5 |
Cl4—Co1—Cl1 | 111.59 (5) | N2—C21—H21A | 109.5 |
Cl3—Co1—Cl1 | 109.17 (4) | N2—C21—H21B | 109.5 |
Cl2—Co1—Cl1 | 104.57 (4) | H21A—C21—H21B | 109.5 |
C11—N1—C12 | 113.2 (4) | N2—C21—H21C | 109.5 |
C11—N1—H1A | 108.9 | H21A—C21—H21C | 109.5 |
C12—N1—H1A | 108.9 | H21B—C21—H21C | 109.5 |
C11—N1—H1B | 108.9 | N2—C22—H22A | 109.5 |
C12—N1—H1B | 108.9 | N2—C22—H22B | 109.5 |
H1A—N1—H1B | 107.7 | H22A—C22—H22B | 109.5 |
C21—N2—C22 | 115.0 (4) | N2—C22—H22C | 109.5 |
C21—N2—H2A | 108.5 | H22A—C22—H22C | 109.5 |
C22—N2—H2A | 108.5 | H22B—C22—H22C | 109.5 |
C21—N2—H2B | 108.5 | N1—C12—H12A | 109.5 |
C22—N2—H2B | 108.5 | N1—C12—H12B | 109.5 |
H2A—N2—H2B | 107.5 | H12A—C12—H12B | 109.5 |
N1—C11—H11A | 109.5 | N1—C12—H12C | 109.5 |
N1—C11—H11B | 109.5 | H12A—C12—H12C | 109.5 |
H11A—C11—H11B | 109.5 | H12B—C12—H12C | 109.5 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1B···Cl2 | 0.90 | 2.35 | 3.222 (4) | 163 |
N1—H1A···Cl1i | 0.90 | 2.49 | 3.297 (4) | 149 |
N2—H2B···Cl1ii | 0.90 | 2.47 | 3.306 (4) | 155 |
N2—H2A···Cl4 | 0.90 | 2.37 | 3.243 (4) | 163 |
C11—H11B···Cl2iii | 0.96 | 2.78 | 3.735 (5) | 171 |
C11—H11C···Cl1iv | 0.96 | 2.83 | 3.749 (5) | 161 |
C11—H11A···Cl4v | 0.96 | 2.88 | 3.561 (5) | 128 |
C22—H22A···Cl3vi | 0.96 | 2.90 | 3.661 (6) | 137 |
Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) x−1/2, −y+3/2, z+1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) x−1/2, −y+3/2, z−1/2; (v) x+1/2, −y+3/2, z−1/2; (vi) −x+3/2, y−1/2, −z+3/2. |
Experimental details
| (297) | (320) | (343) | (366) |
Crystal data |
Chemical formula | 2(C2H8N)·CoCl4 | 2(C2H8N)·CoCl4 | 2(C2H8N)·CoCl4 | 2(C2H8N)·CoCl4 |
Mr | 292.92 | 292.92 | 292.92 | 292.92 |
Crystal system, space group | Monoclinic, P21/n | Monoclinic, P21/n | Monoclinic, P21/n | Monoclinic, P21/n |
Temperature (K) | 297 | 320 | 343 | 366 |
a, b, c (Å) | 8.5313 (2), 11.4382 (2), 13.3070 (1) | 8.5513 (5), 11.4527 (7), 13.3364 (8) | 8.5640 (2), 11.4573 (3), 13.3590 (3) | 8.5775 (5), 11.4679 (6), 13.3855 (6) |
β (°) | 90.038 (1) | 90.010 (1) | 90.037 (1) | 90.021 (1) |
V (Å3) | 1298.53 (4) | 1306.11 (14) | 1310.79 (5) | 1316.68 (12) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 2.10 | 2.09 | 2.08 | 2.07 |
Crystal size (mm) | 0.50 × 0.35 × 0.06 | 0.50 × 0.35 × 0.06 | 0.50 × 0.35 × 0.06 | 0.50 × 0.35 × 0.06 |
|
Data collection |
Diffractometer | Siemens SMART CCD diffractometer | Siemens SMART CCD diffractometer | Siemens SMART CCD diffractometer | Siemens SMART CCD diffractometer |
Absorption correction | Multi-scan (Blessing, 1995; Sheldrick, 1996) Blessing, Acta Cryst. (1995), A51, 33-38. | Multi-scan (Blessing, 1995; Sheldrick, 1996) Blessing, Acta Cryst. (1995), A51, 33-38. | Multi-scan (Blessing, 1995; Sheldrick, 1996) Blessing, Acta Cryst. (1995), A51, 33-38. | Multi-scan (Blessing, 1995; Sheldrick, 1996) Blessing, Acta Cryst. (1995), A51, 33-38. |
Tmin, Tmax | 0.420, 0.884 | 0.422, 0.885 | 0.423, 0.885 | 0.424, 0.886 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 6987, 2372, 1794 | 6082, 2397, 1688 | 6097, 2399, 1639 | 7139, 2412, 1666 |
Rint | 0.036 | 0.036 | 0.039 | 0.038 |
(sin θ/λ)max (Å−1) | 0.603 | 0.603 | 0.602 | 0.602 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.082, 1.00 | 0.034, 0.084, 0.99 | 0.036, 0.085, 1.00 | 0.037, 0.092, 1.01 |
No. of reflections | 2372 | 2397 | 2399 | 2412 |
No. of parameters | 121 | 121 | 121 | 121 |
H-atom treatment | See experimental | See experimental | See experimental | See experimental |
Δρmax, Δρmin (e Å−3) | 0.30, −0.56 | 0.28, −0.34 | 0.31, −0.33 | 0.33, −0.31 |
Selected geometric parameters (Å, º) for (297) topCo1—Cl4 | 2.2529 (9) | N1—C11 | 1.464 (4) |
Co1—Cl3 | 2.2631 (9) | N1—C12 | 1.476 (4) |
Co1—Cl2 | 2.2770 (9) | N2—C21 | 1.464 (5) |
Co1—Cl1 | 2.2911 (9) | N2—C22 | 1.472 (5) |
| | | |
Cl4—Co1—Cl3 | 109.68 (4) | Cl3—Co1—Cl1 | 109.34 (3) |
Cl4—Co1—Cl2 | 110.39 (4) | Cl2—Co1—Cl1 | 104.53 (3) |
Cl3—Co1—Cl2 | 111.37 (3) | C11—N1—C12 | 113.3 (3) |
Cl4—Co1—Cl1 | 111.45 (4) | C21—N2—C22 | 114.4 (3) |
Hydrogen-bond geometry (Å, º) for (297) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1B···Cl2 | 0.90 | 2.33 | 3.203 (3) | 163.1 |
N1—H1A···Cl1i | 0.90 | 2.48 | 3.277 (3) | 148.1 |
N2—H2B···Cl1ii | 0.90 | 2.44 | 3.281 (3) | 156.4 |
N2—H2A···Cl4 | 0.90 | 2.36 | 3.226 (3) | 161.2 |
C11—H11B···Cl2iii | 0.96 | 2.76 | 3.705 (4) | 167.4 |
C11—H11C···Cl1iv | 0.96 | 2.81 | 3.733 (4) | 162.6 |
C11—H11A···Cl4v | 0.96 | 2.85 | 3.545 (4) | 130.0 |
C22—H22A···Cl3vi | 0.96 | 2.89 | 3.643 (5) | 136.1 |
Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) x−1/2, −y+3/2, z+1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) x−1/2, −y+3/2, z−1/2; (v) x+1/2, −y+3/2, z−1/2; (vi) −x+3/2, y−1/2, −z+3/2. |
Selected geometric parameters (Å, º) for (320) topCo1—Cl4 | 2.2533 (10) | N1—C12 | 1.466 (5) |
Co1—Cl3 | 2.2628 (9) | N1—C11 | 1.463 (4) |
Co1—Cl2 | 2.2763 (10) | N2—C21 | 1.465 (5) |
Co1—Cl1 | 2.2910 (10) | N2—C22 | 1.469 (5) |
| | | |
Cl4—Co1—Cl3 | 109.65 (4) | Cl3—Co1—Cl1 | 109.31 (4) |
Cl4—Co1—Cl2 | 110.48 (4) | Cl2—Co1—Cl1 | 104.60 (4) |
Cl3—Co1—Cl2 | 111.30 (4) | C12—N1—C11 | 113.3 (3) |
Cl4—Co1—Cl1 | 111.42 (4) | C21—N2—C22 | 114.4 (4) |
Hydrogen-bond geometry (Å, º) for (320) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···Cl2 | 0.90 | 2.34 | 3.210 (3) | 162.7 |
N1—H1B···Cl1i | 0.90 | 2.48 | 3.286 (3) | 148.8 |
N2—H2B···Cl1ii | 0.90 | 2.44 | 3.287 (3) | 156.4 |
N2—H2A···Cl4 | 0.90 | 2.37 | 3.233 (4) | 161.1 |
C11—H11B···Cl2iii | 0.96 | 2.77 | 3.715 (4) | 168.6 |
C11—H11C···Cl1iv | 0.96 | 2.82 | 3.741 (4) | 162.0 |
C11—H11A···Cl4v | 0.96 | 2.87 | 3.553 (4) | 129.4 |
C22—H22A···Cl3vi | 0.96 | 2.90 | 3.649 (5) | 136.2 |
Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) x−1/2, −y+3/2, z+1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) x−1/2, −y+3/2, z−1/2; (v) x+1/2, −y+3/2, z−1/2; (vi) −x+3/2, y−1/2, −z+3/2. |
Selected geometric parameters (Å, º) for (343) topCo1—Cl4 | 2.2525 (10) | N1—C12 | 1.469 (5) |
Co1—Cl3 | 2.2611 (10) | N1—C11 | 1.471 (5) |
Co1—Cl2 | 2.2738 (10) | N2—C21 | 1.466 (5) |
Co1—Cl1 | 2.2887 (10) | N2—C22 | 1.467 (6) |
| | | |
Cl4—Co1—Cl3 | 109.54 (4) | Cl3—Co1—Cl1 | 109.26 (4) |
Cl4—Co1—Cl2 | 110.53 (4) | Cl2—Co1—Cl1 | 104.65 (4) |
Cl3—Co1—Cl2 | 111.28 (4) | C12—N1—C11 | 113.1 (4) |
Cl4—Co1—Cl1 | 111.51 (4) | C21—N2—C22 | 114.2 (4) |
Hydrogen-bond geometry (Å, º) for (343) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···Cl2 | 0.90 | 2.35 | 3.221 (3) | 161.8 |
N1—H1B···Cl1i | 0.90 | 2.47 | 3.283 (4) | 149.8 |
N2—H2B···Cl1ii | 0.90 | 2.46 | 3.299 (4) | 155.4 |
N2—H2A···Cl4 | 0.90 | 2.36 | 3.231 (4) | 162.0 |
C11—H11B···Cl2iii | 0.96 | 2.77 | 3.718 (5) | 169.6 |
C11—H11C···Cl1iv | 0.96 | 2.82 | 3.742 (5) | 161.8 |
C11—H11A···Cl4v | 0.96 | 2.87 | 3.559 (5) | 129.3 |
C22—H22A···Cl3vi | 0.96 | 2.91 | 3.658 (6) | 135.7 |
Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) x−1/2, −y+3/2, z+1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) x−1/2, −y+3/2, z−1/2; (v) x+1/2, −y+3/2, z−1/2; (vi) −x+3/2, y−1/2, −z+3/2. |
Selected geometric parameters (Å, º) for (366) topCo1—Cl4 | 2.2520 (11) | N1—C11 | 1.463 (5) |
Co1—Cl3 | 2.2602 (10) | N1—C12 | 1.469 (5) |
Co1—Cl2 | 2.2752 (10) | N2—C21 | 1.455 (6) |
Co1—Cl1 | 2.2897 (10) | N2—C22 | 1.466 (6) |
| | | |
Cl4—Co1—Cl3 | 109.52 (4) | Cl3—Co1—Cl1 | 109.17 (4) |
Cl4—Co1—Cl2 | 110.54 (5) | Cl2—Co1—Cl1 | 104.57 (4) |
Cl3—Co1—Cl2 | 111.36 (4) | C11—N1—C12 | 113.2 (4) |
Cl4—Co1—Cl1 | 111.59 (5) | C21—N2—C22 | 115.0 (4) |
Hydrogen-bond geometry (Å, º) for (366) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1B···Cl2 | 0.90 | 2.35 | 3.222 (4) | 162.9 |
N1—H1A···Cl1i | 0.90 | 2.49 | 3.297 (4) | 149.1 |
N2—H2B···Cl1ii | 0.90 | 2.47 | 3.306 (4) | 155.0 |
N2—H2A···Cl4 | 0.90 | 2.37 | 3.243 (4) | 162.6 |
C11—H11B···Cl2iii | 0.96 | 2.78 | 3.735 (5) | 170.6 |
C11—H11C···Cl1iv | 0.96 | 2.83 | 3.749 (5) | 160.8 |
C11—H11A···Cl4v | 0.96 | 2.88 | 3.561 (5) | 128.4 |
C22—H22A···Cl3vi | 0.96 | 2.90 | 3.661 (6) | 136.6 |
Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) x−1/2, −y+3/2, z+1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) x−1/2, −y+3/2, z−1/2; (v) x+1/2, −y+3/2, z−1/2; (vi) −x+3/2, y−1/2, −z+3/2. |