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The crystallization behavior of the title compound, [Co(C2H8N2)3](C2O4)(ClO4)·2H2O, has been studied in order to evaluate the effect of the counter-anion on the crystalline structures of [Co(en)3](C2O4X (en = ethyl­enedi­amine). Two-dimensional intermolecular hydrogen-bonding networks are formed between the amine protons of the [Co(en)3]3+ cations and the O atoms of the oxalate anions. Perchlorate and water mol­ecules fill in the channels between the two-dimensional networks and form hydrogen-bonding interactions with the two-dimensional layers, thus constructing a three-dimensional hydrogen-bonding network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100004200/ln1103sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100004200/ln1103Isup2.hkl
Contains datablock I

CCDC reference: 146044

Computing details top

Data collection: SMART (Bruker, 1998a); cell refinement: SMART; data reduction: SAINT+ (Bruker,1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998b); software used to prepare material for publication: SHELXTL.

Tris(ethylenediamine) cobalt (III) oxalato perchlorate dihydrate top
Crystal data top
[Co(C2H8N2)3](C2O4)(ClO4)·2H2OF(000) = 968
Mr = 462.74Dx = 1.668 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 12.5502 (7) ÅCell parameters from global unit cell refinement reflections
b = 9.5832 (5) Åθ = 2.0–27.0°
c = 15.3950 (8) ŵ = 1.14 mm1
β = 95.734 (1)°T = 293 K
V = 1842.31 (17) Å3Block, red
Z = 40.30 × 0.30 × 0.20 mm
Data collection top
Bruker SMART CCD area detector
diffractometer
4017 independent reflections
Radiation source: fine-focus sealed tube3256 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
φ and ω scansθmax = 27.0°, θmin = 2.0°
Absorption correction: empirical (using intensity measurements)
(Blessing, 1995)
h = 1516
Tmin = 0.727, Tmax = 0.804k = 512
10764 measured reflectionsl = 1919
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.031 w = 1/[σ2(Fo2) + (0.0652P)2 + 0.2357P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.090(Δ/σ)max = 0.006
S = 1.02Δρmax = 0.46 e Å3
4017 reflectionsΔρmin = 0.37 e Å3
235 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Co10.204189 (19)0.25769 (2)0.069605 (15)0.02170 (9)
Cl0.62348 (5)0.13933 (7)0.21236 (4)0.05170 (17)
C10.29927 (19)0.0104 (2)0.07421 (14)0.0383 (5)
H1C0.30010.10340.09910.046*
H1D0.37170.01390.06300.046*
C20.22575 (18)0.0056 (2)0.00915 (13)0.0352 (5)
H2C0.25600.05870.05440.042*
H2D0.15660.04530.00010.042*
C30.25658 (18)0.4870 (3)0.03350 (15)0.0415 (5)
H3C0.24140.58350.04920.050*
H3D0.27750.43850.08440.050*
C40.34462 (18)0.4789 (2)0.04016 (16)0.0417 (5)
H4C0.41210.50830.02040.050*
H4D0.32860.53920.08780.050*
C50.08770 (17)0.3098 (2)0.21409 (13)0.0340 (5)
H5C0.06460.37910.25410.041*
H5D0.09910.22220.24520.041*
C60.00432 (16)0.2921 (2)0.13724 (13)0.0312 (4)
H6C0.05890.24670.15540.037*
H6D0.01640.38230.11230.037*
C70.06625 (15)0.1440 (2)0.16222 (12)0.0266 (4)
C80.10735 (16)0.2912 (2)0.14048 (12)0.0267 (4)
N10.25802 (14)0.09149 (17)0.13512 (10)0.0310 (4)
H1A0.31070.11610.17620.037*
H1B0.20490.05250.16190.037*
N20.21358 (14)0.14248 (17)0.03524 (10)0.0296 (4)
H2A0.15390.15330.07220.035*
H2B0.27010.16950.06280.035*
N30.16109 (13)0.42020 (17)0.00236 (10)0.0285 (3)
H3A0.11580.39350.04840.034*
H3B0.12680.48180.02910.034*
N40.35136 (13)0.33129 (18)0.06955 (12)0.0339 (4)
H4A0.38580.32600.12360.041*
H4B0.38800.28060.03330.041*
N50.18740 (13)0.35532 (17)0.17921 (10)0.0278 (3)
H5A0.24380.33680.21830.033*
H5B0.18520.44800.16980.033*
N60.05353 (13)0.20486 (17)0.07223 (10)0.0265 (3)
H6A0.01800.21720.01900.032*
H6B0.04910.11420.08660.032*
O10.10277 (12)0.08980 (16)0.23318 (9)0.0408 (4)
O20.00388 (12)0.08533 (14)0.10582 (9)0.0359 (3)
O30.05980 (12)0.35217 (15)0.07590 (9)0.0389 (4)
O40.18755 (12)0.33671 (15)0.18644 (10)0.0395 (4)
O50.6656 (4)0.2351 (3)0.1580 (3)0.172 (2)
O60.6814 (3)0.0136 (3)0.21203 (19)0.1154 (11)
O70.5180 (3)0.1149 (4)0.1808 (2)0.1477 (15)
O80.6278 (3)0.1933 (4)0.29642 (16)0.1218 (12)
OW10.07009 (19)0.2845 (2)0.40327 (14)0.0707 (6)
HW10.06320.20350.36890.085*
HW20.06770.35660.37230.085*
OW20.0709 (2)0.0522 (3)0.30038 (16)0.0898 (8)
HW30.01970.01220.27060.108*
HW40.13270.01950.26650.108*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.02281 (15)0.02197 (14)0.01947 (14)0.00003 (9)0.00213 (9)0.00024 (9)
Cl0.0584 (4)0.0520 (4)0.0464 (3)0.0021 (3)0.0138 (3)0.0093 (3)
C10.0417 (12)0.0327 (11)0.0396 (11)0.0117 (9)0.0005 (9)0.0012 (9)
C20.0446 (12)0.0293 (11)0.0315 (10)0.0032 (9)0.0034 (9)0.0065 (8)
C30.0417 (13)0.0384 (12)0.0459 (13)0.0016 (9)0.0110 (10)0.0133 (10)
C40.0328 (11)0.0360 (12)0.0573 (14)0.0091 (9)0.0088 (10)0.0003 (10)
C50.0381 (12)0.0385 (12)0.0257 (9)0.0023 (9)0.0044 (8)0.0053 (9)
C60.0262 (10)0.0343 (11)0.0331 (11)0.0021 (8)0.0032 (8)0.0021 (8)
C70.0248 (9)0.0259 (10)0.0282 (9)0.0029 (7)0.0014 (7)0.0002 (8)
C80.0298 (10)0.0249 (9)0.0247 (9)0.0007 (8)0.0009 (8)0.0014 (7)
N10.0344 (9)0.0298 (9)0.0273 (8)0.0015 (7)0.0046 (7)0.0001 (7)
N20.0322 (9)0.0323 (9)0.0236 (8)0.0015 (7)0.0003 (6)0.0018 (7)
N30.0320 (9)0.0265 (8)0.0266 (8)0.0003 (7)0.0009 (7)0.0027 (6)
N40.0272 (9)0.0360 (10)0.0379 (9)0.0019 (7)0.0003 (7)0.0003 (8)
N50.0294 (8)0.0276 (8)0.0251 (8)0.0003 (7)0.0038 (6)0.0019 (6)
N60.0278 (8)0.0258 (8)0.0249 (8)0.0023 (6)0.0023 (6)0.0008 (6)
O10.0438 (9)0.0391 (9)0.0362 (8)0.0073 (7)0.0125 (7)0.0149 (7)
O20.0419 (8)0.0279 (7)0.0350 (8)0.0031 (6)0.0101 (6)0.0037 (6)
O30.0442 (9)0.0329 (8)0.0359 (8)0.0079 (6)0.0137 (7)0.0119 (6)
O40.0447 (9)0.0338 (8)0.0365 (8)0.0107 (7)0.0135 (7)0.0032 (6)
O50.268 (6)0.083 (2)0.190 (4)0.022 (2)0.150 (4)0.016 (2)
O60.148 (3)0.0859 (19)0.112 (2)0.0424 (18)0.0125 (19)0.0161 (16)
O70.102 (2)0.161 (3)0.164 (3)0.032 (2)0.065 (2)0.007 (2)
O80.132 (3)0.169 (3)0.0617 (15)0.047 (2)0.0032 (16)0.0489 (18)
OW10.0858 (16)0.0592 (12)0.0736 (14)0.0006 (11)0.0402 (12)0.0032 (10)
OW20.0829 (16)0.0863 (18)0.1072 (17)0.0126 (13)0.0440 (13)0.0409 (15)
Geometric parameters (Å, º) top
Co1—N31.9560 (15)C2—N21.479 (3)
Co1—N51.9590 (16)C3—N31.480 (3)
Co1—N61.9617 (16)C3—C41.504 (3)
Co1—N11.9683 (16)C4—N41.485 (3)
Co1—N21.9688 (16)C5—N51.476 (3)
Co1—N41.9772 (17)C5—C61.509 (3)
Cl—O51.382 (3)C6—N61.485 (3)
Cl—O71.384 (3)C7—O21.244 (2)
Cl—O81.390 (2)C7—O11.254 (2)
Cl—O61.407 (3)C7—C81.551 (3)
C1—N11.483 (3)C8—O41.249 (2)
C1—C21.505 (3)C8—O31.252 (2)
N3—Co1—N593.45 (7)O8—Cl—O6110.45 (19)
N3—Co1—N690.26 (7)N1—C1—C2107.23 (17)
N5—Co1—N685.34 (7)N2—C2—C1107.39 (16)
N3—Co1—N1174.79 (7)N3—C3—C4106.94 (17)
N5—Co1—N190.35 (7)N4—C4—C3107.07 (17)
N6—Co1—N193.60 (7)N5—C5—C6107.13 (16)
N3—Co1—N291.03 (7)N6—C6—C5106.80 (16)
N5—Co1—N2173.90 (7)O2—C7—O1124.81 (19)
N6—Co1—N290.51 (7)O2—C7—C8117.41 (16)
N1—Co1—N285.45 (7)O1—C7—C8117.66 (16)
N3—Co1—N485.48 (7)O4—C8—O3125.47 (19)
N5—Co1—N490.62 (7)O4—C8—C7117.49 (16)
N6—Co1—N4173.95 (7)O3—C8—C7116.97 (16)
N1—Co1—N490.92 (7)C1—N1—Co1109.43 (12)
N2—Co1—N493.86 (7)C2—N2—Co1109.18 (12)
O5—Cl—O7108.0 (3)C3—N3—Co1109.92 (13)
O5—Cl—O8109.6 (2)C4—N4—Co1108.37 (12)
O7—Cl—O8109.7 (2)C5—N5—Co1109.89 (12)
O5—Cl—O6109.7 (2)C6—N6—Co1109.57 (12)
O7—Cl—O6109.3 (2)
N1—C1—C2—N250.3 (2)N1—Co1—N3—C333.7 (8)
N3—C3—C4—N451.2 (2)N2—Co1—N3—C381.07 (15)
N5—C5—C6—N650.0 (2)N4—Co1—N3—C312.71 (14)
O2—C7—C8—O4163.65 (19)C3—C4—N4—Co140.5 (2)
O1—C7—C8—O412.6 (3)N3—Co1—N4—C415.81 (14)
O2—C7—C8—O313.5 (3)N5—Co1—N4—C477.60 (15)
O1—C7—C8—O3170.29 (19)N6—Co1—N4—C429.6 (7)
C2—C1—N1—Co138.0 (2)N1—Co1—N4—C4167.96 (14)
N3—Co1—N1—C134.3 (8)N2—Co1—N4—C4106.54 (14)
N5—Co1—N1—C1171.11 (14)C6—C5—N5—Co138.49 (18)
N6—Co1—N1—C1103.54 (14)N3—Co1—N5—C5103.83 (13)
N2—Co1—N1—C113.31 (14)N6—Co1—N5—C513.85 (13)
N4—Co1—N1—C180.48 (15)N1—Co1—N5—C579.73 (14)
C1—C2—N2—Co139.2 (2)N2—Co1—N5—C533.3 (7)
N3—Co1—N2—C2169.12 (14)N4—Co1—N5—C5170.66 (14)
N5—Co1—N2—C231.9 (7)C5—C6—N6—Co138.68 (18)
N6—Co1—N2—C278.85 (14)N3—Co1—N6—C679.10 (13)
N1—Co1—N2—C214.72 (14)N5—Co1—N6—C614.34 (13)
N4—Co1—N2—C2105.34 (14)N1—Co1—N6—C6104.40 (13)
C4—C3—N3—Co138.1 (2)N2—Co1—N6—C6170.13 (13)
N5—Co1—N3—C3103.07 (14)N4—Co1—N6—C633.9 (7)
N6—Co1—N3—C3171.59 (14)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O4i0.902.162.848 (2)133
N1—H1A···O70.902.593.276 (4)133
N1—H1B···O1ii0.902.233.112 (3)165
N2—H2A···O20.902.102.887 (2)146
N2—H2A···O8iii0.902.503.130 (3)128
N2—H2B···OW1iv0.902.173.045 (3)165
N3—H3A···O30.902.242.960 (2)137
N3—H3A···O8iii0.902.553.270 (3)138
N3—H3B···O3v0.901.972.852 (2)166
N4—H4A···O1i0.902.343.127 (2)146
N4—H4B···OW1iv0.902.213.043 (3)154
N5—H5A···O1i0.902.112.885 (2)143
N5—H5A···O4i0.902.323.079 (2)141
N5—H5B···O4v0.902.082.953 (2)164
N6—H6A···O30.902.122.927 (2)149
N6—H6A···O20.902.292.992 (2)134
N6—H6B···O2ii0.902.022.908 (2)167
OW1—HW1···OW20.951.792.732 (3)172
OW1—HW2···O6vi0.842.373.071 (4)141
OW2—HW3···O10.911.962.850 (3)167
OW2—HW4···O6vii0.942.403.287 (4)157
Symmetry codes: (i) x+1/2, y+1/2, z+1/2; (ii) x, y, z; (iii) x1/2, y+1/2, z1/2; (iv) x+1/2, y+1/2, z1/2; (v) x, y+1, z; (vi) x1/2, y1/2, z1/2; (vii) x+1, y, z.
 

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