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The crystal structures and absolute configurations of three cis1 and three cis2 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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768100013896/bm0032sup1.cif
Contains datablocks 1, 2, 3, 4, 5, 6, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013896/bm00321sup2.hkl
Contains datablock 1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013896/bm00322sup3.hkl
Contains datablock 2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013896/bm00323sup4.hkl
Contains datablock 3

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013896/bm00324sup5.hkl
Contains datablock 4

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013896/bm00325sup6.hkl
Contains datablock 5

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013896/bm00326sup7.hkl
Contains datablock 6

CCDC references: 159946; 159947; 159948; 159949; 159950; 159951

Computing details top

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.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
[Figure 10]
[Figure 11]
[Figure 12]
[Figure 13]
(1) (L-isoleucinato)-(triethylenetetramine)-cobalt(III) diperchlorate top
Crystal data top
C12H30CoN5O22+·2(ClO4)Z = 2
Mr = 534.24F(000) = 556
Monoclinic, P21Dx = 1.670 Mg m3
a = 10.7972 (13) ÅMo Kα radiation, λ = 0.71073 Å
b = 8.8272 (11) ŵ = 1.12 mm1
c = 11.9248 (14) ÅT = 293 K
β = 110.794 (2)°Block, red
V = 1062.5 (2) Å30.40 × 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 tubeRint = 0.029
Graphite monochromatorθmax = 27.0°, θmin = 1.8°
ϕ and ω scansh = 1313
6477 measured reflectionsk = 1011
4129 independent reflectionsl = 1512
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.050H 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 reflectionsΔρmax = 0.49 e Å3
280 parametersΔρmin = 0.54 e Å3
1 restraintAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.08 (2)
Crystal data top
C12H30CoN5O22+·2(ClO4)V = 1062.5 (2) Å3
Mr = 534.24Z = 2
Monoclinic, P21Mo Kα radiation
a = 10.7972 (13) ŵ = 1.12 mm1
b = 8.8272 (11) ÅT = 293 K
c = 11.9248 (14) Å0.40 × 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 reflectionsRint = 0.029
4129 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.050H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.127Δρmax = 0.49 e Å3
S = 1.05Δρmin = 0.54 e Å3
4129 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
280 parametersAbsolute 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
xyzUiso*/UeqOcc. (<1)
Co0.13845 (5)0.34207 (7)0.26941 (5)0.02571 (15)
Cl10.87592 (16)0.18784 (16)0.72185 (12)0.0502 (4)
Cl20.37596 (13)0.02414 (16)0.06881 (12)0.0436 (3)
C10.1044 (6)0.3620 (11)0.2233 (5)0.0582 (18)
H1A0.10630.45240.17770.070*
H1B0.19440.32510.26040.070*
C20.0200 (6)0.2433 (7)0.1419 (5)0.0450 (13)
H2A0.04040.14450.17960.054*
H2B0.03710.24040.06730.054*
C30.1710 (7)0.4030 (7)0.0275 (5)0.0530 (15)
H3A0.09780.45390.01420.064*
H3B0.22740.35930.04800.064*
C50.2469 (8)0.6294 (8)0.2624 (6)0.0603 (19)
H5A0.34240.63960.22810.072*
H5B0.20940.72830.25840.072*
C60.2124 (11)0.5903 (8)0.3846 (7)0.082 (3)
H6A0.14990.66420.43330.099*
H6B0.29110.59440.40580.099*
C70.1576 (5)0.0631 (5)0.3596 (4)0.0283 (9)
C80.2982 (5)0.0849 (5)0.2745 (4)0.0280 (10)
H8A0.30980.01810.20580.034*
C90.4023 (5)0.0387 (7)0.3265 (5)0.0409 (12)
H9A0.37830.06250.36130.049*
C100.4062 (6)0.1424 (9)0.4267 (5)0.0522 (15)
H10A0.44610.23780.39180.063*
H10B0.31590.16350.47880.063*
C110.4812 (11)0.0809 (16)0.5022 (9)0.101 (4)
H11A0.47920.15360.56270.151*
H11B0.57140.06170.45210.151*
H11C0.44070.01180.53980.151*
C120.5404 (6)0.0249 (10)0.2257 (6)0.066 (2)
H12A0.60480.00490.26000.100*
H12B0.56510.12100.18630.100*
H12C0.53670.04980.16850.100*
N10.0476 (5)0.3978 (6)0.3168 (4)0.0444 (11)
H1C0.09410.34830.38470.053*
H1D0.05610.49770.33250.053*
N20.1191 (4)0.2809 (5)0.1179 (3)0.0328 (9)
H2C0.16860.19610.09050.039*
N30.2069 (7)0.5290 (6)0.1892 (5)0.0639 (17)
H3C0.12780.57350.19880.077*
N40.1533 (4)0.4380 (5)0.4121 (4)0.0332 (9)
H4C0.07230.44510.46930.040*
H4D0.20380.37990.44080.040*
N50.3143 (4)0.2442 (5)0.2270 (3)0.0305 (8)
H5C0.35490.24300.14670.037*
H5D0.36510.29740.25850.037*
O10.0724 (3)0.1612 (4)0.3565 (3)0.0295 (7)
O20.1273 (4)0.0491 (4)0.4269 (3)0.0420 (8)
O30.7877 (8)0.2682 (7)0.7613 (7)0.109 (3)
O40.8127 (6)0.0502 (6)0.6673 (5)0.0793 (15)
O50.9932 (6)0.1555 (13)0.8165 (5)0.116 (2)
O60.9054 (5)0.2741 (6)0.6316 (4)0.0608 (12)
O70.2373 (5)0.0431 (10)0.0217 (6)0.104 (2)
O80.4018 (8)0.1249 (7)0.0361 (6)0.103 (2)
O90.4385 (7)0.1310 (10)0.0150 (5)0.110 (3)
O100.4262 (6)0.0456 (7)0.1935 (4)0.0762 (15)
C40.2505 (14)0.5179 (17)0.0713 (11)0.042 (3)0.50
H4A0.34290.48760.04280.050*0.50
H4B0.24530.61650.03730.050*0.50
C4A0.1892 (17)0.5430 (16)0.0751 (13)0.043 (3)0.50
H4AA0.11280.60670.08510.052*0.50
H4AB0.26620.59260.01860.052*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co0.0334 (3)0.0199 (3)0.0258 (3)0.0002 (3)0.0129 (2)0.0010 (3)
Cl10.0679 (9)0.0461 (10)0.0434 (7)0.0001 (7)0.0284 (6)0.0064 (5)
Cl20.0448 (7)0.0461 (8)0.0420 (7)0.0058 (6)0.0180 (5)0.0093 (5)
C10.041 (3)0.077 (5)0.064 (4)0.017 (4)0.028 (3)0.013 (4)
C20.047 (3)0.044 (3)0.052 (3)0.001 (3)0.027 (3)0.007 (2)
C30.077 (4)0.055 (4)0.032 (3)0.016 (3)0.025 (3)0.007 (2)
C50.084 (5)0.038 (3)0.054 (4)0.024 (3)0.019 (4)0.005 (3)
C60.168 (9)0.034 (3)0.078 (5)0.029 (4)0.085 (6)0.010 (3)
C70.040 (3)0.020 (2)0.028 (2)0.0032 (19)0.015 (2)0.0024 (17)
C80.030 (2)0.026 (2)0.028 (2)0.0092 (19)0.0100 (19)0.0029 (17)
C90.036 (3)0.048 (3)0.038 (3)0.012 (2)0.012 (2)0.001 (2)
C100.052 (3)0.069 (4)0.043 (3)0.009 (3)0.027 (3)0.003 (3)
C110.097 (7)0.161 (9)0.064 (4)0.064 (7)0.053 (5)0.027 (5)
C120.043 (3)0.102 (6)0.050 (3)0.034 (4)0.011 (3)0.008 (4)
N10.050 (3)0.050 (3)0.038 (2)0.021 (2)0.021 (2)0.0104 (19)
N20.042 (2)0.031 (2)0.0265 (19)0.0054 (17)0.0135 (17)0.0025 (15)
N30.122 (5)0.033 (3)0.060 (3)0.027 (3)0.062 (3)0.022 (2)
N40.036 (2)0.033 (2)0.033 (2)0.0062 (17)0.0152 (17)0.0025 (16)
N50.030 (2)0.029 (2)0.0311 (19)0.0034 (16)0.0088 (16)0.0077 (15)
O10.0253 (16)0.0276 (17)0.0336 (17)0.0022 (13)0.0080 (13)0.0053 (13)
O20.050 (2)0.0289 (19)0.047 (2)0.0065 (17)0.0174 (17)0.0142 (15)
O30.176 (7)0.062 (4)0.145 (6)0.021 (4)0.126 (6)0.010 (4)
O40.091 (4)0.050 (3)0.099 (4)0.017 (3)0.036 (3)0.004 (3)
O50.095 (4)0.160 (6)0.066 (3)0.020 (6)0.007 (3)0.019 (5)
O60.089 (3)0.054 (3)0.052 (2)0.012 (2)0.040 (2)0.007 (2)
O70.059 (3)0.140 (6)0.097 (4)0.023 (4)0.009 (3)0.025 (4)
O80.155 (6)0.058 (4)0.097 (4)0.010 (4)0.046 (4)0.029 (3)
O90.141 (5)0.130 (7)0.073 (3)0.084 (5)0.054 (4)0.027 (4)
O100.094 (4)0.087 (4)0.045 (2)0.013 (3)0.020 (2)0.010 (2)
C40.045 (8)0.043 (7)0.029 (5)0.015 (6)0.004 (6)0.018 (4)
C4A0.062 (10)0.030 (7)0.041 (7)0.003 (7)0.023 (7)0.010 (5)
Geometric parameters (Å, º) top
Co—O11.900 (3)C3—C4A1.402 (16)
Co—N31.919 (5)C3—N21.485 (7)
Co—N11.947 (4)C3—C41.536 (17)
Co—N41.957 (4)C5—C61.413 (10)
Co—N21.967 (4)C5—N31.415 (8)
Co—N51.981 (4)C6—N41.474 (8)
Cl1—O51.394 (6)C7—O21.242 (6)
Cl1—O31.396 (6)C7—O11.274 (6)
Cl1—O41.432 (6)C7—C81.509 (7)
Cl1—O61.443 (4)C8—N51.503 (6)
Cl2—O101.403 (5)C8—C91.520 (7)
Cl2—O71.410 (5)C9—C101.518 (8)
Cl2—O81.428 (6)C9—C121.552 (8)
Cl2—O91.436 (6)C10—C111.510 (10)
C1—N11.484 (7)N3—C41.318 (14)
C1—C21.497 (9)N3—C4A1.444 (14)
C2—N21.464 (7)
O1—Co—N3176.82 (18)C4A—C3—C426.4 (6)
O1—Co—N184.56 (18)N2—C3—C4110.2 (6)
N3—Co—N195.9 (3)C6—C5—N3117.2 (5)
O1—Co—N491.09 (16)C5—C6—N4112.8 (5)
N3—Co—N485.7 (2)O2—C7—O1122.2 (5)
N1—Co—N491.90 (18)O2—C7—C8120.5 (4)
O1—Co—N297.46 (16)O1—C7—C8117.2 (4)
N3—Co—N285.72 (19)N5—C8—C7109.1 (4)
N1—Co—N284.31 (18)N5—C8—C9113.6 (4)
N4—Co—N2170.26 (18)C7—C8—C9113.8 (4)
O1—Co—N585.01 (15)C10—C9—C8113.0 (5)
N3—Co—N594.8 (2)C10—C9—C12111.7 (5)
N1—Co—N5168.74 (19)C8—C9—C12110.6 (4)
N4—Co—N592.50 (17)C11—C10—C9115.0 (7)
N2—Co—N592.88 (17)C1—N1—Co112.8 (3)
O5—Cl1—O3111.3 (5)C2—N2—C3113.7 (5)
O5—Cl1—O4110.1 (5)C2—N2—Co108.6 (3)
O3—Cl1—O4108.2 (4)C3—N2—Co109.4 (3)
O5—Cl1—O6109.5 (4)C4—N3—C5129.2 (9)
O3—Cl1—O6109.9 (3)C4—N3—C4A28.2 (6)
O4—Cl1—O6107.7 (3)C5—N3—C4A134.3 (7)
O10—Cl2—O7111.3 (4)C4—N3—Co113.4 (7)
O10—Cl2—O8112.0 (4)C5—N3—Co112.3 (4)
O7—Cl2—O8106.5 (5)C4A—N3—Co112.8 (6)
O10—Cl2—O9108.5 (3)C6—N4—Co111.3 (4)
O7—Cl2—O9110.2 (5)C8—N5—Co109.8 (3)
O8—Cl2—O9108.3 (5)C7—O1—Co116.9 (3)
N1—C1—C2108.5 (5)N3—C4—C3112.3 (10)
N2—C2—C1108.3 (5)C3—C4A—N3113.0 (10)
C4A—C3—N2114.6 (7)
N1—C1—C2—N241.9 (7)N5—Co—N3—C471.9 (8)
N3—C5—C6—N47.2 (12)O1—Co—N3—C50 (5)
O2—C7—C8—N5166.4 (4)N1—Co—N3—C598.3 (6)
O1—C7—C8—N515.7 (6)N4—Co—N3—C56.8 (6)
O2—C7—C8—C938.3 (6)N2—Co—N3—C5177.9 (6)
O1—C7—C8—C9143.8 (4)N5—Co—N3—C585.3 (6)
N5—C8—C9—C1057.2 (6)O1—Co—N3—C4A172 (4)
C7—C8—C9—C1068.5 (6)N1—Co—N3—C4A73.8 (8)
N5—C8—C9—C1268.8 (6)N4—Co—N3—C4A165.3 (8)
C7—C8—C9—C12165.5 (5)N2—Co—N3—C4A10.0 (8)
C8—C9—C10—C11165.0 (7)N5—Co—N3—C4A102.6 (8)
C12—C9—C10—C1169.6 (9)C5—C6—N4—Co1.4 (10)
C2—C1—N1—Co21.2 (7)O1—Co—N4—C6176.6 (5)
O1—Co—N1—C195.8 (5)N3—Co—N4—C63.0 (6)
N3—Co—N1—C187.3 (5)N1—Co—N4—C698.8 (5)
N4—Co—N1—C1173.2 (5)N2—Co—N4—C632.0 (13)
N2—Co—N1—C12.2 (5)N5—Co—N4—C691.5 (5)
N5—Co—N1—C173.7 (10)C7—C8—N5—Co11.5 (4)
C1—C2—N2—C378.2 (6)C9—C8—N5—Co139.7 (3)
C1—C2—N2—Co43.8 (5)O1—Co—N5—C85.0 (3)
C4A—C3—N2—C2106.4 (9)N3—Co—N5—C8178.2 (3)
C4—C3—N2—C2134.6 (7)N1—Co—N5—C817.1 (10)
C4A—C3—N2—Co15.2 (10)N4—Co—N5—C895.9 (3)
C4—C3—N2—Co13.0 (8)N2—Co—N5—C892.2 (3)
O1—Co—N2—C258.0 (4)O2—C7—O1—Co169.9 (4)
N3—Co—N2—C2122.2 (4)C8—C7—O1—Co12.2 (5)
N1—Co—N2—C225.8 (4)N3—Co—O1—C782 (4)
N4—Co—N2—C293.2 (11)N1—Co—O1—C7179.7 (3)
N5—Co—N2—C2143.3 (4)N4—Co—O1—C788.5 (3)
O1—Co—N2—C3177.4 (4)N2—Co—O1—C796.2 (3)
N3—Co—N2—C32.5 (4)N5—Co—O1—C73.9 (3)
N1—Co—N2—C398.9 (4)C5—N3—C4—C3174.7 (8)
N4—Co—N2—C331.4 (13)C4A—N3—C4—C362 (2)
N5—Co—N2—C392.1 (4)Co—N3—C4—C332.9 (11)
C6—C5—N3—C4162.3 (10)C4A—C3—C4—N374.8 (19)
C6—C5—N3—C4A160.1 (12)N2—C3—C4—N330.1 (12)
C6—C5—N3—Co9.7 (10)N2—C3—C4A—N323.9 (15)
O1—Co—N3—C4157 (4)C4—C3—C4A—N362.2 (17)
N1—Co—N3—C4104.5 (8)C4—N3—C4A—C376 (2)
N4—Co—N3—C4164.0 (8)C5—N3—C4A—C3169.0 (9)
N2—Co—N3—C420.7 (8)Co—N3—C4A—C321.3 (15)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1C···O2i0.902.332.905 (6)122
N1—H1D···O6ii0.902.072.967 (7)174
N2—H2C···O70.912.473.327 (10)157
N2—H2C···O80.912.513.256 (9)139
N4—H4C···O2i0.902.072.958 (6)169
N4—H4D···O6iii0.902.553.096 (6)120
N5—H5C···O80.902.303.120 (8)151
N5—H5C···O9iii0.902.493.152 (7)131
N5—H5D···O10iii0.902.523.264 (7)140
Symmetry codes: (i) x, y1/2, z1; (ii) x1, y1, z1; (iii) x+1, y1/2, z.
(2) (L-valinato)-(triethylenetetramine)-cobalt(III) diperchlorate top
Crystal data top
C11H28CoN5O22+·2(ClO4)Z = 2
Mr = 520.21F(000) = 540
Monoclinic, P21Dx = 1.724 Mg m3
a = 8.9877 (7) ÅMo Kα radiation, λ = 0.71073 Å
b = 8.8829 (7) ŵ = 1.18 mm1
c = 12.8157 (10) ÅT = 293 K
β = 101.577 (1)°Block, red
V = 1002.35 (14) Å30.30 × 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 tubeRint = 0.022
Graphite monochromatorθmax = 27.0°, θmin = 1.6°
ϕ and ω scansh = 1111
6012 measured reflectionsk = 1011
3835 independent reflectionsl = 1316
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.045H 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 reflectionsΔρmax = 0.68 e Å3
262 parametersΔρmin = 0.40 e Å3
1 restraintAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.08 (2)
Crystal data top
C11H28CoN5O22+·2(ClO4)V = 1002.35 (14) Å3
Mr = 520.21Z = 2
Monoclinic, P21Mo Kα radiation
a = 8.9877 (7) ŵ = 1.18 mm1
b = 8.8829 (7) ÅT = 293 K
c = 12.8157 (10) Å0.30 × 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 reflectionsRint = 0.022
3835 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.045H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.123Δρmax = 0.68 e Å3
S = 1.07Δρmin = 0.40 e Å3
3835 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
262 parametersAbsolute 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
xyzUiso*/Ueq
Co0.40564 (5)0.01783 (6)0.79301 (3)0.02989 (14)
Cl10.29331 (16)0.37208 (16)0.47588 (10)0.0575 (3)
Cl21.09219 (16)0.54801 (15)0.89150 (11)0.0640 (4)
C10.1032 (6)0.0237 (7)0.8279 (5)0.0620 (15)
H1A0.04690.00420.88210.074*
H1B0.05610.11250.79140.074*
C20.0989 (5)0.1010 (7)0.7511 (4)0.0527 (12)
H2A0.00100.10380.70260.063*
H2B0.11460.19650.78840.063*
C30.1898 (6)0.0414 (6)0.6059 (4)0.0533 (12)
H3A0.22960.00770.54490.064*
H3B0.08080.05370.58340.064*
C40.2590 (8)0.1875 (7)0.6431 (5)0.0689 (17)
H4A0.26880.24950.58260.083*
H4B0.19490.24030.68370.083*
C50.4935 (9)0.2791 (7)0.7721 (5)0.0687 (17)
H5A0.52980.34990.72530.082*
H5B0.42870.33330.81130.082*
C60.6221 (8)0.2163 (7)0.8465 (5)0.0716 (17)
H6A0.65510.28670.90430.086*
H6B0.70590.20040.81040.086*
C70.4999 (4)0.3001 (5)0.8574 (3)0.0321 (8)
C80.5571 (4)0.2862 (4)0.7530 (3)0.0308 (8)
H8A0.49510.35210.70010.037*
C90.7215 (5)0.3353 (5)0.7663 (3)0.0405 (9)
H9A0.73660.42880.80770.049*
C100.8107 (4)0.2189 (5)0.8245 (3)0.0351 (8)
H10A0.91620.24540.83520.053*
H10B0.78220.20650.89220.053*
H10C0.79370.12640.78510.053*
C110.7677 (6)0.3601 (8)0.6601 (4)0.0583 (13)
H11A0.87210.39090.67200.087*
H11B0.75530.26800.62000.087*
H11C0.70490.43690.62100.087*
N10.2640 (4)0.0571 (5)0.8786 (3)0.0433 (8)
H1C0.28570.01440.94350.052*
H1D0.27580.15730.88700.052*
N20.2217 (4)0.0742 (4)0.6912 (3)0.0378 (7)
H2C0.24030.16280.66050.045*
N30.4062 (5)0.1611 (5)0.7088 (3)0.0487 (9)
H3C0.46460.13530.66130.058*
N40.5796 (4)0.0707 (5)0.8901 (3)0.0413 (8)
H4C0.55590.08620.95420.050*
H4D0.65890.00690.89870.050*
N50.5362 (4)0.1291 (4)0.7137 (3)0.0359 (7)
H5C0.49360.12920.64390.043*
H5D0.62720.08330.72180.043*
O10.4173 (3)0.1932 (4)0.8793 (2)0.0369 (6)
O20.5334 (4)0.4117 (4)0.9135 (2)0.0448 (7)
O30.2141 (9)0.3687 (11)0.5572 (6)0.137 (3)
O40.3867 (10)0.2408 (10)0.4869 (5)0.137 (3)
O50.2195 (9)0.4058 (12)0.3727 (4)0.143 (3)
O60.4082 (11)0.4877 (12)0.5017 (8)0.172 (4)
O70.9607 (9)0.6109 (10)0.8816 (14)0.223 (7)
O81.1279 (15)0.521 (2)0.7914 (5)0.213 (6)
O91.0901 (9)0.4057 (6)0.9399 (5)0.1076 (19)
O101.2149 (6)0.6344 (6)0.9486 (4)0.0865 (16)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co0.0340 (2)0.0246 (2)0.0311 (2)0.0008 (2)0.00662 (15)0.0008 (2)
Cl10.0600 (7)0.0637 (8)0.0484 (6)0.0122 (6)0.0100 (5)0.0177 (5)
Cl20.0631 (7)0.0514 (9)0.0698 (7)0.0138 (6)0.0049 (6)0.0005 (6)
C10.045 (3)0.072 (4)0.077 (3)0.002 (2)0.031 (2)0.008 (3)
C20.037 (2)0.070 (4)0.053 (3)0.011 (2)0.0125 (19)0.004 (2)
C30.058 (3)0.058 (3)0.039 (2)0.004 (2)0.0016 (19)0.011 (2)
C40.086 (4)0.053 (3)0.060 (3)0.004 (3)0.003 (3)0.022 (3)
C50.092 (5)0.038 (3)0.073 (4)0.027 (3)0.010 (3)0.000 (3)
C60.076 (4)0.058 (4)0.077 (4)0.033 (3)0.005 (3)0.006 (3)
C70.0328 (18)0.0328 (19)0.0305 (16)0.0037 (15)0.0061 (13)0.0015 (14)
C80.0338 (19)0.0307 (19)0.0283 (16)0.0016 (15)0.0067 (13)0.0009 (14)
C90.038 (2)0.041 (2)0.044 (2)0.0063 (18)0.0116 (16)0.0023 (17)
C100.0224 (16)0.051 (2)0.0294 (16)0.0030 (16)0.0015 (13)0.0039 (16)
C110.056 (3)0.074 (4)0.049 (2)0.012 (3)0.020 (2)0.009 (2)
N10.052 (2)0.040 (2)0.0400 (17)0.0067 (17)0.0130 (15)0.0077 (15)
N20.0360 (16)0.0366 (17)0.0401 (16)0.0015 (14)0.0059 (13)0.0022 (14)
N30.061 (2)0.0327 (19)0.052 (2)0.0028 (18)0.0093 (18)0.0114 (16)
N40.0437 (19)0.040 (2)0.0386 (17)0.0076 (16)0.0056 (14)0.0036 (15)
N50.0387 (17)0.0360 (18)0.0348 (15)0.0015 (14)0.0114 (12)0.0063 (13)
O10.0427 (15)0.0353 (16)0.0351 (13)0.0047 (13)0.0135 (11)0.0060 (11)
O20.0562 (18)0.0372 (16)0.0420 (14)0.0083 (14)0.0124 (13)0.0138 (12)
O30.140 (6)0.172 (8)0.119 (5)0.045 (6)0.074 (5)0.051 (5)
O40.162 (7)0.130 (6)0.104 (4)0.080 (5)0.009 (4)0.005 (4)
O50.131 (5)0.214 (9)0.072 (3)0.051 (6)0.012 (3)0.031 (5)
O60.155 (7)0.159 (9)0.180 (8)0.079 (7)0.023 (6)0.074 (7)
O70.083 (5)0.097 (6)0.46 (2)0.016 (4)0.013 (8)0.025 (9)
O80.281 (13)0.276 (14)0.077 (4)0.095 (14)0.024 (6)0.012 (8)
O90.144 (5)0.060 (3)0.111 (4)0.029 (4)0.006 (4)0.003 (3)
O100.084 (3)0.061 (3)0.097 (3)0.027 (3)0.024 (3)0.016 (2)
Geometric parameters (Å, º) top
Co—O11.901 (3)C1—N11.491 (7)
Co—N31.921 (4)C2—N21.485 (6)
Co—N21.955 (3)C3—C41.477 (8)
Co—N11.956 (4)C3—N21.484 (6)
Co—N41.957 (4)C4—N31.438 (7)
Co—N51.966 (4)C5—C61.453 (10)
Cl1—O31.376 (6)C5—N31.455 (7)
Cl1—O51.388 (5)C6—N41.489 (7)
Cl1—O41.427 (7)C7—O21.226 (5)
Cl1—O61.447 (8)C7—O11.272 (5)
Cl2—O71.290 (8)C7—C81.531 (5)
Cl2—O81.404 (9)C8—N51.483 (5)
Cl2—O91.410 (6)C8—C91.517 (6)
Cl2—O101.420 (5)C9—C101.423 (6)
C1—C21.477 (8)C9—C111.516 (6)
O1—Co—N3176.69 (16)O9—Cl2—O10109.6 (3)
O1—Co—N296.83 (14)C2—C1—N1109.5 (4)
N3—Co—N286.23 (17)C1—C2—N2107.6 (4)
O1—Co—N185.36 (15)C4—C3—N2111.3 (4)
N3—Co—N196.22 (19)N3—C4—C3108.9 (5)
N2—Co—N184.44 (16)C6—C5—N3111.0 (5)
O1—Co—N490.90 (15)C5—C6—N4110.5 (5)
N3—Co—N486.15 (17)O2—C7—O1124.0 (3)
N2—Co—N4171.15 (17)O2—C7—C8119.5 (4)
N1—Co—N491.91 (16)O1—C7—C8116.5 (3)
O1—Co—N585.41 (13)N5—C8—C9111.3 (3)
N3—Co—N593.23 (17)N5—C8—C7109.3 (3)
N2—Co—N592.21 (15)C9—C8—C7111.6 (3)
N1—Co—N5169.74 (16)C10—C9—C11110.4 (4)
N4—Co—N592.71 (16)C10—C9—C8106.4 (4)
O3—Cl1—O5120.4 (5)C11—C9—C8112.1 (4)
O3—Cl1—O4106.9 (5)C1—N1—Co111.8 (3)
O5—Cl1—O4115.5 (5)C3—N2—C2115.9 (4)
O3—Cl1—O6107.2 (6)C3—N2—Co109.1 (3)
O5—Cl1—O6104.3 (6)C2—N2—Co108.2 (3)
O4—Cl1—O6100.3 (6)C4—N3—C5122.6 (5)
O7—Cl2—O8110.9 (9)C4—N3—Co111.0 (3)
O7—Cl2—O9109.8 (7)C5—N3—Co110.2 (3)
O8—Cl2—O9106.1 (8)C6—N4—Co110.0 (3)
O7—Cl2—O10114.7 (6)C8—N5—Co110.2 (2)
O8—Cl2—O10105.4 (6)C7—O1—Co116.8 (2)
N1—C1—C2—N242.4 (6)C6—C5—N3—C4168.5 (5)
N2—C3—C4—N339.4 (7)C6—C5—N3—Co35.0 (7)
N3—C5—C6—N437.7 (8)O1—Co—N3—C4177 (3)
O2—C7—C8—N5165.9 (4)N2—Co—N3—C419.0 (4)
O1—C7—C8—N515.1 (5)N1—Co—N3—C465.0 (4)
O2—C7—C8—C942.3 (5)N4—Co—N3—C4156.5 (4)
O1—C7—C8—C9138.7 (4)N5—Co—N3—C4111.0 (4)
N5—C8—C9—C1048.8 (4)O1—Co—N3—C544 (3)
C7—C8—C9—C1073.7 (4)N2—Co—N3—C5158.1 (4)
N5—C8—C9—C1172.0 (5)N1—Co—N3—C574.1 (4)
C7—C8—C9—C11165.5 (4)N4—Co—N3—C517.4 (4)
C2—C1—N1—Co20.6 (5)N5—Co—N3—C5109.9 (4)
O1—Co—N1—C193.4 (4)C5—C6—N4—Co22.9 (6)
N3—Co—N1—C189.5 (4)O1—Co—N4—C6175.5 (4)
N2—Co—N1—C13.9 (4)N3—Co—N4—C63.0 (4)
N4—Co—N1—C1175.8 (4)N2—Co—N4—C633.6 (12)
N5—Co—N1—C167.5 (10)N1—Co—N4—C699.1 (4)
C4—C3—N2—C298.5 (5)N5—Co—N4—C690.1 (4)
C4—C3—N2—Co23.9 (6)C9—C8—N5—Co136.1 (3)
C1—C2—N2—C377.5 (5)C7—C8—N5—Co12.3 (4)
C1—C2—N2—Co45.3 (5)O1—Co—N5—C86.4 (3)
O1—Co—N2—C3175.8 (3)N3—Co—N5—C8176.6 (3)
N3—Co—N2—C33.0 (3)N2—Co—N5—C890.3 (3)
N1—Co—N2—C399.6 (3)N1—Co—N5—C819.6 (10)
N4—Co—N2—C333.6 (11)N4—Co—N5—C897.1 (3)
N5—Co—N2—C390.1 (3)O2—C7—O1—Co170.6 (3)
O1—Co—N2—C257.3 (3)C8—C7—O1—Co10.4 (4)
N3—Co—N2—C2124.0 (3)N3—Co—O1—C764 (3)
N1—Co—N2—C227.3 (3)N2—Co—O1—C793.9 (3)
N4—Co—N2—C293.3 (10)N1—Co—O1—C7177.8 (3)
N5—Co—N2—C2143.0 (3)N4—Co—O1—C790.4 (3)
C3—C4—N3—C5169.6 (5)N5—Co—O1—C72.2 (3)
C3—C4—N3—Co36.5 (6)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1C···O2i0.902.292.923 (5)127
N1—H1D···O10ii0.902.132.944 (6)151
N2—H2C···O30.912.243.122 (9)163
N4—H4C···O2i0.902.022.901 (5)168
N4—H4D···O10iii0.902.413.078 (6)131
N5—H5C···O40.902.273.110 (7)154
N5—H5C···O6iv0.902.553.162 (9)126
N5—H5D···O5iv0.902.553.310 (11)142
Symmetry codes: (i) x1, y+1/2, z2; (ii) x+1, y+1, z; (iii) x2, y+1/2, z2; (iv) x1, y+1/2, z1.
(3) (L-pyroglutamicacidato)-(triethylenetetramine)-cobalt(III) perchlorate top
Crystal data top
C11H23CoN5O3+·ClO4F(000) = 896
Mr = 431.72Dx = 1.671 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
a = 9.4009 (5) ŵ = 1.20 mm1
b = 13.3659 (8) ÅT = 293 K
c = 13.6588 (8) ÅBlock, red
V = 1716.25 (17) Å30.30 × 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 tubeRint = 0.044
Graphite monochromatorθmax = 27.5°, θmin = 2.1°
ϕ and ω scansh = 1210
10571 measured reflectionsk = 1517
3939 independent reflectionsl = 1717
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH 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 = 1.05Δρmax = 0.65 e Å3
3939 reflectionsΔρmin = 0.35 e Å3
227 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0015 (8)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.001 (15)
Crystal data top
C11H23CoN5O3+·ClO4V = 1716.25 (17) Å3
Mr = 431.72Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 9.4009 (5) ŵ = 1.20 mm1
b = 13.3659 (8) ÅT = 293 K
c = 13.6588 (8) Å0.30 × 0.25 × 0.23 mm
Data collection top
Bruker SMART CCD area detector
diffractometer
3573 reflections with I > 2σ(I)
10571 measured reflectionsRint = 0.044
3939 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.037H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.094Δρmax = 0.65 e Å3
S = 1.05Δρmin = 0.35 e Å3
3939 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
227 parametersAbsolute 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
xyzUiso*/Ueq
Co10.09692 (4)0.42381 (3)0.06786 (2)0.02530 (11)
Cl10.31468 (10)0.66230 (7)0.17022 (7)0.0512 (2)
C60.3642 (3)0.3419 (3)0.1201 (3)0.0427 (7)
H6A0.36650.34420.19110.051*
H6B0.43720.29590.09790.051*
C50.3898 (3)0.4439 (2)0.0788 (2)0.0408 (7)
H5A0.47290.47430.10870.049*
H5B0.40470.44040.00860.049*
C40.2487 (3)0.6035 (2)0.0569 (3)0.0463 (8)
H4A0.27140.60100.01240.056*
H4B0.31320.65000.08860.056*
C30.0955 (3)0.6358 (2)0.0719 (3)0.0466 (7)
H3A0.08100.65500.13970.056*
H3B0.07470.69320.03090.056*
C20.0562 (4)0.5532 (3)0.0545 (3)0.0511 (9)
H2A0.08170.62110.07220.061*
H2B0.14060.51180.05970.061*
C10.0573 (4)0.5148 (3)0.1226 (2)0.0511 (9)
H1A0.01540.49630.18490.061*
H1B0.12760.56660.13420.061*
C70.1465 (3)0.3202 (2)0.1131 (2)0.0340 (6)
C80.0770 (3)0.3377 (2)0.21145 (19)0.0316 (6)
H8A0.03170.27510.23210.038*
C90.1685 (3)0.3750 (3)0.2949 (2)0.0412 (7)
H9A0.20790.31990.33230.049*
H9B0.24550.41680.27130.049*
C100.0631 (3)0.4347 (3)0.3550 (2)0.0480 (9)
H10A0.02070.39370.40580.058*
H10B0.10850.49220.38500.058*
C110.0485 (3)0.4674 (3)0.2801 (2)0.0361 (7)
N40.2210 (3)0.30781 (18)0.08557 (18)0.0336 (5)
H4C0.18260.26580.12980.040*
H4D0.23000.27470.02850.040*
N30.2609 (3)0.50246 (19)0.10136 (18)0.0326 (5)
H3C0.25900.51100.16740.039*
N20.0025 (3)0.55078 (19)0.04602 (19)0.0377 (6)
H2C0.07850.55310.08730.045*
N10.1264 (2)0.42547 (19)0.07653 (16)0.0343 (5)
H1C0.22030.42640.08950.041*
H1D0.08970.36930.10270.041*
N50.0338 (2)0.41332 (19)0.20015 (16)0.0307 (5)
O10.0722 (2)0.34780 (16)0.03915 (13)0.0356 (5)
O20.2642 (2)0.2797 (2)0.10631 (18)0.0518 (6)
O30.1389 (3)0.5341 (2)0.29426 (17)0.0507 (6)
O40.2419 (10)0.6414 (4)0.2539 (5)0.213 (4)
O50.2278 (6)0.7426 (5)0.1454 (7)0.178 (3)
O60.4496 (5)0.6894 (5)0.1858 (5)0.185 (3)
O70.2997 (4)0.5756 (4)0.1138 (4)0.1223 (18)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.02347 (17)0.02985 (18)0.02259 (16)0.00162 (14)0.00177 (14)0.00275 (14)
Cl10.0433 (4)0.0492 (5)0.0609 (5)0.0002 (4)0.0016 (4)0.0107 (4)
C60.0327 (16)0.0486 (19)0.0468 (18)0.0102 (13)0.0043 (13)0.0042 (15)
C50.0234 (13)0.0503 (18)0.0486 (17)0.0024 (12)0.0038 (13)0.0007 (14)
C40.0420 (16)0.0360 (15)0.061 (2)0.0083 (12)0.0014 (17)0.0037 (15)
C30.0502 (17)0.0336 (15)0.0560 (18)0.0048 (14)0.006 (2)0.0049 (14)
C20.0504 (19)0.053 (2)0.050 (2)0.0138 (15)0.0136 (16)0.0032 (15)
C10.058 (2)0.062 (2)0.0338 (16)0.0100 (17)0.0004 (15)0.0087 (16)
C70.0326 (14)0.0363 (16)0.0332 (15)0.0070 (12)0.0042 (12)0.0083 (12)
C80.0311 (14)0.0338 (13)0.0298 (13)0.0018 (12)0.0037 (11)0.0022 (11)
C90.0351 (16)0.056 (2)0.0322 (15)0.0043 (14)0.0073 (13)0.0015 (14)
C100.0417 (17)0.075 (2)0.0277 (14)0.0068 (17)0.0081 (12)0.0120 (15)
C110.0282 (14)0.0516 (17)0.0285 (14)0.0023 (13)0.0028 (11)0.0050 (13)
N40.0375 (13)0.0336 (12)0.0298 (13)0.0013 (10)0.0044 (10)0.0013 (10)
N30.0268 (11)0.0369 (13)0.0340 (12)0.0052 (10)0.0007 (9)0.0005 (10)
N20.0291 (12)0.0438 (14)0.0401 (15)0.0074 (10)0.0019 (10)0.0002 (11)
N10.0335 (11)0.0416 (12)0.0279 (11)0.0043 (10)0.0030 (9)0.0019 (11)
N50.0270 (11)0.0410 (13)0.0242 (10)0.0043 (10)0.0041 (9)0.0076 (10)
O10.0319 (11)0.0480 (12)0.0269 (9)0.0126 (9)0.0007 (8)0.0073 (8)
O20.0449 (13)0.0629 (16)0.0475 (13)0.0269 (12)0.0081 (10)0.0116 (12)
O30.0468 (14)0.0690 (16)0.0363 (12)0.0188 (12)0.0006 (10)0.0160 (11)
O40.344 (11)0.123 (5)0.171 (6)0.072 (6)0.132 (7)0.026 (4)
O50.140 (5)0.114 (4)0.281 (9)0.044 (4)0.023 (5)0.030 (4)
O60.056 (2)0.206 (6)0.292 (8)0.018 (3)0.004 (3)0.153 (6)
O70.068 (2)0.136 (4)0.162 (4)0.032 (2)0.038 (3)0.096 (3)
Geometric parameters (Å, º) top
Co1—N51.907 (2)C4—C31.517 (4)
Co1—N31.921 (2)C3—N21.505 (4)
Co1—O11.9273 (19)C2—N21.463 (4)
Co1—N41.955 (2)C2—C11.505 (5)
Co1—N21.960 (2)C1—N11.498 (4)
Co1—N11.992 (2)C7—O21.236 (3)
Cl1—O61.336 (4)C7—O11.282 (3)
Cl1—O41.361 (6)C7—C81.512 (4)
Cl1—O51.391 (5)C8—N51.460 (4)
Cl1—O71.399 (4)C8—C91.512 (4)
C6—C51.496 (5)C9—C101.515 (5)
C6—N41.497 (4)C10—C111.529 (4)
C5—N31.476 (4)C11—O31.247 (4)
C4—N31.486 (4)C11—N51.317 (4)
N5—Co1—N393.68 (10)N2—C2—C1109.2 (3)
N5—Co1—O184.11 (9)N1—C1—C2108.6 (3)
N3—Co1—O1177.36 (10)O2—C7—O1123.7 (3)
N5—Co1—N490.58 (11)O2—C7—C8121.4 (3)
N3—Co1—N485.75 (11)O1—C7—C8114.9 (2)
O1—Co1—N495.70 (10)N5—C8—C7108.7 (2)
N5—Co1—N293.41 (11)N5—C8—C9104.9 (2)
N3—Co1—N286.85 (11)C7—C8—C9118.4 (3)
O1—Co1—N291.84 (10)C8—C9—C10102.1 (2)
N4—Co1—N2171.80 (10)C9—C10—C11103.7 (2)
N5—Co1—N1169.22 (10)O3—C11—N5126.4 (3)
N3—Co1—N196.78 (10)O3—C11—C10124.6 (3)
O1—Co1—N185.36 (9)N5—C11—C10109.0 (3)
N4—Co1—N192.77 (10)C6—N4—Co1109.51 (18)
N2—Co1—N184.60 (11)C5—N3—C4117.3 (2)
O6—Cl1—O4113.5 (5)C5—N3—Co1108.63 (18)
O6—Cl1—O5112.8 (4)C4—N3—Co1109.79 (19)
O4—Cl1—O593.9 (5)C2—N2—C3114.6 (3)
O6—Cl1—O7114.1 (3)C2—N2—Co1109.0 (2)
O4—Cl1—O7104.0 (4)C3—N2—Co1109.01 (17)
O5—Cl1—O7116.5 (4)C1—N1—Co1111.38 (19)
C5—C6—N4107.7 (2)C11—N5—C8111.6 (2)
N3—C5—C6105.8 (2)C11—N5—Co1135.4 (2)
N3—C4—C3106.0 (3)C8—N5—Co1111.92 (17)
N2—C3—C4109.6 (2)C7—O1—Co1116.14 (18)
N4—C6—C5—N349.6 (3)N4—Co1—N2—C296.9 (8)
N3—C4—C3—N245.4 (4)N1—Co1—N2—C225.3 (2)
N2—C2—C1—N142.0 (4)N5—Co1—N2—C390.2 (2)
O2—C7—C8—N5161.7 (3)N3—Co1—N2—C33.3 (2)
O1—C7—C8—N520.2 (4)O1—Co1—N2—C3174.4 (2)
O2—C7—C8—C942.2 (4)N4—Co1—N2—C328.8 (9)
O1—C7—C8—C9139.7 (3)N1—Co1—N2—C3100.4 (2)
N5—C8—C9—C1028.7 (3)C2—C1—N1—Co121.1 (3)
C7—C8—C9—C10150.1 (3)N5—Co1—N1—C178.0 (7)
C8—C9—C10—C1126.5 (4)N3—Co1—N1—C188.1 (2)
C9—C10—C11—O3165.1 (3)O1—Co1—N1—C190.4 (2)
C9—C10—C11—N515.6 (4)N4—Co1—N1—C1174.1 (2)
C5—C6—N4—Co130.4 (3)N2—Co1—N1—C11.9 (2)
N5—Co1—N4—C690.0 (2)O3—C11—N5—C8176.2 (3)
N3—Co1—N4—C63.6 (2)C10—C11—N5—C83.1 (4)
O1—Co1—N4—C6174.14 (18)O3—C11—N5—Co117.1 (6)
N2—Co1—N4—C629.2 (8)C10—C11—N5—Co1163.6 (3)
N1—Co1—N4—C6100.2 (2)C7—C8—N5—C11148.2 (3)
C6—C5—N3—C4171.9 (3)C9—C8—N5—C1120.7 (3)
C6—C5—N3—Co146.7 (3)C7—C8—N5—Co121.7 (3)
C3—C4—N3—C5167.1 (3)C9—C8—N5—Co1149.3 (2)
C3—C4—N3—Co142.5 (3)N3—Co1—N5—C1126.3 (3)
N5—Co1—N3—C5114.7 (2)O1—Co1—N5—C11152.3 (3)
O1—Co1—N3—C5148 (2)N4—Co1—N5—C11112.0 (3)
N4—Co1—N3—C524.35 (19)N2—Co1—N5—C1160.8 (3)
N2—Co1—N3—C5152.1 (2)N1—Co1—N5—C11139.8 (5)
N1—Co1—N3—C567.9 (2)N3—Co1—N5—C8167.1 (2)
N5—Co1—N3—C4115.8 (2)O1—Co1—N5—C814.36 (19)
O1—Co1—N3—C483 (2)N4—Co1—N5—C881.3 (2)
N4—Co1—N3—C4153.9 (2)N2—Co1—N5—C8105.9 (2)
N2—Co1—N3—C422.6 (2)N1—Co1—N5—C826.8 (7)
N1—Co1—N3—C461.6 (2)O2—C7—O1—Co1172.7 (3)
C1—C2—N2—C378.7 (4)C8—C7—O1—Co19.2 (3)
C1—C2—N2—Co143.7 (3)N5—Co1—O1—C72.9 (2)
C4—C3—N2—C294.5 (3)N3—Co1—O1—C736 (2)
C4—C3—N2—Co128.0 (3)N4—Co1—O1—C787.1 (2)
N5—Co1—N2—C2144.1 (2)N2—Co1—O1—C796.1 (2)
N3—Co1—N2—C2122.4 (2)N1—Co1—O1—C7179.5 (2)
O1—Co1—N2—C259.8 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N4—H4C···O4i0.902.373.129 (7)143
N4—H4D···O2ii0.901.982.873 (3)171
N4—H4D···O1ii0.902.643.318 (3)132
N3—H3C···O30.912.092.904 (3)148
N2—H2C···O70.912.132.962 (4)151
N1—H1D···O2ii0.902.422.957 (4)119
N1—H1C···O3iii0.902.132.876 (3)139
Symmetry codes: (i) x, y1/2, z+1/2; (ii) x+1/2, y+1/2, z; (iii) x+1/2, y+1, z1/2.
(4) (L-isoleucinato)-(triethylenetetramine)-cobalt(III) diiodide monohydrate top
Crystal data top
C12H30CoN5O22+·2(I)·H2OF(000) = 1180
Mr = 606.15Dx = 1.859 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
a = 10.053 (2) ŵ = 3.66 mm1
b = 11.540 (2) ÅT = 293 K
c = 18.664 (4) ÅBlock, yellow
V = 2165.2 (7) Å30.30 × 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 tubeRint = 0.022
Graphite monochromatorθmax = 27.5°, θmin = 2.1°
ϕ and ω scansh = 135
7861 measured reflectionsk = 1315
4811 independent reflectionsl = 247
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH 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 = 1.02Δρmax = 1.16 e Å3
4811 reflectionsΔρmin = 0.77 e Å3
317 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0022 (2)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.02 (2)
Crystal data top
C12H30CoN5O22+·2(I)·H2OV = 2165.2 (7) Å3
Mr = 606.15Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 10.053 (2) ŵ = 3.66 mm1
b = 11.540 (2) ÅT = 293 K
c = 18.664 (4) Å0.30 × 0.15 × 0.10 mm
Data collection top
Bruker SMART CCD area detector
diffractometer
4240 reflections with I > 2σ(I)
7861 measured reflectionsRint = 0.022
4811 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.032H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.078Δρmax = 1.16 e Å3
S = 1.02Δρmin = 0.77 e Å3
4811 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
317 parametersAbsolute 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
xyzUiso*/Ueq
Co0.37838 (5)0.49364 (5)0.15239 (3)0.02180 (12)
I10.81567 (4)0.72191 (3)0.160537 (19)0.05131 (12)
I20.17425 (4)0.70985 (3)0.439873 (17)0.05258 (12)
C10.1672 (6)0.3324 (5)0.1279 (3)0.0475 (13)
H40.132 (7)0.324 (7)0.081 (4)0.08 (2)*
H30.132 (8)0.251 (7)0.149 (4)0.09 (2)*
C20.1113 (6)0.4310 (5)0.1714 (3)0.0422 (12)
H60.122 (6)0.413 (5)0.226 (3)0.059 (18)*
H50.017 (6)0.459 (4)0.160 (3)0.037 (14)*
C30.1521 (6)0.5937 (6)0.0862 (3)0.0432 (13)
H80.129 (5)0.542 (5)0.065 (3)0.026 (14)*
H90.072 (7)0.642 (6)0.095 (3)0.053 (17)*
C40.2723 (5)0.6436 (5)0.0517 (3)0.0351 (11)
H110.296 (4)0.707 (4)0.073 (2)0.016 (10)*
H100.259 (5)0.674 (4)0.003 (3)0.034 (13)*
C50.5133 (5)0.5837 (5)0.0336 (2)0.0368 (11)
H140.544 (5)0.664 (4)0.065 (2)0.027 (12)*
H130.524 (5)0.602 (5)0.020 (3)0.038 (14)*
C60.5988 (6)0.4847 (5)0.0570 (3)0.0399 (11)
H160.697 (6)0.487 (5)0.053 (3)0.046 (15)*
H150.573 (7)0.412 (6)0.031 (4)0.07 (2)*
C70.4426 (4)0.6553 (4)0.2538 (2)0.0248 (9)
C80.4159 (5)0.5495 (4)0.3007 (2)0.0262 (9)
H190.322 (6)0.574 (4)0.328 (2)0.033 (12)*
C90.5279 (5)0.5289 (4)0.3555 (2)0.0349 (11)
H220.533 (4)0.607 (3)0.3783 (19)0.005 (9)*
C100.4857 (8)0.4327 (6)0.4069 (3)0.0528 (16)
H250.388 (9)0.432 (7)0.421 (4)0.09 (3)*
H240.473 (5)0.353 (5)0.378 (3)0.031 (13)*
H230.540 (9)0.425 (7)0.443 (4)0.08 (2)*
C110.6621 (6)0.5066 (6)0.3198 (3)0.0476 (13)
H270.663 (6)0.444 (5)0.293 (3)0.052 (17)*
H260.689 (6)0.587 (5)0.286 (3)0.051 (16)*
C120.7774 (7)0.4960 (7)0.3728 (4)0.0687 (19)
H300.85850.48230.34700.103*
H290.76090.43260.40490.103*
H280.78510.56660.39980.103*
N10.3132 (4)0.3389 (3)0.1284 (2)0.0294 (8)
H20.349 (5)0.321 (4)0.092 (3)0.031 (14)*
H10.344 (6)0.275 (5)0.159 (3)0.046 (15)*
N20.1910 (4)0.5375 (3)0.15546 (19)0.0308 (8)
H70.170 (5)0.600 (4)0.188 (2)0.022 (11)*
N30.3742 (4)0.5513 (3)0.05455 (18)0.0281 (8)
H120.344 (4)0.488 (4)0.028 (2)0.012 (9)*
N40.5678 (4)0.4598 (4)0.1334 (2)0.0297 (9)
H180.590 (6)0.392 (5)0.139 (3)0.045 (17)*
H170.620 (5)0.509 (4)0.152 (2)0.023 (11)*
N50.3896 (5)0.4486 (3)0.25377 (18)0.0256 (8)
H210.310 (6)0.412 (5)0.267 (3)0.044 (15)*
H200.451 (6)0.402 (5)0.255 (3)0.036 (16)*
O10.4289 (3)0.6428 (3)0.18546 (15)0.0275 (6)
OW10.1273 (6)0.7210 (6)0.2522 (3)0.103 (2)
O20.4702 (4)0.7479 (3)0.28221 (17)0.0349 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co0.0234 (3)0.0203 (2)0.0216 (2)0.0002 (2)0.0011 (2)0.0002 (2)
I10.03795 (19)0.0610 (2)0.0550 (2)0.01032 (19)0.00159 (16)0.01078 (17)
I20.0564 (2)0.0619 (2)0.03946 (17)0.0038 (2)0.00252 (16)0.01354 (16)
C10.043 (3)0.048 (3)0.052 (3)0.015 (3)0.003 (3)0.006 (2)
C20.027 (3)0.052 (3)0.048 (3)0.001 (2)0.001 (2)0.003 (2)
C30.037 (3)0.057 (4)0.036 (2)0.007 (3)0.007 (2)0.002 (2)
C40.041 (3)0.033 (3)0.031 (2)0.011 (2)0.006 (2)0.003 (2)
C50.039 (3)0.043 (3)0.027 (2)0.001 (2)0.007 (2)0.008 (2)
C60.035 (3)0.050 (3)0.035 (2)0.009 (2)0.007 (2)0.003 (2)
C70.024 (2)0.022 (2)0.028 (2)0.0036 (18)0.0017 (17)0.0016 (16)
C80.032 (3)0.021 (2)0.026 (2)0.0009 (19)0.0002 (17)0.0018 (16)
C90.049 (3)0.028 (2)0.028 (2)0.009 (2)0.010 (2)0.0015 (18)
C100.072 (5)0.055 (4)0.031 (3)0.016 (3)0.009 (3)0.016 (3)
C110.038 (3)0.058 (3)0.047 (3)0.000 (3)0.013 (2)0.002 (3)
C120.046 (4)0.075 (4)0.085 (4)0.011 (4)0.030 (3)0.016 (4)
N10.034 (2)0.0245 (18)0.0298 (18)0.0010 (18)0.0036 (18)0.0022 (14)
N20.0221 (19)0.038 (2)0.0318 (17)0.0008 (16)0.0025 (17)0.0014 (16)
N30.032 (2)0.0287 (18)0.0239 (16)0.0034 (17)0.0033 (15)0.0016 (15)
N40.029 (2)0.028 (2)0.0326 (19)0.0023 (18)0.0004 (16)0.0003 (15)
N50.031 (2)0.0204 (17)0.0255 (17)0.0064 (18)0.0020 (16)0.0002 (14)
O10.0343 (18)0.0236 (15)0.0247 (14)0.0012 (14)0.0014 (12)0.0009 (11)
OW10.079 (4)0.155 (6)0.076 (3)0.060 (4)0.022 (3)0.049 (4)
O20.048 (2)0.0198 (15)0.0372 (16)0.0039 (14)0.0027 (15)0.0042 (12)
Geometric parameters (Å, º) top
Co—O11.898 (3)C7—O21.225 (5)
Co—N31.944 (3)C7—O11.291 (5)
Co—N21.951 (4)C7—C81.525 (6)
Co—N11.954 (4)C8—N51.481 (5)
Co—N51.966 (4)C8—C91.540 (6)
Co—N41.976 (4)C8—H191.11 (5)
C1—N11.470 (7)C9—C101.526 (7)
C1—C21.507 (8)C9—C111.527 (8)
C1—H40.96 (7)C9—H221.00 (4)
C1—H31.08 (8)C10—H251.02 (9)
C2—N21.498 (7)C10—H241.08 (5)
C2—H61.05 (6)C10—H230.86 (9)
C2—H51.03 (6)C11—C121.529 (8)
C3—C41.484 (8)C11—H270.88 (6)
C3—N21.498 (6)C11—H261.15 (6)
C3—H80.75 (5)C12—H300.9600
C3—H90.99 (7)C12—H290.9600
C4—N31.479 (6)C12—H280.9600
C4—H110.87 (5)N1—H20.79 (5)
C4—H100.98 (5)N1—H10.99 (6)
C5—C61.495 (8)N2—H70.96 (4)
C5—N31.499 (6)N3—H120.93 (4)
C5—H141.14 (5)N4—H180.82 (6)
C5—H131.02 (5)N4—H170.84 (5)
C6—N41.486 (6)N5—H210.93 (6)
C6—H160.99 (6)N5—H200.82 (6)
C6—H151.01 (7)
O1—Co—N390.05 (14)C7—C8—H19102 (2)
O1—Co—N290.76 (15)C9—C8—H19111 (2)
N3—Co—N285.29 (16)C10—C9—C11113.4 (5)
O1—Co—N1173.26 (16)C10—C9—C8109.1 (5)
N3—Co—N195.17 (16)C11—C9—C8112.4 (4)
N2—Co—N185.44 (17)C10—C9—H22114 (2)
O1—Co—N584.94 (13)C11—C9—H22107 (2)
N3—Co—N5174.93 (16)C8—C9—H22100 (2)
N2—Co—N595.50 (17)C9—C10—H25115 (5)
N1—Co—N589.88 (16)C9—C10—H24110 (3)
O1—Co—N488.84 (17)H25—C10—H2491 (5)
N3—Co—N485.39 (16)C9—C10—H23113 (5)
N2—Co—N4170.67 (16)H25—C10—H23114 (7)
N1—Co—N495.81 (19)H24—C10—H23112 (6)
N5—Co—N493.75 (18)C9—C11—C12113.6 (5)
N1—C1—C2109.3 (4)C9—C11—H27114 (4)
N1—C1—H4112 (4)C12—C11—H27107 (4)
C2—C1—H4116 (5)C9—C11—H26108 (3)
N1—C1—H3112 (4)C12—C11—H26104 (3)
C2—C1—H3110 (4)H27—C11—H26110 (5)
H4—C1—H397 (6)C11—C12—H30109.5
N2—C2—C1108.3 (4)C11—C12—H29109.5
N2—C2—H6107 (3)H30—C12—H29109.5
C1—C2—H6110 (3)C11—C12—H28109.5
N2—C2—H5102 (3)H30—C12—H28109.5
C1—C2—H5118 (3)H29—C12—H28109.5
H6—C2—H5111 (5)C1—N1—Co112.5 (3)
C4—C3—N2109.3 (4)C1—N1—H2116 (4)
C4—C3—H8110 (4)Co—N1—H2106 (4)
N2—C3—H8101 (4)C1—N1—H1106 (3)
C4—C3—H9121 (4)Co—N1—H1116 (3)
N2—C3—H9108 (4)H2—N1—H199 (5)
H8—C3—H9106 (6)C2—N2—C3112.8 (4)
N3—C4—C3105.6 (4)C2—N2—Co108.0 (3)
N3—C4—H11114 (3)C3—N2—Co109.8 (3)
C3—C4—H11111 (3)C2—N2—H7112 (3)
N3—C4—H10112 (3)C3—N2—H799 (2)
C3—C4—H10115 (3)Co—N2—H7115 (3)
H11—C4—H1099 (4)C4—N3—C5117.2 (4)
C6—C5—N3105.6 (4)C4—N3—Co107.2 (3)
C6—C5—H14108 (2)C5—N3—Co108.1 (3)
N3—C5—H14109 (2)C4—N3—H12109 (3)
C6—C5—H13112 (3)C5—N3—H12111 (3)
N3—C5—H13114 (3)Co—N3—H12104 (2)
H14—C5—H13108 (4)C6—N4—Co109.6 (3)
N4—C6—C5107.9 (4)C6—N4—H18105 (4)
N4—C6—H16107 (3)Co—N4—H18115 (4)
C5—C6—H16122 (3)C6—N4—H1798 (3)
N4—C6—H15104 (4)Co—N4—H17113 (3)
C5—C6—H15111 (4)H18—N4—H17115 (5)
H16—C6—H15104 (5)C8—N5—Co111.8 (3)
O2—C7—O1123.3 (4)C8—N5—H21110 (3)
O2—C7—C8119.4 (4)Co—N5—H21109 (3)
O1—C7—C8117.3 (4)C8—N5—H20111 (4)
N5—C8—C7108.8 (3)Co—N5—H20104 (4)
N5—C8—C9113.7 (4)H21—N5—H20110 (5)
C7—C8—C9112.1 (4)C7—O1—Co116.8 (3)
N5—C8—H19108 (3)
N1—C1—C2—N240.7 (6)C3—C4—N3—Co49.1 (4)
N2—C3—C4—N347.7 (6)C6—C5—N3—C4167.5 (4)
N3—C5—C6—N451.1 (5)C6—C5—N3—Co46.4 (4)
O2—C7—C8—N5178.1 (4)O1—Co—N3—C461.5 (3)
O1—C7—C8—N54.8 (6)N2—Co—N3—C429.3 (3)
O2—C7—C8—C951.4 (6)N1—Co—N3—C4114.3 (3)
O1—C7—C8—C9131.5 (4)N5—Co—N3—C470 (2)
N5—C8—C9—C1063.8 (5)N4—Co—N3—C4150.3 (3)
C7—C8—C9—C10172.3 (4)O1—Co—N3—C565.7 (3)
N5—C8—C9—C1162.8 (5)N2—Co—N3—C5156.4 (3)
C7—C8—C9—C1161.1 (5)N1—Co—N3—C5118.6 (3)
C10—C9—C11—C1260.6 (7)N5—Co—N3—C557 (2)
C8—C9—C11—C12175.1 (5)N4—Co—N3—C523.2 (3)
C2—C1—N1—Co20.7 (5)C5—C6—N4—Co32.5 (5)
O1—Co—N1—C153.4 (15)O1—Co—N4—C695.3 (4)
N3—Co—N1—C187.3 (4)N3—Co—N4—C65.2 (4)
N2—Co—N1—C12.4 (4)N2—Co—N4—C67.7 (13)
N5—Co—N1—C193.1 (4)N1—Co—N4—C689.6 (4)
N4—Co—N1—C1173.1 (3)N5—Co—N4—C6179.8 (3)
C1—C2—N2—C379.4 (5)C7—C8—N5—Co6.7 (5)
C1—C2—N2—Co42.2 (5)C9—C8—N5—Co132.4 (3)
C4—C3—N2—C2144.9 (5)O1—Co—N5—C85.5 (3)
C4—C3—N2—Co24.4 (6)N3—Co—N5—C814 (2)
O1—Co—N2—C2149.5 (3)N2—Co—N5—C884.7 (3)
N3—Co—N2—C2120.5 (3)N1—Co—N5—C8170.2 (3)
N1—Co—N2—C224.9 (3)N4—Co—N5—C894.0 (3)
N5—Co—N2—C264.5 (3)O2—C7—O1—Co177.4 (4)
N4—Co—N2—C2123.0 (11)C8—C7—O1—Co0.4 (5)
O1—Co—N2—C387.2 (4)N3—Co—O1—C7177.8 (3)
N3—Co—N2—C32.8 (4)N2—Co—O1—C792.5 (3)
N1—Co—N2—C398.4 (4)N1—Co—O1—C736.9 (15)
N5—Co—N2—C3172.1 (4)N5—Co—O1—C73.0 (3)
N4—Co—N2—C30.3 (13)N4—Co—O1—C796.8 (3)
C3—C4—N3—C5170.7 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N4—H18···O2i0.82 (6)2.30 (6)2.934 (5)134 (5)
N2—H7···OW10.96 (4)1.89 (5)2.856 (6)179 (4)
N5—H21···I1i0.93 (6)2.87 (6)3.695 (4)148 (4)
N4—H17···I10.84 (5)3.16 (6)3.951 (5)158 (4)
N3—H12···I2ii0.93 (4)2.82 (4)3.728 (4)165 (3)
N1—H2···I2ii0.79 (5)2.87 (5)3.565 (4)147 (5)
N1—H1···O2i0.99 (6)2.18 (6)2.937 (5)132 (4)
N5—H20···O2i0.82 (6)2.07 (6)2.793 (5)147 (5)
Symmetry codes: (i) x+1, y1/2, z+1/2; (ii) x+1/2, y+1, z1/2.
(5) (L-isoleucinato)-(triethylenetetramine)-cobalt(III) diperchlorate dihydrate top
Crystal data top
C12H30CoN5O22+·2(ClO4)·2(H2O)F(000) = 1192
Mr = 570.27Dx = 1.631 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
a = 11.5333 (11) ŵ = 1.04 mm1
b = 13.3726 (14) ÅT = 293 K
c = 15.0622 (15) ÅBlock, yellow
V = 2323.0 (4) Å30.35 × 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 tubeRint = 0.032
Graphite monochromatorθmax = 27.0°, θmin = 2.0°
ϕ and ω scansh = 1313
8345 measured reflectionsk = 177
4922 independent reflectionsl = 196
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.041H 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 reflectionsΔρmax = 0.59 e Å3
293 parametersΔρmin = 0.32 e Å3
0 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.007 (17)
Crystal data top
C12H30CoN5O22+·2(ClO4)·2(H2O)V = 2323.0 (4) Å3
Mr = 570.27Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 11.5333 (11) ŵ = 1.04 mm1
b = 13.3726 (14) ÅT = 293 K
c = 15.0622 (15) Å0.35 × 0.30 × 0.28 mm
Data collection top
Buker SMART CCD area detector
diffractometer
3537 reflections with I > 2σ(I)
8345 measured reflectionsRint = 0.032
4922 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.041H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.085Δρmax = 0.59 e Å3
S = 0.90Δρmin = 0.32 e Å3
4922 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
293 parametersAbsolute 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
xyzUiso*/Ueq
Co0.04919 (4)0.58677 (4)0.03034 (3)0.02426 (12)
Cl10.79559 (11)0.70122 (8)0.27852 (7)0.0462 (3)
Cl20.33328 (11)0.74231 (8)0.25777 (7)0.0463 (3)
C10.1916 (4)0.4669 (3)0.1393 (3)0.0410 (11)
H1A0.26560.46550.17000.049*
H1B0.17130.39890.12310.049*
C20.0997 (4)0.5102 (3)0.1993 (3)0.0398 (11)
H2A0.08050.46320.24600.048*
H2B0.12730.57150.22640.048*
C30.0757 (4)0.4395 (3)0.1284 (3)0.0410 (12)
H3A0.14300.44070.16700.049*
H3B0.03090.38010.14200.049*
C40.1142 (4)0.4371 (3)0.0322 (3)0.0416 (11)
H4A0.14160.37090.01630.050*
H4B0.17610.48480.02210.050*
C50.0289 (4)0.4796 (3)0.1167 (3)0.0391 (11)
H5A0.09810.51910.12690.047*
H5B0.03710.41600.14700.047*
C60.0767 (4)0.5341 (3)0.1491 (3)0.0388 (11)
H6A0.14410.49080.14620.047*
H6B0.06590.55490.21030.047*
C70.1051 (3)0.7415 (3)0.0327 (3)0.0253 (8)
C80.0039 (3)0.7898 (3)0.0778 (3)0.0255 (8)
H8A0.02620.79960.14000.031*
C90.0263 (3)0.8928 (2)0.0408 (3)0.0308 (10)
H9A0.04380.93390.04530.037*
C100.0598 (4)0.8892 (3)0.0575 (3)0.0363 (10)
H10A0.00560.84620.08860.044*
H10B0.13630.85960.06280.044*
C110.0606 (4)0.9920 (3)0.1022 (3)0.0542 (13)
H11A0.08230.98480.16340.081*
H11B0.11551.03460.07270.081*
H11C0.01531.02110.09850.081*
C120.1194 (4)0.9436 (3)0.0970 (3)0.0443 (11)
H12A0.13701.00800.07230.067*
H12B0.18820.90310.09730.067*
H12C0.09170.95150.15660.067*
N10.2004 (2)0.5297 (2)0.0586 (2)0.0308 (8)
H1C0.22540.49230.01270.037*
H1D0.25200.57910.06760.037*
N20.0035 (3)0.5307 (2)0.1439 (2)0.0327 (8)
H2C0.04790.57720.17190.039*
N30.0105 (3)0.4638 (2)0.0204 (2)0.0325 (8)
H3C0.04360.41500.01320.039*
N40.0934 (3)0.6222 (2)0.0915 (2)0.0310 (8)
H4C0.04930.67320.11090.037*
H4D0.16810.64150.09290.037*
N50.0954 (2)0.7174 (2)0.0778 (2)0.0265 (7)
H5C0.12180.70980.13360.032*
H5D0.15350.74240.04460.032*
O10.0960 (2)0.64899 (18)0.00997 (17)0.0296 (6)
O20.1949 (2)0.79101 (18)0.01893 (19)0.0367 (7)
O30.2118 (4)0.7632 (4)0.2603 (4)0.1271 (19)
O40.3381 (4)0.6508 (3)0.2116 (3)0.0976 (14)
O50.3891 (7)0.8157 (4)0.2193 (4)0.198 (3)
O60.3616 (5)0.7269 (4)0.3456 (3)0.131 (2)
O70.7679 (3)0.6126 (2)0.2337 (3)0.0876 (13)
O80.7521 (4)0.7845 (3)0.2327 (3)0.0928 (14)
O90.7572 (3)0.6988 (3)0.3676 (2)0.0727 (11)
O100.9200 (3)0.7076 (3)0.2791 (3)0.0875 (13)
OW10.4657 (3)0.7643 (3)0.5126 (2)0.0751 (11)
HW10.41870.79270.47190.14 (3)*
HW20.41600.77630.57620.27 (5)*
OW20.1779 (4)0.6161 (3)0.4460 (3)0.0868 (13)
HW30.11910.66950.47110.23 (4)*
HW40.23110.66340.41400.16 (3)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co0.0206 (2)0.0221 (2)0.0302 (3)0.0002 (2)0.0013 (3)0.0012 (3)
Cl10.0588 (8)0.0422 (6)0.0375 (6)0.0014 (6)0.0010 (6)0.0033 (5)
Cl20.0513 (7)0.0473 (6)0.0402 (6)0.0002 (6)0.0002 (6)0.0045 (6)
C10.037 (3)0.039 (2)0.047 (3)0.004 (2)0.011 (2)0.012 (2)
C20.041 (3)0.045 (2)0.033 (2)0.010 (2)0.008 (2)0.010 (2)
C30.035 (3)0.033 (2)0.055 (3)0.0083 (18)0.006 (2)0.008 (2)
C40.032 (2)0.033 (2)0.060 (3)0.0095 (18)0.001 (2)0.004 (2)
C50.039 (3)0.034 (2)0.044 (3)0.000 (2)0.011 (2)0.007 (2)
C60.046 (3)0.037 (2)0.034 (2)0.006 (2)0.001 (2)0.006 (2)
C70.022 (2)0.026 (2)0.0275 (19)0.0037 (16)0.0028 (19)0.002 (2)
C80.0187 (19)0.0254 (19)0.032 (2)0.0041 (17)0.0016 (17)0.0010 (17)
C90.027 (2)0.023 (2)0.043 (2)0.0011 (15)0.0006 (19)0.0009 (19)
C100.034 (2)0.032 (2)0.042 (2)0.000 (2)0.004 (2)0.0026 (17)
C110.054 (3)0.052 (3)0.057 (3)0.003 (3)0.002 (3)0.022 (2)
C120.045 (3)0.034 (2)0.054 (3)0.0094 (19)0.002 (2)0.003 (2)
N10.0256 (18)0.0295 (17)0.0372 (19)0.0015 (15)0.0015 (15)0.0020 (15)
N20.0319 (19)0.0306 (17)0.0354 (19)0.0010 (16)0.0047 (16)0.0027 (16)
N30.0313 (18)0.0277 (16)0.039 (2)0.0008 (14)0.0007 (17)0.0015 (17)
N40.0301 (19)0.0276 (17)0.035 (2)0.0007 (14)0.0014 (16)0.0009 (15)
N50.0215 (16)0.0265 (17)0.0316 (17)0.0002 (14)0.0048 (14)0.0016 (14)
O10.0198 (13)0.0272 (14)0.0419 (17)0.0012 (11)0.0058 (12)0.0000 (12)
O20.0224 (14)0.0319 (14)0.0559 (18)0.0022 (12)0.0032 (15)0.0023 (14)
O30.099 (4)0.150 (5)0.132 (4)0.044 (3)0.013 (3)0.047 (4)
O40.114 (3)0.072 (2)0.108 (3)0.011 (3)0.003 (3)0.027 (3)
O50.310 (8)0.127 (4)0.158 (5)0.140 (5)0.076 (6)0.012 (4)
O60.186 (5)0.135 (4)0.071 (3)0.031 (4)0.060 (3)0.018 (3)
O70.102 (3)0.057 (2)0.104 (3)0.007 (2)0.012 (3)0.037 (2)
O80.144 (4)0.065 (2)0.069 (3)0.036 (3)0.019 (3)0.004 (2)
O90.087 (3)0.082 (2)0.049 (2)0.010 (2)0.025 (2)0.005 (2)
O100.059 (3)0.125 (3)0.078 (3)0.018 (2)0.010 (2)0.014 (3)
OW10.092 (3)0.069 (2)0.064 (2)0.023 (2)0.003 (3)0.010 (2)
OW20.083 (3)0.078 (3)0.099 (3)0.021 (2)0.020 (3)0.035 (2)
Geometric parameters (Å, º) top
Co—O11.895 (2)C2—N21.479 (5)
Co—N31.940 (3)C3—N21.494 (5)
Co—N11.951 (3)C3—C41.516 (6)
Co—N51.961 (3)C4—N31.478 (5)
Co—N41.963 (3)C5—N31.480 (5)
Co—N21.964 (3)C5—C61.501 (6)
Cl1—O71.401 (3)C6—N41.476 (5)
Cl1—O81.403 (4)C7—O21.247 (4)
Cl1—O91.413 (3)C7—O11.288 (4)
Cl1—O101.437 (4)C7—C81.496 (5)
Cl2—O51.309 (5)C8—N51.499 (4)
Cl2—O61.378 (4)C8—C91.527 (5)
Cl2—O41.408 (4)C9—C121.527 (5)
Cl2—O31.429 (5)C9—C101.531 (5)
C1—N11.482 (5)C10—C111.531 (5)
C1—C21.509 (6)
O1—Co—N389.69 (12)N1—C1—C2108.8 (3)
O1—Co—N1175.75 (13)N2—C2—C1107.4 (3)
N3—Co—N194.09 (13)N2—C3—C4109.3 (3)
O1—Co—N584.72 (11)N3—C4—C3105.7 (3)
N3—Co—N5174.35 (12)N3—C5—C6105.8 (3)
N1—Co—N591.52 (12)N4—C6—C5107.6 (3)
O1—Co—N488.41 (12)O2—C7—O1122.2 (3)
N3—Co—N485.88 (13)O2—C7—C8119.7 (3)
N1—Co—N493.78 (13)O1—C7—C8118.1 (3)
N5—Co—N493.16 (13)C7—C8—N5108.5 (3)
O1—Co—N292.02 (12)C7—C8—C9113.6 (3)
N3—Co—N284.81 (13)N5—C8—C9114.1 (3)
N1—Co—N286.41 (13)C8—C9—C12111.1 (3)
N5—Co—N296.16 (13)C8—C9—C10112.5 (3)
N4—Co—N2170.68 (13)C12—C9—C10111.8 (3)
O7—Cl1—O8110.6 (2)C9—C10—C11113.5 (3)
O7—Cl1—O9111.5 (2)C1—N1—Co109.9 (2)
O8—Cl1—O9111.9 (3)C2—N2—C3112.7 (3)
O7—Cl1—O10106.3 (3)C2—N2—Co108.2 (2)
O8—Cl1—O10108.3 (3)C3—N2—Co110.4 (2)
O9—Cl1—O10108.0 (2)C4—N3—C5116.4 (3)
O5—Cl2—O6114.9 (4)C4—N3—Co106.3 (2)
O5—Cl2—O4114.4 (3)C5—N3—Co108.4 (2)
O6—Cl2—O4109.6 (3)C6—N4—Co108.9 (2)
O5—Cl2—O3110.3 (4)C8—N5—Co111.6 (2)
O6—Cl2—O3103.7 (3)C7—O1—Co116.7 (2)
O4—Cl2—O3102.8 (3)
N1—C1—C2—N247.6 (4)C3—C4—N3—Co51.5 (3)
N2—C3—C4—N344.0 (4)C6—C5—N3—C4163.7 (3)
N3—C5—C6—N452.1 (4)C6—C5—N3—Co43.9 (3)
O2—C7—C8—N5174.5 (3)O1—Co—N3—C457.2 (3)
O1—C7—C8—N56.1 (5)N1—Co—N3—C4120.9 (3)
O2—C7—C8—C946.5 (5)N5—Co—N3—C465.3 (15)
O1—C7—C8—C9134.1 (3)N4—Co—N3—C4145.6 (3)
C7—C8—C9—C12172.7 (3)N2—Co—N3—C434.9 (2)
N5—C8—C9—C1262.3 (4)O1—Co—N3—C568.6 (2)
C7—C8—C9—C1061.1 (4)N1—Co—N3—C5113.3 (2)
N5—C8—C9—C1064.0 (4)N5—Co—N3—C560.5 (15)
C8—C9—C10—C11165.4 (3)N4—Co—N3—C519.8 (2)
C12—C9—C10—C1168.8 (5)N2—Co—N3—C5160.7 (3)
C2—C1—N1—Co31.7 (4)C5—C6—N4—Co36.0 (4)
O1—Co—N1—C175.5 (17)O1—Co—N4—C699.1 (3)
N3—Co—N1—C177.4 (3)N3—Co—N4—C69.3 (3)
N5—Co—N1—C1103.2 (3)N1—Co—N4—C684.6 (3)
N4—Co—N1—C1163.5 (2)N5—Co—N4—C6176.3 (2)
N2—Co—N1—C17.2 (2)N2—Co—N4—C66.2 (10)
C1—C2—N2—C381.5 (4)C7—C8—N5—Co5.6 (4)
C1—C2—N2—Co40.9 (4)C9—C8—N5—Co133.4 (3)
C4—C3—N2—C2137.6 (3)O1—Co—N5—C83.3 (2)
C4—C3—N2—Co16.5 (4)N3—Co—N5—C811.5 (15)
O1—Co—N2—C2156.8 (3)N1—Co—N5—C8174.7 (2)
N3—Co—N2—C2113.7 (3)N4—Co—N5—C891.4 (2)
N1—Co—N2—C219.2 (3)N2—Co—N5—C888.1 (2)
N5—Co—N2—C271.9 (3)O2—C7—O1—Co176.9 (3)
N4—Co—N2—C2110.7 (8)C8—C7—O1—Co3.7 (4)
O1—Co—N2—C379.4 (2)N3—Co—O1—C7179.1 (3)
N3—Co—N2—C310.1 (2)N1—Co—O1—C728.0 (18)
N1—Co—N2—C3104.5 (2)N5—Co—O1—C70.1 (3)
N5—Co—N2—C3164.3 (2)N4—Co—O1—C793.2 (3)
N4—Co—N2—C313.1 (9)N2—Co—O1—C796.1 (3)
C3—C4—N3—C5172.3 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1C···OW2i0.902.092.940 (5)158
N1—H1D···O2ii0.902.262.928 (4)131
N1—H1D···O40.902.573.234 (5)131
N2—H2C···O7iii0.912.373.159 (5)146
N2—H2C···O10iii0.912.403.244 (5)153
N2—H2C···Cl1iii0.912.933.832 (3)171
N3—H3C···OW1i0.912.433.134 (4)134
N4—H4C···O5iv0.902.473.154 (7)133
N4—H4D···O2ii0.902.132.916 (4)145
N4—H4D···O8iv0.902.523.071 (5)120
N5—H5C···O30.902.293.120 (6)154
N5—H5D···O2ii0.902.042.825 (4)145
OW1—HW1···O60.902.202.832 (6)127
OW1—HW2···O9v1.132.053.047 (5)146
OW1—HW2···O10v1.132.193.203 (5)148
OW2—HW3···OW1v1.061.992.989 (5)156
OW2—HW4···O61.002.012.995 (7)166
Symmetry codes: (i) x+1/2, y+1, z1/2; (ii) x+1/2, y+3/2, z; (iii) x1, y, z; (iv) x1/2, y+3/2, z; (v) x1/2, 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 = 570.27Dx = 1.597 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
a = 8.7716 (8) ŵ = 1.01 mm1
b = 12.6294 (15) ÅT = 293 K
c = 21.413 (4) ÅPlate, yellow
V = 2372.1 (5) Å30.34 × 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 tubeRint = 0.022
Graphite monochromatorθmax = 30.1°, θmin = 4.0°
ϕ and ω scansh = 1212
17247 measured reflectionsk = 1711
6815 independent reflectionsl = 3021
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.036H 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 reflectionsΔρmax = 0.55 e Å3
289 parametersΔρmin = 0.27 e Å3
0 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.003 (11)
Crystal data top
C12H30CoN5O22+·2(ClO4)·2(H2O)V = 2372.1 (5) Å3
Mr = 570.27Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 8.7716 (8) ŵ = 1.01 mm1
b = 12.6294 (15) ÅT = 293 K
c = 21.413 (4) Å0.34 × 0.25 × 0.13 mm
Data collection top
Bruker SMART CCD area detector
diffractometer
5824 reflections with I > 2σ(I)
17247 measured reflectionsRint = 0.022
6815 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.036H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.100Δρmax = 0.55 e Å3
S = 1.00Δρmin = 0.27 e Å3
6815 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
289 parametersAbsolute 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
xyzUiso*/Ueq
Co0.07192 (3)0.06767 (2)0.154788 (12)0.03001 (8)
Cl10.38665 (9)0.27409 (7)0.34015 (5)0.0731 (3)
Cl20.67091 (8)0.32902 (6)0.06836 (3)0.04992 (16)
N10.0661 (2)0.21240 (14)0.12129 (8)0.0348 (4)
H1C0.01760.21260.08430.042*
H1D0.01450.25470.14760.042*
N20.2909 (2)0.09097 (16)0.16718 (9)0.0395 (4)
H2C0.31910.06440.20500.047*
N30.1308 (3)0.00597 (15)0.07546 (9)0.0402 (5)
H3C0.14300.05930.04730.048*
N40.1398 (3)0.03772 (18)0.13000 (10)0.0453 (5)
H4C0.17980.01220.15510.054*
H4D0.19670.09670.13350.054*
N50.0111 (3)0.11134 (14)0.23972 (9)0.0370 (4)
H5C0.06280.17000.25060.044*
H5D0.08910.12700.24010.044*
O10.0814 (2)0.06961 (12)0.19010 (7)0.0410 (3)
O20.0515 (3)0.16352 (13)0.27619 (8)0.0520 (5)
O30.2753 (5)0.3414 (4)0.3114 (2)0.153 (2)
O40.3501 (5)0.1691 (3)0.3255 (2)0.1393 (17)
O50.3981 (4)0.2982 (3)0.40336 (17)0.1182 (12)
O60.5311 (3)0.2946 (3)0.31048 (16)0.0928 (9)
O70.8024 (4)0.3647 (3)0.03746 (16)0.1135 (12)
O80.7014 (6)0.2396 (4)0.0978 (3)0.199 (3)
O90.6223 (8)0.4005 (6)0.1105 (3)0.237 (4)
O100.5515 (3)0.3200 (4)0.02568 (15)0.1294 (16)
C10.2246 (3)0.25318 (18)0.11318 (12)0.0413 (5)
H1A0.22570.32990.11490.050*
H1B0.26580.23090.07330.050*
C20.3173 (3)0.2069 (2)0.16640 (12)0.0467 (6)
H2A0.42480.22180.16020.056*
H2B0.28580.23790.20580.056*
C30.3791 (3)0.0351 (2)0.11610 (13)0.0499 (6)
H3A0.41380.08640.08550.060*
H3B0.46800.00070.13390.060*
C40.2798 (4)0.0458 (2)0.08490 (12)0.0510 (7)
H4A0.32330.06700.04520.061*
H4B0.26900.10800.11110.061*
C50.0022 (4)0.0629 (2)0.05405 (12)0.0573 (7)
H5A0.01420.08090.01030.069*
H5B0.00110.12780.07820.069*
C60.1402 (4)0.0001 (2)0.06374 (13)0.0560 (7)
H6A0.22910.04390.05600.067*
H6B0.14280.05960.03530.067*
C70.0576 (3)0.07886 (16)0.24918 (10)0.0358 (4)
C80.0422 (3)0.02600 (17)0.28557 (10)0.0364 (5)
H8A0.14000.04110.30590.044*
C90.0793 (3)0.01882 (19)0.33560 (10)0.0451 (5)
H9A0.05710.04210.36160.054*
H9B0.17640.00570.31530.054*
C100.0973 (4)0.1153 (2)0.37802 (12)0.0570 (8)
H10A0.09460.17930.35220.068*
C110.0312 (7)0.1208 (4)0.4250 (2)0.0994 (15)
H11A0.12680.12550.40340.149*
H11B0.03010.05820.45050.149*
H11C0.01810.18200.45100.149*
C120.2541 (6)0.1091 (4)0.4109 (2)0.1005 (16)
H12A0.26600.16890.43810.151*
H12B0.26000.04490.43480.151*
H12C0.33360.10960.38010.151*
OW10.4488 (4)0.9718 (3)0.26895 (13)0.0972 (10)
H1W0.44350.95890.30740.117*
H2W0.47901.03420.27070.117*
OW20.6685 (3)0.1283 (3)0.23213 (13)0.0854 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co0.04151 (14)0.02479 (11)0.02374 (12)0.00120 (11)0.00463 (12)0.00172 (10)
Cl10.0610 (4)0.0641 (5)0.0941 (6)0.0009 (3)0.0033 (4)0.0371 (5)
Cl20.0584 (4)0.0561 (4)0.0353 (3)0.0052 (3)0.0017 (3)0.0106 (2)
N10.0451 (9)0.0292 (8)0.0300 (8)0.0011 (8)0.0043 (8)0.0045 (6)
N20.0436 (10)0.0401 (10)0.0348 (10)0.0031 (8)0.0015 (8)0.0058 (7)
N30.0594 (13)0.0349 (9)0.0263 (8)0.0021 (9)0.0081 (8)0.0007 (7)
N40.0509 (12)0.0416 (11)0.0436 (11)0.0075 (9)0.0020 (9)0.0032 (8)
N50.0552 (11)0.0251 (8)0.0308 (9)0.0013 (8)0.0106 (8)0.0035 (7)
O10.0654 (10)0.0270 (6)0.0304 (7)0.0005 (8)0.0076 (7)0.0014 (6)
O20.0872 (15)0.0291 (7)0.0396 (9)0.0005 (9)0.0054 (9)0.0091 (6)
O30.145 (3)0.173 (4)0.141 (4)0.098 (3)0.029 (3)0.058 (3)
O40.134 (3)0.081 (2)0.202 (4)0.039 (2)0.029 (3)0.061 (3)
O50.123 (3)0.145 (3)0.086 (2)0.021 (3)0.004 (2)0.033 (2)
O60.0803 (18)0.0913 (19)0.107 (2)0.0078 (15)0.0161 (16)0.0253 (17)
O70.100 (2)0.155 (3)0.086 (2)0.058 (2)0.0219 (18)0.008 (2)
O80.132 (3)0.151 (4)0.315 (8)0.015 (3)0.029 (4)0.167 (5)
O90.241 (7)0.270 (7)0.199 (6)0.004 (6)0.089 (5)0.150 (6)
O100.077 (2)0.232 (5)0.079 (2)0.014 (3)0.0233 (17)0.032 (3)
C10.0485 (13)0.0323 (11)0.0430 (12)0.0024 (9)0.0118 (10)0.0053 (9)
C20.0476 (12)0.0463 (13)0.0463 (14)0.0118 (11)0.0009 (11)0.0016 (10)
C30.0480 (13)0.0502 (14)0.0514 (15)0.0138 (11)0.0109 (11)0.0085 (12)
C40.0735 (18)0.0396 (14)0.0400 (13)0.0133 (12)0.0168 (12)0.0011 (9)
C50.087 (2)0.0486 (14)0.0360 (12)0.0177 (15)0.0008 (13)0.0114 (11)
C60.0647 (18)0.0615 (17)0.0419 (14)0.0171 (14)0.0097 (13)0.0009 (12)
C70.0473 (12)0.0291 (9)0.0309 (9)0.0018 (10)0.0042 (9)0.0046 (7)
C80.0511 (14)0.0308 (9)0.0274 (9)0.0026 (9)0.0055 (9)0.0025 (8)
C90.0601 (14)0.0436 (12)0.0315 (11)0.0016 (11)0.0125 (11)0.0066 (9)
C100.093 (2)0.0457 (14)0.0325 (12)0.0177 (15)0.0148 (14)0.0076 (10)
C110.125 (4)0.091 (3)0.082 (3)0.010 (3)0.011 (3)0.038 (2)
C120.113 (4)0.125 (4)0.064 (2)0.027 (3)0.044 (2)0.002 (2)
OW10.124 (3)0.101 (2)0.0666 (16)0.0244 (19)0.0037 (17)0.0209 (15)
OW20.0781 (17)0.110 (2)0.0680 (16)0.0417 (15)0.0090 (13)0.0126 (14)
Geometric parameters (Å, º) top
Co—O11.8933 (15)N2—C31.515 (3)
Co—N31.9389 (19)N3—C41.475 (4)
Co—N21.961 (2)N3—C51.497 (4)
Co—N11.9642 (17)N4—C61.497 (4)
Co—N41.968 (2)N5—C81.483 (3)
Co—N51.9740 (19)O1—C71.288 (3)
Cl1—O51.391 (3)O2—C71.217 (3)
Cl1—O41.400 (3)C1—C21.517 (4)
Cl1—O31.434 (4)C3—C41.499 (4)
Cl1—O61.441 (3)C5—C61.494 (5)
Cl2—O81.320 (3)C7—C81.542 (3)
Cl2—O91.345 (4)C8—C91.514 (3)
Cl2—O101.395 (3)C9—C101.527 (4)
Cl2—O71.404 (3)C10—C111.512 (6)
N1—C11.492 (3)C10—C121.547 (5)
N2—C21.483 (3)
O1—Co—N388.29 (7)C1—N1—Co109.86 (14)
O1—Co—N292.30 (8)C2—N2—C3111.84 (19)
N3—Co—N285.29 (9)C2—N2—Co107.46 (15)
O1—Co—N1177.62 (8)C3—N2—Co109.45 (16)
N3—Co—N193.49 (8)C4—N3—C5116.9 (2)
N2—Co—N186.28 (8)C4—N3—Co107.11 (15)
O1—Co—N488.47 (9)C5—N3—Co107.51 (16)
N3—Co—N486.45 (10)C6—N4—Co108.60 (18)
N2—Co—N4171.67 (9)C8—N5—Co110.91 (14)
N1—Co—N493.21 (9)C7—O1—Co117.93 (13)
O1—Co—N584.25 (7)N1—C1—C2106.21 (18)
N3—Co—N5172.51 (8)N2—C2—C1107.7 (2)
N2—Co—N595.64 (9)C4—C3—N2110.0 (2)
N1—Co—N593.98 (7)N3—C4—C3105.9 (2)
N4—Co—N592.69 (9)C6—C5—N3106.2 (2)
O5—Cl1—O4116.2 (3)C5—C6—N4107.4 (2)
O5—Cl1—O3109.7 (2)O2—C7—O1123.6 (2)
O4—Cl1—O3108.0 (3)O2—C7—C8120.70 (19)
O5—Cl1—O6109.0 (2)O1—C7—C8115.64 (17)
O4—Cl1—O6105.8 (2)N5—C8—C9112.5 (2)
O3—Cl1—O6107.6 (3)N5—C8—C7107.80 (17)
O8—Cl2—O9108.5 (5)C9—C8—C7111.58 (19)
O8—Cl2—O10113.2 (3)C8—C9—C10116.5 (2)
O9—Cl2—O10104.8 (4)C11—C10—C9110.8 (3)
O8—Cl2—O7109.5 (3)C11—C10—C12111.2 (3)
O9—Cl2—O7111.2 (4)C9—C10—C12108.8 (3)
O10—Cl2—O7109.5 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1C···O10i0.902.413.176 (4)143
N1—H1D···O2ii0.902.022.888 (3)163
N2—H2C···OW1iii0.912.132.989 (3)157
N3—H3C···O10i0.912.333.163 (4)153
N3—H3C···O7i0.912.483.283 (5)147
N4—H4C···O3iv0.902.153.022 (4)162
N4—H4D···O8v0.902.152.986 (4)154
N4—H4D···OW2v0.902.452.986 (4)118
N5—H5C···O2ii0.902.402.916 (3)117
N5—H5D···OW2v0.902.133.017 (4)167
OW1—H1W···O9vi0.841.992.805 (5)162
OW1—H2W···OW2vii0.832.202.871 (5)137
OW1—H2W···O4vii0.832.362.903 (5)124
Symmetry codes: (i) x1/2, y+1/2, z; (ii) x, y+1/2, z+1/2; (iii) x, y1, z; (iv) x, y1/2, z+1/2; (v) x1, 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 formulaC12H30CoN5O22+·2(ClO4)C11H28CoN5O22+·2(ClO4)C11H23CoN5O3+·ClO4C12H30CoN5O22+·2(I)·H2O
Mr534.24520.21431.72606.15
Crystal system, space groupMonoclinic, P21Monoclinic, P21Orthorhombic, P212121Orthorhombic, P212121
Temperature (K)293293293293
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), 9090, 101.577 (1), 9090, 90, 9090, 90, 90
V3)1062.5 (2)1002.35 (14)1716.25 (17)2165.2 (7)
Z2244
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)1.121.181.203.66
Crystal size (mm)0.40 × 0.30 × 0.300.30 × 0.25 × 0.230.30 × 0.25 × 0.230.30 × 0.15 × 0.10
Data collection
DiffractometerBruker 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
Rint0.0290.0220.0440.022
(sin θ/λ)max1)0.6390.6390.6510.649
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 reflections4129383539394811
No. of parameters280262227317
No. of restraints1100
H-atom treatmentH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.49, 0.540.68, 0.400.65, 0.351.16, 0.77
Absolute structureFlack H D (1983), Acta Cryst. A39, 876-881Flack H D (1983), Acta Cryst. A39, 876-881Flack H D (1983), Acta Cryst. A39, 876-881Flack H D (1983), Acta Cryst. A39, 876-881
Absolute structure parameter0.08 (2)0.08 (2)0.001 (15)0.02 (2)


(5)(6)
Crystal data
Chemical formulaC12H30CoN5O22+·2(ClO4)·2(H2O)C12H30CoN5O22+·2(ClO4)·2(H2O)
Mr570.27570.27
Crystal system, space groupOrthorhombic, P212121Orthorhombic, P212121
Temperature (K)293293
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, 9090, 90, 90
V3)2323.0 (4)2372.1 (5)
Z44
Radiation typeMo KαMo Kα
µ (mm1)1.041.01
Crystal size (mm)0.35 × 0.30 × 0.280.34 × 0.25 × 0.13
Data collection
DiffractometerBuker 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
Rint0.0320.022
(sin θ/λ)max1)0.6390.705
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.085, 0.90 0.036, 0.100, 1.00
No. of reflections49226815
No. of parameters293289
No. of restraints00
H-atom treatmentH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.59, 0.320.55, 0.27
Absolute structureFlack H D (1983), Acta Cryst. A39, 876-881Flack H D (1983), Acta Cryst. A39, 876-881
Absolute structure parameter0.007 (17)0.003 (11)

Computer programs: Bruker SMART (Bruker, 1998a), Bruker SAINT+ & SHELXTL(Bruker, 1999 & 1998b), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), Bruker SHELXTL.

Hydrogen-bond geometry (Å, º) for (1) top
D—H···AD—HH···AD···AD—H···A
N1—H1C···O2i0.902.332.905 (6)121.7
N1—H1D···O6ii0.902.072.967 (7)174.3
N2—H2C···O70.912.473.327 (10)157.3
N2—H2C···O80.912.513.256 (9)139.2
N4—H4C···O2i0.902.072.958 (6)168.5
N4—H4D···O6iii0.902.553.096 (6)119.5
N5—H5C···O80.902.303.120 (8)150.6
N5—H5C···O9iii0.902.493.152 (7)130.9
N5—H5D···O10iii0.902.523.264 (7)140.3
Symmetry codes: (i) x, y1/2, z1; (ii) x1, y1, z1; (iii) x+1, y1/2, z.
Hydrogen-bond geometry (Å, º) for (2) top
D—H···AD—HH···AD···AD—H···A
N1—H1C···O2i0.902.292.923 (5)127.3
N1—H1D···O10ii0.902.132.944 (6)150.7
N2—H2C···O30.912.243.122 (9)162.5
N4—H4C···O2i0.902.022.901 (5)167.6
N4—H4D···O10iii0.902.413.078 (6)131.3
N5—H5C···O40.902.273.110 (7)154.1
N5—H5C···O6iv0.902.553.162 (9)125.8
N5—H5D···O5iv0.902.553.310 (11)142.0
Symmetry codes: (i) x1, y+1/2, z2; (ii) x+1, y+1, z; (iii) x2, y+1/2, z2; (iv) x1, y+1/2, z1.
Hydrogen-bond geometry (Å, º) for (3) top
D—H···AD—HH···AD···AD—H···A
N4—H4C···O4i0.902.373.129 (7)142.6
N4—H4D···O2ii0.901.982.873 (3)171.2
N4—H4D···O1ii0.902.643.318 (3)132.3
N3—H3C···O30.912.092.904 (3)148.3
N2—H2C···O70.912.132.962 (4)151.1
N1—H1D···O2ii0.902.422.957 (4)118.5
N1—H1C···O3iii0.902.132.876 (3)139.3
Symmetry codes: (i) x, y1/2, z+1/2; (ii) x+1/2, y+1/2, z; (iii) x+1/2, y+1, z1/2.
Hydrogen-bond geometry (Å, º) for (4) top
D—H···AD—HH···AD···AD—H···A
N4—H18···O2i0.82 (6)2.30 (6)2.934 (5)134 (5)
N2—H7···OW10.96 (4)1.89 (5)2.856 (6)179 (4)
N5—H21···I1i0.93 (6)2.87 (6)3.695 (4)148 (4)
N4—H17···I10.84 (5)3.16 (6)3.951 (5)158 (4)
N3—H12···I2ii0.93 (4)2.82 (4)3.728 (4)165 (3)
N1—H2···I2ii0.79 (5)2.87 (5)3.565 (4)147 (5)
N1—H1···O2i0.99 (6)2.18 (6)2.937 (5)132 (4)
N5—H20···O2i0.82 (6)2.07 (6)2.793 (5)147 (5)
Symmetry codes: (i) x+1, y1/2, z+1/2; (ii) x+1/2, y+1, z1/2.
Hydrogen-bond geometry (Å, º) for (5) top
D—H···AD—HH···AD···AD—H···A
N1—H1C···OW2i0.902.092.940 (5)157.9
N1—H1D···O2ii0.902.262.928 (4)131.1
N1—H1D···O40.902.573.234 (5)131.1
N2—H2C···O7iii0.912.373.159 (5)145.5
N2—H2C···O10iii0.912.403.244 (5)153.4
N2—H2C···Cl1iii0.912.933.832 (3)171.1
N3—H3C···OW1i0.912.433.134 (4)134.1
N4—H4C···O5iv0.902.473.154 (7)133.1
N4—H4D···O2ii0.902.132.916 (4)144.9
N4—H4D···O8iv0.902.523.071 (5)120.1
N5—H5C···O30.902.293.120 (6)153.8
N5—H5D···O2ii0.902.042.825 (4)144.8
OW1—HW1···O60.902.202.832 (6)126.8
OW1—HW2···O9v1.132.053.047 (5)146.1
OW1—HW2···O10v1.132.193.203 (5)148.0
OW2—HW3···OW1v1.061.992.989 (5)156.2
OW2—HW4···O61.002.012.995 (7)165.5
Symmetry codes: (i) x+1/2, y+1, z1/2; (ii) x+1/2, y+3/2, z; (iii) x1, y, z; (iv) x1/2, y+3/2, z; (v) x1/2, y+3/2, z+1.
Hydrogen-bond geometry (Å, º) for (6) top
D—H···AD—HH···AD···AD—H···A
N1—H1C···O10i0.902.413.176 (4)143.3
N1—H1D···O2ii0.902.022.888 (3)163.1
N2—H2C···OW1iii0.912.132.989 (3)156.8
N3—H3C···O10i0.912.333.163 (4)152.8
N3—H3C···O7i0.912.483.283 (5)146.7
N4—H4C···O3iv0.902.153.022 (4)162.3
N4—H4D···O8v0.902.152.986 (4)153.5
N4—H4D···OW2v0.902.452.986 (4)118.2
N5—H5C···O2ii0.902.402.916 (3)116.6
N5—H5D···OW2v0.902.133.017 (4)166.8
OW1—H1W···O9vi0.841.992.805 (5)162.2
OW1—H2W···OW2vii0.832.202.871 (5)137.1
OW1—H2W···O4vii0.832.362.903 (5)123.7
Symmetry codes: (i) x1/2, y+1/2, z; (ii) x, y+1/2, z+1/2; (iii) x, y1, z; (iv) x, y1/2, z+1/2; (v) x1, y, z; (vi) x+1, y+1/2, z+1/2; (vii) x, y+1, z.
 

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