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The Co(II) ion in the title compound, [CoCl(phen)2(H2O)]Cl·C(NH2)2S [phen = 1,10-phenanthroline, (C12H8N2)], has a distorted octa­hedral coordination formed by one Cl atom, one water mol­ecule, and four N atoms of two phen ligands. Ions and mol­ecules are linked into a three-dimensional framework by N—H...S, N—H...Cl and O—H...Cl hydrogen bonds. The supra­molecular network structure is consolidated by π–π stacking inter­actions and hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806041122/hk2146sup1.cif
Contains datablocks I, aa

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806041122/hk2146Isup2.hkl
Contains datablock I

CCDC reference: 1195260

Key indicators

  • Single-crystal X-ray study
  • T = 273 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.048
  • wR factor = 0.181
  • Data-to-parameter ratio = 16.1

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C25 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7 PLAT420_ALERT_2_C D-H Without Acceptor N6 - H6B ... ?
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 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 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: APEX2; software used to prepare material for publication: APEX2.

(I) top
Crystal data top
[CoCl(C12H8N2)2(H2O)]Cl·(NH2)2CSZ = 2
Mr = 584.38F(000) = 598
Triclinic, P1Dx = 1.536 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.8147 (9) ÅCell parameters from 2467 reflections
b = 11.3517 (11) Åθ = 2.6–25.0°
c = 12.8454 (12) ŵ = 1.01 mm1
α = 64.223 (1)°T = 273 K
β = 86.947 (1)°Block, pink
γ = 78.748 (1)°0.21 × 0.20 × 0.09 mm
V = 1263.2 (2) Å3
Data collection top
Bruker APEX-II area-detector
diffractometer
5320 independent reflections
Radiation source: fine-focus sealed tube3160 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.030
φ and ω scansθmax = 26.9°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
h = 1212
Tmin = 0.815, Tmax = 0.915k = 1414
8804 measured reflectionsl = 1615
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)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.181H atoms treated by a mixture of independent and constrained refinement
S = 1.07 w = 1/[σ2(Fo2) + (0.101P)2 + 0.010P]
where P = (Fo2 + 2Fc2)/3
5320 reflections(Δ/σ)max < 0.001
330 parametersΔρmax = 1.17 e Å3
0 restraintsΔρmin = 0.80 e Å3
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
C10.1929 (5)0.0629 (5)0.1418 (4)0.0563 (13)
H10.27960.07110.11000.068*
C20.0953 (5)0.1286 (6)0.1268 (5)0.0667 (15)
H20.11700.17810.08440.080*
C30.0305 (5)0.1208 (6)0.1732 (5)0.0608 (14)
H30.09620.16440.16330.073*
C40.0607 (4)0.0448 (5)0.2376 (4)0.0470 (11)
C50.0421 (4)0.0187 (4)0.2489 (3)0.0408 (10)
C60.0161 (4)0.0952 (4)0.3148 (3)0.0388 (10)
C70.1899 (5)0.0359 (5)0.2944 (4)0.0549 (12)
H70.25950.07610.28520.066*
C80.2111 (4)0.0310 (5)0.3619 (4)0.0521 (12)
H80.29330.03200.40130.063*
C90.1082 (4)0.1004 (4)0.3732 (4)0.0425 (10)
C100.1259 (5)0.1722 (5)0.4391 (4)0.0494 (11)
H100.20630.17640.48010.059*
C110.0239 (5)0.2358 (5)0.4427 (4)0.0513 (12)
H110.03500.28590.48480.062*
C120.0980 (5)0.2260 (5)0.3829 (4)0.0462 (11)
H120.16730.26920.38730.055*
C130.1201 (5)0.3156 (5)0.0115 (4)0.0489 (11)
H130.08530.24080.00100.059*
C140.0788 (5)0.4323 (6)0.1095 (4)0.0581 (14)
H140.01640.43550.16310.070*
C150.1292 (5)0.5427 (5)0.1278 (4)0.0599 (14)
H150.10320.62100.19480.072*
C160.2210 (5)0.5379 (5)0.0450 (4)0.0491 (12)
C170.2583 (4)0.4167 (4)0.0522 (4)0.0409 (10)
C180.3521 (4)0.4038 (4)0.1399 (4)0.0381 (9)
C190.2773 (5)0.6491 (5)0.0554 (5)0.0622 (14)
H190.25400.73030.12010.075*
C200.3649 (6)0.6371 (5)0.0288 (5)0.0638 (15)
H200.39930.71120.02110.077*
C210.4051 (4)0.5146 (5)0.1282 (4)0.0489 (11)
C220.4974 (5)0.4981 (5)0.2164 (5)0.0584 (13)
H220.53680.56840.21150.070*
C230.5271 (5)0.3763 (6)0.3089 (5)0.0590 (13)
H230.58580.36380.36870.071*
C240.4706 (4)0.2709 (5)0.3146 (4)0.0466 (11)
H240.49360.18870.37830.056*
C250.2482 (12)0.4413 (11)0.5281 (8)0.127 (3)
Cl10.42462 (11)0.05267 (12)0.38482 (9)0.0500 (3)
Cl20.37942 (13)0.18632 (13)0.85438 (11)0.0586 (4)
Co10.29819 (5)0.12891 (6)0.22383 (5)0.0369 (2)
N10.1673 (4)0.0111 (4)0.2000 (3)0.0437 (9)
N20.1187 (3)0.1579 (3)0.3204 (3)0.0386 (8)
N30.3846 (3)0.2829 (3)0.2324 (3)0.0376 (8)
N40.2074 (3)0.3056 (3)0.0685 (3)0.0396 (8)
N50.1724 (9)0.4020 (8)0.6134 (7)0.171 (4)
H5A0.20930.35000.68120.206*
H5B0.08360.42720.60430.206*
N60.3857 (10)0.3916 (14)0.5588 (10)0.247 (7)
H6A0.41060.33990.62980.296*
H6B0.44730.41190.50700.296*
O10.4540 (3)0.0967 (4)0.1127 (3)0.0489 (8)
H1A0.42330.13520.04560.073*
S10.1732 (3)0.5482 (3)0.3936 (2)0.1518 (11)
H1B0.510 (5)0.019 (5)0.148 (4)0.052 (15)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.053 (3)0.072 (4)0.060 (3)0.019 (3)0.012 (2)0.042 (3)
C20.066 (3)0.085 (4)0.082 (4)0.031 (3)0.018 (3)0.061 (4)
C30.063 (3)0.069 (4)0.068 (3)0.030 (3)0.007 (3)0.039 (3)
C40.043 (2)0.053 (3)0.046 (3)0.015 (2)0.001 (2)0.019 (2)
C50.039 (2)0.043 (3)0.035 (2)0.0072 (19)0.0002 (18)0.0124 (19)
C60.037 (2)0.038 (2)0.034 (2)0.0057 (18)0.0026 (17)0.0086 (18)
C70.040 (2)0.061 (3)0.063 (3)0.013 (2)0.006 (2)0.024 (3)
C80.034 (2)0.056 (3)0.052 (3)0.007 (2)0.004 (2)0.011 (2)
C90.038 (2)0.039 (3)0.038 (2)0.0016 (19)0.0020 (19)0.0075 (19)
C100.045 (3)0.049 (3)0.042 (2)0.001 (2)0.004 (2)0.012 (2)
C110.061 (3)0.050 (3)0.041 (2)0.005 (2)0.001 (2)0.024 (2)
C120.048 (2)0.045 (3)0.043 (2)0.003 (2)0.001 (2)0.019 (2)
C130.049 (3)0.051 (3)0.045 (3)0.002 (2)0.008 (2)0.021 (2)
C140.056 (3)0.070 (4)0.041 (3)0.010 (3)0.011 (2)0.024 (3)
C150.066 (3)0.050 (3)0.038 (2)0.011 (3)0.001 (2)0.004 (2)
C160.048 (3)0.042 (3)0.041 (2)0.004 (2)0.009 (2)0.009 (2)
C170.039 (2)0.037 (2)0.039 (2)0.0019 (19)0.0067 (18)0.0112 (19)
C180.034 (2)0.037 (2)0.044 (2)0.0072 (18)0.0035 (18)0.019 (2)
C190.065 (3)0.035 (3)0.067 (3)0.001 (2)0.013 (3)0.009 (2)
C200.068 (3)0.041 (3)0.081 (4)0.017 (3)0.023 (3)0.024 (3)
C210.042 (2)0.041 (3)0.062 (3)0.010 (2)0.013 (2)0.020 (2)
C220.049 (3)0.056 (3)0.085 (4)0.019 (2)0.009 (3)0.042 (3)
C230.049 (3)0.070 (4)0.072 (3)0.006 (3)0.010 (2)0.044 (3)
C240.047 (3)0.047 (3)0.048 (3)0.006 (2)0.009 (2)0.023 (2)
C250.138 (8)0.156 (9)0.093 (6)0.011 (7)0.032 (6)0.070 (6)
Cl10.0509 (7)0.0503 (7)0.0393 (6)0.0054 (5)0.0022 (5)0.0122 (5)
Cl20.0631 (8)0.0576 (8)0.0594 (7)0.0054 (6)0.0027 (6)0.0313 (6)
Co10.0375 (3)0.0368 (4)0.0359 (3)0.0087 (2)0.0023 (2)0.0147 (3)
N10.0409 (19)0.050 (2)0.043 (2)0.0121 (17)0.0048 (16)0.0213 (18)
N20.0386 (18)0.040 (2)0.0325 (18)0.0066 (15)0.0041 (14)0.0124 (16)
N30.0371 (18)0.037 (2)0.0389 (19)0.0069 (15)0.0011 (15)0.0165 (16)
N40.0417 (19)0.039 (2)0.0367 (18)0.0060 (16)0.0020 (15)0.0154 (16)
N50.149 (7)0.146 (8)0.139 (8)0.002 (6)0.018 (6)0.001 (6)
N60.158 (8)0.46 (2)0.240 (12)0.087 (11)0.092 (9)0.260 (14)
O10.0492 (18)0.047 (2)0.0443 (17)0.0011 (16)0.0056 (15)0.0182 (17)
S10.187 (3)0.150 (2)0.1045 (18)0.002 (2)0.0128 (17)0.0575 (17)
Geometric parameters (Å, º) top
C1—N11.332 (6)C16—C191.426 (7)
C1—C21.391 (7)C17—N41.375 (6)
C1—H10.9300C17—C181.432 (6)
C2—C31.347 (7)C18—N31.359 (5)
C2—H20.9300C18—C211.399 (6)
C3—C41.418 (7)C19—C201.362 (7)
C3—H30.9300C19—H190.9300
C4—C51.397 (6)C20—C211.419 (7)
C4—C71.437 (6)C20—H200.9300
C5—N11.354 (5)C21—C221.414 (7)
C5—C61.437 (6)C22—C231.363 (7)
C6—N21.364 (5)C22—H220.9300
C6—C91.402 (6)C23—C241.387 (7)
C7—C81.365 (7)C23—H230.9300
C7—H70.9300C24—N31.331 (5)
C8—C91.444 (7)C24—H240.9300
C8—H80.9300C25—N51.253 (10)
C9—C101.393 (6)C25—N61.364 (13)
C10—C111.357 (7)C25—S11.721 (10)
C10—H100.9300Cl1—Co12.3733 (12)
C11—C121.399 (6)Co1—O12.124 (3)
C11—H110.9300Co1—N32.131 (3)
C12—N21.319 (5)Co1—N12.145 (4)
C12—H120.9300Co1—N22.156 (3)
C13—N41.326 (5)Co1—N42.193 (3)
C13—C141.378 (6)N5—H5A0.8600
C13—H130.9300N5—H5B0.8600
C14—C151.358 (7)N6—H6A0.8600
C14—H140.9300N6—H6B0.8600
C15—C161.408 (7)O1—H1A0.8300
C15—H150.9300O1—H1B0.88 (6)
C16—C171.394 (6)
N1—C1—C2122.7 (4)C16—C19—H19119.8
N1—C1—H1118.7C19—C20—C21121.7 (5)
C2—C1—H1118.7C19—C20—H20119.1
C3—C2—C1120.3 (5)C21—C20—H20119.1
C3—C2—H2119.8C18—C21—C22117.9 (4)
C1—C2—H2119.8C18—C21—C20118.9 (4)
C2—C3—C4118.6 (4)C22—C21—C20123.2 (5)
C2—C3—H3120.7C23—C22—C21118.2 (4)
C4—C3—H3120.7C23—C22—H22120.9
C5—C4—C3117.9 (4)C21—C22—H22120.9
C5—C4—C7119.7 (4)C22—C23—C24120.7 (5)
C3—C4—C7122.3 (4)C22—C23—H23119.6
N1—C5—C4122.5 (4)C24—C23—H23119.6
N1—C5—C6118.0 (4)N3—C24—C23122.5 (4)
C4—C5—C6119.5 (4)N3—C24—H24118.8
N2—C6—C9122.2 (4)C23—C24—H24118.8
N2—C6—C5117.1 (4)N5—C25—N6111.9 (10)
C9—C6—C5120.7 (4)N5—C25—S1119.5 (9)
C8—C7—C4120.4 (4)N6—C25—S1128.6 (9)
C8—C7—H7119.8O1—Co1—N392.49 (13)
C4—C7—H7119.8O1—Co1—N194.99 (13)
C7—C8—C9121.2 (4)N3—Co1—N1166.10 (13)
C7—C8—H8119.4O1—Co1—N2171.40 (13)
C9—C8—H8119.4N3—Co1—N294.03 (13)
C10—C9—C6118.2 (4)N1—Co1—N277.51 (13)
C10—C9—C8123.4 (4)O1—Co1—N485.18 (13)
C6—C9—C8118.3 (4)N3—Co1—N477.09 (13)
C11—C10—C9118.9 (4)N1—Co1—N491.87 (13)
C11—C10—H10120.5N2—Co1—N490.80 (12)
C9—C10—H10120.5O1—Co1—Cl189.78 (10)
C10—C11—C12119.9 (4)N3—Co1—Cl197.59 (9)
C10—C11—H11120.0N1—Co1—Cl194.14 (10)
C12—C11—H11120.0N2—Co1—Cl194.92 (9)
N2—C12—C11122.7 (4)N4—Co1—Cl1172.47 (9)
N2—C12—H12118.6C1—N1—C5117.9 (4)
C11—C12—H12118.6C1—N1—Co1128.2 (3)
N4—C13—C14122.7 (5)C5—N1—Co1113.8 (3)
N4—C13—H13118.6C12—N2—C6117.9 (4)
C14—C13—H13118.6C12—N2—Co1128.5 (3)
C15—C14—C13119.9 (5)C6—N2—Co1113.6 (3)
C15—C14—H14120.0C24—N3—C18117.9 (4)
C13—C14—H14120.0C24—N3—Co1127.0 (3)
C14—C15—C16119.7 (4)C18—N3—Co1115.0 (3)
C14—C15—H15120.2C13—N4—C17118.2 (4)
C16—C15—H15120.2C13—N4—Co1129.0 (3)
C17—C16—C15117.3 (5)C17—N4—Co1112.6 (3)
C17—C16—C19118.9 (5)C25—N5—H5A120.0
C15—C16—C19123.8 (5)C25—N5—H5B120.0
N4—C17—C16122.1 (4)H5A—N5—H5B120.0
N4—C17—C18117.3 (4)C25—N6—H6A120.0
C16—C17—C18120.6 (4)C25—N6—H6B120.0
N3—C18—C21122.8 (4)H6A—N6—H6B120.0
N3—C18—C17117.7 (4)Co1—O1—H1A109.5
C21—C18—C17119.5 (4)Co1—O1—H1B112 (3)
C20—C19—C16120.4 (5)H1A—O1—H1B129.2
C20—C19—H19119.8
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···Cl2i0.88 (5)2.39 (5)3.165 (4)148 (4)
O1—H1A···Cl2ii0.822.313.100 (3)162
N6—H6A···Cl20.862.683.491 (12)157
N5—H5B···S1iii0.862.483.328 (9)168
N5—H5A···Cl20.862.603.441 (8)165
Symmetry codes: (i) x+1, y, z+1; (ii) x, y, z1; (iii) x, y+1, z+1.
 

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