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In the structure of the title complex, [Ni(C17H13N2O2)2(C3H7NO)2] or [Ni(PMBP)2(DMF)2], where HPMBP is 4-benzoyl-5-methyl-2-phenyl-2H-pyrazol-3(4H)-one, the CdII atom, which lies on an inversion centre, is in a distorted octa­hedral coordination environment. The metal is coordin­ated by four O atoms from the two symmetry-related chelating PMBP ligands and O atoms from the two symmetry-related DMF ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805024360/sj6124sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805024360/sj6124Isup2.hkl
Contains datablock I

CCDC reference: 283987

Key indicators

  • Single-crystal X-ray study
  • T = 193 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.063
  • wR factor = 0.110
  • Data-to-parameter ratio = 17.6

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.59 Ratio
Alert level C PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N3 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C19 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C20 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C17
0 ALERT level A = In general: serious problem 1 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 2 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 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker 1998); software used to prepare material for publication: SHELXTL.

Bis[4-benzoyl-5-methyl-2-phenyl-2H-pyrazol-3(4H)-onato- κ2O,O']bis(N,N-dimethylformamide-κO)cadmium(II) top
Crystal data top
[Cd(C17H13N2O2)2(C3H7NO)2]F(000) = 836
Mr = 813.18Dx = 1.457 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 6769 reflections
a = 10.4835 (19) Åθ = 3.1–27.5°
b = 9.4768 (18) ŵ = 0.65 mm1
c = 18.660 (4) ÅT = 193 K
β = 90.981 (4)°Block, colourless
V = 1853.6 (6) Å30.34 × 0.21 × 0.20 mm
Z = 2
Data collection top
Rigaku Mercury CCD
diffractometer
4248 independent reflections
Radiation source: fine-focus sealed tube3899 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.047
ω scansθmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan
(North et al., 1968)
h = 1113
Tmin = 0.838, Tmax = 0.883k = 1212
20261 measured reflectionsl = 2424
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)] = 0.063Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.110H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.012P)2 + 9.086P]
where P = (Fo2 + 2Fc2)/3
4248 reflections(Δ/σ)max < 0.001
241 parametersΔρmax = 0.32 e Å3
0 restraintsΔρmin = 0.35 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
Cd10.00000.00000.00000.01838 (11)
O10.1528 (3)0.0991 (3)0.06535 (14)0.0276 (6)
O20.1389 (2)0.0226 (3)0.09178 (13)0.0253 (6)
O30.0763 (3)0.2248 (3)0.02183 (16)0.0373 (8)
N10.3521 (3)0.1998 (4)0.08329 (16)0.0195 (7)
N20.4619 (3)0.2309 (4)0.04455 (18)0.0249 (7)
N30.1898 (4)0.4196 (4)0.0041 (2)0.0326 (8)
C10.3477 (4)0.2429 (4)0.1561 (2)0.0208 (8)
C20.4392 (4)0.3375 (5)0.1824 (2)0.0298 (9)
H2A0.50080.37390.15220.036*
C30.4375 (5)0.3767 (5)0.2540 (2)0.0363 (11)
H3A0.49890.43910.27160.044*
C40.3475 (5)0.3254 (5)0.2992 (2)0.0382 (11)
H4A0.34740.35250.34710.046*
C50.2568 (5)0.2331 (6)0.2728 (2)0.0368 (11)
H5A0.19490.19860.30330.044*
C60.2557 (4)0.1900 (5)0.2014 (2)0.0299 (9)
H6A0.19440.12690.18440.036*
C70.3106 (3)0.0958 (4)0.16240 (19)0.0187 (7)
C80.2863 (4)0.2151 (5)0.2032 (2)0.0294 (9)
H8A0.22750.28160.18780.035*
C90.3497 (5)0.2357 (5)0.2672 (2)0.0386 (11)
H9A0.33470.31690.29400.046*
C100.4349 (4)0.1355 (6)0.2910 (2)0.0369 (11)
H10A0.47860.15020.33330.044*
C110.4549 (4)0.0141 (6)0.2521 (2)0.0364 (10)
H11A0.50990.05490.26890.044*
C120.3931 (4)0.0058 (5)0.1875 (2)0.0293 (8)
H12A0.40730.08780.16110.035*
C130.2602 (3)0.1356 (4)0.04141 (19)0.0192 (8)
C140.3130 (3)0.1271 (4)0.02866 (19)0.0188 (7)
C150.2478 (3)0.0777 (4)0.09083 (19)0.0184 (7)
C160.4379 (4)0.1875 (5)0.0207 (2)0.0240 (8)
C170.5407 (4)0.2059 (6)0.0753 (2)0.0386 (12)
H17A0.61370.25000.05310.058*
H17B0.50930.26420.11390.058*
H17C0.56460.11530.09380.058*
C180.1510 (4)0.2892 (5)0.0163 (2)0.0287 (9)
H18A0.18220.24300.05630.034*
C190.1482 (5)0.4990 (6)0.0579 (3)0.0520 (13)
H19A0.09020.44270.08500.078*
H19B0.22090.52300.08740.078*
H19C0.10600.58380.04220.078*
C200.2794 (6)0.4876 (7)0.0518 (4)0.0660 (18)
H20A0.29920.42470.09040.099*
H20B0.24200.57240.07090.099*
H20C0.35620.51060.02560.099*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.01623 (17)0.02034 (19)0.01858 (18)0.00122 (18)0.00026 (12)0.00021 (18)
O10.0204 (14)0.0436 (18)0.0188 (13)0.0096 (13)0.0028 (11)0.0044 (13)
O20.0238 (13)0.0329 (18)0.0192 (12)0.0089 (12)0.0017 (10)0.0024 (12)
O30.054 (2)0.0292 (17)0.0289 (16)0.0129 (15)0.0030 (15)0.0056 (14)
N10.0170 (15)0.0260 (17)0.0155 (15)0.0014 (13)0.0002 (12)0.0035 (13)
N20.0192 (16)0.036 (2)0.0198 (16)0.0032 (14)0.0014 (13)0.0015 (15)
N30.032 (2)0.0218 (19)0.044 (2)0.0048 (15)0.0038 (17)0.0019 (16)
C10.0227 (19)0.0217 (19)0.0179 (18)0.0058 (15)0.0046 (15)0.0047 (15)
C20.031 (2)0.030 (2)0.028 (2)0.0017 (18)0.0008 (18)0.0044 (18)
C30.040 (3)0.039 (3)0.030 (2)0.001 (2)0.008 (2)0.015 (2)
C40.050 (3)0.045 (3)0.020 (2)0.011 (2)0.007 (2)0.014 (2)
C50.039 (3)0.049 (3)0.023 (2)0.005 (2)0.007 (2)0.004 (2)
C60.027 (2)0.039 (3)0.024 (2)0.0022 (19)0.0023 (17)0.0053 (19)
C70.0173 (17)0.0229 (19)0.0158 (17)0.0002 (15)0.0000 (14)0.0031 (15)
C80.034 (2)0.031 (2)0.023 (2)0.0104 (19)0.0056 (17)0.0031 (18)
C90.047 (3)0.042 (3)0.026 (2)0.005 (2)0.006 (2)0.012 (2)
C100.034 (2)0.057 (3)0.020 (2)0.001 (2)0.0086 (18)0.003 (2)
C110.034 (2)0.048 (3)0.028 (2)0.015 (2)0.0078 (17)0.003 (2)
C120.032 (2)0.029 (2)0.0272 (19)0.007 (2)0.0038 (15)0.006 (2)
C130.0182 (18)0.0207 (19)0.0187 (18)0.0023 (15)0.0016 (14)0.0013 (15)
C140.0173 (17)0.0231 (19)0.0160 (17)0.0017 (15)0.0011 (14)0.0007 (15)
C150.0175 (17)0.0183 (19)0.0193 (18)0.0041 (15)0.0013 (14)0.0013 (15)
C160.0202 (19)0.031 (2)0.0207 (19)0.0030 (17)0.0016 (15)0.0016 (17)
C170.024 (2)0.069 (4)0.022 (2)0.015 (2)0.0041 (18)0.008 (2)
C180.032 (2)0.026 (2)0.027 (2)0.0003 (18)0.0065 (18)0.0006 (18)
C190.068 (3)0.033 (2)0.056 (3)0.012 (3)0.003 (3)0.018 (3)
C200.065 (4)0.037 (3)0.096 (5)0.018 (3)0.029 (3)0.005 (3)
Geometric parameters (Å, º) top
Cd1—O1i2.206 (3)C7—C81.385 (6)
Cd1—O12.206 (3)C7—C121.382 (6)
Cd1—O22.277 (3)C7—C151.509 (5)
Cd1—O2i2.277 (3)C8—C91.389 (6)
Cd1—O3i2.309 (3)C8—H8A0.9300
Cd1—O32.309 (3)C9—C101.382 (7)
O1—C131.267 (4)C9—H9A0.9300
O2—C151.255 (4)C10—C111.375 (7)
O3—C181.229 (5)C10—H10A0.9300
N1—C131.373 (5)C11—C121.390 (5)
N1—N21.401 (4)C11—H11A0.9300
N1—C11.420 (5)C12—H12A0.9300
N2—C161.306 (5)C13—C141.431 (5)
N3—C181.320 (5)C14—C151.416 (5)
N3—C191.453 (6)C14—C161.435 (5)
N3—C201.455 (6)C16—C171.506 (5)
C1—C61.388 (6)C17—H17A0.9600
C1—C21.396 (6)C17—H17B0.9600
C2—C31.387 (6)C17—H17C0.9600
C2—H2A0.9300C18—H18A0.9300
C3—C41.366 (7)C19—H19A0.9600
C3—H3A0.9300C19—H19B0.9600
C4—C51.377 (7)C19—H19C0.9600
C4—H4A0.9300C20—H20A0.9600
C5—C61.393 (6)C20—H20B0.9600
C5—H5A0.9300C20—H20C0.9600
C6—H6A0.9300
O1i—Cd1—O1180.00 (12)C7—C8—H8A120.0
O1i—Cd1—O295.27 (9)C9—C8—H8A120.0
O1—Cd1—O284.73 (9)C10—C9—C8120.1 (4)
O1i—Cd1—O2i84.73 (9)C10—C9—H9A120.0
O1—Cd1—O2i95.27 (9)C8—C9—H9A120.0
O2—Cd1—O2i180.00 (13)C11—C10—C9119.9 (4)
O1i—Cd1—O3i92.81 (12)C11—C10—H10A120.1
O1—Cd1—O3i87.19 (12)C9—C10—H10A120.1
O2—Cd1—O3i90.26 (11)C10—C11—C12120.2 (4)
O2i—Cd1—O3i89.74 (11)C10—C11—H11A119.9
O1i—Cd1—O387.19 (12)C12—C11—H11A119.9
O1—Cd1—O392.81 (12)C7—C12—C11120.2 (4)
O2—Cd1—O389.74 (11)C7—C12—H12A119.9
O2i—Cd1—O390.26 (11)C11—C12—H12A119.9
O3i—Cd1—O3180.00 (16)O1—C13—N1122.7 (3)
C13—O1—Cd1124.3 (2)O1—C13—C14131.8 (3)
C15—O2—Cd1128.4 (2)N1—C13—C14105.4 (3)
C18—O3—Cd1125.3 (3)C15—C14—C13125.4 (3)
C13—N1—N2112.0 (3)C15—C14—C16130.0 (3)
C13—N1—C1129.6 (3)C13—C14—C16104.5 (3)
N2—N1—C1118.3 (3)O2—C15—C14125.1 (3)
C16—N2—N1105.6 (3)O2—C15—C7116.4 (3)
C18—N3—C19121.7 (4)C14—C15—C7118.4 (3)
C18—N3—C20120.7 (4)N2—C16—C14112.5 (3)
C19—N3—C20117.6 (4)N2—C16—C17117.8 (4)
C6—C1—C2119.9 (4)C14—C16—C17129.7 (4)
C6—C1—N1120.9 (3)C16—C17—H17A109.5
C2—C1—N1119.2 (4)C16—C17—H17B109.5
C3—C2—C1119.4 (4)H17A—C17—H17B109.5
C3—C2—H2A120.3C16—C17—H17C109.5
C1—C2—H2A120.3H17A—C17—H17C109.5
C4—C3—C2121.3 (4)H17B—C17—H17C109.5
C4—C3—H3A119.3O3—C18—N3124.3 (4)
C2—C3—H3A119.3O3—C18—H18A117.9
C3—C4—C5119.0 (4)N3—C18—H18A117.9
C3—C4—H4A120.5N3—C19—H19A109.5
C5—C4—H4A120.5N3—C19—H19B109.5
C4—C5—C6121.6 (4)H19A—C19—H19B109.5
C4—C5—H5A119.2N3—C19—H19C109.5
C6—C5—H5A119.2H19A—C19—H19C109.5
C1—C6—C5118.8 (4)H19B—C19—H19C109.5
C1—C6—H6A120.6N3—C20—H20A109.5
C5—C6—H6A120.6N3—C20—H20B109.5
C8—C7—C12119.5 (4)H20A—C20—H20B109.5
C8—C7—C15120.1 (3)N3—C20—H20C109.5
C12—C7—C15120.4 (3)H20A—C20—H20C109.5
C7—C8—C9120.1 (4)H20B—C20—H20C109.5
O2—Cd1—O1—C130.9 (3)C15—C7—C12—C11177.3 (4)
O2i—Cd1—O1—C13179.1 (3)C10—C11—C12—C70.5 (7)
O3i—Cd1—O1—C1391.4 (3)Cd1—O1—C13—N1178.6 (3)
O3—Cd1—O1—C1388.6 (3)Cd1—O1—C13—C140.5 (6)
O1i—Cd1—O2—C15177.6 (3)N2—N1—C13—O1179.5 (4)
O1—Cd1—O2—C152.4 (3)C1—N1—C13—O13.0 (6)
O3i—Cd1—O2—C1584.7 (3)N2—N1—C13—C141.0 (4)
O3—Cd1—O2—C1595.3 (3)C1—N1—C13—C14175.5 (4)
O1i—Cd1—O3—C1887.2 (4)O1—C13—C14—C153.3 (7)
O1—Cd1—O3—C1892.8 (4)N1—C13—C14—C15175.0 (4)
O2—Cd1—O3—C188.1 (4)O1—C13—C14—C16179.4 (4)
O2i—Cd1—O3—C18171.9 (4)N1—C13—C14—C161.1 (4)
C13—N1—N2—C160.5 (4)Cd1—O2—C15—C146.3 (6)
C1—N1—N2—C16176.5 (3)Cd1—O2—C15—C7171.7 (2)
C13—N1—C1—C617.7 (6)C13—C14—C15—O27.0 (6)
N2—N1—C1—C6166.0 (4)C16—C14—C15—O2178.0 (4)
C13—N1—C1—C2163.7 (4)C13—C14—C15—C7171.0 (4)
N2—N1—C1—C212.6 (5)C16—C14—C15—C74.0 (6)
C6—C1—C2—C30.5 (6)C8—C7—C15—O286.3 (5)
N1—C1—C2—C3178.1 (4)C12—C7—C15—O294.0 (4)
C1—C2—C3—C40.5 (7)C8—C7—C15—C1491.8 (5)
C2—C3—C4—C50.0 (7)C12—C7—C15—C1487.8 (5)
C3—C4—C5—C60.6 (7)N1—N2—C16—C140.2 (5)
C2—C1—C6—C50.1 (6)N1—N2—C16—C17179.4 (4)
N1—C1—C6—C5178.6 (4)C15—C14—C16—N2175.0 (4)
C4—C5—C6—C10.6 (7)C13—C14—C16—N20.8 (5)
C12—C7—C8—C93.3 (6)C15—C14—C16—C175.4 (8)
C15—C7—C8—C9176.3 (4)C13—C14—C16—C17178.7 (5)
C7—C8—C9—C101.5 (7)Cd1—O3—C18—N3177.4 (3)
C8—C9—C10—C111.3 (8)C19—N3—C18—O31.3 (7)
C9—C10—C11—C122.3 (7)C20—N3—C18—O3179.5 (5)
C8—C7—C12—C112.4 (6)
Symmetry code: (i) x, y, z.
 

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