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The Co atom in the title complex, [Co(C7H8N4O)2](ClO4)2·H2O, is octahedrally coordinated by two molecules of the neutral Schiff bases derived from the condensation of pyridine-2-carb­aldehyde and semicarbazone; the Schiff base molecules act as meridional tridentate ligands, coordinating the metal through the amido O atom, imine N and pyridyl N atoms. The ligands are perpendicular to each other [dihedral angle = 87.27 (5)°]. The crystal packing is stabilized by intermolecular hydrogen bonds involving the cations, perchlorate counter-ions and water mol­ecules.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804007494/ng6017sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804007494/ng6017Isup2.hkl
Contains datablock I

CCDC reference: 239035

Key indicators

  • Single-crystal X-ray study
  • T = 193 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.051
  • wR factor = 0.105
  • Data-to-parameter ratio = 15.4

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O1W - H1W1 ... ? PLAT731_ALERT_1_B Bond Calc 0.85(5), Rep 0.848(10) ...... 5.00 su-Rat O1W -H1W2 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.85(5), Rep 0.848(10) ...... 5.00 su-Rat O1W -H2# 1.555 1.555
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl1 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl2 PLAT480_ALERT_4_C Long H...A H-Bond Reported H4B .. O4 .. 2.61 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H8B .. O5 .. 2.65 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2 PLAT731_ALERT_1_C Bond Calc 0.84(4), Rep 0.846(10) ...... 4.00 su-Rat O1W -H1W1 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 111(6), Rep 110.9(18) ...... 3.33 su-Rat H1W1 -O1W -H1W2 1.555 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 2.22(5), Rep 2.221(19) ...... 2.63 su-Rat H2# -O4 1.555 2.677
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrystalClear (Rigaku, 1999); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku/MSC, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1994); software used to prepare material for publication: SHELXTL.

Bis{1-[(E)-2-pyridinylmethylidene]semicarbazide}cobalt(II) diperchlorate monohydrate top
Crystal data top
[Co(C7H8N4O)2](ClO4)2·H2OZ = 2
Mr = 604.19F(000) = 614
Triclinic, P1Dx = 1.769 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.984 (3) ÅCell parameters from 4571 reflections
b = 11.082 (4) Åθ = 3.3–27.5°
c = 12.196 (5) ŵ = 1.07 mm1
α = 112.954 (4)°T = 193 K
β = 110.050 (4)°Chip, orange–red
γ = 94.017 (3)°0.31 × 0.30 × 0.09 mm
V = 1134.4 (7) Å3
Data collection top
Rigaku Mercury
diffractometer
5106 independent reflections
Radiation source: fine-focus sealed tube4358 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
Detector resolution: 7.31 pixels mm-1θmax = 27.5°, θmin = 3.3°
ω scansh = 1112
Absorption correction: multi-scan
(Jacobson, 1998)
k = 1414
Tmin = 0.733, Tmax = 0.910l = 1513
12785 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.051Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.105H atoms treated by a mixture of independent and constrained refinement
S = 1.14 w = 1/[σ2(Fo2) + (0.0346P)2 + 1.3252P]
where P = (Fo2 + 2Fc2)/3
5106 reflections(Δ/σ)max = 0.001
331 parametersΔρmax = 0.39 e Å3
3 restraintsΔρmin = 0.48 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Co10.44207 (4)0.49908 (4)0.72939 (3)0.01993 (11)
Cl10.09103 (8)0.79693 (8)0.97529 (8)0.03300 (18)
Cl20.40605 (10)0.98753 (8)0.69923 (7)0.0371 (2)
O10.6161 (2)0.4026 (2)0.78164 (19)0.0288 (5)
O20.5844 (2)0.6898 (2)0.79851 (19)0.0313 (5)
O30.0833 (3)0.6730 (3)0.9842 (4)0.0686 (9)
O40.1644 (3)0.9066 (3)1.1036 (3)0.0631 (8)
O50.0527 (3)0.8105 (3)0.9213 (4)0.0855 (12)
O60.1698 (4)0.8001 (3)0.8992 (3)0.0712 (10)
O70.3314 (4)0.9512 (3)0.7669 (3)0.0707 (10)
O80.4743 (3)1.1283 (2)0.7714 (2)0.0436 (6)
O90.3032 (3)0.9589 (3)0.5714 (2)0.0509 (7)
O100.5154 (3)0.9114 (3)0.6867 (2)0.0646 (9)
O1W0.9163 (6)0.8906 (4)0.6892 (4)0.0952 (13)
H1W11.005 (2)0.911 (5)0.702 (6)0.114*
H1W20.894 (5)0.955 (4)0.740 (5)0.114*
N10.2813 (3)0.5382 (2)0.5888 (2)0.0241 (5)
N20.4445 (3)0.3686 (2)0.5563 (2)0.0231 (5)
N30.5383 (3)0.2863 (2)0.5632 (2)0.0279 (6)
H3B0.54250.22300.49390.033*
N40.7206 (3)0.2332 (3)0.6990 (3)0.0374 (7)
H4B0.78130.24590.77660.045*
H4C0.72280.16940.62890.045*
N50.2835 (3)0.3720 (2)0.7458 (2)0.0223 (5)
N60.4363 (3)0.6161 (2)0.9043 (2)0.0213 (5)
N70.5187 (3)0.7440 (2)0.9685 (2)0.0256 (5)
H7A0.52290.80141.04450.031*
N80.6749 (3)0.9012 (3)0.9646 (3)0.0395 (7)
H8B0.72560.92770.92830.047*
H8C0.67760.95781.04030.047*
C10.2020 (3)0.6307 (3)0.6085 (3)0.0318 (7)
H10.21390.68560.69510.038*
C20.1040 (4)0.6501 (4)0.5089 (4)0.0393 (8)
H20.05040.71760.52670.047*
C30.0850 (4)0.5696 (4)0.3824 (3)0.0391 (8)
H30.01700.58050.31220.047*
C40.1657 (3)0.4731 (3)0.3589 (3)0.0339 (7)
H40.15480.41710.27280.041*
C50.2627 (3)0.4602 (3)0.4641 (3)0.0246 (6)
C60.3548 (3)0.3627 (3)0.4493 (3)0.0258 (6)
H60.34820.30000.36680.031*
C70.6260 (3)0.3103 (3)0.6875 (3)0.0253 (6)
C80.2069 (3)0.2461 (3)0.6630 (3)0.0291 (7)
H80.21440.20520.58150.035*
C90.1169 (4)0.1723 (3)0.6909 (3)0.0336 (7)
H90.06270.08310.62920.040*
C100.1071 (3)0.2303 (3)0.8096 (3)0.0330 (7)
H100.04810.18040.83160.040*
C110.1837 (3)0.3612 (3)0.8961 (3)0.0290 (7)
H110.17640.40380.97750.035*
C120.2713 (3)0.4293 (3)0.8618 (3)0.0216 (6)
C130.3557 (3)0.5684 (3)0.9468 (3)0.0223 (6)
H130.35110.61981.02800.027*
C140.5952 (3)0.7772 (3)0.9060 (3)0.0250 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0266 (2)0.0190 (2)0.01370 (18)0.00440 (15)0.01079 (15)0.00462 (14)
Cl10.0333 (4)0.0306 (4)0.0358 (4)0.0068 (3)0.0150 (3)0.0145 (3)
Cl20.0598 (5)0.0256 (4)0.0234 (4)0.0120 (4)0.0217 (4)0.0039 (3)
O10.0373 (12)0.0341 (12)0.0179 (10)0.0154 (10)0.0148 (9)0.0100 (9)
O20.0446 (13)0.0237 (11)0.0203 (10)0.0043 (9)0.0188 (10)0.0017 (9)
O30.075 (2)0.0523 (18)0.120 (3)0.0293 (16)0.059 (2)0.059 (2)
O40.0701 (19)0.066 (2)0.0325 (14)0.0130 (15)0.0202 (14)0.0074 (13)
O50.0481 (18)0.071 (2)0.094 (3)0.0282 (17)0.0038 (18)0.020 (2)
O60.116 (3)0.0487 (18)0.068 (2)0.0059 (17)0.071 (2)0.0161 (15)
O70.127 (3)0.0387 (16)0.0523 (17)0.0033 (17)0.0586 (19)0.0098 (14)
O80.0623 (16)0.0271 (12)0.0338 (13)0.0044 (11)0.0254 (12)0.0020 (10)
O90.0639 (17)0.0495 (16)0.0245 (12)0.0209 (14)0.0139 (12)0.0042 (11)
O100.088 (2)0.0586 (18)0.0298 (13)0.0477 (17)0.0177 (14)0.0028 (13)
O1W0.147 (4)0.057 (2)0.063 (2)0.009 (2)0.043 (3)0.0129 (18)
N10.0271 (12)0.0218 (12)0.0223 (12)0.0024 (10)0.0097 (10)0.0095 (10)
N20.0291 (13)0.0217 (12)0.0195 (12)0.0046 (10)0.0145 (10)0.0061 (10)
N30.0370 (14)0.0253 (13)0.0199 (12)0.0130 (11)0.0158 (11)0.0039 (10)
N40.0504 (17)0.0452 (17)0.0328 (15)0.0273 (14)0.0279 (14)0.0207 (13)
N50.0265 (12)0.0217 (12)0.0207 (12)0.0057 (10)0.0121 (10)0.0090 (10)
N60.0257 (12)0.0209 (12)0.0161 (11)0.0060 (10)0.0098 (10)0.0059 (9)
N70.0340 (14)0.0200 (12)0.0168 (11)0.0012 (10)0.0142 (10)0.0003 (9)
N80.0588 (19)0.0258 (14)0.0265 (14)0.0079 (13)0.0234 (14)0.0020 (11)
C10.0365 (17)0.0257 (16)0.0320 (17)0.0080 (13)0.0132 (14)0.0120 (13)
C20.0355 (18)0.038 (2)0.047 (2)0.0121 (15)0.0120 (16)0.0256 (17)
C30.0280 (17)0.050 (2)0.0394 (19)0.0049 (15)0.0036 (15)0.0290 (17)
C40.0294 (16)0.0427 (19)0.0235 (15)0.0038 (14)0.0044 (13)0.0160 (14)
C50.0275 (15)0.0244 (15)0.0184 (13)0.0023 (12)0.0080 (12)0.0085 (12)
C60.0331 (16)0.0258 (15)0.0134 (13)0.0003 (12)0.0098 (12)0.0047 (11)
C70.0334 (16)0.0253 (15)0.0239 (14)0.0086 (13)0.0170 (13)0.0122 (12)
C80.0320 (16)0.0257 (16)0.0282 (16)0.0044 (13)0.0148 (14)0.0086 (13)
C90.0333 (17)0.0235 (16)0.0388 (18)0.0015 (13)0.0128 (15)0.0111 (14)
C100.0305 (16)0.0372 (18)0.0388 (18)0.0065 (14)0.0157 (14)0.0228 (15)
C110.0306 (16)0.0371 (18)0.0270 (15)0.0087 (14)0.0157 (13)0.0180 (14)
C120.0233 (14)0.0269 (15)0.0195 (13)0.0099 (12)0.0101 (11)0.0131 (12)
C130.0246 (14)0.0281 (15)0.0167 (13)0.0089 (12)0.0104 (11)0.0101 (11)
C140.0295 (15)0.0231 (15)0.0171 (13)0.0018 (12)0.0080 (12)0.0058 (11)
Geometric parameters (Å, º) top
Co1—N12.120 (2)N5—C121.359 (3)
Co1—N22.051 (2)N6—C131.278 (4)
Co1—N52.158 (2)N6—N71.352 (3)
Co1—N62.043 (2)N7—C141.370 (4)
Co1—O12.145 (2)N7—H7A0.8800
Co1—O22.136 (2)N8—C141.312 (4)
Cl1—O51.406 (3)N8—H8B0.8800
Cl1—O61.415 (3)N8—H8C0.8800
Cl1—O31.418 (3)C1—C21.377 (5)
Cl1—O41.438 (3)C1—H10.9500
Cl2—O71.428 (3)C2—C31.383 (5)
Cl2—O81.429 (2)C2—H20.9500
Cl2—O91.434 (3)C3—C41.384 (5)
Cl2—O101.439 (3)C3—H30.9500
C7—O11.245 (3)C4—C51.384 (4)
C14—O21.253 (3)C4—H40.9500
O1W—H1W10.846 (10)C5—C61.465 (4)
O1W—H1W20.848 (10)C6—H60.9500
N1—C11.337 (4)C8—C91.384 (4)
N1—C51.361 (4)C8—H80.9500
N2—C61.277 (4)C9—C101.377 (5)
N2—N31.357 (3)C9—H90.9500
N3—C71.370 (4)C10—C111.379 (4)
N3—H3B0.8800C10—H100.9500
N4—C71.326 (4)C11—C121.383 (4)
N4—H4B0.8800C11—H110.9500
N4—H4C0.8800C12—C131.461 (4)
N5—C81.332 (4)C13—H130.9500
N1—Co1—N276.26 (10)N6—N7—C14114.7 (2)
N1—Co1—N593.98 (9)N6—N7—H7A122.6
N1—Co1—N6106.22 (9)C14—N7—H7A122.6
N2—Co1—N5100.11 (9)C14—N8—H8B120.0
N2—Co1—N6175.45 (10)C14—N8—H8C120.0
N5—Co1—N676.04 (9)H8B—N8—H8C120.0
N1—Co1—O1150.79 (8)N1—C1—C2122.9 (3)
N1—Co1—O290.59 (9)N1—C1—H1118.5
N2—Co1—O174.83 (9)C2—C1—H1118.5
N2—Co1—O2108.96 (9)C1—C2—C3118.9 (3)
N5—Co1—O195.03 (9)C1—C2—H2120.6
N5—Co1—O2150.82 (8)C3—C2—H2120.6
N6—Co1—O1102.90 (9)C2—C3—C4119.6 (3)
N6—Co1—O275.01 (9)C2—C3—H3120.2
O1—Co1—O294.87 (9)C4—C3—H3120.2
O5—Cl1—O6111.6 (2)C5—C4—C3118.2 (3)
O5—Cl1—O3108.4 (2)C5—C4—H4120.9
O6—Cl1—O3109.94 (18)C3—C4—H4120.9
O5—Cl1—O4108.1 (2)N1—C5—C4122.7 (3)
O6—Cl1—O4109.27 (18)N1—C5—C6115.1 (2)
O3—Cl1—O4109.4 (2)C4—C5—C6122.2 (3)
O7—Cl2—O8108.32 (15)N2—C6—C5114.6 (2)
O7—Cl2—O9109.7 (2)N2—C6—H6122.7
O8—Cl2—O9110.20 (16)C5—C6—H6122.7
O7—Cl2—O10110.3 (2)O1—C7—N4123.9 (3)
O8—Cl2—O10109.79 (18)O1—C7—N3119.8 (3)
O9—Cl2—O10108.50 (15)N4—C7—N3116.3 (3)
C7—O1—Co1114.42 (19)N5—C8—C9122.6 (3)
C14—O2—Co1114.86 (18)N5—C8—H8118.7
H1W1—O1W—H1W2110.9 (18)C9—C8—H8118.7
C1—N1—C5117.7 (3)C10—C9—C8119.0 (3)
C1—N1—Co1128.3 (2)C10—C9—H9120.5
C5—N1—Co1113.97 (19)C8—C9—H9120.5
C6—N2—N3123.6 (2)C9—C10—C11119.4 (3)
C6—N2—Co1120.0 (2)C9—C10—H10120.3
N3—N2—Co1116.29 (17)C11—C10—H10120.3
N2—N3—C7114.2 (2)C10—C11—C12118.6 (3)
N2—N3—H3B122.9C10—C11—H11120.7
C7—N3—H3B122.9C12—C11—H11120.7
C7—N4—H4B120.0N5—C12—C11122.4 (3)
C7—N4—H4C120.0N5—C12—C13115.2 (2)
H4B—N4—H4C120.0C11—C12—C13122.5 (3)
C8—N5—C12118.0 (2)N6—C13—C12115.4 (2)
C8—N5—Co1128.82 (19)N6—C13—H13122.3
C12—N5—Co1112.99 (18)C12—C13—H13122.3
C13—N6—N7123.4 (2)O2—C14—N8124.6 (3)
C13—N6—Co1120.2 (2)O2—C14—N7118.9 (3)
N7—N6—Co1116.45 (17)N8—C14—N7116.5 (2)
N6—Co1—O1—C7169.9 (2)N1—Co1—N6—N786.0 (2)
N2—Co1—O1—C76.0 (2)O2—Co1—N6—N70.20 (18)
N1—Co1—O1—C714.3 (3)O1—Co1—N6—N791.9 (2)
O2—Co1—O1—C7114.3 (2)N5—Co1—N6—N7176.1 (2)
N5—Co1—O1—C793.1 (2)C13—N6—N7—C14178.6 (3)
N6—Co1—O2—C140.5 (2)Co1—N6—N7—C140.0 (3)
N2—Co1—O2—C14178.1 (2)C5—N1—C1—C20.1 (5)
N1—Co1—O2—C14106.2 (2)Co1—N1—C1—C2177.5 (2)
O1—Co1—O2—C14102.5 (2)N1—C1—C2—C30.7 (5)
N5—Co1—O2—C146.9 (3)C1—C2—C3—C40.8 (5)
N6—Co1—N1—C17.0 (3)C2—C3—C4—C50.4 (5)
N2—Co1—N1—C1177.0 (3)C1—N1—C5—C40.3 (4)
O2—Co1—N1—C167.6 (3)Co1—N1—C5—C4178.3 (2)
O1—Co1—N1—C1168.7 (2)C1—N1—C5—C6178.8 (3)
N5—Co1—N1—C183.6 (3)Co1—N1—C5—C60.9 (3)
N6—Co1—N1—C5175.35 (19)C3—C4—C5—N10.2 (4)
N2—Co1—N1—C50.71 (19)C3—C4—C5—C6178.9 (3)
O2—Co1—N1—C5110.1 (2)N3—N2—C6—C5179.6 (2)
O1—Co1—N1—C59.0 (3)Co1—N2—C6—C53.8 (3)
N5—Co1—N1—C598.7 (2)N1—C5—C6—N23.0 (4)
N1—Co1—N2—C62.6 (2)C4—C5—C6—N2176.2 (3)
O2—Co1—N2—C688.4 (2)Co1—O1—C7—N4176.1 (2)
O1—Co1—N2—C6178.4 (2)Co1—O1—C7—N35.7 (3)
N5—Co1—N2—C689.1 (2)N2—N3—C7—O10.9 (4)
N1—Co1—N2—N3178.7 (2)N2—N3—C7—N4179.3 (3)
O2—Co1—N2—N395.5 (2)C12—N5—C8—C90.2 (4)
O1—Co1—N2—N35.52 (19)Co1—N5—C8—C9174.7 (2)
N5—Co1—N2—N387.0 (2)N5—C8—C9—C100.9 (5)
C6—N2—N3—C7179.5 (3)C8—C9—C10—C111.8 (5)
Co1—N2—N3—C74.6 (3)C9—C10—C11—C121.6 (5)
N6—Co1—N5—C8179.5 (3)C8—N5—C12—C110.4 (4)
N2—Co1—N5—C81.9 (3)Co1—N5—C12—C11175.3 (2)
N1—Co1—N5—C874.8 (3)C8—N5—C12—C13178.8 (2)
O2—Co1—N5—C8173.2 (2)Co1—N5—C12—C135.5 (3)
O1—Co1—N5—C877.4 (3)C10—C11—C12—N50.5 (4)
N6—Co1—N5—C124.36 (18)C10—C11—C12—C13179.6 (3)
N2—Co1—N5—C12173.17 (19)N7—N6—C13—C12178.2 (2)
N1—Co1—N5—C12110.10 (19)Co1—N6—C13—C120.5 (3)
O2—Co1—N5—C1211.7 (3)N5—C12—C13—N63.6 (4)
O1—Co1—N5—C1297.71 (19)C11—C12—C13—N6177.2 (3)
N1—Co1—N6—C1392.7 (2)Co1—O2—C14—N8178.9 (3)
O2—Co1—N6—C13178.9 (2)Co1—O2—C14—N70.6 (4)
O1—Co1—N6—C1389.4 (2)N6—N7—C14—O20.5 (4)
N5—Co1—N6—C132.6 (2)N6—N7—C14—N8179.2 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w2···O4i0.85 (1)2.22 (2)3.052 (5)166 (6)
N3—H3b···O10ii0.881.962.808 (3)161
N4—H4b···O3iii0.882.503.353 (5)165
N4—H4b···O4iii0.882.613.283 (4)134
N4—H4c···O9ii0.882.213.063 (4)165
N7—H7a···O8i0.882.062.899 (3)159
N8—H8b···O4i0.882.303.102 (4)151
N8—H8b···O5iv0.882.653.104 (5)113
N8—H8c···O7i0.882.203.062 (4)165
Symmetry codes: (i) x+1, y+2, z+2; (ii) x+1, y+1, z+1; (iii) x+1, y+1, z+2; (iv) x+1, y, z.
 

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