Literature DB >> 21201036

Tetra-aquabis-(2-sulfamoylbenzoato)manganese(II).

Rehana Akram, Waseeq Ahmad Siddiqui, M Nawaz Tahir, Hamid Latif Siddiqui, Amjid Iqbal.   

Abstract

In the title compound, [Mn(C(7)H(6)NO(4)S)(2)(H(2)O)(4)], the Mn atom, lying on an inversion center, exhibits a distorted octa-hedral coordination by six O atoms, two from carboxyl-ate groups and four from water mol-ecules. The SO(2)NH(2) group is involved in a three dimensional polymeric hydrogen bonding network along with the water mol-ecules. π-Stacking inter-actions parallel to the c axis lead to a separation of 4.0050 (12) Å between the centroids of the benzene rings.

Entities:  

Year:  2008        PMID： 21201036      PMCID： PMC2959390          DOI： 10.1107/S1600536808029450

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For related literature, see: Allen (2002 ▶); Aurengzeb et al. (1994 ▶); Eltayeb et al. (2008 ▶); Hulme et al. (1997 ▶); Siddiqui et al. (2007 ▶, 2008 ▶); Tahir et al. (1997 ▶); Zhang & Janiak (2001 ▶).

Experimental

Crystal data

[Mn(C7H6NO4S)2(H2O)4] M = 527.38 Monoclinic, a = 15.2442 (4) Å b = 8.2835 (2) Å c = 7.9188 (2) Å β = 99.971 (1)° V = 984.85 (4) Å3 Z = 2 Mo Kα radiation μ = 0.95 mm−1 T = 296 (2) K 0.20 × 0.15 × 0.12 mm

Data collection

Bruker KAPPA APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2007 ▶) T min = 0.840, T max = 0.895 10903 measured reflections 2445 independent reflections 2174 reflections with I > 2σ(I) R int = 0.027

Refinement

R[F 2 > 2σ(F 2)] = 0.029 wR(F 2) = 0.106 S = 1.05 2445 reflections 148 parameters H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.46 e Å−3 Δρmin = −0.40 e Å−3 Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: APEX2; data reduction: SAINT (Bruker, 2007 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶) and PLATON (Spek, 2003 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶) and PLATON. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808029450/fj2154sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808029450/fj2154Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Mn(C7H6NO4S)2(H2O)4]F(000) = 542
Mr = 527.38Dx = 1.778 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2445 reflections
a = 15.2442 (4) Åθ = 1.4–28.3°
b = 8.2835 (2) ŵ = 0.95 mm−1
c = 7.9188 (2) ÅT = 296 K
β = 99.971 (1)°Prismatic, colourless
V = 984.85 (4) Å30.20 × 0.15 × 0.12 mm
Z = 2
Bruker KAPPA APEXII CCD diffractometer2445 independent reflections
Radiation source: fine-focus sealed tube2174 reflections with I > 2σ(I)
graphiteRint = 0.027
Detector resolution: 7.50 pixels mm-1θmax = 28.3°, θmin = 1.4°
ω scansh = −20→20
Absorption correction: multi-scan (SADABS; Bruker, 2007)k = −11→7
Tmin = 0.840, Tmax = 0.895l = −10→8
10903 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.029Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.106H atoms treated by a mixture of independent and constrained refinement
S = 1.05w = 1/[σ2(Fo2) + (0.0727P)2 + 0.2877P] where P = (Fo2 + 2Fc2)/3
2445 reflections(Δ/σ)max < 0.001
148 parametersΔρmax = 0.46 e Å−3
0 restraintsΔρmin = −0.40 e Å−3
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles
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.
xyzUiso*/Ueq
Mn10.000001.000000.000000.0202 (1)
S10.26720 (3)0.44810 (6)0.04336 (6)0.0258 (1)
O10.13332 (8)0.92172 (17)0.01231 (17)0.0292 (4)
O20.13202 (9)0.68245 (19)0.1401 (2)0.0399 (4)
O30.19410 (10)0.46089 (19)−0.09625 (18)0.0352 (4)
O40.33501 (10)0.33230 (18)0.0254 (2)0.0415 (5)
O50.00686 (10)0.99300 (17)0.28706 (18)0.0334 (4)
O60.05852 (9)1.23701 (17)0.0481 (2)0.0411 (5)
N10.22897 (12)0.3966 (2)0.2145 (2)0.0324 (5)
C10.26985 (10)0.7841 (2)0.0847 (2)0.0213 (4)
C20.31781 (10)0.6410 (2)0.0774 (2)0.0226 (4)
C30.41025 (11)0.6438 (3)0.0899 (3)0.0330 (5)
C40.45577 (12)0.7888 (3)0.1114 (3)0.0407 (7)
C50.40934 (13)0.9313 (3)0.1195 (3)0.0363 (6)
C60.31757 (12)0.9290 (2)0.1056 (2)0.0275 (5)
C70.16968 (10)0.7939 (2)0.0780 (2)0.0224 (4)
H30.441300.547920.083740.0395*
H40.517410.790500.120510.0488*
H50.439861.028860.134170.0436*
H5A0.060461.016460.334530.0400*
H5B−0.034441.075960.310530.0400*
H60.287071.025660.110380.0330*
H6A0.027841.310740.106100.0493*
H6B0.114781.246150.082460.0493*
H110.2043 (19)0.467 (4)0.248 (3)0.0389*
H120.2695 (16)0.353 (3)0.288 (3)0.0389*
U11U22U33U12U13U23
Mn10.0192 (2)0.0176 (2)0.0239 (2)0.0011 (1)0.0040 (1)0.0001 (1)
S10.0248 (2)0.0198 (3)0.0320 (2)−0.0007 (2)0.0028 (2)−0.0006 (2)
O10.0223 (6)0.0287 (7)0.0359 (7)0.0066 (5)0.0028 (5)0.0026 (5)
O20.0246 (6)0.0393 (8)0.0591 (9)0.0024 (6)0.0169 (6)0.0163 (7)
O30.0339 (7)0.0389 (8)0.0303 (7)−0.0078 (6)−0.0011 (5)−0.0005 (6)
O40.0396 (8)0.0245 (7)0.0612 (10)0.0071 (6)0.0114 (7)−0.0040 (7)
O50.0280 (7)0.0441 (9)0.0276 (7)0.0002 (5)0.0035 (5)−0.0005 (5)
O60.0301 (7)0.0257 (7)0.0684 (10)−0.0049 (6)0.0112 (6)−0.0081 (7)
N10.0351 (9)0.0273 (9)0.0343 (8)−0.0006 (7)0.0046 (7)0.0067 (7)
C10.0197 (7)0.0219 (8)0.0224 (7)0.0007 (6)0.0037 (5)0.0033 (6)
C20.0185 (7)0.0216 (8)0.0274 (8)−0.0005 (6)0.0030 (6)0.0009 (6)
C30.0199 (8)0.0326 (10)0.0461 (10)0.0038 (7)0.0049 (7)0.0028 (8)
C40.0189 (8)0.0454 (13)0.0571 (13)−0.0060 (8)0.0050 (8)0.0049 (10)
C50.0304 (9)0.0318 (11)0.0460 (11)−0.0121 (8)0.0045 (8)0.0016 (9)
C60.0287 (8)0.0223 (9)0.0313 (9)−0.0013 (7)0.0045 (7)0.0011 (7)
C70.0195 (7)0.0248 (8)0.0232 (7)0.0035 (6)0.0042 (5)−0.0023 (6)
Mn1—O12.1194 (13)O6—H6B0.8600
Mn1—O52.2582 (14)N1—H110.77 (3)
Mn1—O62.1628 (14)N1—H120.85 (2)
Mn1—O1i2.1194 (13)C1—C71.521 (2)
Mn1—O5i2.2582 (14)C1—C21.399 (2)
Mn1—O6i2.1628 (14)C1—C61.398 (2)
S1—O31.4313 (15)C2—C31.396 (2)
S1—O41.4352 (16)C3—C41.383 (3)
S1—N11.6223 (17)C4—C51.384 (3)
S1—C21.7746 (17)C5—C61.384 (3)
O1—C71.265 (2)C3—H30.9300
O2—C71.234 (2)C4—H40.9300
O5—H5A0.8600C5—H50.9300
O5—H5B0.9700C6—H60.9300
O6—H6A0.9400
S1···O23.0246 (16)O4···H6ii2.7600
S1···H6Bii2.9200O4···H32.4000
O1···O53.202 (2)O4···H4xi2.8900
O1···O62.883 (2)O5···H6Av1.8500
O1···O6i3.1663 (19)O6···H5A2.9100
O1···O5i2.989 (2)O6···H5Aix2.6500
O1···O3iii3.228 (2)O6···H5Bix2.6500
O1···O2iv3.068 (2)N1···O22.799 (2)
O2···O1iii3.068 (2)N1···O6ii3.008 (2)
O2···N12.799 (2)N1···H6Bii2.2500
O2···O6i3.099 (2)C6···O4viii3.420 (2)
O2···S13.0246 (16)C6···O3iii3.389 (2)
O2···O32.895 (2)C7···O3iii3.254 (2)
O2···O5v2.775 (2)C7···O33.135 (2)
O3···C73.135 (2)C3···H5xii3.0300
O3···O5iv2.869 (2)C6···H12iv3.08 (2)
O3···O6ii3.136 (2)C7···H113.03 (3)
O3···C6iv3.389 (2)C7···H5Bv2.9900
O3···O1iv3.228 (2)H3···O42.4000
O3···C7iv3.254 (2)H3···H3xi2.5300
O3···O22.895 (2)H4···O4xi2.8900
O4···C6ii3.420 (2)H5···C3xiii3.0300
O5···O6v2.765 (2)H5A···H6Av2.2700
O5···O1i2.989 (2)H5A···O3iii2.0200
O5···O62.967 (2)H5A···O6vi2.6500
O5···O6vi3.055 (2)H5B···O2vii1.8300
O5···O2vii2.775 (2)H5B···C7vii2.9900
O5···O13.202 (2)H5B···H6Av2.2900
O5···O3iii2.869 (2)H5B···O6vi2.6500
O6···O5vii2.765 (2)H5B···H6Avi2.5500
O6···O3viii3.136 (2)H6···O12.4900
O6···O52.967 (2)H6···O4viii2.7600
O6···O1i3.1663 (19)H6A···O5vii1.8500
O6···O2i3.099 (2)H6A···H5Avii2.2700
O6···N1viii3.008 (2)H6A···H5Bvii2.2900
O6···O5ix3.055 (2)H6A···O2i2.8500
O6···O12.883 (2)H6A···H5Bix2.5500
O1···H62.4900H6B···S1viii2.9200
O1···H6B2.7700H6B···O3viii2.6900
O1···H11iv2.68 (3)H6B···N1viii2.2500
O1···H5Bi2.7300H6B···H11viii2.5100
O2···H112.19 (3)H11···O22.19 (3)
O2···H5Bv1.8300H11···C73.03 (3)
O2···H6Ai2.8500H11···H6Bii2.5100
O3···H6Bii2.6900H11···O1iii2.68 (3)
O3···H5Aiv2.0200H12···O4xiv2.50 (2)
O4···H12x2.50 (2)H12···C6iii3.08 (2)
O1—Mn1—O593.95 (5)Mn1—O6—H6A117.00
O1—Mn1—O684.64 (5)H6A—O6—H6B110.00
O1—Mn1—O1i180.00S1—N1—H12111.1 (16)
O1—Mn1—O5i86.05 (5)S1—N1—H11111 (2)
O1—Mn1—O6i95.36 (5)H11—N1—H12115 (2)
O5—Mn1—O684.27 (5)C2—C1—C6117.85 (15)
O1i—Mn1—O586.05 (5)C2—C1—C7124.92 (14)
O5—Mn1—O5i180.00C6—C1—C7117.19 (15)
O5—Mn1—O6i95.73 (5)S1—C2—C1123.55 (12)
O1i—Mn1—O695.36 (5)S1—C2—C3115.65 (14)
O5i—Mn1—O695.73 (5)C1—C2—C3120.76 (17)
O6—Mn1—O6i180.00C2—C3—C4120.1 (2)
O1i—Mn1—O5i93.95 (5)C3—C4—C5119.80 (18)
O1i—Mn1—O6i84.64 (5)C4—C5—C6120.2 (2)
O5i—Mn1—O6i84.27 (5)C1—C6—C5121.27 (17)
O3—S1—O4116.79 (9)O2—C7—C1118.68 (15)
O3—S1—N1108.69 (9)O1—C7—O2126.13 (15)
O3—S1—C2108.09 (9)O1—C7—C1115.15 (14)
O4—S1—N1106.03 (9)C2—C3—H3120.00
O4—S1—C2108.37 (8)C4—C3—H3120.00
N1—S1—C2108.63 (8)C3—C4—H4120.00
Mn1—O1—C7128.58 (11)C5—C4—H4120.00
H5A—O5—H5B111.00C4—C5—H5120.00
Mn1—O5—H5B105.00C6—C5—H5120.00
Mn1—O5—H5A108.00C1—C6—H6119.00
Mn1—O6—H6B120.00C5—C6—H6119.00
O5—Mn1—O1—C757.48 (15)C7—C1—C2—S14.8 (2)
O6—Mn1—O1—C7141.35 (15)C7—C1—C2—C3−177.97 (17)
O5i—Mn1—O1—C7−122.52 (15)C2—C1—C6—C5−0.3 (2)
O6i—Mn1—O1—C7−38.65 (15)C7—C1—C6—C5177.57 (17)
O3—S1—C2—C146.54 (16)C2—C1—C7—O1−150.20 (16)
O3—S1—C2—C3−130.87 (15)C2—C1—C7—O232.0 (2)
O4—S1—C2—C1174.00 (14)C6—C1—C7—O132.1 (2)
O4—S1—C2—C3−3.41 (17)C6—C1—C7—O2−145.67 (16)
N1—S1—C2—C1−71.23 (16)S1—C2—C3—C4178.11 (17)
N1—S1—C2—C3111.36 (16)C1—C2—C3—C40.6 (3)
Mn1—O1—C7—O24.9 (3)C2—C3—C4—C5−0.4 (3)
Mn1—O1—C7—C1−172.72 (10)C3—C4—C5—C6−0.2 (3)
C6—C1—C2—S1−177.56 (12)C4—C5—C6—C10.6 (3)
C6—C1—C2—C3−0.3 (2)
D—H···AD—HH···AD···AD—H···A
O5—H5A···O3iii0.862.022.869 (2)167
O5—H5B···O2vii0.971.832.775 (2)164
O6—H6A···O5vii0.941.852.765 (2)164
O6—H6B···N1viii0.862.253.008 (2)148
N1—H11···O20.77 (3)2.19 (3)2.799 (2)137 (2)
N1—H12···O4xiv0.85 (2)2.50 (2)3.300 (2)157 (2)
C3—H3···O40.932.402.834 (3)108
Mn1—O12.1194 (13)
Mn1—O52.2582 (14)
Mn1—O62.1628 (14)
Mn1—O1i2.1194 (13)
Mn1—O5i2.2582 (14)
Mn1—O6i2.1628 (14)
S1—O31.4313 (15)
S1—O41.4352 (16)
S1—N11.6223 (17)
O1—Mn1—O593.95 (5)
O1—Mn1—O684.64 (5)
O1—Mn1—O5i86.05 (5)
O1—Mn1—O6i95.36 (5)
O5—Mn1—O684.27 (5)
Mn1—O1—C7128.58 (11)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O5—H5A⋯O3ii0.862.022.869 (2)167
O5—H5B⋯O2iii0.971.832.775 (2)164
O6—H6A⋯O5iii0.941.852.765 (2)164
O6—H6B⋯N1iv0.862.253.008 (2)148
N1—H11⋯O20.77 (3)2.19 (3)2.799 (2)137 (2)
N1—H12⋯O4v0.85 (2)2.50 (2)3.300 (2)157 (2)
C3—H3⋯O40.932.402.834 (3)108

Symmetry codes: (ii) ; (iii) ; (iv) ; (v) .

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5.  Chlorido{4,4'-dichloro-2,2'-[1,2-phenyl-enebis(nitrilo-methyl-idyne)]diphenolato-κO,N,N',O'}(methanol-κO)manganese(III).

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2.  4-Hy-droxy-2-methyl-1,1-dioxo-2H-1λ,2- benzothia-zine-3-carb-oxy-lic acid hemihydrate.

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