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The title compound, [Mn(C19H27N6O3S)2]·2CH2Cl2 or [Mn(TpmsiPr)2]·2CH2Cl2, contains a distorted octa­hedral Mn atom bound to two N atoms and an O atom from each ligand. The Mn atom lies on a center of symmetry. This structure is compared with previously reported octa­hedral complexes of the same ligand and other octa­hedral manganese complexes containing N4O2 donor sets.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806044606/bv2037sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806044606/bv2037Isup2.hkl
Contains datablock I

CCDC reference: 629454

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.076
  • wR factor = 0.209
  • Data-to-parameter ratio = 14.2

checkCIF/PLATON results

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Alert level C PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.22 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.23 Ratio PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C20 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7
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: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL, Sheldrick (2001); software used to prepare material for publication: SHELXTL.

Bis[tris(3-isopropylpyrazolyl)methanesulfonato]manganese(II) dichloromethane disolvate top
Crystal data top
[Mn(C19H27N6O3S)2]·2CH2Cl2F(000) = 1110
Mr = 1063.84Dx = 1.441 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 994 reflections
a = 10.437 (6) Åθ = 2.7–24.3°
b = 21.860 (8) ŵ = 0.63 mm1
c = 11.341 (6) ÅT = 120 K
β = 108.626 (7)°Block, colourless
V = 2452 (2) Å30.20 × 0.10 × 0.05 mm
Z = 2
Data collection top
Bruker APEX
diffractometer
4285 independent reflections
Radiation source: fine-focus sealed tube3243 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.092
Detector resolution: 835.6 pixels mm-1θmax = 25.0°, θmin = 1.9°
ω scansh = 1112
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
k = 2525
Tmin = 0.884, Tmax = 0.969l = 1313
11367 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)] = 0.076Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.209H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.1003P)2 + 2.0495P]
where P = (Fo2 + 2Fc2)/3
4285 reflections(Δ/σ)max = 0.002
301 parametersΔρmax = 1.64 e Å3
0 restraintsΔρmin = 1.11 e Å3
Special details top

Experimental. Data collection is performed with four batch runs at φ = 0.00 ° (600 frames), at φ = 90.00 ° (600 frames), at φ = 180 ° (600 frames) and at φ = 270 ° (600 frames). Frame width = 0.30 \& in ω. Data is merged, corrected for decay, and treated with multi-scan absorption corrections.

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
Mn0.00000.00000.00000.0141 (3)
S10.08215 (12)0.00068 (5)0.25618 (9)0.0168 (3)
O10.0261 (3)0.02936 (13)0.1691 (3)0.0184 (7)
O20.0191 (3)0.01686 (15)0.3710 (3)0.0220 (8)
O30.2020 (3)0.02863 (15)0.2642 (3)0.0238 (8)
N10.2124 (4)0.03593 (15)0.0369 (3)0.0142 (8)
N20.2463 (4)0.06339 (16)0.0575 (3)0.0140 (8)
N30.0378 (3)0.09350 (16)0.0876 (3)0.0145 (8)
N40.0332 (4)0.11151 (16)0.1651 (3)0.0143 (8)
N50.2617 (4)0.16620 (17)0.2121 (3)0.0212 (9)
N60.2076 (4)0.10980 (16)0.2547 (3)0.0161 (8)
C10.1458 (4)0.07549 (19)0.1790 (4)0.0148 (9)
C20.3280 (4)0.02938 (19)0.1301 (4)0.0150 (9)
C30.4367 (5)0.0514 (2)0.0953 (4)0.0193 (10)
H3A0.52930.05230.14470.023*
C40.3818 (4)0.0712 (2)0.0245 (4)0.0188 (10)
H4A0.43000.08750.07550.023*
C50.3289 (5)0.0036 (2)0.2544 (4)0.0214 (11)
H5A0.25610.02800.23930.026*
C60.3004 (5)0.0540 (2)0.3356 (4)0.0279 (12)
H6A0.21170.07210.29340.042*
H6B0.30100.03660.41540.042*
H6C0.37030.08560.35010.042*
C70.4650 (5)0.0268 (2)0.3206 (4)0.0299 (12)
H7A0.48340.05810.26630.045*
H7B0.53670.00410.33990.045*
H7C0.46190.04580.39790.045*
C80.1312 (4)0.13703 (19)0.0981 (4)0.0160 (10)
C90.1240 (5)0.1812 (2)0.1858 (4)0.0205 (10)
H9A0.18020.21610.21170.025*
C100.0193 (5)0.1636 (2)0.2259 (4)0.0179 (10)
H10A0.01110.18420.28580.022*
C110.2227 (5)0.1366 (2)0.0192 (4)0.0206 (10)
H11A0.24220.09310.00320.025*
C120.1527 (5)0.1677 (2)0.1055 (4)0.0264 (11)
H12A0.06740.14670.14760.040*
H12B0.13430.21060.09110.040*
H12C0.21150.16590.15770.040*
C130.3557 (5)0.1684 (2)0.0858 (5)0.0283 (12)
H13A0.40010.14780.16500.042*
H13B0.41460.16690.03370.042*
H13C0.33820.21120.10160.042*
C140.2936 (5)0.1904 (2)0.3065 (4)0.0177 (10)
C150.2621 (5)0.1496 (2)0.4085 (4)0.0259 (11)
H15A0.27810.15600.48550.031*
C160.2045 (5)0.0996 (2)0.3751 (4)0.0207 (10)
H16A0.16920.06470.42480.025*
C170.3467 (5)0.2546 (2)0.2996 (4)0.0228 (11)
H17A0.39180.26500.21010.027*
C180.2275 (6)0.2978 (3)0.3514 (6)0.0473 (16)
H18A0.16490.29340.30340.071*
H18B0.26030.34000.34540.071*
H18C0.18060.28770.43880.071*
C190.4487 (6)0.2628 (3)0.3676 (5)0.0344 (13)
H19A0.52420.23440.33350.052*
H19B0.40550.25430.45630.052*
H19C0.48260.30490.35690.052*
C200.7734 (6)0.3825 (2)0.0264 (5)0.0355 (13)
H20A0.74890.41380.09290.043*
H20B0.81600.40360.05380.043*
Cl10.89005 (15)0.33138 (7)0.05427 (12)0.0411 (4)
Cl20.62625 (18)0.34507 (8)0.0215 (2)0.0694 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn0.0198 (6)0.0126 (5)0.0105 (5)0.0005 (4)0.0055 (4)0.0010 (3)
S10.0244 (7)0.0145 (6)0.0130 (5)0.0010 (5)0.0078 (5)0.0012 (4)
O10.0266 (18)0.0141 (16)0.0152 (14)0.0042 (13)0.0076 (13)0.0030 (13)
O20.0310 (19)0.0217 (17)0.0127 (15)0.0050 (15)0.0061 (14)0.0015 (12)
O30.0312 (19)0.0186 (18)0.0249 (17)0.0020 (15)0.0138 (15)0.0040 (13)
N10.020 (2)0.0111 (19)0.0122 (17)0.0017 (15)0.0070 (15)0.0008 (14)
N20.018 (2)0.0138 (19)0.0122 (16)0.0009 (15)0.0072 (15)0.0007 (14)
N30.0151 (19)0.018 (2)0.0116 (16)0.0010 (15)0.0058 (14)0.0003 (14)
N40.023 (2)0.0127 (19)0.0099 (16)0.0014 (16)0.0085 (15)0.0000 (14)
N50.030 (2)0.018 (2)0.0181 (18)0.0028 (17)0.0120 (17)0.0019 (16)
N60.023 (2)0.0138 (19)0.0132 (17)0.0020 (16)0.0081 (16)0.0002 (14)
C10.019 (2)0.015 (2)0.0125 (19)0.0026 (18)0.0088 (17)0.0006 (17)
C20.018 (2)0.009 (2)0.016 (2)0.0002 (18)0.0029 (18)0.0015 (17)
C30.020 (2)0.017 (2)0.017 (2)0.0021 (19)0.0010 (18)0.0030 (18)
C40.020 (2)0.017 (2)0.022 (2)0.0027 (19)0.0097 (19)0.0019 (18)
C50.027 (3)0.022 (3)0.012 (2)0.001 (2)0.0012 (19)0.0029 (17)
C60.034 (3)0.033 (3)0.017 (2)0.003 (2)0.009 (2)0.001 (2)
C70.031 (3)0.031 (3)0.023 (2)0.002 (2)0.003 (2)0.004 (2)
C80.019 (2)0.012 (2)0.015 (2)0.0008 (18)0.0026 (18)0.0011 (17)
C90.029 (3)0.018 (2)0.016 (2)0.007 (2)0.011 (2)0.0057 (18)
C100.026 (3)0.014 (2)0.013 (2)0.0025 (19)0.0061 (19)0.0044 (17)
C110.025 (3)0.012 (2)0.028 (2)0.0011 (19)0.013 (2)0.0005 (19)
C120.038 (3)0.024 (3)0.023 (2)0.000 (2)0.017 (2)0.001 (2)
C130.029 (3)0.029 (3)0.031 (3)0.000 (2)0.016 (2)0.001 (2)
C140.022 (2)0.015 (2)0.021 (2)0.0059 (19)0.0125 (19)0.0060 (18)
C150.042 (3)0.023 (3)0.019 (2)0.000 (2)0.018 (2)0.002 (2)
C160.029 (3)0.019 (2)0.018 (2)0.003 (2)0.014 (2)0.0018 (18)
C170.031 (3)0.017 (2)0.022 (2)0.006 (2)0.010 (2)0.0035 (19)
C180.055 (4)0.022 (3)0.068 (4)0.003 (3)0.024 (3)0.008 (3)
C190.045 (3)0.029 (3)0.036 (3)0.009 (2)0.021 (3)0.007 (2)
C200.047 (3)0.028 (3)0.030 (3)0.005 (3)0.010 (3)0.006 (2)
Cl10.0509 (9)0.0486 (9)0.0255 (7)0.0045 (7)0.0145 (6)0.0007 (6)
Cl20.0451 (10)0.0409 (10)0.1214 (17)0.0059 (8)0.0252 (10)0.0126 (10)
Geometric parameters (Å, º) top
Mn—O12.121 (3)C7—H7B0.9800
Mn—O1i2.121 (3)C7—H7C0.9800
Mn—N32.252 (4)C8—C91.405 (6)
Mn—N3i2.252 (4)C8—C111.503 (6)
Mn—N12.261 (4)C9—C101.367 (6)
Mn—N1i2.261 (4)C9—H9A0.9500
S1—O31.434 (3)C10—H10A0.9500
S1—O21.434 (3)C11—C131.521 (6)
S1—O11.455 (3)C11—C121.529 (6)
S1—C11.873 (4)C11—H11A1.0000
N1—C21.334 (5)C12—H12A0.9800
N1—N21.369 (5)C12—H12B0.9800
N2—C41.353 (6)C12—H12C0.9800
N2—C11.466 (5)C13—H13A0.9800
N3—C81.340 (5)C13—H13B0.9800
N3—N41.376 (5)C13—H13C0.9800
N4—C101.353 (5)C14—C151.413 (6)
N4—C11.464 (5)C14—C171.503 (6)
N5—C141.328 (6)C15—C161.359 (7)
N5—N61.378 (5)C15—H15A0.9500
N6—C161.373 (5)C16—H16A0.9500
N6—C11.439 (5)C17—C191.510 (7)
C2—C31.399 (6)C17—C181.522 (7)
C2—C51.515 (6)C17—H17A1.0000
C3—C41.366 (6)C18—H18A0.9800
C3—H3A0.9500C18—H18B0.9800
C4—H4A0.9500C18—H18C0.9800
C5—C61.524 (7)C19—H19A0.9800
C5—C71.530 (7)C19—H19B0.9800
C5—H5A1.0000C19—H19C0.9800
C6—H6A0.9800C20—Cl11.753 (6)
C6—H6B0.9800C20—Cl21.756 (6)
C6—H6C0.9800C20—H20A0.9900
C7—H7A0.9800C20—H20B0.9900
O1—Mn—O1i180.00 (16)C5—C7—H7B109.5
O1—Mn—N386.02 (12)H7A—C7—H7B109.5
O1i—Mn—N393.98 (12)C5—C7—H7C109.5
O1—Mn—N3i93.98 (12)H7A—C7—H7C109.5
O1i—Mn—N3i86.02 (12)H7B—C7—H7C109.5
N3—Mn—N3i180.0 (3)N3—C8—C9110.4 (4)
O1—Mn—N182.60 (12)N3—C8—C11121.7 (4)
O1i—Mn—N197.40 (12)C9—C8—C11127.8 (4)
N3—Mn—N177.86 (12)C10—C9—C8105.7 (4)
N3i—Mn—N1102.14 (12)C10—C9—H9A127.1
O1—Mn—N1i97.40 (12)C8—C9—H9A127.1
O1i—Mn—N1i82.60 (12)N4—C10—C9107.7 (4)
N3—Mn—N1i102.14 (12)N4—C10—H10A126.1
N3i—Mn—N1i77.86 (12)C9—C10—H10A126.1
N1—Mn—N1i180.00 (18)C8—C11—C13110.8 (4)
O3—S1—O2117.24 (19)C8—C11—C12109.9 (4)
O3—S1—O1112.91 (19)C13—C11—C12110.3 (4)
O2—S1—O1112.8 (2)C8—C11—H11A108.6
O3—S1—C1103.5 (2)C13—C11—H11A108.6
O2—S1—C1104.90 (19)C12—C11—H11A108.6
O1—S1—C1103.68 (18)C11—C12—H12A109.5
S1—O1—Mn132.26 (18)C11—C12—H12B109.5
C2—N1—N2105.8 (3)H12A—C12—H12B109.5
C2—N1—Mn134.0 (3)C11—C12—H12C109.5
N2—N1—Mn119.4 (2)H12A—C12—H12C109.5
C4—N2—N1110.4 (3)H12B—C12—H12C109.5
C4—N2—C1127.5 (4)C11—C13—H13A109.5
N1—N2—C1121.9 (3)C11—C13—H13B109.5
C8—N3—N4105.4 (3)H13A—C13—H13B109.5
C8—N3—Mn134.7 (3)C11—C13—H13C109.5
N4—N3—Mn119.2 (3)H13A—C13—H13C109.5
C10—N4—N3110.7 (4)H13B—C13—H13C109.5
C10—N4—C1127.3 (4)N5—C14—C15110.9 (4)
N3—N4—C1122.0 (3)N5—C14—C17120.9 (4)
C14—N5—N6104.7 (3)C15—C14—C17128.1 (4)
C16—N6—N5111.8 (4)C16—C15—C14106.7 (4)
C16—N6—C1129.5 (4)C16—C15—H15A126.7
N5—N6—C1118.0 (3)C14—C15—H15A126.7
N6—C1—N4108.2 (3)C15—C16—N6105.9 (4)
N6—C1—N2109.4 (3)C15—C16—H16A127.0
N4—C1—N2110.7 (3)N6—C16—H16A127.0
N6—C1—S1109.6 (3)C14—C17—C19113.1 (4)
N4—C1—S1110.1 (3)C14—C17—C18108.5 (4)
N2—C1—S1108.8 (3)C19—C17—C18110.6 (4)
N1—C2—C3110.4 (4)C14—C17—H17A108.2
N1—C2—C5120.8 (4)C19—C17—H17A108.2
C3—C2—C5128.7 (4)C18—C17—H17A108.2
C4—C3—C2105.6 (4)C17—C18—H18A109.5
C4—C3—H3A127.2C17—C18—H18B109.5
C2—C3—H3A127.2H18A—C18—H18B109.5
N2—C4—C3107.7 (4)C17—C18—H18C109.5
N2—C4—H4A126.1H18A—C18—H18C109.5
C3—C4—H4A126.1H18B—C18—H18C109.5
C2—C5—C6110.4 (4)C17—C19—H19A109.5
C2—C5—C7110.3 (4)C17—C19—H19B109.5
C6—C5—C7110.3 (4)H19A—C19—H19B109.5
C2—C5—H5A108.6C17—C19—H19C109.5
C6—C5—H5A108.6H19A—C19—H19C109.5
C7—C5—H5A108.6H19B—C19—H19C109.5
C5—C6—H6A109.5Cl1—C20—Cl2112.0 (3)
C5—C6—H6B109.5Cl1—C20—H20A109.2
H6A—C6—H6B109.5Cl2—C20—H20A109.2
C5—C6—H6C109.5Cl1—C20—H20B109.2
H6A—C6—H6C109.5Cl2—C20—H20B109.2
H6B—C6—H6C109.5H20A—C20—H20B107.9
C5—C7—H7A109.5
O3—S1—O1—Mn115.8 (3)C4—N2—C1—S1107.5 (4)
O2—S1—O1—Mn108.4 (3)N1—N2—C1—S165.8 (4)
C1—S1—O1—Mn4.5 (3)O3—S1—C1—N660.6 (3)
N3—Mn—O1—S134.2 (3)O2—S1—C1—N662.9 (3)
N3i—Mn—O1—S1145.8 (3)O1—S1—C1—N6178.6 (3)
N1—Mn—O1—S144.1 (3)O3—S1—C1—N4179.5 (3)
N1i—Mn—O1—S1135.9 (3)O2—S1—C1—N456.1 (3)
O1—Mn—N1—C2126.9 (4)O1—S1—C1—N462.4 (3)
O1i—Mn—N1—C253.1 (4)O3—S1—C1—N259.0 (3)
N3—Mn—N1—C2145.6 (4)O2—S1—C1—N2177.5 (3)
N3i—Mn—N1—C234.4 (4)O1—S1—C1—N259.0 (3)
O1—Mn—N1—N241.1 (3)N2—N1—C2—C31.2 (5)
O1i—Mn—N1—N2138.9 (3)Mn—N1—C2—C3168.0 (3)
N3—Mn—N1—N246.4 (3)N2—N1—C2—C5176.4 (4)
N3i—Mn—N1—N2133.6 (3)Mn—N1—C2—C514.4 (6)
C2—N1—N2—C42.6 (5)N1—C2—C3—C40.6 (5)
Mn—N1—N2—C4168.5 (3)C5—C2—C3—C4178.0 (4)
C2—N1—N2—C1176.9 (4)N1—N2—C4—C33.0 (5)
Mn—N1—N2—C15.9 (5)C1—N2—C4—C3177.0 (4)
O1—Mn—N3—C8133.0 (4)C2—C3—C4—N22.2 (5)
O1i—Mn—N3—C847.0 (4)N1—C2—C5—C684.4 (5)
N1—Mn—N3—C8143.7 (4)C3—C2—C5—C692.8 (6)
N1i—Mn—N3—C836.3 (4)N1—C2—C5—C7153.5 (4)
O1—Mn—N3—N435.6 (3)C3—C2—C5—C729.3 (6)
O1i—Mn—N3—N4144.4 (3)N4—N3—C8—C92.6 (5)
N1—Mn—N3—N447.6 (3)Mn—N3—C8—C9167.1 (3)
N1i—Mn—N3—N4132.4 (3)N4—N3—C8—C11174.9 (4)
C8—N3—N4—C102.7 (4)Mn—N3—C8—C1115.3 (6)
Mn—N3—N4—C10169.0 (3)N3—C8—C9—C101.6 (5)
C8—N3—N4—C1179.7 (3)C11—C8—C9—C10175.7 (4)
Mn—N3—N4—C18.6 (5)N3—N4—C10—C91.7 (5)
C14—N5—N6—C160.8 (5)C1—N4—C10—C9179.1 (4)
C14—N5—N6—C1171.6 (4)C8—C9—C10—N40.1 (5)
C16—N6—C1—N4108.4 (5)N3—C8—C11—C13152.5 (4)
N5—N6—C1—N460.5 (4)C9—C8—C11—C1330.4 (6)
C16—N6—C1—N2130.9 (4)N3—C8—C11—C1285.4 (5)
N5—N6—C1—N260.2 (5)C9—C8—C11—C1291.7 (5)
C16—N6—C1—S111.7 (6)N6—N5—C14—C150.8 (5)
N5—N6—C1—S1179.4 (3)N6—N5—C14—C17175.4 (4)
C10—N4—C1—N69.2 (5)N5—C14—C15—C162.1 (6)
N3—N4—C1—N6173.6 (3)C17—C14—C15—C16173.8 (5)
C10—N4—C1—N2129.1 (4)C14—C15—C16—N62.5 (5)
N3—N4—C1—N253.7 (5)N5—N6—C16—C152.1 (5)
C10—N4—C1—S1110.6 (4)C1—N6—C16—C15171.6 (4)
N3—N4—C1—S166.6 (4)N5—C14—C17—C19146.2 (4)
C4—N2—C1—N612.2 (6)C15—C14—C17—C1938.4 (7)
N1—N2—C1—N6174.4 (3)N5—C14—C17—C1890.7 (5)
C4—N2—C1—N4131.4 (4)C15—C14—C17—C1884.8 (6)
N1—N2—C1—N455.3 (5)
Symmetry code: (i) x, y, z.
 

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