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The Co ion in the title compound, [CoCl(phen)2(H2O)]Cl·DMF [phen = 1,10-phenanthroline (C12H8N2) and DMF is di­methyl­form­amide (C3H7NO)], exists in a distorted octahedral coordination environment. The cations and anions are linked by O—H...Cl hydrogen-bond interactions across a center of inversion, forming a dimeric entity. A 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/S1600536804007263/hg6031sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804007263/hg6031Isup2.hkl
Contains datablock I

CCDC reference: 238683

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.048
  • wR factor = 0.133
  • Data-to-parameter ratio = 17.6

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT241_ALERT_2_A Check High U(eq) as Compared to Neighbors .... C27
Author Response: ...Because the lattice DMF molecule is disordered.
PLAT241_ALERT_2_A Check High   U(eq) as Compared to Neighbors ....       C27'
Author Response: ...Because the lattice DMF molecule is disordered.
PLAT242_ALERT_2_A Check Low    U(eq) as Compared to Neighbors ....         N5
Author Response: ...Because the lattice DMF molecule is disordered.
PLAT242_ALERT_2_A Check Low    U(eq) as Compared to Neighbors ....        N5'
Author Response: ...Because the lattice DMF molecule is disordered.

Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C25
Author Response: ...Because the lattice DMF molecule is disordered.
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....       C25'
Author Response: ...Because the lattice DMF molecule is disordered.
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....        C26
Author Response: ...Because the lattice DMF molecule is disordered.
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....       C26'
Author Response: ...Because the lattice DMF molecule is disordered.
PLAT301_ALERT_3_C Main Residue  Disorder .........................      12.00 Perc.
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........         O1
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........        O1'
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          2
PLAT731_ALERT_1_C Bond    Calc     0.84(3), Rep   0.840(10) ......       3.00 su-Rat
              O1W  -H1W1    1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.84(3), Rep   0.840(10) ......       3.00 su-Rat
              O1W  -H1#     1.555   1.555
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          2
              C6 H14 N2 O2

4 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 10 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Aquachlorobis(1,10-phenanthroline)cobalt(II) chloride dimethylformamide hemisolvate top
Crystal data top
[CoCl(C12H8N2)2(H2O)]Cl·0.5C6H14N2O2Z = 2
Mr = 581.35F(000) = 598
Triclinic, P1Dx = 1.491 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.632 (4) ÅCell parameters from 5907 reflections
b = 11.612 (4) Åθ = 3.1–27.5°
c = 12.777 (5) ŵ = 0.91 mm1
α = 66.97 (3)°T = 293 K
β = 85.63 (3)°Prism, pink
γ = 79.87 (3)°0.36 × 0.24 × 0.19 mm
V = 1294.6 (9) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
5881 independent reflections
Radiation source: fine-focus sealed tube4687 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
Detector resolution: 10 pixels mm-1θmax = 27.5°, θmin = 3.1°
ω scansh = 1212
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1415
Tmin = 0.737, Tmax = 0.847l = 1616
9430 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)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.133H atoms treated by a mixture of independent and constrained refinement
S = 1.05 w = 1/[σ2(Fo2) + (0.0902P)2]
where P = (Fo2 + 2Fc2)/3
5881 reflections(Δ/σ)max < 0.001
334 parametersΔρmax = 0.64 e Å3
10 restraintsΔρmin = 0.61 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Co10.69758 (3)0.16993 (3)0.71532 (2)0.0311 (1)
Cl10.58182 (6)0.18922 (6)0.88135 (5)0.0424 (2)
Cl20.40111 (8)0.55236 (6)0.64188 (6)0.0505 (2)
N10.8856 (2)0.0573 (2)0.8050 (2)0.0348 (4)
N20.8331 (2)0.3099 (2)0.6888 (2)0.0379 (4)
N30.6144 (2)0.0051 (2)0.7293 (2)0.0344 (4)
N40.7821 (2)0.1365 (2)0.5636 (2)0.0342 (4)
N50.7433 (7)0.4659 (7)0.9534 (6)0.069 (1)*0.50
N5'0.7810 (7)0.4842 (7)0.9763 (6)0.069 (1)*0.50
O10.8528 (8)0.3161 (7)0.8281 (6)0.104 (2)*0.50
O1'0.9131 (8)0.3428 (7)0.8567 (6)0.104 (2)*0.50
O1W0.5381 (2)0.3019 (2)0.6116 (2)0.0412 (4)
C10.9886 (2)0.1248 (2)0.8009 (2)0.0365 (5)
C20.9085 (3)0.0662 (3)0.8642 (2)0.0440 (6)
C31.0335 (3)0.1286 (3)0.9238 (2)0.0513 (7)
C41.1381 (3)0.0620 (3)0.9207 (2)0.0508 (7)
C51.1188 (3)0.0685 (3)0.8571 (2)0.0439 (6)
C61.2225 (3)0.1474 (3)0.8476 (3)0.0548 (7)
C71.1987 (3)0.2724 (3)0.7860 (3)0.0570 (8)
C81.0662 (3)0.3337 (3)0.7296 (2)0.0484 (6)
C91.0348 (3)0.4643 (3)0.6685 (3)0.0572 (8)
C100.9043 (3)0.5146 (3)0.6196 (3)0.0578 (7)
C110.8063 (3)0.4344 (3)0.6317 (2)0.0478 (6)
C120.9616 (2)0.2595 (2)0.7379 (2)0.0371 (5)
C130.6451 (2)0.0327 (2)0.6412 (2)0.0345 (5)
C140.5363 (3)0.0622 (3)0.8142 (2)0.0452 (6)
C150.4838 (3)0.1674 (3)0.8144 (3)0.0559 (8)
C160.5109 (3)0.2033 (3)0.7245 (3)0.0554 (7)
C170.5959 (3)0.1360 (2)0.6344 (2)0.0426 (6)
C180.6329 (3)0.1689 (3)0.5374 (3)0.0565 (8)
C190.7173 (3)0.1033 (3)0.4545 (3)0.0568 (8)
C200.7716 (3)0.0021 (3)0.4589 (2)0.0435 (6)
C210.8622 (3)0.0734 (3)0.3762 (2)0.0559 (7)
C220.9092 (3)0.1715 (3)0.3879 (2)0.0544 (7)
C230.8662 (3)0.2002 (3)0.4839 (2)0.0446 (6)
C240.7355 (2)0.0380 (2)0.5525 (2)0.0353 (5)
C250.838 (1)0.377 (1)0.9355 (9)0.120 (3)*0.50
C260.726 (2)0.528 (1)0.890 (1)0.128 (3)*0.50
C270.726 (2)0.545 (1)1.0860 (9)0.145 (3)*0.50
C25'0.825 (1)0.415 (1)0.8610 (9)0.120 (3)*0.50
C26'0.765 (1)0.433 (1)1.052 (1)0.128 (3)*0.50
C27'0.678 (2)0.560 (1)0.946 (1)0.145 (3)*0.50
H1W10.506 (3)0.353 (2)0.643 (2)0.049*
H1W20.557 (3)0.335 (3)0.542 (1)0.049*
H20.83900.11340.86620.053*
H31.04520.21560.96560.062*
H41.22130.10290.96050.061*
H61.30810.11080.88490.066*
H71.26900.32040.77970.068*
H91.10110.51630.66110.069*
H100.88130.60140.57870.069*
H110.71830.46990.59820.057*
H140.51570.03840.87590.054*
H150.43060.21260.87580.067*
H160.47390.27120.72260.067*
H180.59840.23620.53170.068*
H190.74100.12690.39300.068*
H210.88990.05310.31330.067*
H220.96870.21880.33340.065*
H230.89870.26740.49150.054*
H250.88120.36480.99240.144*0.50
H25'0.79170.42130.79730.144*0.50
H26A0.78610.50310.82360.192*0.50
H26B0.62940.50820.86590.192*0.50
H26C0.74960.61730.93220.192*0.50
H26D0.84740.46201.09890.192*0.50
H26E0.68380.45791.09840.192*0.50
H26F0.75240.34271.01430.192*0.50
H27A0.71320.62971.09790.217*0.50
H27B0.64540.50521.11500.217*0.50
H27C0.80910.54901.12490.217*0.50
H27D0.61230.50210.88900.217*0.50
H27E0.62660.60481.01330.217*0.50
H27F0.73200.62020.91810.217*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0292 (2)0.0350 (2)0.0325 (2)0.0085 (1)0.0000 (1)0.0152 (1)
Cl10.0384 (3)0.0568 (4)0.0365 (3)0.0074 (3)0.0014 (2)0.0233 (3)
Cl20.0602 (4)0.0424 (3)0.0486 (4)0.0088 (3)0.0064 (3)0.0182 (3)
O1W0.0438 (9)0.044 (1)0.0364 (9)0.0020 (8)0.0028 (7)0.0174 (8)
N10.0322 (9)0.041 (1)0.033 (1)0.0059 (8)0.0003 (8)0.0169 (8)
N20.035 (1)0.042 (1)0.041 (1)0.0105 (9)0.0004 (8)0.0193 (9)
N30.034 (1)0.037 (1)0.037 (1)0.0105 (8)0.0019 (8)0.0169 (8)
N40.0348 (9)0.036 (1)0.032 (1)0.0070 (8)0.0017 (8)0.0137 (8)
C10.031 (1)0.051 (1)0.033 (1)0.008 (1)0.0033 (9)0.022 (1)
C20.043 (1)0.047 (1)0.040 (1)0.008 (1)0.002 (1)0.014 (1)
C30.050 (2)0.052 (2)0.042 (1)0.004 (1)0.004 (1)0.012 (1)
C40.038 (1)0.071 (2)0.040 (1)0.008 (1)0.007 (1)0.023 (1)
C50.032 (1)0.067 (2)0.039 (1)0.002 (1)0.001 (1)0.030 (1)
C60.031 (1)0.083 (2)0.063 (2)0.006 (1)0.005 (1)0.042 (2)
C70.035 (1)0.085 (2)0.069 (2)0.023 (2)0.005 (1)0.044 (2)
C80.041 (1)0.067 (2)0.053 (2)0.024 (1)0.009 (1)0.034 (1)
C90.055 (2)0.062 (2)0.068 (2)0.033 (2)0.010 (1)0.031 (2)
C100.063 (2)0.047 (2)0.067 (2)0.021 (1)0.005 (2)0.021 (1)
C110.047 (1)0.043 (1)0.054 (2)0.010 (1)0.001 (1)0.018 (1)
C120.034 (1)0.049 (1)0.038 (1)0.014 (1)0.0050 (9)0.024 (1)
C130.031 (1)0.038 (1)0.039 (1)0.0039 (9)0.0047 (9)0.020 (1)
C140.045 (1)0.047 (1)0.050 (2)0.016 (1)0.011 (1)0.024 (1)
C150.053 (2)0.049 (2)0.071 (2)0.025 (1)0.021 (2)0.025 (2)
C160.051 (2)0.047 (2)0.079 (2)0.020 (1)0.006 (2)0.031 (2)
C170.038 (1)0.042 (1)0.056 (2)0.007 (1)0.004 (1)0.026 (1)
C180.056 (2)0.056 (2)0.076 (2)0.006 (1)0.011 (2)0.045 (2)
C190.063 (2)0.068 (2)0.056 (2)0.009 (2)0.009 (1)0.045 (2)
C200.045 (1)0.050 (1)0.038 (1)0.002 (1)0.002 (1)0.023 (1)
C210.062 (2)0.069 (2)0.040 (1)0.001 (2)0.006 (1)0.029 (1)
C220.056 (2)0.062 (2)0.038 (1)0.010 (1)0.016 (1)0.014 (1)
C230.044 (1)0.045 (1)0.043 (1)0.009 (1)0.008 (1)0.016 (1)
C240.032 (1)0.041 (1)0.034 (1)0.001 (1)0.0031 (9)0.017 (1)
Geometric parameters (Å, º) top
Co1—Cl12.391 (1)C9—C101.374 (5)
Co1—N32.141 (2)C9—H90.9300
Co1—N12.148 (2)C10—C111.400 (4)
Co1—N22.169 (2)C10—H100.9300
Co1—N42.192 (2)C11—H110.9300
Co1—O1W2.087 (2)C13—C171.399 (3)
N5—C251.44 (1)C13—C241.445 (3)
N5—C261.32 (1)C14—C151.401 (4)
N5—C271.59 (1)C14—H140.9300
N1—C11.354 (3)C15—C161.360 (4)
N1—C21.320 (3)C15—H150.9300
N2—C111.327 (3)C16—C171.408 (4)
N2—C121.358 (3)C16—H160.9300
N3—C131.356 (3)C17—C181.438 (4)
N3—C141.331 (3)C18—C191.348 (5)
N4—C231.318 (3)C18—H180.9300
N4—C241.360 (3)C19—C201.434 (4)
N5'—C25'1.45 (1)C19—H190.9300
N5'—C26'1.30 (1)C20—C211.411 (4)
N5'—C27'1.60 (1)C20—C241.414 (3)
O1—C251.28 (1)C21—C221.361 (5)
O1'—C25'1.28 (1)C21—H210.9300
O1W—H1W10.84 (1)C22—C231.407 (4)
O1W—H1W20.84 (1)C22—H220.9300
C1—C51.413 (3)C23—H230.9300
C1—C121.437 (4)C25—H250.9300
C2—C31.398 (4)C25'—H25'0.9300
C2—H20.9300C26—H26A0.9600
C3—C41.364 (4)C26—H26B0.9600
C3—H30.9300C26—H26C0.9600
C4—C51.397 (4)C26'—H26D0.9600
C4—H40.9300C26'—H26E0.9600
C5—C61.438 (4)C26'—H26F0.9600
C6—C71.340 (5)C27—H27A0.9600
C6—H60.9300C27—H27B0.9600
C7—C81.440 (4)C27—H27C0.9600
C7—H70.9300C27'—H27D0.9600
C8—C91.396 (4)C27'—H27E0.9600
C8—C121.409 (3)C27'—H27F0.9600
N1—Co1—Cl193.81 (6)C7—C6—H6119.3
N1—Co1—N277.14 (8)C8—C7—H7119.4
N1—Co1—N489.16 (8)C8—C9—H9120.5
N2—Co1—Cl195.74 (6)C8—C12—C1120.0 (2)
N2—Co1—N491.95 (8)C9—C8—C7123.1 (3)
N3—Co1—Cl195.94 (6)C9—C8—C12118.0 (3)
N3—Co1—N192.04 (8)C9—C10—C11119.5 (3)
N3—Co1—N2164.56 (8)C9—C10—H10120.3
N3—Co1—N476.72 (8)C10—C9—C8119.0 (3)
N4—Co1—Cl1172.20 (6)C10—C9—H9120.5
O1W—Co1—Cl191.10 (6)C10—C11—H11118.5
O1W—Co1—N1169.97 (8)C11—N2—Co1128.6 (2)
O1W—Co1—N293.68 (8)C11—N2—C12117.8 (2)
O1W—Co1—N396.15 (8)C11—C10—H10120.3
O1W—Co1—N487.10 (8)C12—N2—Co1113.6 (2)
Co1—O1W—H1W1108 (2)C12—C8—C7118.9 (3)
Co1—O1W—H1W2116 (2)C13—N3—Co1115.5 (2)
N1—C1—C5122.7 (2)C13—C17—C16117.6 (2)
N1—C1—C12117.8 (2)C13—C17—C18119.5 (2)
N1—C2—C3122.4 (3)C14—N3—Co1126.9 (2)
N1—C2—H2118.8C14—N3—C13117.6 (2)
N2—C11—C10123.0 (3)C14—C15—H15120.1
N2—C11—H11118.5C15—C14—H14118.6
N2—C12—C1117.3 (2)C15—C16—C17119.0 (3)
N2—C12—C8122.7 (2)C15—C16—H16120.5
N3—C13—C17123.2 (2)C16—C15—C14119.8 (3)
N3—C13—C24116.7 (2)C16—C15—H15120.1
N3—C14—C15122.8 (3)C16—C17—C18122.9 (2)
N3—C14—H14118.6C17—C13—C24120.1 (2)
N4—C23—C22123.2 (3)C17—C16—H16120.5
N4—C23—H23118.4C17—C18—H18119.7
N4—C24—C13117.9 (2)C18—C19—C20121.7 (3)
N4—C24—C20123.0 (2)C18—C19—H19119.2
N5—C25—H25125.6C19—C18—C17120.6 (3)
N5'—C25'—H25'123.9C19—C18—H18119.7
N5'—C26'—H26D109.5C20—C19—H19119.2
N5'—C26'—H26E109.5C20—C21—H21119.8
N5'—C26'—H26F109.5C20—C24—C13119.1 (2)
N5'—C27'—H27D109.5C21—C20—C19124.5 (2)
N5'—C27'—H27E109.5C21—C20—C24116.4 (3)
N5'—C27'—H27F109.5C21—C22—C23118.8 (2)
O1—C25—N5108.8 (9)C21—C22—H22120.6
O1—C25—H25125.6C22—C21—C20120.4 (2)
O1'—C25'—N5'112.2 (9)C22—C21—H21119.8
O1'—C25'—H25'123.9C22—C23—H23118.4
C1—N1—Co1114.2 (2)C23—N4—Co1128.8 (2)
C1—C5—C6119.0 (3)C23—N4—C24118.2 (2)
C2—N1—Co1127.5 (2)C23—C22—H22120.6
C2—N1—C1118.3 (2)C24—N4—Co1113.1 (2)
C2—C3—H3120.0C24—C20—C19119.1 (2)
C3—C2—H2118.8C25—N5—C27110.0 (8)
C3—C4—C5119.2 (3)C25'—N5'—C27'97.0 (8)
C3—C4—H4120.4C26—N5—C25128.4 (9)
C4—C3—C2120.0 (3)C26—N5—C27113.5 (9)
C4—C3—H3120.0C26'—N5'—C25'121.2 (9)
C4—C5—C1117.3 (3)C26'—N5'—C27'129.1 (9)
C4—C5—C6123.6 (3)H1W1—O1W—H1W2116 (3)
C5—C1—C12119.4 (2)H26D—C26'—H26E109.5
C5—C4—H4120.4H26D—C26'—H26F109.5
C5—C6—H6119.3H26E—C26'—H26F109.5
C6—C7—C8121.2 (3)H27D—C27'—H27E109.5
C6—C7—H7119.4H27D—C27'—H27F109.5
C7—C6—C5121.4 (3)H27E—C27'—H27F109.5
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···Cl20.84 (1)2.35 (2)3.131 (2)154 (3)
O1W—H1W2···Cl2i0.84 (1)2.24 (1)3.077 (2)172 (3)
Symmetry code: (i) x+1, y+1, z+1.
 

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