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In the title compound, [Co(C18H37N4O3)](ClO4)Cl·H2O, the CoIII ion has a distorted octahedral geometry, with four N atoms and two O atoms constituting the coordination sphere. The crystal structure is stabilized by a three-dimensional network of hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S010827010000398X/gd1092sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010827010000398X/gd1092Isup2.hkl
Contains datablock I

CCDC reference: 146043

Computing details top

Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: NRCVAX (Gabe et al., 1989); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: NRCVAX (Gabe et al., 1989); software used to prepare material for publication: SHELXL97.

(12-hydroxymethyl-5,5,7,12,14-pentamethyl-1,4,8,11- tetraazacyclotetradecane-N-acetato-N,N',N'',N''',O,O')cobalt(III) Chloride Perchlorate Monohydrate top
Crystal data top
[Co(C18H37N4O3)]Cl(ClO4)·H2OF(000) = 1200
Mr = 569.36Dx = 1.521 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 10.789 (3) ÅCell parameters from 25 reflections
b = 8.918 (2) Åθ = 6.0–15.8°
c = 25.847 (4) ŵ = 0.96 mm1
β = 91.79 (2)°T = 293 K
V = 2485.6 (8) Å3Pillar, purple
Z = 40.25 × 0.22 × 0.16 mm
Data collection top
Enraf Nonius CAD4
diffractometer
2981 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.047
Graphite monochromatorθmax = 25.0°, θmin = 1.6°
ω/2θ scansh = 1212
Absorption correction: ψ scan
(North et al., 1968)
k = 010
Tmin = 0.795, Tmax = 0.858l = 030
4613 measured reflections3 standard reflections every 100 reflections
4361 independent reflections intensity decay: 1%
Refinement top
Refinement on F2Primary atom site location: heavy atom method
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.109H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0518P)2]
where P = (Fo2 + 2Fc2)/3
4361 reflections(Δ/σ)max = 0.001
339 parametersΔρmax = 0.51 e Å3
0 restraintsΔρmin = 0.33 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Co10.35162 (4)0.23138 (5)0.12338 (2)0.0222 (1)
O10.2239 (2)0.2980 (3)0.16836 (9)0.0303 (6)
H1O10.24240.38450.19110.056*
O20.4656 (2)0.1600 (3)0.07639 (9)0.0306 (6)
O30.5471 (3)0.2080 (3)0.00021 (10)0.0471 (7)
N10.3308 (3)0.4106 (3)0.07671 (10)0.0234 (6)
N20.4849 (3)0.3481 (3)0.16052 (11)0.0284 (7)
H1N20.44200.40220.18390.034*
N30.3764 (3)0.0471 (3)0.16416 (11)0.0288 (7)
H1N30.32620.05530.19170.035*
N40.2097 (3)0.1266 (3)0.09025 (11)0.0286 (7)
H1N40.22500.11500.05610.034*
C10.4126 (3)0.5314 (4)0.09899 (14)0.0294 (8)
H1A0.43560.59980.07170.035*
H1B0.36780.58790.12450.035*
C20.5265 (3)0.4651 (4)0.12382 (14)0.0320 (9)
H2A0.57820.42080.09780.038*
H2B0.57410.54170.14220.038*
C30.5905 (3)0.2829 (5)0.19331 (15)0.0374 (9)
C40.5435 (4)0.1441 (5)0.22045 (15)0.0411 (10)
H4A0.60850.10900.24430.049*
H4B0.47370.17320.24100.049*
C50.5034 (4)0.0142 (4)0.18619 (15)0.0369 (10)
H50.56060.00650.15760.044*
C60.3244 (4)0.0756 (4)0.13172 (16)0.0414 (10)
H6A0.31900.16740.15170.050*
H6B0.37610.09390.10240.050*
C70.1973 (4)0.0249 (4)0.11370 (17)0.0436 (11)
H7A0.16270.09460.08830.052*
H7B0.14250.02070.14270.052*
C80.0965 (3)0.2221 (4)0.09477 (13)0.0315 (8)
C90.1050 (3)0.3546 (4)0.05843 (14)0.0347 (9)
H9A0.12070.31610.02420.042*
H9B0.02440.40300.05660.042*
C100.2010 (3)0.4735 (4)0.07092 (14)0.0293 (8)
H100.18040.51650.10450.035*
C110.3765 (3)0.3579 (4)0.02593 (13)0.0312 (9)
H11A0.41310.44140.00780.037*
H11B0.30720.32060.00480.037*
C120.4719 (3)0.2347 (4)0.03347 (14)0.0326 (8)
C130.7006 (4)0.2449 (5)0.15996 (18)0.0517 (12)
H13A0.76020.18770.18000.062*
H13B0.73840.33580.14840.062*
H13C0.67240.18710.13050.062*
C140.6276 (5)0.4000 (5)0.23429 (18)0.0596 (13)
H14A0.68860.35800.25790.071*
H14B0.55580.42890.25290.071*
H14C0.66150.48640.21770.071*
C150.5061 (4)0.1328 (5)0.21600 (18)0.0541 (12)
H15A0.58920.15310.22830.065*
H15B0.47810.21270.19360.065*
H15C0.45260.12560.24490.065*
C160.0964 (3)0.2710 (4)0.15172 (13)0.0327 (9)
H16A0.04770.36160.15530.039*
H16B0.06050.19300.17270.039*
C170.0235 (4)0.1366 (5)0.08067 (17)0.0483 (11)
H17A0.09350.20100.08540.058*
H17B0.02990.05030.10260.058*
H17C0.02210.10520.04520.058*
C180.1914 (4)0.6007 (5)0.03109 (16)0.0454 (11)
H18A0.25710.67140.03770.055*
H18B0.11290.65030.03380.055*
H18C0.19810.56010.00310.055*
Cl10.85040 (14)0.69656 (15)0.11615 (5)0.0613 (3)
O40.8849 (14)0.7726 (12)0.0704 (4)0.118 (4)0.50
O50.8391 (16)0.5471 (13)0.1018 (8)0.157 (8)0.50
O60.7661 (13)0.755 (2)0.1428 (7)0.169 (8)0.50
O70.9689 (14)0.687 (2)0.1413 (5)0.165 (8)0.50
O410.9513 (17)0.762 (2)0.1237 (11)0.267 (14)0.50
O510.759 (2)0.804 (3)0.1065 (8)0.235 (13)0.50
O610.8067 (15)0.6334 (18)0.1619 (4)0.148 (7)0.50
O710.811 (2)0.610 (3)0.0775 (5)0.203 (11)0.50
Cl20.29129 (12)0.55192 (14)0.23104 (5)0.0644 (4)
OW10.7332 (3)0.0163 (4)0.00986 (10)0.0567 (9)
H1OW0.67490.04000.01870.054*
H2OW0.76630.04000.04020.054*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0237 (2)0.0215 (2)0.0216 (2)0.0025 (2)0.00278 (17)0.0002 (2)
O10.0295 (14)0.0346 (15)0.0268 (13)0.0030 (11)0.0035 (11)0.0093 (11)
O20.0370 (15)0.0278 (14)0.0275 (13)0.0041 (12)0.0089 (11)0.0012 (11)
O30.0540 (18)0.0488 (18)0.0400 (15)0.0087 (15)0.0241 (14)0.0053 (14)
N10.0241 (16)0.0262 (16)0.0201 (14)0.0007 (13)0.0030 (12)0.0006 (12)
N20.0247 (16)0.0332 (17)0.0272 (16)0.0031 (14)0.0004 (13)0.0019 (14)
N30.0319 (18)0.0255 (16)0.0293 (16)0.0003 (14)0.0053 (13)0.0035 (13)
N40.0305 (18)0.0279 (16)0.0273 (16)0.0058 (14)0.0006 (13)0.0060 (13)
C10.033 (2)0.0223 (19)0.033 (2)0.0061 (16)0.0045 (16)0.0035 (16)
C20.029 (2)0.031 (2)0.036 (2)0.0078 (17)0.0025 (17)0.0050 (17)
C30.026 (2)0.044 (2)0.042 (2)0.0027 (18)0.0124 (17)0.0073 (19)
C40.036 (2)0.052 (3)0.035 (2)0.001 (2)0.0066 (18)0.014 (2)
C50.029 (2)0.040 (2)0.042 (2)0.0045 (18)0.0067 (18)0.0137 (19)
C60.051 (3)0.0212 (19)0.052 (3)0.0064 (19)0.002 (2)0.0005 (18)
C70.047 (3)0.029 (2)0.054 (3)0.012 (2)0.000 (2)0.0024 (19)
C80.025 (2)0.036 (2)0.0338 (19)0.0050 (17)0.0003 (15)0.0042 (17)
C90.028 (2)0.043 (2)0.033 (2)0.0012 (18)0.0029 (16)0.0005 (18)
C100.029 (2)0.029 (2)0.0298 (19)0.0030 (17)0.0008 (16)0.0015 (16)
C110.037 (2)0.034 (2)0.0225 (18)0.0013 (18)0.0065 (16)0.0037 (16)
C120.033 (2)0.033 (2)0.0328 (19)0.0058 (18)0.0069 (16)0.0031 (18)
C130.027 (2)0.060 (3)0.068 (3)0.001 (2)0.006 (2)0.015 (2)
C140.057 (3)0.062 (3)0.059 (3)0.014 (3)0.022 (2)0.003 (2)
C150.040 (3)0.048 (3)0.074 (3)0.009 (2)0.002 (2)0.024 (2)
C160.0254 (19)0.040 (2)0.0337 (19)0.0045 (18)0.0062 (15)0.0047 (18)
C170.034 (2)0.054 (3)0.056 (3)0.014 (2)0.007 (2)0.003 (2)
C180.045 (3)0.042 (3)0.049 (3)0.008 (2)0.000 (2)0.010 (2)
Cl10.0699 (9)0.0605 (8)0.0533 (8)0.0107 (8)0.0003 (7)0.0059 (6)
O40.196 (12)0.091 (7)0.066 (6)0.035 (8)0.001 (7)0.024 (5)
O50.167 (15)0.045 (6)0.27 (2)0.038 (7)0.100 (15)0.019 (9)
O60.119 (10)0.23 (2)0.161 (16)0.049 (14)0.033 (12)0.119 (15)
O70.112 (10)0.30 (2)0.083 (7)0.052 (13)0.048 (7)0.003 (10)
O410.128 (14)0.23 (2)0.44 (4)0.138 (15)0.035 (16)0.16 (2)
O510.26 (2)0.26 (2)0.188 (17)0.167 (17)0.106 (17)0.141 (17)
O610.200 (15)0.200 (14)0.043 (5)0.137 (12)0.025 (7)0.037 (7)
O710.225 (18)0.31 (3)0.070 (8)0.02 (2)0.043 (10)0.097 (13)
Cl20.0647 (8)0.0656 (8)0.0648 (7)0.0246 (7)0.0313 (6)0.0378 (6)
OW10.061 (2)0.065 (2)0.0430 (17)0.0169 (17)0.0037 (15)0.0203 (16)
Geometric parameters (Å, º) top
Co1—O21.867 (2)C7—H7B0.97
Co1—O11.925 (2)C8—C91.514 (5)
Co1—N31.966 (3)C8—C161.535 (5)
Co1—N41.967 (3)C8—C171.537 (5)
Co1—N21.997 (3)C9—C101.509 (5)
Co1—N12.011 (3)C9—H9A0.97
O1—C161.449 (4)C9—H9B0.97
O1—H1O10.99C10—C181.534 (5)
O2—C121.297 (4)C10—H100.98
O3—C121.223 (4)C11—C121.514 (5)
N1—C111.492 (4)C11—H11A0.97
N1—C11.496 (4)C11—H11B0.97
N1—C101.512 (4)C13—H13A0.96
N2—C21.489 (4)C13—H13B0.96
N2—C31.515 (4)C13—H13C0.96
N2—H1N20.91C14—H14A0.96
N3—C61.479 (5)C14—H14B0.96
N3—C51.496 (5)C14—H14C0.96
N3—H1N30.91C15—H15A0.96
N4—C71.489 (5)C15—H15B0.96
N4—C81.497 (5)C15—H15C0.96
N4—H1N40.91C16—H16A0.97
C1—C21.492 (5)C16—H16B0.97
C1—H1A0.97C17—H17A0.96
C1—H1B0.97C17—H17B0.96
C2—H2A0.97C17—H17C0.96
C2—H2B0.97C18—H18A0.96
C3—C41.517 (5)C18—H18B0.96
C3—C131.527 (5)C18—H18C0.96
C3—C141.532 (6)Cl1—O411.246 (15)
C4—C51.514 (6)Cl1—O61.271 (11)
C4—H4A0.97Cl1—O711.318 (14)
C4—H4B0.97Cl1—O51.388 (12)
C5—C151.521 (5)Cl1—O511.388 (16)
C5—H50.98Cl1—O611.404 (9)
C6—C71.503 (6)Cl1—O71.418 (13)
C6—H6A0.97Cl1—O41.422 (8)
C6—H6B0.97OW1—H1OW0.84
C7—H7A0.97OW1—H2OW0.88
O2—Co1—O1175.4 (1)C6—C7—H7A110.1
O2—Co1—N389.0 (1)N4—C7—H7B110.1
O1—Co1—N391.3 (1)C6—C7—H7B110.1
O2—Co1—N494.3 (1)H7A—C7—H7B108.4
O1—Co1—N481.2 (1)N4—C8—C9109.3 (3)
N3—Co1—N485.8 (1)N4—C8—C16105.2 (3)
O2—Co1—N290.6 (1)C9—C8—C16112.0 (3)
O1—Co1—N293.8 (1)N4—C8—C17112.5 (3)
N3—Co1—N295.4 (1)C9—C8—C17107.9 (3)
N4—Co1—N2174.9 (1)C16—C8—C17110.0 (3)
O2—Co1—N186.8 (1)C10—C9—C8118.0 (3)
O1—Co1—N192.8 (1)C10—C9—H9A107.8
N3—Co1—N1175.4 (1)C8—C9—H9A107.8
N4—Co1—N192.6 (1)C10—C9—H9B107.8
N2—Co1—N186.5 (1)C8—C9—H9B107.8
C16—O1—Co1117.4 (2)H9A—C9—H9B107.1
C16—O1—H1O1118.7C9—C10—N1112.8 (3)
Co1—O1—H1O1117.8C9—C10—C18110.2 (3)
C12—O2—Co1115.7 (2)N1—C10—C18112.6 (3)
C11—N1—C1111.0 (3)C9—C10—H10107.0
C11—N1—C10111.1 (3)N1—C10—H10107.0
C1—N1—C10107.7 (3)C18—C10—H10107.0
C11—N1—Co1104.1 (2)N1—C11—C12110.9 (3)
C1—N1—Co1106.8 (2)N1—C11—H11A109.5
C10—N1—Co1116.1 (2)C12—C11—H11A109.5
C2—N2—C3112.9 (3)N1—C11—H11B109.5
C2—N2—Co1106.6 (2)C12—C11—H11B109.5
C3—N2—Co1125.9 (2)H11A—C11—H11B108.0
C2—N2—H1N2102.8O3—C12—O2123.7 (4)
C3—N2—H1N2102.8O3—C12—C11120.9 (3)
Co1—N2—H1N2102.8O2—C12—C11115.4 (3)
C6—N3—C5113.4 (3)C3—C13—H13A109.5
C6—N3—Co1105.8 (2)C3—C13—H13B109.5
C5—N3—Co1118.4 (2)H13A—C13—H13B109.5
C6—N3—H1N3106.1C3—C13—H13C109.5
C5—N3—H1N3106.1H13A—C13—H13C109.5
Co1—N3—H1N3106.1H13B—C13—H13C109.5
C7—N4—C8113.6 (3)C3—C14—H14A109.5
C7—N4—Co1109.4 (2)C3—C14—H14B109.5
C8—N4—Co1108.8 (2)H14A—C14—H14B109.5
C7—N4—H1N4108.3C3—C14—H14C109.5
C8—N4—H1N4108.3H14A—C14—H14C109.5
Co1—N4—H1N4108.3H14B—C14—H14C109.5
C2—C1—N1110.3 (3)C5—C15—H15A109.5
C2—C1—H1A109.6C5—C15—H15B109.5
N1—C1—H1A109.6H15A—C15—H15B109.5
C2—C1—H1B109.6C5—C15—H15C109.5
N1—C1—H1B109.6H15A—C15—H15C109.5
H1A—C1—H1B108.1H15B—C15—H15C109.5
N2—C2—C1106.9 (3)O1—C16—C8107.6 (3)
N2—C2—H2A110.3O1—C16—H16A110.2
C1—C2—H2A110.3C8—C16—H16A110.2
N2—C2—H2B110.3O1—C16—H16B110.2
C1—C2—H2B110.3C8—C16—H16B110.2
H2A—C2—H2B108.6H16A—C16—H16B108.5
N2—C3—C4108.4 (3)C8—C17—H17A109.5
N2—C3—C13110.7 (3)C8—C17—H17B109.5
C4—C3—C13110.9 (4)H17A—C17—H17B109.5
N2—C3—C14107.5 (3)C8—C17—H17C109.5
C4—C3—C14108.7 (3)H17A—C17—H17C109.5
C13—C3—C14110.6 (3)H17B—C17—H17C109.5
C5—C4—C3116.6 (3)C10—C18—H18A109.5
C5—C4—H4A108.1C10—C18—H18B109.5
C3—C4—H4A108.1H18A—C18—H18B109.5
C5—C4—H4B108.1C10—C18—H18C109.5
C3—C4—H4B108.1H18A—C18—H18C109.5
H4A—C4—H4B107.3H18B—C18—H18C109.5
N3—C5—C4108.3 (3)O6—Cl1—O5118.9 (12)
N3—C5—C15111.4 (3)O6—Cl1—O7115.3 (10)
C4—C5—C15111.3 (3)O5—Cl1—O797.6 (11)
N3—C5—H5108.6O6—Cl1—O4117.6 (13)
C4—C5—H5108.6O5—Cl1—O4105.0 (8)
C15—C5—H5108.6O7—Cl1—O498.9 (8)
N3—C6—C7106.2 (3)O41—Cl1—O71130.4 (17)
N3—C6—H6A110.5O41—Cl1—O51108.4 (16)
C7—C6—H6A110.5O71—Cl1—O5193.4 (14)
N3—C6—H6B110.5O41—Cl1—O61111.8 (13)
C7—C6—H6B110.5O71—Cl1—O61107.2 (11)
H6A—C6—H6B108.7O51—Cl1—O61100.0 (9)
N4—C7—C6107.9 (3)H1OW—OW1—H2OW100.8
N4—C7—H7A110.1
Co1—N1—C1—C233.5 (3)Co1—N4—C8—C972.5 (3)
N1—C1—C2—N252.5 (4)N4—C8—C9—C1069.3 (4)
C1—C2—N2—Co144 (3)C8—C9—C10—N155.6 (4)
C2—N2—Co1—N121.2 (2)C9—C10—N1—Co149.5 (3)
N2—Co1—N1—C16.3 (2)C10—N1—Co1—N448.6 (2)
Co1—N2—C3—C434.5 (4)N1—Co1—N4—C858.4 (2)
N2—C3—C4—C564.1 (4)Co1—N1—C11—C1227.5 (3)
C3—C4—C5—N379.0 (4)N1—C11—C12—O224.0 (4)
C4—C5—N3—Co157.9 (3)C11—C12—O2—Co16.1 (4)
C5—N3—Co1—N229.5 (3)C12—O2—Co1—N18.8 (2)
N3—Co1—N2—C318.8 (3)O2—Co1—N1—C1120.3 (2)
Co1—N3—C6—C749.4 (3)Co1—N4—C8—C1647.9 (3)
N3—C6—C7—N451.9 (4)N4—C8—C16—O137.4 (4)
C6—C7—N4—Co129.2 (4)C8—C16—O1—Co111.8 (4)
C7—N4—Co1—N31.3 (2)C16—O1—Co1—N412.3 (2)
N4—Co1—N3—C627.0 (2)O1—Co1—N4—C834.0 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1O1···CL20.991.882.865 (2)174.7
N2—H1N2···CL20.912.463.350 (3)167
N3—H1N3···CL2i0.912.403.304 (3)173
N4—H1N4···OW1ii0.911.982.854 (4)160
OW1—H1OW···O30.842.082.840 (4)149.5
OW1—H2OW···O4iii0.882.232.918 (12)135.0
OW1—H2OW···O51iii0.882.212.975 (14)145.2
Symmetry codes: (i) x+1/2, y1/2, z+1/2; (ii) x+1, y, z; (iii) x, y1, z.
 

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