The crystal structures and absolute configurations of three cis-β1 and three cis-β2 isomers of [Co(trien)(L-aminoacidato)]2+, namely β1-Λ(SSS)(λλδ)/(λδδ)-[Co(trien)(L-isoleucinato)](ClO4)2, L-isoleucinato(triethylenetetramine)cobalt(III) diperchlorate (1), β1-Λ(SRS)(λδλ)-[Co(trien)(L-valinato)](ClO4)2, L-valinato(triethylenetetramine)cobalt(III) diperchlorate (2), β1-Δ(RSS)(δλδ)-[Co(trien)(L-pyroglutamato)]ClO4, L-pyroglutamato(triethylenetetramine)cobalt(III) perchlorate (3), β2-Δ(RRS)(δδλ)-[Co(trien)(L-isoleucinato)]I2·H2O, L-isoleucinato(triethylenetetramine)cobalt(III) diiodide monohydrate (4), β2-Δ(RRS)(δδλ)-[Co(trien)(L-isoleucinato)](ClO4)2·2H2O, L-isoleucinato(triethylenetetramine)cobalt(III) diperchlorate dihydrate (5), and β2-Λ(SSS)(δλλ)[Co(trien)(L-leucinato)](ClO4)2·2H2O, L-leucinato(triethylenetetramine)cobalt(III) diperchlorate dihydrate (6), have been determined. Both β1 and β2 isomers form inter-cation hydrogen-bonding interactions through double or triple hydrogen bonds which link the cations into helices. However, the motifs of the interactions are different in β1 and β2 isomers, resulting in different packing structures. A localized hydrophobic area is observed in the packing structure of (1), a unique feature amongst these six structures. This work describes the first synthesis of the β1 isomer by direct reaction between amino acids and cis-α-[Co(trien)Cl2]Cl in mildly basic solution.
Supporting information
CCDC references: 159946; 159947; 159948; 159949; 159950; 159951
For all compounds, data collection: Bruker SMART (Bruker, 1998a); cell refinement: Bruker SMART (Bruker, 1998a); data reduction: Bruker SAINT+ & SHELXTL(Bruker, 1999 & 1998b); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Bruker SHELXTL; software used to prepare material for publication: Bruker SHELXTL.
(1) (
L-isoleucinato)-(triethylenetetramine)-cobalt(III) diperchlorate
top
Crystal data top
C12H30CoN5O22+·2(ClO4−) | Z = 2 |
Mr = 534.24 | F(000) = 556 |
Monoclinic, P21 | Dx = 1.670 Mg m−3 |
a = 10.7972 (13) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.8272 (11) Å | µ = 1.12 mm−1 |
c = 11.9248 (14) Å | T = 293 K |
β = 110.794 (2)° | Block, red |
V = 1062.5 (2) Å3 | 0.40 × 0.30 × 0.30 mm |
Data collection top
Bruker SMART CCD area detector diffractometer | 3818 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.029 |
Graphite monochromator | θmax = 27.0°, θmin = 1.8° |
ϕ and ω scans | h = −13→13 |
6477 measured reflections | k = −10→11 |
4129 independent reflections | l = −15→12 |
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)] = 0.050 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.127 | w = 1/[σ2(Fo2) + (0.0712P)2 + 1.0375P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.008 |
4129 reflections | Δρmax = 0.49 e Å−3 |
280 parameters | Δρmin = −0.54 e Å−3 |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.08 (2) |
Crystal data top
C12H30CoN5O22+·2(ClO4−) | V = 1062.5 (2) Å3 |
Mr = 534.24 | Z = 2 |
Monoclinic, P21 | Mo Kα radiation |
a = 10.7972 (13) Å | µ = 1.12 mm−1 |
b = 8.8272 (11) Å | T = 293 K |
c = 11.9248 (14) Å | 0.40 × 0.30 × 0.30 mm |
β = 110.794 (2)° | |
Data collection top
Bruker SMART CCD area detector diffractometer | 3818 reflections with I > 2σ(I) |
6477 measured reflections | Rint = 0.029 |
4129 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.050 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.127 | Δρmax = 0.49 e Å−3 |
S = 1.05 | Δρmin = −0.54 e Å−3 |
4129 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
280 parameters | Absolute structure parameter: 0.08 (2) |
1 restraint | |
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 | Occ. (<1) |
Co | 0.13845 (5) | −0.34207 (7) | −0.26941 (5) | 0.02571 (15) | |
Cl1 | 0.87592 (16) | 0.18784 (16) | 0.72185 (12) | 0.0502 (4) | |
Cl2 | 0.37596 (13) | 0.02414 (16) | 0.06881 (12) | 0.0436 (3) | |
C1 | −0.1044 (6) | −0.3620 (11) | −0.2233 (5) | 0.0582 (18) | |
H1A | −0.1063 | −0.4524 | −0.1777 | 0.070* | |
H1B | −0.1944 | −0.3251 | −0.2604 | 0.070* | |
C2 | −0.0200 (6) | −0.2433 (7) | −0.1419 (5) | 0.0450 (13) | |
H2A | −0.0404 | −0.1445 | −0.1796 | 0.054* | |
H2B | −0.0371 | −0.2404 | −0.0673 | 0.054* | |
C3 | 0.1710 (7) | −0.4030 (7) | −0.0275 (5) | 0.0530 (15) | |
H3A | 0.0978 | −0.4539 | −0.0142 | 0.064* | |
H3B | 0.2274 | −0.3593 | 0.0480 | 0.064* | |
C5 | 0.2469 (8) | −0.6294 (8) | −0.2624 (6) | 0.0603 (19) | |
H5A | 0.3424 | −0.6396 | −0.2281 | 0.072* | |
H5B | 0.2094 | −0.7283 | −0.2584 | 0.072* | |
C6 | 0.2124 (11) | −0.5903 (8) | −0.3846 (7) | 0.082 (3) | |
H6A | 0.1499 | −0.6642 | −0.4333 | 0.099* | |
H6B | 0.2911 | −0.5944 | −0.4058 | 0.099* | |
C7 | 0.1576 (5) | −0.0631 (5) | −0.3596 (4) | 0.0283 (9) | |
C8 | 0.2982 (5) | −0.0849 (5) | −0.2745 (4) | 0.0280 (10) | |
H8A | 0.3098 | −0.0181 | −0.2058 | 0.034* | |
C9 | 0.4023 (5) | −0.0387 (7) | −0.3265 (5) | 0.0409 (12) | |
H9A | 0.3783 | 0.0625 | −0.3613 | 0.049* | |
C10 | 0.4062 (6) | −0.1424 (9) | −0.4267 (5) | 0.0522 (15) | |
H10A | 0.4461 | −0.2378 | −0.3918 | 0.063* | |
H10B | 0.3159 | −0.1635 | −0.4788 | 0.063* | |
C11 | 0.4812 (11) | −0.0809 (16) | −0.5022 (9) | 0.101 (4) | |
H11A | 0.4792 | −0.1536 | −0.5627 | 0.151* | |
H11B | 0.5714 | −0.0617 | −0.4521 | 0.151* | |
H11C | 0.4407 | 0.0118 | −0.5398 | 0.151* | |
C12 | 0.5404 (6) | −0.0249 (10) | −0.2257 (6) | 0.066 (2) | |
H12A | 0.6048 | 0.0049 | −0.2600 | 0.100* | |
H12B | 0.5651 | −0.1210 | −0.1863 | 0.100* | |
H12C | 0.5367 | 0.0498 | −0.1685 | 0.100* | |
N1 | −0.0476 (5) | −0.3978 (6) | −0.3168 (4) | 0.0444 (11) | |
H1C | −0.0941 | −0.3483 | −0.3847 | 0.053* | |
H1D | −0.0561 | −0.4977 | −0.3325 | 0.053* | |
N2 | 0.1191 (4) | −0.2809 (5) | −0.1179 (3) | 0.0328 (9) | |
H2C | 0.1686 | −0.1961 | −0.0905 | 0.039* | |
N3 | 0.2069 (7) | −0.5290 (6) | −0.1892 (5) | 0.0639 (17) | |
H3C | 0.1278 | −0.5735 | −0.1988 | 0.077* | |
N4 | 0.1533 (4) | −0.4380 (5) | −0.4121 (4) | 0.0332 (9) | |
H4C | 0.0723 | −0.4451 | −0.4693 | 0.040* | |
H4D | 0.2038 | −0.3799 | −0.4408 | 0.040* | |
N5 | 0.3143 (4) | −0.2442 (5) | −0.2270 (3) | 0.0305 (8) | |
H5C | 0.3549 | −0.2430 | −0.1467 | 0.037* | |
H5D | 0.3651 | −0.2974 | −0.2585 | 0.037* | |
O1 | 0.0724 (3) | −0.1612 (4) | −0.3565 (3) | 0.0295 (7) | |
O2 | 0.1273 (4) | 0.0491 (4) | −0.4269 (3) | 0.0420 (8) | |
O3 | 0.7877 (8) | 0.2682 (7) | 0.7613 (7) | 0.109 (3) | |
O4 | 0.8127 (6) | 0.0502 (6) | 0.6673 (5) | 0.0793 (15) | |
O5 | 0.9932 (6) | 0.1555 (13) | 0.8165 (5) | 0.116 (2) | |
O6 | 0.9054 (5) | 0.2741 (6) | 0.6316 (4) | 0.0608 (12) | |
O7 | 0.2373 (5) | 0.0431 (10) | 0.0217 (6) | 0.104 (2) | |
O8 | 0.4018 (8) | −0.1249 (7) | 0.0361 (6) | 0.103 (2) | |
O9 | 0.4385 (7) | 0.1310 (10) | 0.0150 (5) | 0.110 (3) | |
O10 | 0.4262 (6) | 0.0456 (7) | 0.1935 (4) | 0.0762 (15) | |
C4 | 0.2505 (14) | −0.5179 (17) | −0.0713 (11) | 0.042 (3) | 0.50 |
H4A | 0.3429 | −0.4876 | −0.0428 | 0.050* | 0.50 |
H4B | 0.2453 | −0.6165 | −0.0373 | 0.050* | 0.50 |
C4A | 0.1892 (17) | −0.5430 (16) | −0.0751 (13) | 0.043 (3) | 0.50 |
H4AA | 0.1128 | −0.6067 | −0.0851 | 0.052* | 0.50 |
H4AB | 0.2662 | −0.5926 | −0.0186 | 0.052* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co | 0.0334 (3) | 0.0199 (3) | 0.0258 (3) | −0.0002 (3) | 0.0129 (2) | 0.0010 (3) |
Cl1 | 0.0679 (9) | 0.0461 (10) | 0.0434 (7) | 0.0001 (7) | 0.0284 (6) | 0.0064 (5) |
Cl2 | 0.0448 (7) | 0.0461 (8) | 0.0420 (7) | −0.0058 (6) | 0.0180 (5) | −0.0093 (5) |
C1 | 0.041 (3) | 0.077 (5) | 0.064 (4) | −0.017 (4) | 0.028 (3) | −0.013 (4) |
C2 | 0.047 (3) | 0.044 (3) | 0.052 (3) | 0.001 (3) | 0.027 (3) | −0.007 (2) |
C3 | 0.077 (4) | 0.055 (4) | 0.032 (3) | 0.016 (3) | 0.025 (3) | 0.007 (2) |
C5 | 0.084 (5) | 0.038 (3) | 0.054 (4) | 0.024 (3) | 0.019 (4) | −0.005 (3) |
C6 | 0.168 (9) | 0.034 (3) | 0.078 (5) | 0.029 (4) | 0.085 (6) | 0.010 (3) |
C7 | 0.040 (3) | 0.020 (2) | 0.028 (2) | 0.0032 (19) | 0.015 (2) | 0.0024 (17) |
C8 | 0.030 (2) | 0.026 (2) | 0.028 (2) | −0.0092 (19) | 0.0100 (19) | −0.0029 (17) |
C9 | 0.036 (3) | 0.048 (3) | 0.038 (3) | −0.012 (2) | 0.012 (2) | 0.001 (2) |
C10 | 0.052 (3) | 0.069 (4) | 0.043 (3) | −0.009 (3) | 0.027 (3) | −0.003 (3) |
C11 | 0.097 (7) | 0.161 (9) | 0.064 (4) | −0.064 (7) | 0.053 (5) | −0.027 (5) |
C12 | 0.043 (3) | 0.102 (6) | 0.050 (3) | −0.034 (4) | 0.011 (3) | −0.008 (4) |
N1 | 0.050 (3) | 0.050 (3) | 0.038 (2) | −0.021 (2) | 0.021 (2) | −0.0104 (19) |
N2 | 0.042 (2) | 0.031 (2) | 0.0265 (19) | −0.0054 (17) | 0.0135 (17) | −0.0025 (15) |
N3 | 0.122 (5) | 0.033 (3) | 0.060 (3) | 0.027 (3) | 0.062 (3) | 0.022 (2) |
N4 | 0.036 (2) | 0.033 (2) | 0.033 (2) | −0.0062 (17) | 0.0152 (17) | −0.0025 (16) |
N5 | 0.030 (2) | 0.029 (2) | 0.0311 (19) | 0.0034 (16) | 0.0088 (16) | 0.0077 (15) |
O1 | 0.0253 (16) | 0.0276 (17) | 0.0336 (17) | 0.0022 (13) | 0.0080 (13) | 0.0053 (13) |
O2 | 0.050 (2) | 0.0289 (19) | 0.047 (2) | 0.0065 (17) | 0.0174 (17) | 0.0142 (15) |
O3 | 0.176 (7) | 0.062 (4) | 0.145 (6) | 0.021 (4) | 0.126 (6) | 0.010 (4) |
O4 | 0.091 (4) | 0.050 (3) | 0.099 (4) | −0.017 (3) | 0.036 (3) | 0.004 (3) |
O5 | 0.095 (4) | 0.160 (6) | 0.066 (3) | −0.020 (6) | −0.007 (3) | 0.019 (5) |
O6 | 0.089 (3) | 0.054 (3) | 0.052 (2) | −0.012 (2) | 0.040 (2) | 0.007 (2) |
O7 | 0.059 (3) | 0.140 (6) | 0.097 (4) | 0.023 (4) | 0.009 (3) | 0.025 (4) |
O8 | 0.155 (6) | 0.058 (4) | 0.097 (4) | 0.010 (4) | 0.046 (4) | −0.029 (3) |
O9 | 0.141 (5) | 0.130 (7) | 0.073 (3) | −0.084 (5) | 0.054 (4) | −0.027 (4) |
O10 | 0.094 (4) | 0.087 (4) | 0.045 (2) | −0.013 (3) | 0.020 (2) | −0.010 (2) |
C4 | 0.045 (8) | 0.043 (7) | 0.029 (5) | −0.015 (6) | 0.004 (6) | 0.018 (4) |
C4A | 0.062 (10) | 0.030 (7) | 0.041 (7) | 0.003 (7) | 0.023 (7) | 0.010 (5) |
Geometric parameters (Å, º) top
Co—O1 | 1.900 (3) | C3—C4A | 1.402 (16) |
Co—N3 | 1.919 (5) | C3—N2 | 1.485 (7) |
Co—N1 | 1.947 (4) | C3—C4 | 1.536 (17) |
Co—N4 | 1.957 (4) | C5—C6 | 1.413 (10) |
Co—N2 | 1.967 (4) | C5—N3 | 1.415 (8) |
Co—N5 | 1.981 (4) | C6—N4 | 1.474 (8) |
Cl1—O5 | 1.394 (6) | C7—O2 | 1.242 (6) |
Cl1—O3 | 1.396 (6) | C7—O1 | 1.274 (6) |
Cl1—O4 | 1.432 (6) | C7—C8 | 1.509 (7) |
Cl1—O6 | 1.443 (4) | C8—N5 | 1.503 (6) |
Cl2—O10 | 1.403 (5) | C8—C9 | 1.520 (7) |
Cl2—O7 | 1.410 (5) | C9—C10 | 1.518 (8) |
Cl2—O8 | 1.428 (6) | C9—C12 | 1.552 (8) |
Cl2—O9 | 1.436 (6) | C10—C11 | 1.510 (10) |
C1—N1 | 1.484 (7) | N3—C4 | 1.318 (14) |
C1—C2 | 1.497 (9) | N3—C4A | 1.444 (14) |
C2—N2 | 1.464 (7) | | |
| | | |
O1—Co—N3 | 176.82 (18) | C4A—C3—C4 | 26.4 (6) |
O1—Co—N1 | 84.56 (18) | N2—C3—C4 | 110.2 (6) |
N3—Co—N1 | 95.9 (3) | C6—C5—N3 | 117.2 (5) |
O1—Co—N4 | 91.09 (16) | C5—C6—N4 | 112.8 (5) |
N3—Co—N4 | 85.7 (2) | O2—C7—O1 | 122.2 (5) |
N1—Co—N4 | 91.90 (18) | O2—C7—C8 | 120.5 (4) |
O1—Co—N2 | 97.46 (16) | O1—C7—C8 | 117.2 (4) |
N3—Co—N2 | 85.72 (19) | N5—C8—C7 | 109.1 (4) |
N1—Co—N2 | 84.31 (18) | N5—C8—C9 | 113.6 (4) |
N4—Co—N2 | 170.26 (18) | C7—C8—C9 | 113.8 (4) |
O1—Co—N5 | 85.01 (15) | C10—C9—C8 | 113.0 (5) |
N3—Co—N5 | 94.8 (2) | C10—C9—C12 | 111.7 (5) |
N1—Co—N5 | 168.74 (19) | C8—C9—C12 | 110.6 (4) |
N4—Co—N5 | 92.50 (17) | C11—C10—C9 | 115.0 (7) |
N2—Co—N5 | 92.88 (17) | C1—N1—Co | 112.8 (3) |
O5—Cl1—O3 | 111.3 (5) | C2—N2—C3 | 113.7 (5) |
O5—Cl1—O4 | 110.1 (5) | C2—N2—Co | 108.6 (3) |
O3—Cl1—O4 | 108.2 (4) | C3—N2—Co | 109.4 (3) |
O5—Cl1—O6 | 109.5 (4) | C4—N3—C5 | 129.2 (9) |
O3—Cl1—O6 | 109.9 (3) | C4—N3—C4A | 28.2 (6) |
O4—Cl1—O6 | 107.7 (3) | C5—N3—C4A | 134.3 (7) |
O10—Cl2—O7 | 111.3 (4) | C4—N3—Co | 113.4 (7) |
O10—Cl2—O8 | 112.0 (4) | C5—N3—Co | 112.3 (4) |
O7—Cl2—O8 | 106.5 (5) | C4A—N3—Co | 112.8 (6) |
O10—Cl2—O9 | 108.5 (3) | C6—N4—Co | 111.3 (4) |
O7—Cl2—O9 | 110.2 (5) | C8—N5—Co | 109.8 (3) |
O8—Cl2—O9 | 108.3 (5) | C7—O1—Co | 116.9 (3) |
N1—C1—C2 | 108.5 (5) | N3—C4—C3 | 112.3 (10) |
N2—C2—C1 | 108.3 (5) | C3—C4A—N3 | 113.0 (10) |
C4A—C3—N2 | 114.6 (7) | | |
| | | |
N1—C1—C2—N2 | −41.9 (7) | N5—Co—N3—C4 | 71.9 (8) |
N3—C5—C6—N4 | 7.2 (12) | O1—Co—N3—C5 | 0 (5) |
O2—C7—C8—N5 | −166.4 (4) | N1—Co—N3—C5 | 98.3 (6) |
O1—C7—C8—N5 | 15.7 (6) | N4—Co—N3—C5 | 6.8 (6) |
O2—C7—C8—C9 | −38.3 (6) | N2—Co—N3—C5 | −177.9 (6) |
O1—C7—C8—C9 | 143.8 (4) | N5—Co—N3—C5 | −85.3 (6) |
N5—C8—C9—C10 | 57.2 (6) | O1—Co—N3—C4A | −172 (4) |
C7—C8—C9—C10 | −68.5 (6) | N1—Co—N3—C4A | −73.8 (8) |
N5—C8—C9—C12 | −68.8 (6) | N4—Co—N3—C4A | −165.3 (8) |
C7—C8—C9—C12 | 165.5 (5) | N2—Co—N3—C4A | 10.0 (8) |
C8—C9—C10—C11 | 165.0 (7) | N5—Co—N3—C4A | 102.6 (8) |
C12—C9—C10—C11 | −69.6 (9) | C5—C6—N4—Co | −1.4 (10) |
C2—C1—N1—Co | 21.2 (7) | O1—Co—N4—C6 | 176.6 (5) |
O1—Co—N1—C1 | −95.8 (5) | N3—Co—N4—C6 | −3.0 (6) |
N3—Co—N1—C1 | 87.3 (5) | N1—Co—N4—C6 | −98.8 (5) |
N4—Co—N1—C1 | 173.2 (5) | N2—Co—N4—C6 | −32.0 (13) |
N2—Co—N1—C1 | 2.2 (5) | N5—Co—N4—C6 | 91.5 (5) |
N5—Co—N1—C1 | −73.7 (10) | C7—C8—N5—Co | −11.5 (4) |
C1—C2—N2—C3 | −78.2 (6) | C9—C8—N5—Co | −139.7 (3) |
C1—C2—N2—Co | 43.8 (5) | O1—Co—N5—C8 | 5.0 (3) |
C4A—C3—N2—C2 | 106.4 (9) | N3—Co—N5—C8 | −178.2 (3) |
C4—C3—N2—C2 | 134.6 (7) | N1—Co—N5—C8 | −17.1 (10) |
C4A—C3—N2—Co | −15.2 (10) | N4—Co—N5—C8 | 95.9 (3) |
C4—C3—N2—Co | 13.0 (8) | N2—Co—N5—C8 | −92.2 (3) |
O1—Co—N2—C2 | 58.0 (4) | O2—C7—O1—Co | 169.9 (4) |
N3—Co—N2—C2 | −122.2 (4) | C8—C7—O1—Co | −12.2 (5) |
N1—Co—N2—C2 | −25.8 (4) | N3—Co—O1—C7 | −82 (4) |
N4—Co—N2—C2 | −93.2 (11) | N1—Co—O1—C7 | 179.7 (3) |
N5—Co—N2—C2 | 143.3 (4) | N4—Co—O1—C7 | −88.5 (3) |
O1—Co—N2—C3 | −177.4 (4) | N2—Co—O1—C7 | 96.2 (3) |
N3—Co—N2—C3 | 2.5 (4) | N5—Co—O1—C7 | 3.9 (3) |
N1—Co—N2—C3 | 98.9 (4) | C5—N3—C4—C3 | −174.7 (8) |
N4—Co—N2—C3 | 31.4 (13) | C4A—N3—C4—C3 | −62 (2) |
N5—Co—N2—C3 | −92.1 (4) | Co—N3—C4—C3 | 32.9 (11) |
C6—C5—N3—C4 | −162.3 (10) | C4A—C3—C4—N3 | 74.8 (19) |
C6—C5—N3—C4A | 160.1 (12) | N2—C3—C4—N3 | −30.1 (12) |
C6—C5—N3—Co | −9.7 (10) | N2—C3—C4A—N3 | 23.9 (15) |
O1—Co—N3—C4 | 157 (4) | C4—C3—C4A—N3 | −62.2 (17) |
N1—Co—N3—C4 | −104.5 (8) | C4—N3—C4A—C3 | 76 (2) |
N4—Co—N3—C4 | 164.0 (8) | C5—N3—C4A—C3 | 169.0 (9) |
N2—Co—N3—C4 | −20.7 (8) | Co—N3—C4A—C3 | −21.3 (15) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1C···O2i | 0.90 | 2.33 | 2.905 (6) | 122 |
N1—H1D···O6ii | 0.90 | 2.07 | 2.967 (7) | 174 |
N2—H2C···O7 | 0.91 | 2.47 | 3.327 (10) | 157 |
N2—H2C···O8 | 0.91 | 2.51 | 3.256 (9) | 139 |
N4—H4C···O2i | 0.90 | 2.07 | 2.958 (6) | 169 |
N4—H4D···O6iii | 0.90 | 2.55 | 3.096 (6) | 120 |
N5—H5C···O8 | 0.90 | 2.30 | 3.120 (8) | 151 |
N5—H5C···O9iii | 0.90 | 2.49 | 3.152 (7) | 131 |
N5—H5D···O10iii | 0.90 | 2.52 | 3.264 (7) | 140 |
Symmetry codes: (i) −x, y−1/2, −z−1; (ii) x−1, y−1, z−1; (iii) −x+1, y−1/2, −z. |
(2) (
L-valinato)-(triethylenetetramine)-cobalt(III) diperchlorate
top
Crystal data top
C11H28CoN5O22+·2(ClO4−) | Z = 2 |
Mr = 520.21 | F(000) = 540 |
Monoclinic, P21 | Dx = 1.724 Mg m−3 |
a = 8.9877 (7) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.8829 (7) Å | µ = 1.18 mm−1 |
c = 12.8157 (10) Å | T = 293 K |
β = 101.577 (1)° | Block, red |
V = 1002.35 (14) Å3 | 0.30 × 0.25 × 0.23 mm |
Data collection top
Bruker SMART CCD area detector diffractometer | 3672 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.022 |
Graphite monochromator | θmax = 27.0°, θmin = 1.6° |
ϕ and ω scans | h = −11→11 |
6012 measured reflections | k = −10→11 |
3835 independent reflections | l = −13→16 |
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)] = 0.045 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.123 | w = 1/[σ2(Fo2) + (0.0821P)2 + 0.5521P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max = 0.002 |
3835 reflections | Δρmax = 0.68 e Å−3 |
262 parameters | Δρmin = −0.40 e Å−3 |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.08 (2) |
Crystal data top
C11H28CoN5O22+·2(ClO4−) | V = 1002.35 (14) Å3 |
Mr = 520.21 | Z = 2 |
Monoclinic, P21 | Mo Kα radiation |
a = 8.9877 (7) Å | µ = 1.18 mm−1 |
b = 8.8829 (7) Å | T = 293 K |
c = 12.8157 (10) Å | 0.30 × 0.25 × 0.23 mm |
β = 101.577 (1)° | |
Data collection top
Bruker SMART CCD area detector diffractometer | 3672 reflections with I > 2σ(I) |
6012 measured reflections | Rint = 0.022 |
3835 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.045 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.123 | Δρmax = 0.68 e Å−3 |
S = 1.07 | Δρmin = −0.40 e Å−3 |
3835 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
262 parameters | Absolute structure parameter: 0.08 (2) |
1 restraint | |
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 | |
Co | −0.40564 (5) | −0.01783 (6) | −0.79301 (3) | 0.02989 (14) | |
Cl1 | −0.29331 (16) | −0.37208 (16) | −0.47588 (10) | 0.0575 (3) | |
Cl2 | −1.09219 (16) | −0.54801 (15) | −0.89150 (11) | 0.0640 (4) | |
C1 | −0.1032 (6) | 0.0237 (7) | −0.8279 (5) | 0.0620 (15) | |
H1A | −0.0469 | −0.0042 | −0.8821 | 0.074* | |
H1B | −0.0561 | 0.1125 | −0.7914 | 0.074* | |
C2 | −0.0989 (5) | −0.1010 (7) | −0.7511 (4) | 0.0527 (12) | |
H2A | −0.0010 | −0.1038 | −0.7026 | 0.063* | |
H2B | −0.1146 | −0.1965 | −0.7884 | 0.063* | |
C3 | −0.1898 (6) | 0.0414 (6) | −0.6059 (4) | 0.0533 (12) | |
H3A | −0.2296 | 0.0077 | −0.5449 | 0.064* | |
H3B | −0.0808 | 0.0537 | −0.5834 | 0.064* | |
C4 | −0.2590 (8) | 0.1875 (7) | −0.6431 (5) | 0.0689 (17) | |
H4A | −0.2688 | 0.2495 | −0.5826 | 0.083* | |
H4B | −0.1949 | 0.2403 | −0.6837 | 0.083* | |
C5 | −0.4935 (9) | 0.2791 (7) | −0.7721 (5) | 0.0687 (17) | |
H5A | −0.5298 | 0.3499 | −0.7253 | 0.082* | |
H5B | −0.4287 | 0.3333 | −0.8113 | 0.082* | |
C6 | −0.6221 (8) | 0.2163 (7) | −0.8465 (5) | 0.0716 (17) | |
H6A | −0.6551 | 0.2867 | −0.9043 | 0.086* | |
H6B | −0.7059 | 0.2004 | −0.8104 | 0.086* | |
C7 | −0.4999 (4) | −0.3001 (5) | −0.8574 (3) | 0.0321 (8) | |
C8 | −0.5571 (4) | −0.2862 (4) | −0.7530 (3) | 0.0308 (8) | |
H8A | −0.4951 | −0.3521 | −0.7001 | 0.037* | |
C9 | −0.7215 (5) | −0.3353 (5) | −0.7663 (3) | 0.0405 (9) | |
H9A | −0.7366 | −0.4288 | −0.8077 | 0.049* | |
C10 | −0.8107 (4) | −0.2189 (5) | −0.8245 (3) | 0.0351 (8) | |
H10A | −0.9162 | −0.2454 | −0.8352 | 0.053* | |
H10B | −0.7822 | −0.2065 | −0.8922 | 0.053* | |
H10C | −0.7937 | −0.1264 | −0.7851 | 0.053* | |
C11 | −0.7677 (6) | −0.3601 (8) | −0.6601 (4) | 0.0583 (13) | |
H11A | −0.8721 | −0.3909 | −0.6720 | 0.087* | |
H11B | −0.7553 | −0.2680 | −0.6200 | 0.087* | |
H11C | −0.7049 | −0.4369 | −0.6210 | 0.087* | |
N1 | −0.2640 (4) | 0.0571 (5) | −0.8786 (3) | 0.0433 (8) | |
H1C | −0.2857 | 0.0144 | −0.9435 | 0.052* | |
H1D | −0.2758 | 0.1573 | −0.8870 | 0.052* | |
N2 | −0.2217 (4) | −0.0742 (4) | −0.6912 (3) | 0.0378 (7) | |
H2C | −0.2403 | −0.1628 | −0.6605 | 0.045* | |
N3 | −0.4062 (5) | 0.1611 (5) | −0.7088 (3) | 0.0487 (9) | |
H3C | −0.4646 | 0.1353 | −0.6613 | 0.058* | |
N4 | −0.5796 (4) | 0.0707 (5) | −0.8901 (3) | 0.0413 (8) | |
H4C | −0.5559 | 0.0862 | −0.9542 | 0.050* | |
H4D | −0.6589 | 0.0069 | −0.8987 | 0.050* | |
N5 | −0.5362 (4) | −0.1291 (4) | −0.7137 (3) | 0.0359 (7) | |
H5C | −0.4936 | −0.1292 | −0.6439 | 0.043* | |
H5D | −0.6272 | −0.0833 | −0.7218 | 0.043* | |
O1 | −0.4173 (3) | −0.1932 (4) | −0.8793 (2) | 0.0369 (6) | |
O2 | −0.5334 (4) | −0.4117 (4) | −0.9135 (2) | 0.0448 (7) | |
O3 | −0.2141 (9) | −0.3687 (11) | −0.5572 (6) | 0.137 (3) | |
O4 | −0.3867 (10) | −0.2408 (10) | −0.4869 (5) | 0.137 (3) | |
O5 | −0.2195 (9) | −0.4058 (12) | −0.3727 (4) | 0.143 (3) | |
O6 | −0.4082 (11) | −0.4877 (12) | −0.5017 (8) | 0.172 (4) | |
O7 | −0.9607 (9) | −0.6109 (10) | −0.8816 (14) | 0.223 (7) | |
O8 | −1.1279 (15) | −0.521 (2) | −0.7914 (5) | 0.213 (6) | |
O9 | −1.0901 (9) | −0.4057 (6) | −0.9399 (5) | 0.1076 (19) | |
O10 | −1.2149 (6) | −0.6344 (6) | −0.9486 (4) | 0.0865 (16) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co | 0.0340 (2) | 0.0246 (2) | 0.0311 (2) | 0.0008 (2) | 0.00662 (15) | −0.0008 (2) |
Cl1 | 0.0600 (7) | 0.0637 (8) | 0.0484 (6) | 0.0122 (6) | 0.0100 (5) | 0.0177 (5) |
Cl2 | 0.0631 (7) | 0.0514 (9) | 0.0698 (7) | −0.0138 (6) | −0.0049 (6) | 0.0005 (6) |
C1 | 0.045 (3) | 0.072 (4) | 0.077 (3) | −0.002 (2) | 0.031 (2) | 0.008 (3) |
C2 | 0.037 (2) | 0.070 (4) | 0.053 (3) | 0.011 (2) | 0.0125 (19) | −0.004 (2) |
C3 | 0.058 (3) | 0.058 (3) | 0.039 (2) | −0.004 (2) | −0.0016 (19) | −0.011 (2) |
C4 | 0.086 (4) | 0.053 (3) | 0.060 (3) | −0.004 (3) | −0.003 (3) | −0.022 (3) |
C5 | 0.092 (5) | 0.038 (3) | 0.073 (4) | 0.027 (3) | 0.010 (3) | 0.000 (3) |
C6 | 0.076 (4) | 0.058 (4) | 0.077 (4) | 0.033 (3) | 0.005 (3) | 0.006 (3) |
C7 | 0.0328 (18) | 0.0328 (19) | 0.0305 (16) | 0.0037 (15) | 0.0061 (13) | −0.0015 (14) |
C8 | 0.0338 (19) | 0.0307 (19) | 0.0283 (16) | −0.0016 (15) | 0.0067 (13) | −0.0009 (14) |
C9 | 0.038 (2) | 0.041 (2) | 0.044 (2) | −0.0063 (18) | 0.0116 (16) | −0.0023 (17) |
C10 | 0.0224 (16) | 0.051 (2) | 0.0294 (16) | 0.0030 (16) | −0.0015 (13) | 0.0039 (16) |
C11 | 0.056 (3) | 0.074 (4) | 0.049 (2) | −0.012 (3) | 0.020 (2) | 0.009 (2) |
N1 | 0.052 (2) | 0.040 (2) | 0.0400 (17) | −0.0067 (17) | 0.0130 (15) | 0.0077 (15) |
N2 | 0.0360 (16) | 0.0366 (17) | 0.0401 (16) | 0.0015 (14) | 0.0059 (13) | 0.0022 (14) |
N3 | 0.061 (2) | 0.0327 (19) | 0.052 (2) | 0.0028 (18) | 0.0093 (18) | −0.0114 (16) |
N4 | 0.0437 (19) | 0.040 (2) | 0.0386 (17) | 0.0076 (16) | 0.0056 (14) | 0.0036 (15) |
N5 | 0.0387 (17) | 0.0360 (18) | 0.0348 (15) | −0.0015 (14) | 0.0114 (12) | −0.0063 (13) |
O1 | 0.0427 (15) | 0.0353 (16) | 0.0351 (13) | −0.0047 (13) | 0.0135 (11) | −0.0060 (11) |
O2 | 0.0562 (18) | 0.0372 (16) | 0.0420 (14) | −0.0083 (14) | 0.0124 (13) | −0.0138 (12) |
O3 | 0.140 (6) | 0.172 (8) | 0.119 (5) | 0.045 (6) | 0.074 (5) | 0.051 (5) |
O4 | 0.162 (7) | 0.130 (6) | 0.104 (4) | 0.080 (5) | −0.009 (4) | −0.005 (4) |
O5 | 0.131 (5) | 0.214 (9) | 0.072 (3) | 0.051 (6) | −0.012 (3) | 0.031 (5) |
O6 | 0.155 (7) | 0.159 (9) | 0.180 (8) | −0.079 (7) | −0.023 (6) | 0.074 (7) |
O7 | 0.083 (5) | 0.097 (6) | 0.46 (2) | 0.016 (4) | −0.013 (8) | −0.025 (9) |
O8 | 0.281 (13) | 0.276 (14) | 0.077 (4) | −0.095 (14) | 0.024 (6) | 0.012 (8) |
O9 | 0.144 (5) | 0.060 (3) | 0.111 (4) | −0.029 (4) | 0.006 (4) | 0.003 (3) |
O10 | 0.084 (3) | 0.061 (3) | 0.097 (3) | −0.027 (3) | −0.024 (3) | 0.016 (2) |
Geometric parameters (Å, º) top
Co—O1 | 1.901 (3) | C1—N1 | 1.491 (7) |
Co—N3 | 1.921 (4) | C2—N2 | 1.485 (6) |
Co—N2 | 1.955 (3) | C3—C4 | 1.477 (8) |
Co—N1 | 1.956 (4) | C3—N2 | 1.484 (6) |
Co—N4 | 1.957 (4) | C4—N3 | 1.438 (7) |
Co—N5 | 1.966 (4) | C5—C6 | 1.453 (10) |
Cl1—O3 | 1.376 (6) | C5—N3 | 1.455 (7) |
Cl1—O5 | 1.388 (5) | C6—N4 | 1.489 (7) |
Cl1—O4 | 1.427 (7) | C7—O2 | 1.226 (5) |
Cl1—O6 | 1.447 (8) | C7—O1 | 1.272 (5) |
Cl2—O7 | 1.290 (8) | C7—C8 | 1.531 (5) |
Cl2—O8 | 1.404 (9) | C8—N5 | 1.483 (5) |
Cl2—O9 | 1.410 (6) | C8—C9 | 1.517 (6) |
Cl2—O10 | 1.420 (5) | C9—C10 | 1.423 (6) |
C1—C2 | 1.477 (8) | C9—C11 | 1.516 (6) |
| | | |
O1—Co—N3 | 176.69 (16) | O9—Cl2—O10 | 109.6 (3) |
O1—Co—N2 | 96.83 (14) | C2—C1—N1 | 109.5 (4) |
N3—Co—N2 | 86.23 (17) | C1—C2—N2 | 107.6 (4) |
O1—Co—N1 | 85.36 (15) | C4—C3—N2 | 111.3 (4) |
N3—Co—N1 | 96.22 (19) | N3—C4—C3 | 108.9 (5) |
N2—Co—N1 | 84.44 (16) | C6—C5—N3 | 111.0 (5) |
O1—Co—N4 | 90.90 (15) | C5—C6—N4 | 110.5 (5) |
N3—Co—N4 | 86.15 (17) | O2—C7—O1 | 124.0 (3) |
N2—Co—N4 | 171.15 (17) | O2—C7—C8 | 119.5 (4) |
N1—Co—N4 | 91.91 (16) | O1—C7—C8 | 116.5 (3) |
O1—Co—N5 | 85.41 (13) | N5—C8—C9 | 111.3 (3) |
N3—Co—N5 | 93.23 (17) | N5—C8—C7 | 109.3 (3) |
N2—Co—N5 | 92.21 (15) | C9—C8—C7 | 111.6 (3) |
N1—Co—N5 | 169.74 (16) | C10—C9—C11 | 110.4 (4) |
N4—Co—N5 | 92.71 (16) | C10—C9—C8 | 106.4 (4) |
O3—Cl1—O5 | 120.4 (5) | C11—C9—C8 | 112.1 (4) |
O3—Cl1—O4 | 106.9 (5) | C1—N1—Co | 111.8 (3) |
O5—Cl1—O4 | 115.5 (5) | C3—N2—C2 | 115.9 (4) |
O3—Cl1—O6 | 107.2 (6) | C3—N2—Co | 109.1 (3) |
O5—Cl1—O6 | 104.3 (6) | C2—N2—Co | 108.2 (3) |
O4—Cl1—O6 | 100.3 (6) | C4—N3—C5 | 122.6 (5) |
O7—Cl2—O8 | 110.9 (9) | C4—N3—Co | 111.0 (3) |
O7—Cl2—O9 | 109.8 (7) | C5—N3—Co | 110.2 (3) |
O8—Cl2—O9 | 106.1 (8) | C6—N4—Co | 110.0 (3) |
O7—Cl2—O10 | 114.7 (6) | C8—N5—Co | 110.2 (2) |
O8—Cl2—O10 | 105.4 (6) | C7—O1—Co | 116.8 (2) |
| | | |
N1—C1—C2—N2 | −42.4 (6) | C6—C5—N3—C4 | 168.5 (5) |
N2—C3—C4—N3 | 39.4 (7) | C6—C5—N3—Co | 35.0 (7) |
N3—C5—C6—N4 | −37.7 (8) | O1—Co—N3—C4 | 177 (3) |
O2—C7—C8—N5 | −165.9 (4) | N2—Co—N3—C4 | 19.0 (4) |
O1—C7—C8—N5 | 15.1 (5) | N1—Co—N3—C4 | −65.0 (4) |
O2—C7—C8—C9 | −42.3 (5) | N4—Co—N3—C4 | −156.5 (4) |
O1—C7—C8—C9 | 138.7 (4) | N5—Co—N3—C4 | 111.0 (4) |
N5—C8—C9—C10 | 48.8 (4) | O1—Co—N3—C5 | −44 (3) |
C7—C8—C9—C10 | −73.7 (4) | N2—Co—N3—C5 | 158.1 (4) |
N5—C8—C9—C11 | −72.0 (5) | N1—Co—N3—C5 | 74.1 (4) |
C7—C8—C9—C11 | 165.5 (4) | N4—Co—N3—C5 | −17.4 (4) |
C2—C1—N1—Co | 20.6 (5) | N5—Co—N3—C5 | −109.9 (4) |
O1—Co—N1—C1 | −93.4 (4) | C5—C6—N4—Co | 22.9 (6) |
N3—Co—N1—C1 | 89.5 (4) | O1—Co—N4—C6 | 175.5 (4) |
N2—Co—N1—C1 | 3.9 (4) | N3—Co—N4—C6 | −3.0 (4) |
N4—Co—N1—C1 | 175.8 (4) | N2—Co—N4—C6 | −33.6 (12) |
N5—Co—N1—C1 | −67.5 (10) | N1—Co—N4—C6 | −99.1 (4) |
C4—C3—N2—C2 | 98.5 (5) | N5—Co—N4—C6 | 90.1 (4) |
C4—C3—N2—Co | −23.9 (6) | C9—C8—N5—Co | −136.1 (3) |
C1—C2—N2—C3 | −77.5 (5) | C7—C8—N5—Co | −12.3 (4) |
C1—C2—N2—Co | 45.3 (5) | O1—Co—N5—C8 | 6.4 (3) |
O1—Co—N2—C3 | −175.8 (3) | N3—Co—N5—C8 | −176.6 (3) |
N3—Co—N2—C3 | 3.0 (3) | N2—Co—N5—C8 | −90.3 (3) |
N1—Co—N2—C3 | 99.6 (3) | N1—Co—N5—C8 | −19.6 (10) |
N4—Co—N2—C3 | 33.6 (11) | N4—Co—N5—C8 | 97.1 (3) |
N5—Co—N2—C3 | −90.1 (3) | O2—C7—O1—Co | 170.6 (3) |
O1—Co—N2—C2 | 57.3 (3) | C8—C7—O1—Co | −10.4 (4) |
N3—Co—N2—C2 | −124.0 (3) | N3—Co—O1—C7 | −64 (3) |
N1—Co—N2—C2 | −27.3 (3) | N2—Co—O1—C7 | 93.9 (3) |
N4—Co—N2—C2 | −93.3 (10) | N1—Co—O1—C7 | 177.8 (3) |
N5—Co—N2—C2 | 143.0 (3) | N4—Co—O1—C7 | −90.4 (3) |
C3—C4—N3—C5 | −169.6 (5) | N5—Co—O1—C7 | 2.2 (3) |
C3—C4—N3—Co | −36.5 (6) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1C···O2i | 0.90 | 2.29 | 2.923 (5) | 127 |
N1—H1D···O10ii | 0.90 | 2.13 | 2.944 (6) | 151 |
N2—H2C···O3 | 0.91 | 2.24 | 3.122 (9) | 163 |
N4—H4C···O2i | 0.90 | 2.02 | 2.901 (5) | 168 |
N4—H4D···O10iii | 0.90 | 2.41 | 3.078 (6) | 131 |
N5—H5C···O4 | 0.90 | 2.27 | 3.110 (7) | 154 |
N5—H5C···O6iv | 0.90 | 2.55 | 3.162 (9) | 126 |
N5—H5D···O5iv | 0.90 | 2.55 | 3.310 (11) | 142 |
Symmetry codes: (i) −x−1, y+1/2, −z−2; (ii) x+1, y+1, z; (iii) −x−2, y+1/2, −z−2; (iv) −x−1, y+1/2, −z−1. |
(3) (
L-pyroglutamicacidato)-(triethylenetetramine)-cobalt(III) perchlorate
top
Crystal data top
C11H23CoN5O3+·ClO4− | F(000) = 896 |
Mr = 431.72 | Dx = 1.671 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.4009 (5) Å | µ = 1.20 mm−1 |
b = 13.3659 (8) Å | T = 293 K |
c = 13.6588 (8) Å | Block, red |
V = 1716.25 (17) Å3 | 0.30 × 0.25 × 0.23 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD area detector diffractometer | 3573 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.044 |
Graphite monochromator | θmax = 27.5°, θmin = 2.1° |
ϕ and ω scans | h = −12→10 |
10571 measured reflections | k = −15→17 |
3939 independent reflections | l = −17→17 |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.037 | w = 1/[σ2(Fo2) + (0.061P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.094 | (Δ/σ)max < 0.001 |
S = 1.05 | Δρmax = 0.65 e Å−3 |
3939 reflections | Δρmin = −0.35 e Å−3 |
227 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0015 (8) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.001 (15) |
Crystal data top
C11H23CoN5O3+·ClO4− | V = 1716.25 (17) Å3 |
Mr = 431.72 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 9.4009 (5) Å | µ = 1.20 mm−1 |
b = 13.3659 (8) Å | T = 293 K |
c = 13.6588 (8) Å | 0.30 × 0.25 × 0.23 mm |
Data collection top
Bruker SMART CCD area detector diffractometer | 3573 reflections with I > 2σ(I) |
10571 measured reflections | Rint = 0.044 |
3939 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.037 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.094 | Δρmax = 0.65 e Å−3 |
S = 1.05 | Δρmin = −0.35 e Å−3 |
3939 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
227 parameters | Absolute structure parameter: 0.001 (15) |
0 restraints | |
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 | 0.09692 (4) | 0.42381 (3) | 0.06786 (2) | 0.02530 (11) | |
Cl1 | −0.31468 (10) | 0.66230 (7) | 0.17022 (7) | 0.0512 (2) | |
C6 | 0.3642 (3) | 0.3419 (3) | 0.1201 (3) | 0.0427 (7) | |
H6A | 0.3665 | 0.3442 | 0.1911 | 0.051* | |
H6B | 0.4372 | 0.2959 | 0.0979 | 0.051* | |
C5 | 0.3898 (3) | 0.4439 (2) | 0.0788 (2) | 0.0408 (7) | |
H5A | 0.4729 | 0.4743 | 0.1087 | 0.049* | |
H5B | 0.4047 | 0.4404 | 0.0086 | 0.049* | |
C4 | 0.2487 (3) | 0.6035 (2) | 0.0569 (3) | 0.0463 (8) | |
H4A | 0.2714 | 0.6010 | −0.0124 | 0.056* | |
H4B | 0.3132 | 0.6500 | 0.0886 | 0.056* | |
C3 | 0.0955 (3) | 0.6358 (2) | 0.0719 (3) | 0.0466 (7) | |
H3A | 0.0810 | 0.6550 | 0.1397 | 0.056* | |
H3B | 0.0747 | 0.6932 | 0.0309 | 0.056* | |
C2 | −0.0562 (4) | 0.5532 (3) | −0.0545 (3) | 0.0511 (9) | |
H2A | −0.0817 | 0.6211 | −0.0722 | 0.061* | |
H2B | −0.1406 | 0.5118 | −0.0597 | 0.061* | |
C1 | 0.0573 (4) | 0.5148 (3) | −0.1226 (2) | 0.0511 (9) | |
H1A | 0.0154 | 0.4963 | −0.1849 | 0.061* | |
H1B | 0.1276 | 0.5666 | −0.1342 | 0.061* | |
C7 | −0.1465 (3) | 0.3202 (2) | 0.1131 (2) | 0.0340 (6) | |
C8 | −0.0770 (3) | 0.3377 (2) | 0.21145 (19) | 0.0316 (6) | |
H8A | −0.0317 | 0.2751 | 0.2321 | 0.038* | |
C9 | −0.1685 (3) | 0.3750 (3) | 0.2949 (2) | 0.0412 (7) | |
H9A | −0.2079 | 0.3199 | 0.3323 | 0.049* | |
H9B | −0.2455 | 0.4168 | 0.2713 | 0.049* | |
C10 | −0.0631 (3) | 0.4347 (3) | 0.3550 (2) | 0.0480 (9) | |
H10A | −0.0207 | 0.3937 | 0.4058 | 0.058* | |
H10B | −0.1085 | 0.4922 | 0.3850 | 0.058* | |
C11 | 0.0485 (3) | 0.4674 (3) | 0.2801 (2) | 0.0361 (7) | |
N4 | 0.2210 (3) | 0.30781 (18) | 0.08557 (18) | 0.0336 (5) | |
H4C | 0.1826 | 0.2658 | 0.1298 | 0.040* | |
H4D | 0.2300 | 0.2747 | 0.0285 | 0.040* | |
N3 | 0.2609 (3) | 0.50246 (19) | 0.10136 (18) | 0.0326 (5) | |
H3C | 0.2590 | 0.5110 | 0.1674 | 0.039* | |
N2 | −0.0025 (3) | 0.55078 (19) | 0.04602 (19) | 0.0377 (6) | |
H2C | −0.0785 | 0.5531 | 0.0873 | 0.045* | |
N1 | 0.1264 (2) | 0.42547 (19) | −0.07653 (16) | 0.0343 (5) | |
H1C | 0.2203 | 0.4264 | −0.0895 | 0.041* | |
H1D | 0.0897 | 0.3693 | −0.1027 | 0.041* | |
N5 | 0.0338 (2) | 0.41332 (19) | 0.20015 (16) | 0.0307 (5) | |
O1 | −0.0722 (2) | 0.34780 (16) | 0.03915 (13) | 0.0356 (5) | |
O2 | −0.2642 (2) | 0.2797 (2) | 0.10631 (18) | 0.0518 (6) | |
O3 | 0.1389 (3) | 0.5341 (2) | 0.29426 (17) | 0.0507 (6) | |
O4 | −0.2419 (10) | 0.6414 (4) | 0.2539 (5) | 0.213 (4) | |
O5 | −0.2278 (6) | 0.7426 (5) | 0.1454 (7) | 0.178 (3) | |
O6 | −0.4496 (5) | 0.6894 (5) | 0.1858 (5) | 0.185 (3) | |
O7 | −0.2997 (4) | 0.5756 (4) | 0.1138 (4) | 0.1223 (18) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.02347 (17) | 0.02985 (18) | 0.02259 (16) | −0.00162 (14) | 0.00177 (14) | −0.00275 (14) |
Cl1 | 0.0433 (4) | 0.0492 (5) | 0.0609 (5) | 0.0002 (4) | −0.0016 (4) | −0.0107 (4) |
C6 | 0.0327 (16) | 0.0486 (19) | 0.0468 (18) | 0.0102 (13) | −0.0043 (13) | −0.0042 (15) |
C5 | 0.0234 (13) | 0.0503 (18) | 0.0486 (17) | −0.0024 (12) | 0.0038 (13) | −0.0007 (14) |
C4 | 0.0420 (16) | 0.0360 (15) | 0.061 (2) | −0.0083 (12) | 0.0014 (17) | 0.0037 (15) |
C3 | 0.0502 (17) | 0.0336 (15) | 0.0560 (18) | 0.0048 (14) | −0.006 (2) | −0.0049 (14) |
C2 | 0.0504 (19) | 0.053 (2) | 0.050 (2) | 0.0138 (15) | −0.0136 (16) | 0.0032 (15) |
C1 | 0.058 (2) | 0.062 (2) | 0.0338 (16) | 0.0100 (17) | −0.0004 (15) | 0.0087 (16) |
C7 | 0.0326 (14) | 0.0363 (16) | 0.0332 (15) | −0.0070 (12) | 0.0042 (12) | −0.0083 (12) |
C8 | 0.0311 (14) | 0.0338 (13) | 0.0298 (13) | −0.0018 (12) | 0.0037 (11) | −0.0022 (11) |
C9 | 0.0351 (16) | 0.056 (2) | 0.0322 (15) | −0.0043 (14) | 0.0073 (13) | −0.0015 (14) |
C10 | 0.0417 (17) | 0.075 (2) | 0.0277 (14) | −0.0068 (17) | 0.0081 (12) | −0.0120 (15) |
C11 | 0.0282 (14) | 0.0516 (17) | 0.0285 (14) | −0.0023 (13) | −0.0028 (11) | −0.0050 (13) |
N4 | 0.0375 (13) | 0.0336 (12) | 0.0298 (13) | 0.0013 (10) | 0.0044 (10) | −0.0013 (10) |
N3 | 0.0268 (11) | 0.0369 (13) | 0.0340 (12) | −0.0052 (10) | 0.0007 (9) | 0.0005 (10) |
N2 | 0.0291 (12) | 0.0438 (14) | 0.0401 (15) | 0.0074 (10) | 0.0019 (10) | 0.0002 (11) |
N1 | 0.0335 (11) | 0.0416 (12) | 0.0279 (11) | −0.0043 (10) | 0.0030 (9) | −0.0019 (11) |
N5 | 0.0270 (11) | 0.0410 (13) | 0.0242 (10) | −0.0043 (10) | 0.0041 (9) | −0.0076 (10) |
O1 | 0.0319 (11) | 0.0480 (12) | 0.0269 (9) | −0.0126 (9) | 0.0007 (8) | −0.0073 (8) |
O2 | 0.0449 (13) | 0.0629 (16) | 0.0475 (13) | −0.0269 (12) | 0.0081 (10) | −0.0116 (12) |
O3 | 0.0468 (14) | 0.0690 (16) | 0.0363 (12) | −0.0188 (12) | −0.0006 (10) | −0.0160 (11) |
O4 | 0.344 (11) | 0.123 (5) | 0.171 (6) | 0.072 (6) | −0.132 (7) | −0.026 (4) |
O5 | 0.140 (5) | 0.114 (4) | 0.281 (9) | −0.044 (4) | 0.023 (5) | 0.030 (4) |
O6 | 0.056 (2) | 0.206 (6) | 0.292 (8) | 0.018 (3) | −0.004 (3) | −0.153 (6) |
O7 | 0.068 (2) | 0.136 (4) | 0.162 (4) | −0.032 (2) | 0.038 (3) | −0.096 (3) |
Geometric parameters (Å, º) top
Co1—N5 | 1.907 (2) | C4—C3 | 1.517 (4) |
Co1—N3 | 1.921 (2) | C3—N2 | 1.505 (4) |
Co1—O1 | 1.9273 (19) | C2—N2 | 1.463 (4) |
Co1—N4 | 1.955 (2) | C2—C1 | 1.505 (5) |
Co1—N2 | 1.960 (2) | C1—N1 | 1.498 (4) |
Co1—N1 | 1.992 (2) | C7—O2 | 1.236 (3) |
Cl1—O6 | 1.336 (4) | C7—O1 | 1.282 (3) |
Cl1—O4 | 1.361 (6) | C7—C8 | 1.512 (4) |
Cl1—O5 | 1.391 (5) | C8—N5 | 1.460 (4) |
Cl1—O7 | 1.399 (4) | C8—C9 | 1.512 (4) |
C6—C5 | 1.496 (5) | C9—C10 | 1.515 (5) |
C6—N4 | 1.497 (4) | C10—C11 | 1.529 (4) |
C5—N3 | 1.476 (4) | C11—O3 | 1.247 (4) |
C4—N3 | 1.486 (4) | C11—N5 | 1.317 (4) |
| | | |
N5—Co1—N3 | 93.68 (10) | N2—C2—C1 | 109.2 (3) |
N5—Co1—O1 | 84.11 (9) | N1—C1—C2 | 108.6 (3) |
N3—Co1—O1 | 177.36 (10) | O2—C7—O1 | 123.7 (3) |
N5—Co1—N4 | 90.58 (11) | O2—C7—C8 | 121.4 (3) |
N3—Co1—N4 | 85.75 (11) | O1—C7—C8 | 114.9 (2) |
O1—Co1—N4 | 95.70 (10) | N5—C8—C7 | 108.7 (2) |
N5—Co1—N2 | 93.41 (11) | N5—C8—C9 | 104.9 (2) |
N3—Co1—N2 | 86.85 (11) | C7—C8—C9 | 118.4 (3) |
O1—Co1—N2 | 91.84 (10) | C8—C9—C10 | 102.1 (2) |
N4—Co1—N2 | 171.80 (10) | C9—C10—C11 | 103.7 (2) |
N5—Co1—N1 | 169.22 (10) | O3—C11—N5 | 126.4 (3) |
N3—Co1—N1 | 96.78 (10) | O3—C11—C10 | 124.6 (3) |
O1—Co1—N1 | 85.36 (9) | N5—C11—C10 | 109.0 (3) |
N4—Co1—N1 | 92.77 (10) | C6—N4—Co1 | 109.51 (18) |
N2—Co1—N1 | 84.60 (11) | C5—N3—C4 | 117.3 (2) |
O6—Cl1—O4 | 113.5 (5) | C5—N3—Co1 | 108.63 (18) |
O6—Cl1—O5 | 112.8 (4) | C4—N3—Co1 | 109.79 (19) |
O4—Cl1—O5 | 93.9 (5) | C2—N2—C3 | 114.6 (3) |
O6—Cl1—O7 | 114.1 (3) | C2—N2—Co1 | 109.0 (2) |
O4—Cl1—O7 | 104.0 (4) | C3—N2—Co1 | 109.01 (17) |
O5—Cl1—O7 | 116.5 (4) | C1—N1—Co1 | 111.38 (19) |
C5—C6—N4 | 107.7 (2) | C11—N5—C8 | 111.6 (2) |
N3—C5—C6 | 105.8 (2) | C11—N5—Co1 | 135.4 (2) |
N3—C4—C3 | 106.0 (3) | C8—N5—Co1 | 111.92 (17) |
N2—C3—C4 | 109.6 (2) | C7—O1—Co1 | 116.14 (18) |
| | | |
N4—C6—C5—N3 | 49.6 (3) | N4—Co1—N2—C2 | 96.9 (8) |
N3—C4—C3—N2 | −45.4 (4) | N1—Co1—N2—C2 | 25.3 (2) |
N2—C2—C1—N1 | 42.0 (4) | N5—Co1—N2—C3 | 90.2 (2) |
O2—C7—C8—N5 | −161.7 (3) | N3—Co1—N2—C3 | −3.3 (2) |
O1—C7—C8—N5 | 20.2 (4) | O1—Co1—N2—C3 | 174.4 (2) |
O2—C7—C8—C9 | −42.2 (4) | N4—Co1—N2—C3 | −28.8 (9) |
O1—C7—C8—C9 | 139.7 (3) | N1—Co1—N2—C3 | −100.4 (2) |
N5—C8—C9—C10 | −28.7 (3) | C2—C1—N1—Co1 | −21.1 (3) |
C7—C8—C9—C10 | −150.1 (3) | N5—Co1—N1—C1 | 78.0 (7) |
C8—C9—C10—C11 | 26.5 (4) | N3—Co1—N1—C1 | −88.1 (2) |
C9—C10—C11—O3 | 165.1 (3) | O1—Co1—N1—C1 | 90.4 (2) |
C9—C10—C11—N5 | −15.6 (4) | N4—Co1—N1—C1 | −174.1 (2) |
C5—C6—N4—Co1 | −30.4 (3) | N2—Co1—N1—C1 | −1.9 (2) |
N5—Co1—N4—C6 | −90.0 (2) | O3—C11—N5—C8 | 176.2 (3) |
N3—Co1—N4—C6 | 3.6 (2) | C10—C11—N5—C8 | −3.1 (4) |
O1—Co1—N4—C6 | −174.14 (18) | O3—C11—N5—Co1 | −17.1 (6) |
N2—Co1—N4—C6 | 29.2 (8) | C10—C11—N5—Co1 | 163.6 (3) |
N1—Co1—N4—C6 | 100.2 (2) | C7—C8—N5—C11 | 148.2 (3) |
C6—C5—N3—C4 | −171.9 (3) | C9—C8—N5—C11 | 20.7 (3) |
C6—C5—N3—Co1 | −46.7 (3) | C7—C8—N5—Co1 | −21.7 (3) |
C3—C4—N3—C5 | 167.1 (3) | C9—C8—N5—Co1 | −149.3 (2) |
C3—C4—N3—Co1 | 42.5 (3) | N3—Co1—N5—C11 | 26.3 (3) |
N5—Co1—N3—C5 | 114.7 (2) | O1—Co1—N5—C11 | −152.3 (3) |
O1—Co1—N3—C5 | 148 (2) | N4—Co1—N5—C11 | 112.0 (3) |
N4—Co1—N3—C5 | 24.35 (19) | N2—Co1—N5—C11 | −60.8 (3) |
N2—Co1—N3—C5 | −152.1 (2) | N1—Co1—N5—C11 | −139.8 (5) |
N1—Co1—N3—C5 | −67.9 (2) | N3—Co1—N5—C8 | −167.1 (2) |
N5—Co1—N3—C4 | −115.8 (2) | O1—Co1—N5—C8 | 14.36 (19) |
O1—Co1—N3—C4 | −83 (2) | N4—Co1—N5—C8 | −81.3 (2) |
N4—Co1—N3—C4 | 153.9 (2) | N2—Co1—N5—C8 | 105.9 (2) |
N2—Co1—N3—C4 | −22.6 (2) | N1—Co1—N5—C8 | 26.8 (7) |
N1—Co1—N3—C4 | 61.6 (2) | O2—C7—O1—Co1 | 172.7 (3) |
C1—C2—N2—C3 | 78.7 (4) | C8—C7—O1—Co1 | −9.2 (3) |
C1—C2—N2—Co1 | −43.7 (3) | N5—Co1—O1—C7 | −2.9 (2) |
C4—C3—N2—C2 | −94.5 (3) | N3—Co1—O1—C7 | −36 (2) |
C4—C3—N2—Co1 | 28.0 (3) | N4—Co1—O1—C7 | 87.1 (2) |
N5—Co1—N2—C2 | −144.1 (2) | N2—Co1—O1—C7 | −96.1 (2) |
N3—Co1—N2—C2 | 122.4 (2) | N1—Co1—O1—C7 | 179.5 (2) |
O1—Co1—N2—C2 | −59.8 (2) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H4C···O4i | 0.90 | 2.37 | 3.129 (7) | 143 |
N4—H4D···O2ii | 0.90 | 1.98 | 2.873 (3) | 171 |
N4—H4D···O1ii | 0.90 | 2.64 | 3.318 (3) | 132 |
N3—H3C···O3 | 0.91 | 2.09 | 2.904 (3) | 148 |
N2—H2C···O7 | 0.91 | 2.13 | 2.962 (4) | 151 |
N1—H1D···O2ii | 0.90 | 2.42 | 2.957 (4) | 119 |
N1—H1C···O3iii | 0.90 | 2.13 | 2.876 (3) | 139 |
Symmetry codes: (i) −x, y−1/2, −z+1/2; (ii) x+1/2, −y+1/2, −z; (iii) −x+1/2, −y+1, z−1/2. |
(4) (
L-isoleucinato)-(triethylenetetramine)-cobalt(III) diiodide monohydrate
top
Crystal data top
C12H30CoN5O22+·2(I−)·H2O | F(000) = 1180 |
Mr = 606.15 | Dx = 1.859 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.053 (2) Å | µ = 3.66 mm−1 |
b = 11.540 (2) Å | T = 293 K |
c = 18.664 (4) Å | Block, yellow |
V = 2165.2 (7) Å3 | 0.30 × 0.15 × 0.10 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD area detector diffractometer | 4240 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.022 |
Graphite monochromator | θmax = 27.5°, θmin = 2.1° |
ϕ and ω scans | h = −13→5 |
7861 measured reflections | k = −13→15 |
4811 independent reflections | l = −24→7 |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.032 | w = 1/[σ2(Fo2) + (0.0437P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.078 | (Δ/σ)max = 0.021 |
S = 1.02 | Δρmax = 1.16 e Å−3 |
4811 reflections | Δρmin = −0.77 e Å−3 |
317 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0022 (2) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.02 (2) |
Crystal data top
C12H30CoN5O22+·2(I−)·H2O | V = 2165.2 (7) Å3 |
Mr = 606.15 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 10.053 (2) Å | µ = 3.66 mm−1 |
b = 11.540 (2) Å | T = 293 K |
c = 18.664 (4) Å | 0.30 × 0.15 × 0.10 mm |
Data collection top
Bruker SMART CCD area detector diffractometer | 4240 reflections with I > 2σ(I) |
7861 measured reflections | Rint = 0.022 |
4811 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.032 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.078 | Δρmax = 1.16 e Å−3 |
S = 1.02 | Δρmin = −0.77 e Å−3 |
4811 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
317 parameters | Absolute structure parameter: 0.02 (2) |
0 restraints | |
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 | |
Co | 0.37838 (5) | 0.49364 (5) | 0.15239 (3) | 0.02180 (12) | |
I1 | 0.81567 (4) | 0.72191 (3) | 0.160537 (19) | 0.05131 (12) | |
I2 | 0.17425 (4) | 0.70985 (3) | 0.439873 (17) | 0.05258 (12) | |
C1 | 0.1672 (6) | 0.3324 (5) | 0.1279 (3) | 0.0475 (13) | |
H4 | 0.132 (7) | 0.324 (7) | 0.081 (4) | 0.08 (2)* | |
H3 | 0.132 (8) | 0.251 (7) | 0.149 (4) | 0.09 (2)* | |
C2 | 0.1113 (6) | 0.4310 (5) | 0.1714 (3) | 0.0422 (12) | |
H6 | 0.122 (6) | 0.413 (5) | 0.226 (3) | 0.059 (18)* | |
H5 | 0.017 (6) | 0.459 (4) | 0.160 (3) | 0.037 (14)* | |
C3 | 0.1521 (6) | 0.5937 (6) | 0.0862 (3) | 0.0432 (13) | |
H8 | 0.129 (5) | 0.542 (5) | 0.065 (3) | 0.026 (14)* | |
H9 | 0.072 (7) | 0.642 (6) | 0.095 (3) | 0.053 (17)* | |
C4 | 0.2723 (5) | 0.6436 (5) | 0.0517 (3) | 0.0351 (11) | |
H11 | 0.296 (4) | 0.707 (4) | 0.073 (2) | 0.016 (10)* | |
H10 | 0.259 (5) | 0.674 (4) | 0.003 (3) | 0.034 (13)* | |
C5 | 0.5133 (5) | 0.5837 (5) | 0.0336 (2) | 0.0368 (11) | |
H14 | 0.544 (5) | 0.664 (4) | 0.065 (2) | 0.027 (12)* | |
H13 | 0.524 (5) | 0.602 (5) | −0.020 (3) | 0.038 (14)* | |
C6 | 0.5988 (6) | 0.4847 (5) | 0.0570 (3) | 0.0399 (11) | |
H16 | 0.697 (6) | 0.487 (5) | 0.053 (3) | 0.046 (15)* | |
H15 | 0.573 (7) | 0.412 (6) | 0.031 (4) | 0.07 (2)* | |
C7 | 0.4426 (4) | 0.6553 (4) | 0.2538 (2) | 0.0248 (9) | |
C8 | 0.4159 (5) | 0.5495 (4) | 0.3007 (2) | 0.0262 (9) | |
H19 | 0.322 (6) | 0.574 (4) | 0.328 (2) | 0.033 (12)* | |
C9 | 0.5279 (5) | 0.5289 (4) | 0.3555 (2) | 0.0349 (11) | |
H22 | 0.533 (4) | 0.607 (3) | 0.3783 (19) | 0.005 (9)* | |
C10 | 0.4857 (8) | 0.4327 (6) | 0.4069 (3) | 0.0528 (16) | |
H25 | 0.388 (9) | 0.432 (7) | 0.421 (4) | 0.09 (3)* | |
H24 | 0.473 (5) | 0.353 (5) | 0.378 (3) | 0.031 (13)* | |
H23 | 0.540 (9) | 0.425 (7) | 0.443 (4) | 0.08 (2)* | |
C11 | 0.6621 (6) | 0.5066 (6) | 0.3198 (3) | 0.0476 (13) | |
H27 | 0.663 (6) | 0.444 (5) | 0.293 (3) | 0.052 (17)* | |
H26 | 0.689 (6) | 0.587 (5) | 0.286 (3) | 0.051 (16)* | |
C12 | 0.7774 (7) | 0.4960 (7) | 0.3728 (4) | 0.0687 (19) | |
H30 | 0.8585 | 0.4823 | 0.3470 | 0.103* | |
H29 | 0.7609 | 0.4326 | 0.4049 | 0.103* | |
H28 | 0.7851 | 0.5666 | 0.3998 | 0.103* | |
N1 | 0.3132 (4) | 0.3389 (3) | 0.1284 (2) | 0.0294 (8) | |
H2 | 0.349 (5) | 0.321 (4) | 0.092 (3) | 0.031 (14)* | |
H1 | 0.344 (6) | 0.275 (5) | 0.159 (3) | 0.046 (15)* | |
N2 | 0.1910 (4) | 0.5375 (3) | 0.15546 (19) | 0.0308 (8) | |
H7 | 0.170 (5) | 0.600 (4) | 0.188 (2) | 0.022 (11)* | |
N3 | 0.3742 (4) | 0.5513 (3) | 0.05455 (18) | 0.0281 (8) | |
H12 | 0.344 (4) | 0.488 (4) | 0.028 (2) | 0.012 (9)* | |
N4 | 0.5678 (4) | 0.4598 (4) | 0.1334 (2) | 0.0297 (9) | |
H18 | 0.590 (6) | 0.392 (5) | 0.139 (3) | 0.045 (17)* | |
H17 | 0.620 (5) | 0.509 (4) | 0.152 (2) | 0.023 (11)* | |
N5 | 0.3896 (5) | 0.4486 (3) | 0.25377 (18) | 0.0256 (8) | |
H21 | 0.310 (6) | 0.412 (5) | 0.267 (3) | 0.044 (15)* | |
H20 | 0.451 (6) | 0.402 (5) | 0.255 (3) | 0.036 (16)* | |
O1 | 0.4289 (3) | 0.6428 (3) | 0.18546 (15) | 0.0275 (6) | |
OW1 | 0.1273 (6) | 0.7210 (6) | 0.2522 (3) | 0.103 (2) | |
O2 | 0.4702 (4) | 0.7479 (3) | 0.28221 (17) | 0.0349 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co | 0.0234 (3) | 0.0203 (2) | 0.0216 (2) | 0.0002 (2) | −0.0011 (2) | −0.0002 (2) |
I1 | 0.03795 (19) | 0.0610 (2) | 0.0550 (2) | 0.01032 (19) | 0.00159 (16) | −0.01078 (17) |
I2 | 0.0564 (2) | 0.0619 (2) | 0.03946 (17) | 0.0038 (2) | 0.00252 (16) | 0.01354 (16) |
C1 | 0.043 (3) | 0.048 (3) | 0.052 (3) | −0.015 (3) | −0.003 (3) | −0.006 (2) |
C2 | 0.027 (3) | 0.052 (3) | 0.048 (3) | −0.001 (2) | 0.001 (2) | 0.003 (2) |
C3 | 0.037 (3) | 0.057 (4) | 0.036 (2) | 0.007 (3) | −0.007 (2) | −0.002 (2) |
C4 | 0.041 (3) | 0.033 (3) | 0.031 (2) | 0.011 (2) | −0.006 (2) | 0.003 (2) |
C5 | 0.039 (3) | 0.043 (3) | 0.027 (2) | 0.001 (2) | 0.007 (2) | 0.008 (2) |
C6 | 0.035 (3) | 0.050 (3) | 0.035 (2) | 0.009 (2) | 0.007 (2) | −0.003 (2) |
C7 | 0.024 (2) | 0.022 (2) | 0.028 (2) | 0.0036 (18) | −0.0017 (17) | −0.0016 (16) |
C8 | 0.032 (3) | 0.021 (2) | 0.026 (2) | 0.0009 (19) | −0.0002 (17) | −0.0018 (16) |
C9 | 0.049 (3) | 0.028 (2) | 0.028 (2) | −0.009 (2) | −0.010 (2) | −0.0015 (18) |
C10 | 0.072 (5) | 0.055 (4) | 0.031 (3) | −0.016 (3) | −0.009 (3) | 0.016 (3) |
C11 | 0.038 (3) | 0.058 (3) | 0.047 (3) | 0.000 (3) | −0.013 (2) | 0.002 (3) |
C12 | 0.046 (4) | 0.075 (4) | 0.085 (4) | −0.011 (4) | −0.030 (3) | 0.016 (4) |
N1 | 0.034 (2) | 0.0245 (18) | 0.0298 (18) | −0.0010 (18) | −0.0036 (18) | −0.0022 (14) |
N2 | 0.0221 (19) | 0.038 (2) | 0.0318 (17) | −0.0008 (16) | 0.0025 (17) | −0.0014 (16) |
N3 | 0.032 (2) | 0.0287 (18) | 0.0239 (16) | −0.0034 (17) | −0.0033 (15) | 0.0016 (15) |
N4 | 0.029 (2) | 0.028 (2) | 0.0326 (19) | 0.0023 (18) | 0.0004 (16) | 0.0003 (15) |
N5 | 0.031 (2) | 0.0204 (17) | 0.0255 (17) | −0.0064 (18) | 0.0020 (16) | −0.0002 (14) |
O1 | 0.0343 (18) | 0.0236 (15) | 0.0247 (14) | −0.0012 (14) | 0.0014 (12) | 0.0009 (11) |
OW1 | 0.079 (4) | 0.155 (6) | 0.076 (3) | 0.060 (4) | −0.022 (3) | −0.049 (4) |
O2 | 0.048 (2) | 0.0198 (15) | 0.0372 (16) | −0.0039 (14) | −0.0027 (15) | −0.0042 (12) |
Geometric parameters (Å, º) top
Co—O1 | 1.898 (3) | C7—O2 | 1.225 (5) |
Co—N3 | 1.944 (3) | C7—O1 | 1.291 (5) |
Co—N2 | 1.951 (4) | C7—C8 | 1.525 (6) |
Co—N1 | 1.954 (4) | C8—N5 | 1.481 (5) |
Co—N5 | 1.966 (4) | C8—C9 | 1.540 (6) |
Co—N4 | 1.976 (4) | C8—H19 | 1.11 (5) |
C1—N1 | 1.470 (7) | C9—C10 | 1.526 (7) |
C1—C2 | 1.507 (8) | C9—C11 | 1.527 (8) |
C1—H4 | 0.96 (7) | C9—H22 | 1.00 (4) |
C1—H3 | 1.08 (8) | C10—H25 | 1.02 (9) |
C2—N2 | 1.498 (7) | C10—H24 | 1.08 (5) |
C2—H6 | 1.05 (6) | C10—H23 | 0.86 (9) |
C2—H5 | 1.03 (6) | C11—C12 | 1.529 (8) |
C3—C4 | 1.484 (8) | C11—H27 | 0.88 (6) |
C3—N2 | 1.498 (6) | C11—H26 | 1.15 (6) |
C3—H8 | 0.75 (5) | C12—H30 | 0.9600 |
C3—H9 | 0.99 (7) | C12—H29 | 0.9600 |
C4—N3 | 1.479 (6) | C12—H28 | 0.9600 |
C4—H11 | 0.87 (5) | N1—H2 | 0.79 (5) |
C4—H10 | 0.98 (5) | N1—H1 | 0.99 (6) |
C5—C6 | 1.495 (8) | N2—H7 | 0.96 (4) |
C5—N3 | 1.499 (6) | N3—H12 | 0.93 (4) |
C5—H14 | 1.14 (5) | N4—H18 | 0.82 (6) |
C5—H13 | 1.02 (5) | N4—H17 | 0.84 (5) |
C6—N4 | 1.486 (6) | N5—H21 | 0.93 (6) |
C6—H16 | 0.99 (6) | N5—H20 | 0.82 (6) |
C6—H15 | 1.01 (7) | | |
| | | |
O1—Co—N3 | 90.05 (14) | C7—C8—H19 | 102 (2) |
O1—Co—N2 | 90.76 (15) | C9—C8—H19 | 111 (2) |
N3—Co—N2 | 85.29 (16) | C10—C9—C11 | 113.4 (5) |
O1—Co—N1 | 173.26 (16) | C10—C9—C8 | 109.1 (5) |
N3—Co—N1 | 95.17 (16) | C11—C9—C8 | 112.4 (4) |
N2—Co—N1 | 85.44 (17) | C10—C9—H22 | 114 (2) |
O1—Co—N5 | 84.94 (13) | C11—C9—H22 | 107 (2) |
N3—Co—N5 | 174.93 (16) | C8—C9—H22 | 100 (2) |
N2—Co—N5 | 95.50 (17) | C9—C10—H25 | 115 (5) |
N1—Co—N5 | 89.88 (16) | C9—C10—H24 | 110 (3) |
O1—Co—N4 | 88.84 (17) | H25—C10—H24 | 91 (5) |
N3—Co—N4 | 85.39 (16) | C9—C10—H23 | 113 (5) |
N2—Co—N4 | 170.67 (16) | H25—C10—H23 | 114 (7) |
N1—Co—N4 | 95.81 (19) | H24—C10—H23 | 112 (6) |
N5—Co—N4 | 93.75 (18) | C9—C11—C12 | 113.6 (5) |
N1—C1—C2 | 109.3 (4) | C9—C11—H27 | 114 (4) |
N1—C1—H4 | 112 (4) | C12—C11—H27 | 107 (4) |
C2—C1—H4 | 116 (5) | C9—C11—H26 | 108 (3) |
N1—C1—H3 | 112 (4) | C12—C11—H26 | 104 (3) |
C2—C1—H3 | 110 (4) | H27—C11—H26 | 110 (5) |
H4—C1—H3 | 97 (6) | C11—C12—H30 | 109.5 |
N2—C2—C1 | 108.3 (4) | C11—C12—H29 | 109.5 |
N2—C2—H6 | 107 (3) | H30—C12—H29 | 109.5 |
C1—C2—H6 | 110 (3) | C11—C12—H28 | 109.5 |
N2—C2—H5 | 102 (3) | H30—C12—H28 | 109.5 |
C1—C2—H5 | 118 (3) | H29—C12—H28 | 109.5 |
H6—C2—H5 | 111 (5) | C1—N1—Co | 112.5 (3) |
C4—C3—N2 | 109.3 (4) | C1—N1—H2 | 116 (4) |
C4—C3—H8 | 110 (4) | Co—N1—H2 | 106 (4) |
N2—C3—H8 | 101 (4) | C1—N1—H1 | 106 (3) |
C4—C3—H9 | 121 (4) | Co—N1—H1 | 116 (3) |
N2—C3—H9 | 108 (4) | H2—N1—H1 | 99 (5) |
H8—C3—H9 | 106 (6) | C2—N2—C3 | 112.8 (4) |
N3—C4—C3 | 105.6 (4) | C2—N2—Co | 108.0 (3) |
N3—C4—H11 | 114 (3) | C3—N2—Co | 109.8 (3) |
C3—C4—H11 | 111 (3) | C2—N2—H7 | 112 (3) |
N3—C4—H10 | 112 (3) | C3—N2—H7 | 99 (2) |
C3—C4—H10 | 115 (3) | Co—N2—H7 | 115 (3) |
H11—C4—H10 | 99 (4) | C4—N3—C5 | 117.2 (4) |
C6—C5—N3 | 105.6 (4) | C4—N3—Co | 107.2 (3) |
C6—C5—H14 | 108 (2) | C5—N3—Co | 108.1 (3) |
N3—C5—H14 | 109 (2) | C4—N3—H12 | 109 (3) |
C6—C5—H13 | 112 (3) | C5—N3—H12 | 111 (3) |
N3—C5—H13 | 114 (3) | Co—N3—H12 | 104 (2) |
H14—C5—H13 | 108 (4) | C6—N4—Co | 109.6 (3) |
N4—C6—C5 | 107.9 (4) | C6—N4—H18 | 105 (4) |
N4—C6—H16 | 107 (3) | Co—N4—H18 | 115 (4) |
C5—C6—H16 | 122 (3) | C6—N4—H17 | 98 (3) |
N4—C6—H15 | 104 (4) | Co—N4—H17 | 113 (3) |
C5—C6—H15 | 111 (4) | H18—N4—H17 | 115 (5) |
H16—C6—H15 | 104 (5) | C8—N5—Co | 111.8 (3) |
O2—C7—O1 | 123.3 (4) | C8—N5—H21 | 110 (3) |
O2—C7—C8 | 119.4 (4) | Co—N5—H21 | 109 (3) |
O1—C7—C8 | 117.3 (4) | C8—N5—H20 | 111 (4) |
N5—C8—C7 | 108.8 (3) | Co—N5—H20 | 104 (4) |
N5—C8—C9 | 113.7 (4) | H21—N5—H20 | 110 (5) |
C7—C8—C9 | 112.1 (4) | C7—O1—Co | 116.8 (3) |
N5—C8—H19 | 108 (3) | | |
| | | |
N1—C1—C2—N2 | 40.7 (6) | C3—C4—N3—Co | −49.1 (4) |
N2—C3—C4—N3 | 47.7 (6) | C6—C5—N3—C4 | 167.5 (4) |
N3—C5—C6—N4 | −51.1 (5) | C6—C5—N3—Co | 46.4 (4) |
O2—C7—C8—N5 | −178.1 (4) | O1—Co—N3—C4 | −61.5 (3) |
O1—C7—C8—N5 | 4.8 (6) | N2—Co—N3—C4 | 29.3 (3) |
O2—C7—C8—C9 | −51.4 (6) | N1—Co—N3—C4 | 114.3 (3) |
O1—C7—C8—C9 | 131.5 (4) | N5—Co—N3—C4 | −70 (2) |
N5—C8—C9—C10 | −63.8 (5) | N4—Co—N3—C4 | −150.3 (3) |
C7—C8—C9—C10 | 172.3 (4) | O1—Co—N3—C5 | 65.7 (3) |
N5—C8—C9—C11 | 62.8 (5) | N2—Co—N3—C5 | 156.4 (3) |
C7—C8—C9—C11 | −61.1 (5) | N1—Co—N3—C5 | −118.6 (3) |
C10—C9—C11—C12 | −60.6 (7) | N5—Co—N3—C5 | 57 (2) |
C8—C9—C11—C12 | 175.1 (5) | N4—Co—N3—C5 | −23.2 (3) |
C2—C1—N1—Co | −20.7 (5) | C5—C6—N4—Co | 32.5 (5) |
O1—Co—N1—C1 | 53.4 (15) | O1—Co—N4—C6 | −95.3 (4) |
N3—Co—N1—C1 | −87.3 (4) | N3—Co—N4—C6 | −5.2 (4) |
N2—Co—N1—C1 | −2.4 (4) | N2—Co—N4—C6 | −7.7 (13) |
N5—Co—N1—C1 | 93.1 (4) | N1—Co—N4—C6 | 89.6 (4) |
N4—Co—N1—C1 | −173.1 (3) | N5—Co—N4—C6 | 179.8 (3) |
C1—C2—N2—C3 | 79.4 (5) | C7—C8—N5—Co | −6.7 (5) |
C1—C2—N2—Co | −42.2 (5) | C9—C8—N5—Co | −132.4 (3) |
C4—C3—N2—C2 | −144.9 (5) | O1—Co—N5—C8 | 5.5 (3) |
C4—C3—N2—Co | −24.4 (6) | N3—Co—N5—C8 | 14 (2) |
O1—Co—N2—C2 | −149.5 (3) | N2—Co—N5—C8 | −84.7 (3) |
N3—Co—N2—C2 | 120.5 (3) | N1—Co—N5—C8 | −170.2 (3) |
N1—Co—N2—C2 | 24.9 (3) | N4—Co—N5—C8 | 94.0 (3) |
N5—Co—N2—C2 | −64.5 (3) | O2—C7—O1—Co | −177.4 (4) |
N4—Co—N2—C2 | 123.0 (11) | C8—C7—O1—Co | −0.4 (5) |
O1—Co—N2—C3 | 87.2 (4) | N3—Co—O1—C7 | 177.8 (3) |
N3—Co—N2—C3 | −2.8 (4) | N2—Co—O1—C7 | 92.5 (3) |
N1—Co—N2—C3 | −98.4 (4) | N1—Co—O1—C7 | 36.9 (15) |
N5—Co—N2—C3 | 172.1 (4) | N5—Co—O1—C7 | −3.0 (3) |
N4—Co—N2—C3 | −0.3 (13) | N4—Co—O1—C7 | −96.8 (3) |
C3—C4—N3—C5 | −170.7 (4) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H18···O2i | 0.82 (6) | 2.30 (6) | 2.934 (5) | 134 (5) |
N2—H7···OW1 | 0.96 (4) | 1.89 (5) | 2.856 (6) | 179 (4) |
N5—H21···I1i | 0.93 (6) | 2.87 (6) | 3.695 (4) | 148 (4) |
N4—H17···I1 | 0.84 (5) | 3.16 (6) | 3.951 (5) | 158 (4) |
N3—H12···I2ii | 0.93 (4) | 2.82 (4) | 3.728 (4) | 165 (3) |
N1—H2···I2ii | 0.79 (5) | 2.87 (5) | 3.565 (4) | 147 (5) |
N1—H1···O2i | 0.99 (6) | 2.18 (6) | 2.937 (5) | 132 (4) |
N5—H20···O2i | 0.82 (6) | 2.07 (6) | 2.793 (5) | 147 (5) |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x+1/2, −y+1, z−1/2. |
(5) (
L-isoleucinato)-(triethylenetetramine)-cobalt(III) diperchlorate
dihydrate
top
Crystal data top
C12H30CoN5O22+·2(ClO4−)·2(H2O) | F(000) = 1192 |
Mr = 570.27 | Dx = 1.631 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.5333 (11) Å | µ = 1.04 mm−1 |
b = 13.3726 (14) Å | T = 293 K |
c = 15.0622 (15) Å | Block, yellow |
V = 2323.0 (4) Å3 | 0.35 × 0.30 × 0.28 mm |
Z = 4 | |
Data collection top
Buker SMART CCD area detector diffractometer | 3537 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.032 |
Graphite monochromator | θmax = 27.0°, θmin = 2.0° |
ϕ and ω scans | h = −13→13 |
8345 measured reflections | k = −17→7 |
4922 independent reflections | l = −19→6 |
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)] = 0.041 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.085 | w = 1/[σ2(Fo2) + (0.0367P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.90 | (Δ/σ)max < 0.001 |
4922 reflections | Δρmax = 0.59 e Å−3 |
293 parameters | Δρmin = −0.32 e Å−3 |
0 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.007 (17) |
Crystal data top
C12H30CoN5O22+·2(ClO4−)·2(H2O) | V = 2323.0 (4) Å3 |
Mr = 570.27 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 11.5333 (11) Å | µ = 1.04 mm−1 |
b = 13.3726 (14) Å | T = 293 K |
c = 15.0622 (15) Å | 0.35 × 0.30 × 0.28 mm |
Data collection top
Buker SMART CCD area detector diffractometer | 3537 reflections with I > 2σ(I) |
8345 measured reflections | Rint = 0.032 |
4922 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.041 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.085 | Δρmax = 0.59 e Å−3 |
S = 0.90 | Δρmin = −0.32 e Å−3 |
4922 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
293 parameters | Absolute structure parameter: −0.007 (17) |
0 restraints | |
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 | |
Co | 0.04919 (4) | 0.58677 (4) | 0.03034 (3) | 0.02426 (12) | |
Cl1 | 0.79559 (11) | 0.70122 (8) | 0.27852 (7) | 0.0462 (3) | |
Cl2 | 0.33328 (11) | 0.74231 (8) | 0.25777 (7) | 0.0463 (3) | |
C1 | 0.1916 (4) | 0.4669 (3) | 0.1393 (3) | 0.0410 (11) | |
H1A | 0.2656 | 0.4655 | 0.1700 | 0.049* | |
H1B | 0.1713 | 0.3989 | 0.1231 | 0.049* | |
C2 | 0.0997 (4) | 0.5102 (3) | 0.1993 (3) | 0.0398 (11) | |
H2A | 0.0805 | 0.4632 | 0.2460 | 0.048* | |
H2B | 0.1273 | 0.5715 | 0.2264 | 0.048* | |
C3 | −0.0757 (4) | 0.4395 (3) | 0.1284 (3) | 0.0410 (12) | |
H3A | −0.1430 | 0.4407 | 0.1670 | 0.049* | |
H3B | −0.0309 | 0.3801 | 0.1420 | 0.049* | |
C4 | −0.1142 (4) | 0.4371 (3) | 0.0322 (3) | 0.0416 (11) | |
H4A | −0.1416 | 0.3709 | 0.0163 | 0.050* | |
H4B | −0.1761 | 0.4848 | 0.0221 | 0.050* | |
C5 | −0.0289 (4) | 0.4796 (3) | −0.1167 (3) | 0.0391 (11) | |
H5A | −0.0981 | 0.5191 | −0.1269 | 0.047* | |
H5B | −0.0371 | 0.4160 | −0.1470 | 0.047* | |
C6 | 0.0767 (4) | 0.5341 (3) | −0.1491 (3) | 0.0388 (11) | |
H6A | 0.1441 | 0.4908 | −0.1462 | 0.047* | |
H6B | 0.0659 | 0.5549 | −0.2103 | 0.047* | |
C7 | −0.1051 (3) | 0.7415 (3) | 0.0327 (3) | 0.0253 (8) | |
C8 | −0.0039 (3) | 0.7898 (3) | 0.0778 (3) | 0.0255 (8) | |
H8A | −0.0262 | 0.7996 | 0.1400 | 0.031* | |
C9 | 0.0263 (3) | 0.8928 (2) | 0.0408 (3) | 0.0308 (10) | |
H9A | −0.0438 | 0.9339 | 0.0453 | 0.037* | |
C10 | 0.0598 (4) | 0.8892 (3) | −0.0575 (3) | 0.0363 (10) | |
H10A | 0.0056 | 0.8462 | −0.0886 | 0.044* | |
H10B | 0.1363 | 0.8596 | −0.0628 | 0.044* | |
C11 | 0.0606 (4) | 0.9920 (3) | −0.1022 (3) | 0.0542 (13) | |
H11A | 0.0823 | 0.9848 | −0.1634 | 0.081* | |
H11B | 0.1155 | 1.0346 | −0.0727 | 0.081* | |
H11C | −0.0153 | 1.0211 | −0.0985 | 0.081* | |
C12 | 0.1194 (4) | 0.9436 (3) | 0.0970 (3) | 0.0443 (11) | |
H12A | 0.1370 | 1.0080 | 0.0723 | 0.067* | |
H12B | 0.1882 | 0.9031 | 0.0973 | 0.067* | |
H12C | 0.0917 | 0.9515 | 0.1566 | 0.067* | |
N1 | 0.2004 (2) | 0.5297 (2) | 0.0586 (2) | 0.0308 (8) | |
H1C | 0.2254 | 0.4923 | 0.0127 | 0.037* | |
H1D | 0.2520 | 0.5791 | 0.0676 | 0.037* | |
N2 | −0.0035 (3) | 0.5307 (2) | 0.1439 (2) | 0.0327 (8) | |
H2C | −0.0479 | 0.5772 | 0.1719 | 0.039* | |
N3 | −0.0105 (3) | 0.4638 (2) | −0.0204 (2) | 0.0325 (8) | |
H3C | 0.0436 | 0.4150 | −0.0132 | 0.039* | |
N4 | 0.0934 (3) | 0.6222 (2) | −0.0915 (2) | 0.0310 (8) | |
H4C | 0.0493 | 0.6732 | −0.1109 | 0.037* | |
H4D | 0.1681 | 0.6415 | −0.0929 | 0.037* | |
N5 | 0.0954 (2) | 0.7174 (2) | 0.0778 (2) | 0.0265 (7) | |
H5C | 0.1218 | 0.7098 | 0.1336 | 0.032* | |
H5D | 0.1535 | 0.7424 | 0.0446 | 0.032* | |
O1 | −0.0960 (2) | 0.64899 (18) | 0.00997 (17) | 0.0296 (6) | |
O2 | −0.1949 (2) | 0.79101 (18) | 0.01893 (19) | 0.0367 (7) | |
O3 | 0.2118 (4) | 0.7632 (4) | 0.2603 (4) | 0.1271 (19) | |
O4 | 0.3381 (4) | 0.6508 (3) | 0.2116 (3) | 0.0976 (14) | |
O5 | 0.3891 (7) | 0.8157 (4) | 0.2193 (4) | 0.198 (3) | |
O6 | 0.3616 (5) | 0.7269 (4) | 0.3456 (3) | 0.131 (2) | |
O7 | 0.7679 (3) | 0.6126 (2) | 0.2337 (3) | 0.0876 (13) | |
O8 | 0.7521 (4) | 0.7845 (3) | 0.2327 (3) | 0.0928 (14) | |
O9 | 0.7572 (3) | 0.6988 (3) | 0.3676 (2) | 0.0727 (11) | |
O10 | 0.9200 (3) | 0.7076 (3) | 0.2791 (3) | 0.0875 (13) | |
OW1 | 0.4657 (3) | 0.7643 (3) | 0.5126 (2) | 0.0751 (11) | |
HW1 | 0.4187 | 0.7927 | 0.4719 | 0.14 (3)* | |
HW2 | 0.4160 | 0.7763 | 0.5762 | 0.27 (5)* | |
OW2 | 0.1779 (4) | 0.6161 (3) | 0.4460 (3) | 0.0868 (13) | |
HW3 | 0.1191 | 0.6695 | 0.4711 | 0.23 (4)* | |
HW4 | 0.2311 | 0.6634 | 0.4140 | 0.16 (3)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co | 0.0206 (2) | 0.0221 (2) | 0.0302 (3) | 0.0002 (2) | −0.0013 (3) | 0.0012 (3) |
Cl1 | 0.0588 (8) | 0.0422 (6) | 0.0375 (6) | −0.0014 (6) | 0.0010 (6) | −0.0033 (5) |
Cl2 | 0.0513 (7) | 0.0473 (6) | 0.0402 (6) | 0.0002 (6) | 0.0002 (6) | 0.0045 (6) |
C1 | 0.037 (3) | 0.039 (2) | 0.047 (3) | 0.004 (2) | −0.011 (2) | 0.012 (2) |
C2 | 0.041 (3) | 0.045 (2) | 0.033 (2) | −0.010 (2) | −0.008 (2) | 0.010 (2) |
C3 | 0.035 (3) | 0.033 (2) | 0.055 (3) | −0.0083 (18) | 0.006 (2) | 0.008 (2) |
C4 | 0.032 (2) | 0.033 (2) | 0.060 (3) | −0.0095 (18) | 0.001 (2) | −0.004 (2) |
C5 | 0.039 (3) | 0.034 (2) | 0.044 (3) | 0.000 (2) | −0.011 (2) | −0.007 (2) |
C6 | 0.046 (3) | 0.037 (2) | 0.034 (2) | 0.006 (2) | 0.001 (2) | −0.006 (2) |
C7 | 0.022 (2) | 0.026 (2) | 0.0275 (19) | 0.0037 (16) | 0.0028 (19) | 0.002 (2) |
C8 | 0.0187 (19) | 0.0254 (19) | 0.032 (2) | 0.0041 (17) | 0.0016 (17) | 0.0010 (17) |
C9 | 0.027 (2) | 0.023 (2) | 0.043 (2) | 0.0011 (15) | 0.0006 (19) | −0.0009 (19) |
C10 | 0.034 (2) | 0.032 (2) | 0.042 (2) | 0.000 (2) | −0.004 (2) | 0.0026 (17) |
C11 | 0.054 (3) | 0.052 (3) | 0.057 (3) | 0.003 (3) | −0.002 (3) | 0.022 (2) |
C12 | 0.045 (3) | 0.034 (2) | 0.054 (3) | −0.0094 (19) | −0.002 (2) | −0.003 (2) |
N1 | 0.0256 (18) | 0.0295 (17) | 0.0372 (19) | −0.0015 (15) | −0.0015 (15) | 0.0020 (15) |
N2 | 0.0319 (19) | 0.0306 (17) | 0.0354 (19) | −0.0010 (16) | 0.0047 (16) | 0.0027 (16) |
N3 | 0.0313 (18) | 0.0277 (16) | 0.039 (2) | −0.0008 (14) | −0.0007 (17) | 0.0015 (17) |
N4 | 0.0301 (19) | 0.0276 (17) | 0.035 (2) | 0.0007 (14) | 0.0014 (16) | −0.0009 (15) |
N5 | 0.0215 (16) | 0.0265 (17) | 0.0316 (17) | 0.0002 (14) | −0.0048 (14) | 0.0016 (14) |
O1 | 0.0198 (13) | 0.0272 (14) | 0.0419 (17) | −0.0012 (11) | −0.0058 (12) | 0.0000 (12) |
O2 | 0.0224 (14) | 0.0319 (14) | 0.0559 (18) | 0.0022 (12) | −0.0032 (15) | 0.0023 (14) |
O3 | 0.099 (4) | 0.150 (5) | 0.132 (4) | 0.044 (3) | −0.013 (3) | −0.047 (4) |
O4 | 0.114 (3) | 0.072 (2) | 0.108 (3) | −0.011 (3) | 0.003 (3) | −0.027 (3) |
O5 | 0.310 (8) | 0.127 (4) | 0.158 (5) | −0.140 (5) | 0.076 (6) | 0.012 (4) |
O6 | 0.186 (5) | 0.135 (4) | 0.071 (3) | −0.031 (4) | −0.060 (3) | 0.018 (3) |
O7 | 0.102 (3) | 0.057 (2) | 0.104 (3) | −0.007 (2) | −0.012 (3) | −0.037 (2) |
O8 | 0.144 (4) | 0.065 (2) | 0.069 (3) | 0.036 (3) | −0.019 (3) | 0.004 (2) |
O9 | 0.087 (3) | 0.082 (2) | 0.049 (2) | −0.010 (2) | 0.025 (2) | 0.005 (2) |
O10 | 0.059 (3) | 0.125 (3) | 0.078 (3) | −0.018 (2) | 0.010 (2) | 0.014 (3) |
OW1 | 0.092 (3) | 0.069 (2) | 0.064 (2) | 0.023 (2) | −0.003 (3) | 0.010 (2) |
OW2 | 0.083 (3) | 0.078 (3) | 0.099 (3) | 0.021 (2) | 0.020 (3) | 0.035 (2) |
Geometric parameters (Å, º) top
Co—O1 | 1.895 (2) | C2—N2 | 1.479 (5) |
Co—N3 | 1.940 (3) | C3—N2 | 1.494 (5) |
Co—N1 | 1.951 (3) | C3—C4 | 1.516 (6) |
Co—N5 | 1.961 (3) | C4—N3 | 1.478 (5) |
Co—N4 | 1.963 (3) | C5—N3 | 1.480 (5) |
Co—N2 | 1.964 (3) | C5—C6 | 1.501 (6) |
Cl1—O7 | 1.401 (3) | C6—N4 | 1.476 (5) |
Cl1—O8 | 1.403 (4) | C7—O2 | 1.247 (4) |
Cl1—O9 | 1.413 (3) | C7—O1 | 1.288 (4) |
Cl1—O10 | 1.437 (4) | C7—C8 | 1.496 (5) |
Cl2—O5 | 1.309 (5) | C8—N5 | 1.499 (4) |
Cl2—O6 | 1.378 (4) | C8—C9 | 1.527 (5) |
Cl2—O4 | 1.408 (4) | C9—C12 | 1.527 (5) |
Cl2—O3 | 1.429 (5) | C9—C10 | 1.531 (5) |
C1—N1 | 1.482 (5) | C10—C11 | 1.531 (5) |
C1—C2 | 1.509 (6) | | |
| | | |
O1—Co—N3 | 89.69 (12) | N1—C1—C2 | 108.8 (3) |
O1—Co—N1 | 175.75 (13) | N2—C2—C1 | 107.4 (3) |
N3—Co—N1 | 94.09 (13) | N2—C3—C4 | 109.3 (3) |
O1—Co—N5 | 84.72 (11) | N3—C4—C3 | 105.7 (3) |
N3—Co—N5 | 174.35 (12) | N3—C5—C6 | 105.8 (3) |
N1—Co—N5 | 91.52 (12) | N4—C6—C5 | 107.6 (3) |
O1—Co—N4 | 88.41 (12) | O2—C7—O1 | 122.2 (3) |
N3—Co—N4 | 85.88 (13) | O2—C7—C8 | 119.7 (3) |
N1—Co—N4 | 93.78 (13) | O1—C7—C8 | 118.1 (3) |
N5—Co—N4 | 93.16 (13) | C7—C8—N5 | 108.5 (3) |
O1—Co—N2 | 92.02 (12) | C7—C8—C9 | 113.6 (3) |
N3—Co—N2 | 84.81 (13) | N5—C8—C9 | 114.1 (3) |
N1—Co—N2 | 86.41 (13) | C8—C9—C12 | 111.1 (3) |
N5—Co—N2 | 96.16 (13) | C8—C9—C10 | 112.5 (3) |
N4—Co—N2 | 170.68 (13) | C12—C9—C10 | 111.8 (3) |
O7—Cl1—O8 | 110.6 (2) | C9—C10—C11 | 113.5 (3) |
O7—Cl1—O9 | 111.5 (2) | C1—N1—Co | 109.9 (2) |
O8—Cl1—O9 | 111.9 (3) | C2—N2—C3 | 112.7 (3) |
O7—Cl1—O10 | 106.3 (3) | C2—N2—Co | 108.2 (2) |
O8—Cl1—O10 | 108.3 (3) | C3—N2—Co | 110.4 (2) |
O9—Cl1—O10 | 108.0 (2) | C4—N3—C5 | 116.4 (3) |
O5—Cl2—O6 | 114.9 (4) | C4—N3—Co | 106.3 (2) |
O5—Cl2—O4 | 114.4 (3) | C5—N3—Co | 108.4 (2) |
O6—Cl2—O4 | 109.6 (3) | C6—N4—Co | 108.9 (2) |
O5—Cl2—O3 | 110.3 (4) | C8—N5—Co | 111.6 (2) |
O6—Cl2—O3 | 103.7 (3) | C7—O1—Co | 116.7 (2) |
O4—Cl2—O3 | 102.8 (3) | | |
| | | |
N1—C1—C2—N2 | 47.6 (4) | C3—C4—N3—Co | −51.5 (3) |
N2—C3—C4—N3 | 44.0 (4) | C6—C5—N3—C4 | 163.7 (3) |
N3—C5—C6—N4 | −52.1 (4) | C6—C5—N3—Co | 43.9 (3) |
O2—C7—C8—N5 | −174.5 (3) | O1—Co—N3—C4 | −57.2 (3) |
O1—C7—C8—N5 | 6.1 (5) | N1—Co—N3—C4 | 120.9 (3) |
O2—C7—C8—C9 | −46.5 (5) | N5—Co—N3—C4 | −65.3 (15) |
O1—C7—C8—C9 | 134.1 (3) | N4—Co—N3—C4 | −145.6 (3) |
C7—C8—C9—C12 | 172.7 (3) | N2—Co—N3—C4 | 34.9 (2) |
N5—C8—C9—C12 | −62.3 (4) | O1—Co—N3—C5 | 68.6 (2) |
C7—C8—C9—C10 | −61.1 (4) | N1—Co—N3—C5 | −113.3 (2) |
N5—C8—C9—C10 | 64.0 (4) | N5—Co—N3—C5 | 60.5 (15) |
C8—C9—C10—C11 | 165.4 (3) | N4—Co—N3—C5 | −19.8 (2) |
C12—C9—C10—C11 | −68.8 (5) | N2—Co—N3—C5 | 160.7 (3) |
C2—C1—N1—Co | −31.7 (4) | C5—C6—N4—Co | 36.0 (4) |
O1—Co—N1—C1 | 75.5 (17) | O1—Co—N4—C6 | −99.1 (3) |
N3—Co—N1—C1 | −77.4 (3) | N3—Co—N4—C6 | −9.3 (3) |
N5—Co—N1—C1 | 103.2 (3) | N1—Co—N4—C6 | 84.6 (3) |
N4—Co—N1—C1 | −163.5 (2) | N5—Co—N4—C6 | 176.3 (2) |
N2—Co—N1—C1 | 7.2 (2) | N2—Co—N4—C6 | −6.2 (10) |
C1—C2—N2—C3 | 81.5 (4) | C7—C8—N5—Co | −5.6 (4) |
C1—C2—N2—Co | −40.9 (4) | C9—C8—N5—Co | −133.4 (3) |
C4—C3—N2—C2 | −137.6 (3) | O1—Co—N5—C8 | 3.3 (2) |
C4—C3—N2—Co | −16.5 (4) | N3—Co—N5—C8 | 11.5 (15) |
O1—Co—N2—C2 | −156.8 (3) | N1—Co—N5—C8 | −174.7 (2) |
N3—Co—N2—C2 | 113.7 (3) | N4—Co—N5—C8 | 91.4 (2) |
N1—Co—N2—C2 | 19.2 (3) | N2—Co—N5—C8 | −88.1 (2) |
N5—Co—N2—C2 | −71.9 (3) | O2—C7—O1—Co | 176.9 (3) |
N4—Co—N2—C2 | 110.7 (8) | C8—C7—O1—Co | −3.7 (4) |
O1—Co—N2—C3 | 79.4 (2) | N3—Co—O1—C7 | −179.1 (3) |
N3—Co—N2—C3 | −10.1 (2) | N1—Co—O1—C7 | 28.0 (18) |
N1—Co—N2—C3 | −104.5 (2) | N5—Co—O1—C7 | 0.1 (3) |
N5—Co—N2—C3 | 164.3 (2) | N4—Co—O1—C7 | −93.2 (3) |
N4—Co—N2—C3 | −13.1 (9) | N2—Co—O1—C7 | 96.1 (3) |
C3—C4—N3—C5 | −172.3 (3) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1C···OW2i | 0.90 | 2.09 | 2.940 (5) | 158 |
N1—H1D···O2ii | 0.90 | 2.26 | 2.928 (4) | 131 |
N1—H1D···O4 | 0.90 | 2.57 | 3.234 (5) | 131 |
N2—H2C···O7iii | 0.91 | 2.37 | 3.159 (5) | 146 |
N2—H2C···O10iii | 0.91 | 2.40 | 3.244 (5) | 153 |
N2—H2C···Cl1iii | 0.91 | 2.93 | 3.832 (3) | 171 |
N3—H3C···OW1i | 0.91 | 2.43 | 3.134 (4) | 134 |
N4—H4C···O5iv | 0.90 | 2.47 | 3.154 (7) | 133 |
N4—H4D···O2ii | 0.90 | 2.13 | 2.916 (4) | 145 |
N4—H4D···O8iv | 0.90 | 2.52 | 3.071 (5) | 120 |
N5—H5C···O3 | 0.90 | 2.29 | 3.120 (6) | 154 |
N5—H5D···O2ii | 0.90 | 2.04 | 2.825 (4) | 145 |
OW1—HW1···O6 | 0.90 | 2.20 | 2.832 (6) | 127 |
OW1—HW2···O9v | 1.13 | 2.05 | 3.047 (5) | 146 |
OW1—HW2···O10v | 1.13 | 2.19 | 3.203 (5) | 148 |
OW2—HW3···OW1v | 1.06 | 1.99 | 2.989 (5) | 156 |
OW2—HW4···O6 | 1.00 | 2.01 | 2.995 (7) | 166 |
Symmetry codes: (i) −x+1/2, −y+1, z−1/2; (ii) x+1/2, −y+3/2, −z; (iii) x−1, y, z; (iv) x−1/2, −y+3/2, −z; (v) x−1/2, −y+3/2, −z+1. |
(6) (
L-leucinato)-(triethylenetetramine)-cobalt(III) diperchlorate dihydrate
top
Crystal data top
C12H30CoN5O22+·2(ClO4−)·2(H2O) | F(000) = 1192 |
Mr = 570.27 | Dx = 1.597 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.7716 (8) Å | µ = 1.01 mm−1 |
b = 12.6294 (15) Å | T = 293 K |
c = 21.413 (4) Å | Plate, yellow |
V = 2372.1 (5) Å3 | 0.34 × 0.25 × 0.13 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD area detector diffractometer | 5824 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.022 |
Graphite monochromator | θmax = 30.1°, θmin = 4.0° |
ϕ and ω scans | h = −12→12 |
17247 measured reflections | k = −17→11 |
6815 independent reflections | l = −30→21 |
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 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.100 | w = 1/[σ2(Fo2) + (0.0662P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.001 |
6815 reflections | Δρmax = 0.55 e Å−3 |
289 parameters | Δρmin = −0.27 e Å−3 |
0 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.003 (11) |
Crystal data top
C12H30CoN5O22+·2(ClO4−)·2(H2O) | V = 2372.1 (5) Å3 |
Mr = 570.27 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 8.7716 (8) Å | µ = 1.01 mm−1 |
b = 12.6294 (15) Å | T = 293 K |
c = 21.413 (4) Å | 0.34 × 0.25 × 0.13 mm |
Data collection top
Bruker SMART CCD area detector diffractometer | 5824 reflections with I > 2σ(I) |
17247 measured reflections | Rint = 0.022 |
6815 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.036 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.100 | Δρmax = 0.55 e Å−3 |
S = 1.00 | Δρmin = −0.27 e Å−3 |
6815 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
289 parameters | Absolute structure parameter: −0.003 (11) |
0 restraints | |
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 | |
Co | 0.07192 (3) | 0.06767 (2) | 0.154788 (12) | 0.03001 (8) | |
Cl1 | 0.38665 (9) | 0.27409 (7) | 0.34015 (5) | 0.0731 (3) | |
Cl2 | 0.67091 (8) | 0.32902 (6) | 0.06836 (3) | 0.04992 (16) | |
N1 | 0.0661 (2) | 0.21240 (14) | 0.12129 (8) | 0.0348 (4) | |
H1C | 0.0176 | 0.2126 | 0.0843 | 0.042* | |
H1D | 0.0145 | 0.2547 | 0.1476 | 0.042* | |
N2 | 0.2909 (2) | 0.09097 (16) | 0.16718 (9) | 0.0395 (4) | |
H2C | 0.3191 | 0.0644 | 0.2050 | 0.047* | |
N3 | 0.1308 (3) | 0.00597 (15) | 0.07546 (9) | 0.0402 (5) | |
H3C | 0.1430 | 0.0593 | 0.0473 | 0.048* | |
N4 | −0.1398 (3) | 0.03772 (18) | 0.13000 (10) | 0.0453 (5) | |
H4C | −0.1798 | −0.0122 | 0.1551 | 0.054* | |
H4D | −0.1967 | 0.0967 | 0.1335 | 0.054* | |
N5 | 0.0111 (3) | 0.11134 (14) | 0.23972 (9) | 0.0370 (4) | |
H5C | 0.0628 | 0.1700 | 0.2506 | 0.044* | |
H5D | −0.0891 | 0.1270 | 0.2401 | 0.044* | |
O1 | 0.0814 (2) | −0.06961 (12) | 0.19010 (7) | 0.0410 (3) | |
O2 | 0.0515 (3) | −0.16352 (13) | 0.27619 (8) | 0.0520 (5) | |
O3 | 0.2753 (5) | 0.3414 (4) | 0.3114 (2) | 0.153 (2) | |
O4 | 0.3501 (5) | 0.1691 (3) | 0.3255 (2) | 0.1393 (17) | |
O5 | 0.3981 (4) | 0.2982 (3) | 0.40336 (17) | 0.1182 (12) | |
O6 | 0.5311 (3) | 0.2946 (3) | 0.31048 (16) | 0.0928 (9) | |
O7 | 0.8024 (4) | 0.3647 (3) | 0.03746 (16) | 0.1135 (12) | |
O8 | 0.7014 (6) | 0.2396 (4) | 0.0978 (3) | 0.199 (3) | |
O9 | 0.6223 (8) | 0.4005 (6) | 0.1105 (3) | 0.237 (4) | |
O10 | 0.5515 (3) | 0.3200 (4) | 0.02568 (15) | 0.1294 (16) | |
C1 | 0.2246 (3) | 0.25318 (18) | 0.11318 (12) | 0.0413 (5) | |
H1A | 0.2257 | 0.3299 | 0.1149 | 0.050* | |
H1B | 0.2658 | 0.2309 | 0.0733 | 0.050* | |
C2 | 0.3173 (3) | 0.2069 (2) | 0.16640 (12) | 0.0467 (6) | |
H2A | 0.4248 | 0.2218 | 0.1602 | 0.056* | |
H2B | 0.2858 | 0.2379 | 0.2058 | 0.056* | |
C3 | 0.3791 (3) | 0.0351 (2) | 0.11610 (13) | 0.0499 (6) | |
H3A | 0.4138 | 0.0864 | 0.0855 | 0.060* | |
H3B | 0.4680 | 0.0007 | 0.1339 | 0.060* | |
C4 | 0.2798 (4) | −0.0458 (2) | 0.08490 (12) | 0.0510 (7) | |
H4A | 0.3233 | −0.0670 | 0.0452 | 0.061* | |
H4B | 0.2690 | −0.1080 | 0.1111 | 0.061* | |
C5 | 0.0022 (4) | −0.0629 (2) | 0.05405 (12) | 0.0573 (7) | |
H5A | 0.0142 | −0.0809 | 0.0103 | 0.069* | |
H5B | −0.0011 | −0.1278 | 0.0782 | 0.069* | |
C6 | −0.1402 (4) | −0.0001 (2) | 0.06374 (13) | 0.0560 (7) | |
H6A | −0.2291 | −0.0439 | 0.0560 | 0.067* | |
H6B | −0.1428 | 0.0596 | 0.0353 | 0.067* | |
C7 | 0.0576 (3) | −0.07886 (16) | 0.24918 (10) | 0.0358 (4) | |
C8 | 0.0422 (3) | 0.02600 (17) | 0.28557 (10) | 0.0364 (5) | |
H8A | 0.1400 | 0.0411 | 0.3059 | 0.044* | |
C9 | −0.0793 (3) | 0.01882 (19) | 0.33560 (10) | 0.0451 (5) | |
H9A | −0.0571 | −0.0421 | 0.3616 | 0.054* | |
H9B | −0.1764 | 0.0057 | 0.3153 | 0.054* | |
C10 | −0.0973 (4) | 0.1153 (2) | 0.37802 (12) | 0.0570 (8) | |
H10A | −0.0946 | 0.1793 | 0.3522 | 0.068* | |
C11 | 0.0312 (7) | 0.1208 (4) | 0.4250 (2) | 0.0994 (15) | |
H11A | 0.1268 | 0.1255 | 0.4034 | 0.149* | |
H11B | 0.0301 | 0.0582 | 0.4505 | 0.149* | |
H11C | 0.0181 | 0.1820 | 0.4510 | 0.149* | |
C12 | −0.2541 (6) | 0.1091 (4) | 0.4109 (2) | 0.1005 (16) | |
H12A | −0.2660 | 0.1689 | 0.4381 | 0.151* | |
H12B | −0.2600 | 0.0449 | 0.4348 | 0.151* | |
H12C | −0.3336 | 0.1096 | 0.3801 | 0.151* | |
OW1 | 0.4488 (4) | 0.9718 (3) | 0.26895 (13) | 0.0972 (10) | |
H1W | 0.4435 | 0.9589 | 0.3074 | 0.117* | |
H2W | 0.4790 | 1.0342 | 0.2707 | 0.117* | |
OW2 | 0.6685 (3) | 0.1283 (3) | 0.23213 (13) | 0.0854 (8) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co | 0.04151 (14) | 0.02479 (11) | 0.02374 (12) | −0.00120 (11) | 0.00463 (12) | 0.00172 (10) |
Cl1 | 0.0610 (4) | 0.0641 (5) | 0.0941 (6) | 0.0009 (3) | −0.0033 (4) | −0.0371 (5) |
Cl2 | 0.0584 (4) | 0.0561 (4) | 0.0353 (3) | 0.0052 (3) | 0.0017 (3) | 0.0106 (2) |
N1 | 0.0451 (9) | 0.0292 (8) | 0.0300 (8) | 0.0011 (8) | 0.0043 (8) | 0.0045 (6) |
N2 | 0.0436 (10) | 0.0401 (10) | 0.0348 (10) | 0.0031 (8) | 0.0015 (8) | 0.0058 (7) |
N3 | 0.0594 (13) | 0.0349 (9) | 0.0263 (8) | 0.0021 (9) | 0.0081 (8) | 0.0007 (7) |
N4 | 0.0509 (12) | 0.0416 (11) | 0.0436 (11) | −0.0075 (9) | 0.0020 (9) | 0.0032 (8) |
N5 | 0.0552 (11) | 0.0251 (8) | 0.0308 (9) | −0.0013 (8) | 0.0106 (8) | 0.0035 (7) |
O1 | 0.0654 (10) | 0.0270 (6) | 0.0304 (7) | −0.0005 (8) | 0.0076 (7) | 0.0014 (6) |
O2 | 0.0872 (15) | 0.0291 (7) | 0.0396 (9) | −0.0005 (9) | 0.0054 (9) | 0.0091 (6) |
O3 | 0.145 (3) | 0.173 (4) | 0.141 (4) | 0.098 (3) | −0.029 (3) | −0.058 (3) |
O4 | 0.134 (3) | 0.081 (2) | 0.202 (4) | −0.039 (2) | 0.029 (3) | −0.061 (3) |
O5 | 0.123 (3) | 0.145 (3) | 0.086 (2) | −0.021 (3) | 0.004 (2) | −0.033 (2) |
O6 | 0.0803 (18) | 0.0913 (19) | 0.107 (2) | −0.0078 (15) | 0.0161 (16) | −0.0253 (17) |
O7 | 0.100 (2) | 0.155 (3) | 0.086 (2) | −0.058 (2) | 0.0219 (18) | 0.008 (2) |
O8 | 0.132 (3) | 0.151 (4) | 0.315 (8) | 0.015 (3) | −0.029 (4) | 0.167 (5) |
O9 | 0.241 (7) | 0.270 (7) | 0.199 (6) | 0.004 (6) | 0.089 (5) | −0.150 (6) |
O10 | 0.077 (2) | 0.232 (5) | 0.079 (2) | −0.014 (3) | −0.0233 (17) | 0.032 (3) |
C1 | 0.0485 (13) | 0.0323 (11) | 0.0430 (12) | −0.0024 (9) | 0.0118 (10) | 0.0053 (9) |
C2 | 0.0476 (12) | 0.0463 (13) | 0.0463 (14) | −0.0118 (11) | −0.0009 (11) | 0.0016 (10) |
C3 | 0.0480 (13) | 0.0502 (14) | 0.0514 (15) | 0.0138 (11) | 0.0109 (11) | 0.0085 (12) |
C4 | 0.0735 (18) | 0.0396 (14) | 0.0400 (13) | 0.0133 (12) | 0.0168 (12) | −0.0011 (9) |
C5 | 0.087 (2) | 0.0486 (14) | 0.0360 (12) | −0.0177 (15) | 0.0008 (13) | −0.0114 (11) |
C6 | 0.0647 (18) | 0.0615 (17) | 0.0419 (14) | −0.0171 (14) | −0.0097 (13) | −0.0009 (12) |
C7 | 0.0473 (12) | 0.0291 (9) | 0.0309 (9) | −0.0018 (10) | 0.0042 (9) | 0.0046 (7) |
C8 | 0.0511 (14) | 0.0308 (9) | 0.0274 (9) | −0.0026 (9) | 0.0055 (9) | 0.0025 (8) |
C9 | 0.0601 (14) | 0.0436 (12) | 0.0315 (11) | −0.0016 (11) | 0.0125 (11) | 0.0066 (9) |
C10 | 0.093 (2) | 0.0457 (14) | 0.0325 (12) | 0.0177 (15) | 0.0148 (14) | 0.0076 (10) |
C11 | 0.125 (4) | 0.091 (3) | 0.082 (3) | 0.010 (3) | −0.011 (3) | −0.038 (2) |
C12 | 0.113 (4) | 0.125 (4) | 0.064 (2) | 0.027 (3) | 0.044 (2) | −0.002 (2) |
OW1 | 0.124 (3) | 0.101 (2) | 0.0666 (16) | 0.0244 (19) | 0.0037 (17) | 0.0209 (15) |
OW2 | 0.0781 (17) | 0.110 (2) | 0.0680 (16) | 0.0417 (15) | −0.0090 (13) | −0.0126 (14) |
Geometric parameters (Å, º) top
Co—O1 | 1.8933 (15) | N2—C3 | 1.515 (3) |
Co—N3 | 1.9389 (19) | N3—C4 | 1.475 (4) |
Co—N2 | 1.961 (2) | N3—C5 | 1.497 (4) |
Co—N1 | 1.9642 (17) | N4—C6 | 1.497 (4) |
Co—N4 | 1.968 (2) | N5—C8 | 1.483 (3) |
Co—N5 | 1.9740 (19) | O1—C7 | 1.288 (3) |
Cl1—O5 | 1.391 (3) | O2—C7 | 1.217 (3) |
Cl1—O4 | 1.400 (3) | C1—C2 | 1.517 (4) |
Cl1—O3 | 1.434 (4) | C3—C4 | 1.499 (4) |
Cl1—O6 | 1.441 (3) | C5—C6 | 1.494 (5) |
Cl2—O8 | 1.320 (3) | C7—C8 | 1.542 (3) |
Cl2—O9 | 1.345 (4) | C8—C9 | 1.514 (3) |
Cl2—O10 | 1.395 (3) | C9—C10 | 1.527 (4) |
Cl2—O7 | 1.404 (3) | C10—C11 | 1.512 (6) |
N1—C1 | 1.492 (3) | C10—C12 | 1.547 (5) |
N2—C2 | 1.483 (3) | | |
| | | |
O1—Co—N3 | 88.29 (7) | C1—N1—Co | 109.86 (14) |
O1—Co—N2 | 92.30 (8) | C2—N2—C3 | 111.84 (19) |
N3—Co—N2 | 85.29 (9) | C2—N2—Co | 107.46 (15) |
O1—Co—N1 | 177.62 (8) | C3—N2—Co | 109.45 (16) |
N3—Co—N1 | 93.49 (8) | C4—N3—C5 | 116.9 (2) |
N2—Co—N1 | 86.28 (8) | C4—N3—Co | 107.11 (15) |
O1—Co—N4 | 88.47 (9) | C5—N3—Co | 107.51 (16) |
N3—Co—N4 | 86.45 (10) | C6—N4—Co | 108.60 (18) |
N2—Co—N4 | 171.67 (9) | C8—N5—Co | 110.91 (14) |
N1—Co—N4 | 93.21 (9) | C7—O1—Co | 117.93 (13) |
O1—Co—N5 | 84.25 (7) | N1—C1—C2 | 106.21 (18) |
N3—Co—N5 | 172.51 (8) | N2—C2—C1 | 107.7 (2) |
N2—Co—N5 | 95.64 (9) | C4—C3—N2 | 110.0 (2) |
N1—Co—N5 | 93.98 (7) | N3—C4—C3 | 105.9 (2) |
N4—Co—N5 | 92.69 (9) | C6—C5—N3 | 106.2 (2) |
O5—Cl1—O4 | 116.2 (3) | C5—C6—N4 | 107.4 (2) |
O5—Cl1—O3 | 109.7 (2) | O2—C7—O1 | 123.6 (2) |
O4—Cl1—O3 | 108.0 (3) | O2—C7—C8 | 120.70 (19) |
O5—Cl1—O6 | 109.0 (2) | O1—C7—C8 | 115.64 (17) |
O4—Cl1—O6 | 105.8 (2) | N5—C8—C9 | 112.5 (2) |
O3—Cl1—O6 | 107.6 (3) | N5—C8—C7 | 107.80 (17) |
O8—Cl2—O9 | 108.5 (5) | C9—C8—C7 | 111.58 (19) |
O8—Cl2—O10 | 113.2 (3) | C8—C9—C10 | 116.5 (2) |
O9—Cl2—O10 | 104.8 (4) | C11—C10—C9 | 110.8 (3) |
O8—Cl2—O7 | 109.5 (3) | C11—C10—C12 | 111.2 (3) |
O9—Cl2—O7 | 111.2 (4) | C9—C10—C12 | 108.8 (3) |
O10—Cl2—O7 | 109.5 (2) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1C···O10i | 0.90 | 2.41 | 3.176 (4) | 143 |
N1—H1D···O2ii | 0.90 | 2.02 | 2.888 (3) | 163 |
N2—H2C···OW1iii | 0.91 | 2.13 | 2.989 (3) | 157 |
N3—H3C···O10i | 0.91 | 2.33 | 3.163 (4) | 153 |
N3—H3C···O7i | 0.91 | 2.48 | 3.283 (5) | 147 |
N4—H4C···O3iv | 0.90 | 2.15 | 3.022 (4) | 162 |
N4—H4D···O8v | 0.90 | 2.15 | 2.986 (4) | 154 |
N4—H4D···OW2v | 0.90 | 2.45 | 2.986 (4) | 118 |
N5—H5C···O2ii | 0.90 | 2.40 | 2.916 (3) | 117 |
N5—H5D···OW2v | 0.90 | 2.13 | 3.017 (4) | 167 |
OW1—H1W···O9vi | 0.84 | 1.99 | 2.805 (5) | 162 |
OW1—H2W···OW2vii | 0.83 | 2.20 | 2.871 (5) | 137 |
OW1—H2W···O4vii | 0.83 | 2.36 | 2.903 (5) | 124 |
Symmetry codes: (i) x−1/2, −y+1/2, −z; (ii) −x, y+1/2, −z+1/2; (iii) x, y−1, z; (iv) −x, y−1/2, −z+1/2; (v) x−1, y, z; (vi) −x+1, y+1/2, −z+1/2; (vii) x, y+1, z. |
Experimental details
| (1) | (2) | (3) | (4) |
Crystal data |
Chemical formula | C12H30CoN5O22+·2(ClO4−) | C11H28CoN5O22+·2(ClO4−) | C11H23CoN5O3+·ClO4− | C12H30CoN5O22+·2(I−)·H2O |
Mr | 534.24 | 520.21 | 431.72 | 606.15 |
Crystal system, space group | Monoclinic, P21 | Monoclinic, P21 | Orthorhombic, P212121 | Orthorhombic, P212121 |
Temperature (K) | 293 | 293 | 293 | 293 |
a, b, c (Å) | 10.7972 (13), 8.8272 (11), 11.9248 (14) | 8.9877 (7), 8.8829 (7), 12.8157 (10) | 9.4009 (5), 13.3659 (8), 13.6588 (8) | 10.053 (2), 11.540 (2), 18.664 (4) |
α, β, γ (°) | 90, 110.794 (2), 90 | 90, 101.577 (1), 90 | 90, 90, 90 | 90, 90, 90 |
V (Å3) | 1062.5 (2) | 1002.35 (14) | 1716.25 (17) | 2165.2 (7) |
Z | 2 | 2 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 1.12 | 1.18 | 1.20 | 3.66 |
Crystal size (mm) | 0.40 × 0.30 × 0.30 | 0.30 × 0.25 × 0.23 | 0.30 × 0.25 × 0.23 | 0.30 × 0.15 × 0.10 |
|
Data collection |
Diffractometer | Bruker SMART CCD area detector diffractometer | Bruker SMART CCD area detector diffractometer | Bruker SMART CCD area detector diffractometer | Bruker SMART CCD area detector diffractometer |
Absorption correction | – | – | – | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 6477, 4129, 3818 | 6012, 3835, 3672 | 10571, 3939, 3573 | 7861, 4811, 4240 |
Rint | 0.029 | 0.022 | 0.044 | 0.022 |
(sin θ/λ)max (Å−1) | 0.639 | 0.639 | 0.651 | 0.649 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.050, 0.127, 1.05 | 0.045, 0.123, 1.07 | 0.037, 0.094, 1.05 | 0.032, 0.078, 1.02 |
No. of reflections | 4129 | 3835 | 3939 | 4811 |
No. of parameters | 280 | 262 | 227 | 317 |
No. of restraints | 1 | 1 | 0 | 0 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.49, −0.54 | 0.68, −0.40 | 0.65, −0.35 | 1.16, −0.77 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 |
Absolute structure parameter | 0.08 (2) | 0.08 (2) | 0.001 (15) | 0.02 (2) |
| (5) | (6) |
Crystal data |
Chemical formula | C12H30CoN5O22+·2(ClO4−)·2(H2O) | C12H30CoN5O22+·2(ClO4−)·2(H2O) |
Mr | 570.27 | 570.27 |
Crystal system, space group | Orthorhombic, P212121 | Orthorhombic, P212121 |
Temperature (K) | 293 | 293 |
a, b, c (Å) | 11.5333 (11), 13.3726 (14), 15.0622 (15) | 8.7716 (8), 12.6294 (15), 21.413 (4) |
α, β, γ (°) | 90, 90, 90 | 90, 90, 90 |
V (Å3) | 2323.0 (4) | 2372.1 (5) |
Z | 4 | 4 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 1.04 | 1.01 |
Crystal size (mm) | 0.35 × 0.30 × 0.28 | 0.34 × 0.25 × 0.13 |
|
Data collection |
Diffractometer | Buker SMART CCD area detector diffractometer | Bruker SMART CCD area detector diffractometer |
Absorption correction | – | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8345, 4922, 3537 | 17247, 6815, 5824 |
Rint | 0.032 | 0.022 |
(sin θ/λ)max (Å−1) | 0.639 | 0.705 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.085, 0.90 | 0.036, 0.100, 1.00 |
No. of reflections | 4922 | 6815 |
No. of parameters | 293 | 289 |
No. of restraints | 0 | 0 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.59, −0.32 | 0.55, −0.27 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 |
Absolute structure parameter | −0.007 (17) | −0.003 (11) |
Hydrogen-bond geometry (Å, º) for (1) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1C···O2i | 0.90 | 2.33 | 2.905 (6) | 121.7 |
N1—H1D···O6ii | 0.90 | 2.07 | 2.967 (7) | 174.3 |
N2—H2C···O7 | 0.91 | 2.47 | 3.327 (10) | 157.3 |
N2—H2C···O8 | 0.91 | 2.51 | 3.256 (9) | 139.2 |
N4—H4C···O2i | 0.90 | 2.07 | 2.958 (6) | 168.5 |
N4—H4D···O6iii | 0.90 | 2.55 | 3.096 (6) | 119.5 |
N5—H5C···O8 | 0.90 | 2.30 | 3.120 (8) | 150.6 |
N5—H5C···O9iii | 0.90 | 2.49 | 3.152 (7) | 130.9 |
N5—H5D···O10iii | 0.90 | 2.52 | 3.264 (7) | 140.3 |
Symmetry codes: (i) −x, y−1/2, −z−1; (ii) x−1, y−1, z−1; (iii) −x+1, y−1/2, −z. |
Hydrogen-bond geometry (Å, º) for (2) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1C···O2i | 0.90 | 2.29 | 2.923 (5) | 127.3 |
N1—H1D···O10ii | 0.90 | 2.13 | 2.944 (6) | 150.7 |
N2—H2C···O3 | 0.91 | 2.24 | 3.122 (9) | 162.5 |
N4—H4C···O2i | 0.90 | 2.02 | 2.901 (5) | 167.6 |
N4—H4D···O10iii | 0.90 | 2.41 | 3.078 (6) | 131.3 |
N5—H5C···O4 | 0.90 | 2.27 | 3.110 (7) | 154.1 |
N5—H5C···O6iv | 0.90 | 2.55 | 3.162 (9) | 125.8 |
N5—H5D···O5iv | 0.90 | 2.55 | 3.310 (11) | 142.0 |
Symmetry codes: (i) −x−1, y+1/2, −z−2; (ii) x+1, y+1, z; (iii) −x−2, y+1/2, −z−2; (iv) −x−1, y+1/2, −z−1. |
Hydrogen-bond geometry (Å, º) for (3) top
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H4C···O4i | 0.90 | 2.37 | 3.129 (7) | 142.6 |
N4—H4D···O2ii | 0.90 | 1.98 | 2.873 (3) | 171.2 |
N4—H4D···O1ii | 0.90 | 2.64 | 3.318 (3) | 132.3 |
N3—H3C···O3 | 0.91 | 2.09 | 2.904 (3) | 148.3 |
N2—H2C···O7 | 0.91 | 2.13 | 2.962 (4) | 151.1 |
N1—H1D···O2ii | 0.90 | 2.42 | 2.957 (4) | 118.5 |
N1—H1C···O3iii | 0.90 | 2.13 | 2.876 (3) | 139.3 |
Symmetry codes: (i) −x, y−1/2, −z+1/2; (ii) x+1/2, −y+1/2, −z; (iii) −x+1/2, −y+1, z−1/2. |
Hydrogen-bond geometry (Å, º) for (4) top
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H18···O2i | 0.82 (6) | 2.30 (6) | 2.934 (5) | 134 (5) |
N2—H7···OW1 | 0.96 (4) | 1.89 (5) | 2.856 (6) | 179 (4) |
N5—H21···I1i | 0.93 (6) | 2.87 (6) | 3.695 (4) | 148 (4) |
N4—H17···I1 | 0.84 (5) | 3.16 (6) | 3.951 (5) | 158 (4) |
N3—H12···I2ii | 0.93 (4) | 2.82 (4) | 3.728 (4) | 165 (3) |
N1—H2···I2ii | 0.79 (5) | 2.87 (5) | 3.565 (4) | 147 (5) |
N1—H1···O2i | 0.99 (6) | 2.18 (6) | 2.937 (5) | 132 (4) |
N5—H20···O2i | 0.82 (6) | 2.07 (6) | 2.793 (5) | 147 (5) |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x+1/2, −y+1, z−1/2. |
Hydrogen-bond geometry (Å, º) for (5) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1C···OW2i | 0.90 | 2.09 | 2.940 (5) | 157.9 |
N1—H1D···O2ii | 0.90 | 2.26 | 2.928 (4) | 131.1 |
N1—H1D···O4 | 0.90 | 2.57 | 3.234 (5) | 131.1 |
N2—H2C···O7iii | 0.91 | 2.37 | 3.159 (5) | 145.5 |
N2—H2C···O10iii | 0.91 | 2.40 | 3.244 (5) | 153.4 |
N2—H2C···Cl1iii | 0.91 | 2.93 | 3.832 (3) | 171.1 |
N3—H3C···OW1i | 0.91 | 2.43 | 3.134 (4) | 134.1 |
N4—H4C···O5iv | 0.90 | 2.47 | 3.154 (7) | 133.1 |
N4—H4D···O2ii | 0.90 | 2.13 | 2.916 (4) | 144.9 |
N4—H4D···O8iv | 0.90 | 2.52 | 3.071 (5) | 120.1 |
N5—H5C···O3 | 0.90 | 2.29 | 3.120 (6) | 153.8 |
N5—H5D···O2ii | 0.90 | 2.04 | 2.825 (4) | 144.8 |
OW1—HW1···O6 | 0.90 | 2.20 | 2.832 (6) | 126.8 |
OW1—HW2···O9v | 1.13 | 2.05 | 3.047 (5) | 146.1 |
OW1—HW2···O10v | 1.13 | 2.19 | 3.203 (5) | 148.0 |
OW2—HW3···OW1v | 1.06 | 1.99 | 2.989 (5) | 156.2 |
OW2—HW4···O6 | 1.00 | 2.01 | 2.995 (7) | 165.5 |
Symmetry codes: (i) −x+1/2, −y+1, z−1/2; (ii) x+1/2, −y+3/2, −z; (iii) x−1, y, z; (iv) x−1/2, −y+3/2, −z; (v) x−1/2, −y+3/2, −z+1. |
Hydrogen-bond geometry (Å, º) for (6) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1C···O10i | 0.90 | 2.41 | 3.176 (4) | 143.3 |
N1—H1D···O2ii | 0.90 | 2.02 | 2.888 (3) | 163.1 |
N2—H2C···OW1iii | 0.91 | 2.13 | 2.989 (3) | 156.8 |
N3—H3C···O10i | 0.91 | 2.33 | 3.163 (4) | 152.8 |
N3—H3C···O7i | 0.91 | 2.48 | 3.283 (5) | 146.7 |
N4—H4C···O3iv | 0.90 | 2.15 | 3.022 (4) | 162.3 |
N4—H4D···O8v | 0.90 | 2.15 | 2.986 (4) | 153.5 |
N4—H4D···OW2v | 0.90 | 2.45 | 2.986 (4) | 118.2 |
N5—H5C···O2ii | 0.90 | 2.40 | 2.916 (3) | 116.6 |
N5—H5D···OW2v | 0.90 | 2.13 | 3.017 (4) | 166.8 |
OW1—H1W···O9vi | 0.84 | 1.99 | 2.805 (5) | 162.2 |
OW1—H2W···OW2vii | 0.83 | 2.20 | 2.871 (5) | 137.1 |
OW1—H2W···O4vii | 0.83 | 2.36 | 2.903 (5) | 123.7 |
Symmetry codes: (i) x−1/2, −y+1/2, −z; (ii) −x, y+1/2, −z+1/2; (iii) x, y−1, z; (iv) −x, y−1/2, −z+1/2; (v) x−1, y, z; (vi) −x+1, y+1/2, −z+1/2; (vii) x, y+1, z. |