Literature DB >> 25249880

Di-aqua-[5,10,15,20-tetra-kis-(4-chloro-phen-yl)porphyrinato-κ(4) N]iron(III) tri-fluoro-methane-sulfonate-4-hy-droxy-3-meth-oxy-benzaldehyde-water (1/1/2).

Leila Ben Haj Hassen1, Khaireddine Ezzayani1, Yoann Rousselin2, Habib Nasri1.   

Abstract

In the title compound, [Fe(C44H24Cl4N4)(H2O)2](SO3CF3)·C8H8O3·2H2O, the Fe(III) cation is chelated by the four N atoms of the deprotonated tetra-kis-(4-chloro-tetra-phen-yl)porphyrin (TClPP) and further coordinated by two water mol-ecules in a distorted octa-hedral geometry. In the crystal, the cations, anions, 4-hy-droxy-3-meth-oxy-benzaldehyde and water mol-ecules of crystallization are linked by classical O-H⋯O hydrogen bonds and weak C-H⋯O and C-H⋯Cl hydrogen bonds into a three-dimensional supra-molecular architecture. The crystal packing is further stabilized by weak C-H⋯π inter-actions involving pyrrole and benzene rings. π-π stacking between parallel benzene rings of adjacent 4-hy-droxy-3-meth-oxy-benzaldehyde mol-ecules is also observed, the centroid-centroid distance being 3.8003 (13) Å. The three F atoms of the anion are disordered over two sets of sites, with a refined occupancy ratio 0.527 (12):0.473 (12). The O atom of one water mol-ecule of crystallization is also disordered over two positions in an occupancy ratio of 0.68 (5):0.32 (5).

Entities:  

Keywords:  crystal structure

Year:  2014        PMID： 25249880      PMCID： PMC4158530          DOI： 10.1107/S1600536814015335

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


Related literature

For the synthesis, see: Gismelseed et al. (1990 ▶). For related structures, see: Gismelseed et al. (1990 ▶); Scheidt et al. (1979 ▶); Scheidt & Reed (1981 ▶); Scheidt & Finnegan (1989 ▶); Dhifet et al. (2009 ▶); Xu et al. (2011 ▶); Nasri et al. (1990 ▶); Cheng et al. (1994 ▶). For a description of the Cambridge Structural Database, see: Allen (2002 ▶).

Experimental

Crystal data

[Fe(C44H24Cl4N4)(H2O)2](CF3O3S)·C8H8O3·2H2O M = 1179.60 Monoclinic, a = 10.9998 (4) Å b = 17.8613 (6) Å c = 26.6592 (9) Å β = 97.9013 (11)° V = 5188.0 (3) Å3 Z = 4 Mo Kα radiation μ = 0.61 mm−1 T = 115 K 0.2 × 0.2 × 0.1 mm

Data collection

Nonius KappaAPEXII diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2012 ▶) T min = 0.885, T max = 0.941 95018 measured reflections 11916 independent reflections 8821 reflections with I > 2σ(I) R int = 0.061

Refinement

R[F 2 > 2σ(F 2)] = 0.040 wR(F 2) = 0.101 S = 1.02 11916 reflections 709 parameters H-atom parameters constrained Δρmax = 0.76 e Å−3 Δρmin = −0.74 e Å−3 Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: OLEX2.solve (Puschmann et al., 2013 ▶); program(s) used to refine structure: SHELXTL (Sheldrick, 2008 ▶); molecular graphics: ORTEPIII (Burnett & Johnson, 1996 ▶) and ORTEP-3 for Windows (Farrugia, 2012 ▶); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009 ▶). Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536814015335/xu5800sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536814015335/xu5800Isup2.hkl CCDC reference: 975656 Additional supporting information: crystallographic information; 3D view; checkCIF report
[Fe(C44H24Cl4N4)(H2O)2](CF3O3S)·C8H8O3·2H2OF(000) = 2412
Mr = 1179.60Dx = 1.510 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 10.9998 (4) ÅCell parameters from 9872 reflections
b = 17.8613 (6) Åθ = 2.5–27.4°
c = 26.6592 (9) ŵ = 0.61 mm−1
β = 97.9013 (11)°T = 115 K
V = 5188.0 (3) Å3Prism, dark violet
Z = 40.2 × 0.2 × 0.1 mm
Nonius KappaAPEXII diffractometer11916 independent reflections
Radiation source: X-ray tube, Siemens KFF Mo 2K-1808821 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.061
φ and ω scansθmax = 27.5°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Bruker, 2012)h = −14→14
Tmin = 0.885, Tmax = 0.941k = −23→23
95018 measured reflectionsl = −34→34
Refinement on F26 constraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.040H-atom parameters constrained
wR(F2) = 0.101w = 1/[σ2(Fo2) + (0.0399P)2 + 6.1729P] where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.002
11916 reflectionsΔρmax = 0.76 e Å−3
709 parametersΔρmin = −0.74 e Å−3
0 restraints
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.
xyzUiso*/UeqOcc. (<1)
C10.7091 (2)0.75273 (13)0.22709 (8)0.0148 (4)
C20.6504 (2)0.76670 (13)0.17385 (8)0.0159 (5)
C30.5374 (2)0.80365 (13)0.16516 (9)0.0167 (5)
H30.49950.82030.19310.020*
C40.4800 (2)0.81620 (13)0.11625 (9)0.0189 (5)
H40.40270.84080.11060.023*
C4EA0.2576 (2)0.59674 (13)0.39721 (9)0.0193 (5)
H4EA0.19280.62700.40610.023*
C50.5364 (2)0.79256 (14)0.07589 (9)0.0193 (5)
C60.6483 (2)0.75627 (14)0.08291 (9)0.0211 (5)
H60.68600.74050.05470.025*
C70.7051 (2)0.74313 (14)0.13225 (9)0.0197 (5)
H70.78180.71790.13760.024*
C80.8235 (2)0.78571 (12)0.24315 (8)0.0135 (4)
C90.8903 (2)0.83203 (14)0.21212 (9)0.0192 (5)
H90.86300.84770.17840.023*
C100.9989 (2)0.84900 (14)0.23989 (8)0.0194 (5)
H101.06260.87810.22900.023*
C111.0008 (2)0.81518 (12)0.28879 (8)0.0140 (4)
C121.0996 (2)0.81831 (12)0.32806 (8)0.0133 (4)
C131.2167 (2)0.85384 (13)0.31672 (8)0.0143 (4)
C141.2242 (2)0.92948 (13)0.30468 (8)0.0165 (5)
H141.15390.96050.30420.020*
C151.3339 (2)0.96011 (14)0.29332 (9)0.0193 (5)
H151.33811.01150.28460.023*
C161.4362 (2)0.91480 (14)0.29486 (9)0.0205 (5)
C171.4318 (2)0.83969 (14)0.30698 (9)0.0201 (5)
H171.50300.80930.30820.024*
C181.3217 (2)0.80948 (13)0.31731 (8)0.0161 (5)
H181.31750.75770.32490.019*
C191.0996 (2)0.78766 (12)0.37654 (8)0.0131 (4)
C201.1960 (2)0.79639 (13)0.41813 (8)0.0161 (5)
H201.27000.82370.41780.019*
C211.1622 (2)0.75870 (13)0.45793 (8)0.0159 (5)
H211.20830.75450.49070.019*
C221.0437 (2)0.72617 (12)0.44171 (8)0.0131 (4)
C230.9787 (2)0.68094 (12)0.47167 (8)0.0135 (4)
C241.0435 (2)0.65774 (13)0.52273 (8)0.0140 (4)
C251.0415 (2)0.70133 (13)0.56561 (9)0.0196 (5)
H250.99670.74700.56320.024*
C261.1043 (2)0.67914 (14)0.61238 (8)0.0197 (5)
H261.10350.70950.64160.024*
C271.1674 (2)0.61222 (14)0.61515 (8)0.0173 (5)
C281.1707 (2)0.56756 (14)0.57324 (9)0.0216 (5)
H281.21490.52170.57600.026*
C291.1086 (2)0.59058 (14)0.52690 (9)0.0187 (5)
H291.11050.56020.49780.022*
C300.8601 (2)0.65259 (12)0.45727 (8)0.0133 (4)
C310.7898 (2)0.61143 (13)0.48957 (8)0.0158 (5)
H310.81600.59740.52370.019*
C320.6794 (2)0.59620 (13)0.46239 (8)0.0154 (5)
H320.61350.57010.47400.019*
C330.6804 (2)0.62697 (12)0.41259 (8)0.0130 (4)
C340.5852 (2)0.62091 (12)0.37230 (8)0.0134 (4)
C350.4675 (2)0.58381 (13)0.38095 (8)0.0147 (5)
C360.4471 (2)0.50808 (14)0.37200 (11)0.0281 (6)
H360.51200.47730.36370.034*
C370.3326 (2)0.47665 (14)0.37508 (11)0.0280 (6)
H370.31900.42470.36900.034*
C380.2394 (2)0.52161 (13)0.38702 (8)0.0156 (5)
C390.3724 (2)0.62737 (13)0.39432 (9)0.0174 (5)
H390.38620.67900.40160.021*
C400.5879 (2)0.64867 (12)0.32326 (8)0.0143 (4)
C410.4945 (2)0.63557 (13)0.28105 (9)0.0177 (5)
H410.42150.60730.28160.021*
C420.5291 (2)0.67066 (13)0.24049 (9)0.0178 (5)
H420.48580.67100.20710.021*
C430.6443 (2)0.70764 (12)0.25718 (8)0.0140 (4)
N10.89170 (16)0.77736 (10)0.29038 (7)0.0125 (4)
N20.67932 (17)0.69230 (10)0.30781 (7)0.0133 (4)
N30.79152 (16)0.66139 (10)0.41031 (7)0.0122 (4)
N41.00622 (16)0.74539 (10)0.39191 (7)0.0128 (4)
O10.76299 (15)0.81594 (9)0.37720 (6)0.0187 (3)
H1A0.81870.85220.38390.028*
H1B0.73190.80590.40570.028*
O20.91879 (16)0.62112 (9)0.32428 (6)0.0216 (4)
H2A0.91000.62030.29090.032*
H2B0.86630.59050.33560.032*
Cl10.46219 (6)0.80909 (4)0.01479 (2)0.02837 (15)
Cl20.09344 (5)0.48365 (3)0.38831 (2)0.02059 (13)
Cl31.24603 (6)0.58219 (4)0.67323 (2)0.02717 (15)
Cl41.57458 (6)0.95266 (4)0.28187 (3)0.03687 (18)
Fe10.84010 (3)0.72182 (2)0.35080 (2)0.01104 (8)
C440.5613 (2)0.89392 (16)0.43434 (10)0.0278 (6)
H440.58680.91630.40520.033*
C450.4549 (2)0.92685 (14)0.45329 (9)0.0223 (5)
C460.4162 (2)0.90025 (14)0.49835 (9)0.0213 (5)
H460.46130.86230.51780.026*
C470.3121 (2)0.93010 (14)0.51372 (9)0.0204 (5)
C480.2449 (2)0.98641 (14)0.48501 (9)0.0211 (5)
C490.2843 (2)1.01260 (15)0.44081 (9)0.0249 (5)
H490.23971.05070.42140.030*
C500.3895 (2)0.98248 (15)0.42550 (9)0.0247 (6)
H500.41691.00040.39540.030*
C510.3268 (3)0.85316 (16)0.58774 (10)0.0322 (6)
H51A0.33130.80730.56790.048*
H51B0.28260.84290.61650.048*
H51C0.40990.87050.60020.048*
O70.14350 (17)1.01146 (11)0.50295 (6)0.0269 (4)
H7A0.10671.04220.48240.040*
O80.26317 (17)0.90970 (11)0.55642 (7)0.0281 (4)
O90.62056 (18)0.84012 (11)0.45260 (8)0.0351 (5)
C520.1484 (3)0.61624 (19)0.22889 (11)0.0362 (7)
O3−0.08765 (17)0.60737 (11)0.22290 (7)0.0312 (4)
O4−0.00031 (18)0.65653 (11)0.15053 (7)0.0342 (5)
O50.0170 (2)0.52536 (11)0.17085 (8)0.0390 (5)
S0AA0.00338 (6)0.60012 (3)0.18920 (2)0.01966 (13)
O60.00468 (17)0.10763 (11)0.44911 (7)0.0289 (4)
H6A−0.07020.09690.45370.043*
H6B0.00710.11620.41710.043*
O100.149 (5)0.0536 (15)0.6090 (10)0.044 (8)0.32 (5)
H10A0.16070.04490.57790.066*0.32 (5)
H10B0.10760.01660.61980.066*0.32 (5)
O10B0.0901 (17)0.0701 (5)0.5980 (4)0.034 (2)0.68 (5)
H10C0.06530.03970.61990.050*0.68 (5)
H10D0.10340.04520.57130.050*0.68 (5)
F1_10.2374 (6)0.6047 (3)0.19998 (16)0.0441 (12)0.473 (12)
F2_10.1574 (4)0.6952 (3)0.2380 (2)0.0441 (12)0.473 (12)
F3_10.1719 (4)0.5850 (4)0.27147 (15)0.0441 (12)0.473 (12)
F1A_20.2464 (6)0.6124 (3)0.20575 (19)0.0448 (11)0.527 (12)
F2A_20.1492 (4)0.6758 (3)0.2566 (2)0.0448 (11)0.527 (12)
F3A_20.1597 (4)0.5563 (4)0.26316 (17)0.0448 (11)0.527 (12)
U11U22U33U12U13U23
C10.0134 (11)0.0175 (11)0.0136 (10)0.0021 (9)0.0019 (8)0.0003 (9)
C20.0138 (11)0.0182 (12)0.0155 (11)−0.0042 (9)0.0007 (9)0.0045 (9)
C30.0131 (11)0.0188 (12)0.0183 (11)−0.0022 (9)0.0022 (9)0.0005 (9)
C40.0121 (11)0.0208 (12)0.0222 (12)−0.0009 (9)−0.0030 (9)0.0043 (10)
C4EA0.0146 (12)0.0217 (12)0.0228 (12)0.0003 (10)0.0073 (9)−0.0018 (10)
C50.0177 (12)0.0238 (13)0.0141 (11)−0.0067 (10)−0.0054 (9)0.0065 (9)
C60.0203 (12)0.0287 (13)0.0146 (11)−0.0031 (10)0.0030 (9)−0.0013 (10)
C70.0137 (11)0.0267 (13)0.0180 (11)0.0014 (10)−0.0005 (9)0.0015 (10)
C80.0119 (11)0.0168 (11)0.0115 (10)0.0007 (9)0.0015 (8)0.0004 (8)
C90.0169 (12)0.0267 (13)0.0135 (11)−0.0029 (10)0.0007 (9)0.0056 (9)
C100.0168 (12)0.0259 (13)0.0157 (11)−0.0046 (10)0.0030 (9)0.0044 (10)
C110.0133 (11)0.0155 (11)0.0137 (10)−0.0010 (9)0.0037 (8)0.0004 (9)
C120.0099 (10)0.0150 (11)0.0154 (11)−0.0014 (9)0.0032 (8)−0.0013 (9)
C130.0131 (11)0.0195 (12)0.0100 (10)−0.0039 (9)0.0006 (8)−0.0024 (9)
C140.0148 (11)0.0194 (12)0.0147 (11)0.0002 (9)−0.0001 (9)−0.0003 (9)
C150.0213 (13)0.0178 (12)0.0182 (11)−0.0055 (10)0.0005 (9)0.0023 (9)
C160.0142 (12)0.0285 (13)0.0190 (12)−0.0079 (10)0.0034 (9)0.0021 (10)
C170.0145 (12)0.0253 (13)0.0212 (12)0.0004 (10)0.0050 (9)−0.0001 (10)
C180.0160 (11)0.0158 (11)0.0169 (11)−0.0018 (9)0.0042 (9)0.0003 (9)
C190.0105 (10)0.0152 (11)0.0135 (10)0.0005 (9)0.0020 (8)−0.0008 (8)
C200.0123 (11)0.0196 (12)0.0159 (11)−0.0036 (9)0.0004 (9)−0.0022 (9)
C210.0137 (11)0.0210 (12)0.0123 (10)−0.0015 (9)−0.0008 (8)−0.0018 (9)
C220.0120 (10)0.0171 (11)0.0101 (10)0.0019 (9)0.0009 (8)−0.0019 (8)
C230.0125 (11)0.0159 (11)0.0119 (10)0.0018 (9)0.0013 (8)−0.0019 (8)
C240.0112 (11)0.0185 (11)0.0126 (10)−0.0033 (9)0.0031 (8)0.0020 (9)
C250.0231 (13)0.0184 (12)0.0168 (11)0.0023 (10)0.0012 (10)−0.0002 (9)
C260.0217 (12)0.0258 (13)0.0110 (10)−0.0002 (10)0.0008 (9)−0.0025 (9)
C270.0100 (11)0.0297 (13)0.0118 (10)0.0001 (10)0.0003 (8)0.0058 (9)
C280.0197 (13)0.0261 (13)0.0191 (12)0.0072 (10)0.0036 (10)0.0037 (10)
C290.0185 (12)0.0247 (13)0.0132 (11)0.0031 (10)0.0027 (9)−0.0023 (9)
C300.0140 (11)0.0143 (11)0.0118 (10)0.0021 (9)0.0022 (8)−0.0002 (8)
C310.0154 (11)0.0182 (12)0.0140 (11)−0.0010 (9)0.0027 (9)0.0015 (9)
C320.0145 (11)0.0165 (11)0.0160 (11)−0.0021 (9)0.0048 (9)0.0017 (9)
C330.0122 (11)0.0124 (10)0.0148 (11)−0.0006 (8)0.0037 (8)−0.0006 (8)
C340.0093 (10)0.0127 (11)0.0186 (11)−0.0009 (8)0.0029 (8)0.0003 (9)
C350.0126 (11)0.0176 (11)0.0141 (10)−0.0025 (9)0.0020 (8)0.0030 (9)
C360.0150 (12)0.0176 (12)0.0531 (17)0.0019 (10)0.0101 (12)−0.0008 (12)
C370.0181 (13)0.0131 (12)0.0540 (18)−0.0043 (10)0.0091 (12)−0.0024 (11)
C380.0106 (11)0.0208 (12)0.0153 (11)−0.0047 (9)0.0009 (8)0.0044 (9)
C390.0177 (12)0.0160 (11)0.0191 (11)−0.0040 (9)0.0052 (9)−0.0021 (9)
C400.0110 (11)0.0149 (11)0.0172 (11)−0.0004 (9)0.0022 (9)0.0002 (9)
C410.0121 (11)0.0206 (12)0.0193 (11)−0.0041 (9)−0.0012 (9)0.0005 (9)
C420.0133 (11)0.0223 (12)0.0166 (11)−0.0037 (9)−0.0022 (9)−0.0012 (9)
C430.0114 (11)0.0162 (11)0.0138 (10)0.0003 (9)−0.0011 (8)0.0000 (8)
N10.0091 (9)0.0166 (9)0.0117 (9)−0.0006 (7)0.0010 (7)0.0006 (7)
N20.0109 (9)0.0154 (9)0.0135 (9)−0.0006 (7)0.0008 (7)0.0018 (7)
N30.0099 (9)0.0153 (9)0.0112 (9)−0.0013 (7)0.0012 (7)0.0003 (7)
N40.0106 (9)0.0170 (9)0.0110 (9)−0.0008 (7)0.0021 (7)−0.0004 (7)
O10.0178 (9)0.0177 (8)0.0225 (9)−0.0001 (7)0.0089 (7)−0.0012 (7)
O20.0272 (10)0.0221 (9)0.0164 (8)0.0054 (7)0.0065 (7)−0.0012 (7)
Cl10.0245 (3)0.0417 (4)0.0164 (3)−0.0080 (3)−0.0063 (2)0.0101 (3)
Cl20.0119 (3)0.0247 (3)0.0254 (3)−0.0047 (2)0.0032 (2)0.0052 (2)
Cl30.0195 (3)0.0486 (4)0.0133 (3)0.0091 (3)0.0017 (2)0.0083 (3)
Cl40.0188 (3)0.0420 (4)0.0512 (4)−0.0106 (3)0.0098 (3)0.0146 (3)
Fe10.00874 (15)0.01416 (16)0.01025 (14)−0.00075 (12)0.00145 (11)0.00049 (12)
C440.0209 (13)0.0363 (16)0.0282 (14)−0.0101 (12)0.0108 (11)−0.0109 (12)
C450.0167 (12)0.0276 (13)0.0228 (12)−0.0064 (10)0.0038 (10)−0.0108 (10)
C460.0180 (12)0.0230 (13)0.0227 (12)−0.0004 (10)0.0024 (10)−0.0071 (10)
C470.0202 (12)0.0257 (13)0.0156 (11)−0.0019 (10)0.0037 (9)−0.0060 (10)
C480.0180 (12)0.0269 (13)0.0189 (12)0.0003 (10)0.0040 (9)−0.0058 (10)
C490.0241 (13)0.0304 (14)0.0201 (12)−0.0008 (11)0.0026 (10)−0.0015 (11)
C500.0228 (13)0.0347 (15)0.0176 (12)−0.0087 (11)0.0062 (10)−0.0058 (11)
C510.0333 (16)0.0409 (17)0.0228 (13)0.0130 (13)0.0055 (12)0.0078 (12)
O70.0252 (10)0.0352 (11)0.0219 (9)0.0115 (8)0.0086 (8)0.0060 (8)
O80.0278 (10)0.0369 (11)0.0217 (9)0.0136 (8)0.0109 (8)0.0063 (8)
O90.0289 (11)0.0360 (11)0.0441 (12)0.0035 (9)0.0185 (9)−0.0037 (9)
C520.0267 (15)0.057 (2)0.0242 (14)0.0059 (14)0.0021 (12)−0.0089 (14)
O30.0255 (10)0.0480 (12)0.0209 (9)0.0048 (9)0.0065 (8)−0.0075 (8)
O40.0347 (11)0.0356 (11)0.0319 (10)0.0032 (9)0.0028 (9)0.0093 (9)
O50.0449 (13)0.0284 (11)0.0494 (13)−0.0089 (9)0.0271 (10)−0.0135 (9)
S0AA0.0197 (3)0.0235 (3)0.0162 (3)−0.0002 (2)0.0040 (2)−0.0025 (2)
O60.0299 (11)0.0314 (10)0.0266 (10)0.0053 (9)0.0079 (8)0.0060 (8)
O100.074 (18)0.027 (7)0.038 (6)−0.026 (9)0.032 (9)−0.011 (5)
O10B0.052 (6)0.024 (2)0.030 (3)−0.013 (3)0.021 (3)−0.0083 (18)
F1_10.0317 (16)0.072 (2)0.0259 (16)−0.0074 (13)−0.0058 (10)−0.0084 (12)
F2_10.0317 (16)0.072 (2)0.0259 (16)−0.0074 (13)−0.0058 (10)−0.0084 (12)
F3_10.0317 (16)0.072 (2)0.0259 (16)−0.0074 (13)−0.0058 (10)−0.0084 (12)
F1A_20.0330 (14)0.071 (2)0.0279 (15)−0.0038 (12)−0.0032 (10)−0.0091 (11)
F2A_20.0330 (14)0.071 (2)0.0279 (15)−0.0038 (12)−0.0032 (10)−0.0091 (11)
F3A_20.0330 (14)0.071 (2)0.0279 (15)−0.0038 (12)−0.0032 (10)−0.0091 (11)
C1—C21.497 (3)C33—C341.398 (3)
C1—C81.402 (3)C33—N31.377 (3)
C1—C431.399 (3)C34—C351.500 (3)
C2—C31.399 (3)C34—C401.402 (3)
C2—C71.397 (3)C35—C361.386 (3)
C3—H30.9500C35—C391.389 (3)
C3—C41.386 (3)C36—H360.9500
C4—H40.9500C36—C371.392 (3)
C4—C51.380 (3)C37—H370.9500
C4EA—H4EA0.9500C37—C381.373 (3)
C4EA—C381.378 (3)C38—Cl21.747 (2)
C4EA—C391.388 (3)C39—H390.9500
C5—C61.381 (3)C40—C411.435 (3)
C5—Cl11.744 (2)C40—N21.379 (3)
C6—H60.9500C41—H410.9500
C6—C71.396 (3)C41—C421.349 (3)
C7—H70.9500C42—H420.9500
C8—C91.441 (3)C42—C431.443 (3)
C8—N11.382 (3)C43—N21.379 (3)
C9—H90.9500N1—Fe12.0377 (18)
C9—C101.351 (3)N2—Fe12.0402 (18)
C10—H100.9500N3—Fe12.0497 (18)
C10—C111.434 (3)N4—Fe12.0412 (18)
C11—C121.403 (3)O1—H1A0.8932
C11—N11.383 (3)O1—H1B0.8931
C12—C131.504 (3)O1—Fe12.0506 (16)
C12—C191.404 (3)O2—H2A0.8809
C13—C141.394 (3)O2—H2B0.8779
C13—C181.398 (3)O2—Fe12.1570 (16)
C14—H140.9500C44—H440.9500
C14—C151.395 (3)C44—C451.460 (3)
C15—H150.9500C44—O91.224 (3)
C15—C161.383 (3)C45—C461.411 (3)
C16—C171.382 (3)C45—C501.381 (4)
C16—Cl41.743 (2)C46—H460.9500
C17—H170.9500C46—C471.376 (3)
C17—C181.388 (3)C47—C481.410 (4)
C18—H180.9500C47—O81.373 (3)
C19—C201.433 (3)C48—C491.391 (3)
C19—N41.382 (3)C48—O71.349 (3)
C20—H200.9500C49—H490.9500
C20—C211.351 (3)C49—C501.387 (4)
C21—H210.9500C50—H500.9500
C21—C221.438 (3)C51—H51A0.9800
C22—C231.399 (3)C51—H51B0.9800
C22—N41.378 (3)C51—H51C0.9800
C23—C241.506 (3)C51—O81.430 (3)
C23—C301.403 (3)O7—H7A0.8400
C24—C251.386 (3)C52—S0AA1.812 (3)
C24—C291.394 (3)C52—F1_11.342 (5)
C25—H250.9500C52—F2_11.431 (5)
C25—C261.397 (3)C52—F3_11.259 (4)
C26—H260.9500C52—F1A_21.315 (6)
C26—C271.379 (3)C52—F2A_21.293 (5)
C27—C281.377 (3)C52—F3A_21.403 (6)
C27—Cl31.751 (2)O3—S0AA1.4402 (18)
C28—H280.9500O4—S0AA1.4380 (19)
C28—C291.389 (3)O5—S0AA1.437 (2)
C29—H290.9500O6—H6A0.8699
C30—C311.436 (3)O6—H6B0.8702
C30—N31.379 (3)O10—H10A0.8696
C31—H310.9500O10—H10B0.8701
C31—C321.354 (3)O10B—H10C0.8703
C32—H320.9500O10B—H10D0.8697
C32—C331.438 (3)
C8—C1—C2118.1 (2)C35—C36—H36119.7
C43—C1—C2116.9 (2)C35—C36—C37120.6 (2)
C43—C1—C8125.0 (2)C37—C36—H36119.7
C3—C2—C1119.6 (2)C36—C37—H37120.4
C7—C2—C1121.7 (2)C38—C37—C36119.2 (2)
C7—C2—C3118.7 (2)C38—C37—H37120.4
C2—C3—H3119.6C4EA—C38—Cl2118.87 (18)
C4—C3—C2120.8 (2)C37—C38—C4EA121.5 (2)
C4—C3—H3119.6C37—C38—Cl2119.65 (18)
C3—C4—H4120.4C4EA—C39—C35121.1 (2)
C5—C4—C3119.2 (2)C4EA—C39—H39119.5
C5—C4—H4120.4C35—C39—H39119.5
C38—C4EA—H4EA120.6C34—C40—C41124.7 (2)
C38—C4EA—C39118.8 (2)N2—C40—C34126.0 (2)
C39—C4EA—H4EA120.6N2—C40—C41109.33 (19)
C4—C5—C6121.7 (2)C40—C41—H41126.2
C4—C5—Cl1118.26 (19)C42—C41—C40107.6 (2)
C6—C5—Cl1120.00 (19)C42—C41—H41126.2
C5—C6—H6120.6C41—C42—H42126.3
C5—C6—C7118.8 (2)C41—C42—C43107.3 (2)
C7—C6—H6120.6C43—C42—H42126.3
C2—C7—H7119.6C1—C43—C42125.5 (2)
C6—C7—C2120.8 (2)N2—C43—C1125.4 (2)
C6—C7—H7119.6N2—C43—C42109.03 (19)
C1—C8—C9125.0 (2)C8—N1—C11106.51 (17)
N1—C8—C1125.8 (2)C8—N1—Fe1126.67 (15)
N1—C8—C9109.22 (19)C11—N1—Fe1126.81 (14)
C8—C9—H9126.4C40—N2—C43106.70 (18)
C10—C9—C8107.2 (2)C40—N2—Fe1126.14 (15)
C10—C9—H9126.4C43—N2—Fe1127.04 (15)
C9—C10—H10126.1C30—N3—Fe1126.49 (15)
C9—C10—C11107.8 (2)C33—N3—C30106.68 (18)
C11—C10—H10126.1C33—N3—Fe1126.64 (14)
C12—C11—C10125.1 (2)C19—N4—Fe1126.93 (14)
N1—C11—C10109.22 (19)C22—N4—C19106.61 (18)
N1—C11—C12125.69 (19)C22—N4—Fe1126.34 (15)
C11—C12—C13117.66 (19)H1A—O1—H1B107.9
C11—C12—C19125.0 (2)Fe1—O1—H1A111.0
C19—C12—C13117.27 (19)Fe1—O1—H1B110.7
C14—C13—C12122.3 (2)H2A—O2—H2B110.5
C14—C13—C18118.5 (2)Fe1—O2—H2A110.5
C18—C13—C12119.2 (2)Fe1—O2—H2B95.4
C13—C14—H14119.7N1—Fe1—N289.77 (7)
C13—C14—C15120.7 (2)N1—Fe1—N3177.28 (7)
C15—C14—H14119.7N1—Fe1—N489.88 (7)
C14—C15—H15120.4N1—Fe1—O192.61 (7)
C16—C15—C14119.3 (2)N1—Fe1—O288.79 (7)
C16—C15—H15120.4N2—Fe1—N390.03 (7)
C15—C16—Cl4119.78 (19)N2—Fe1—N4176.22 (8)
C17—C16—C15121.4 (2)N2—Fe1—O192.13 (7)
C17—C16—Cl4118.86 (19)N2—Fe1—O287.49 (7)
C16—C17—H17120.5N3—Fe1—O190.11 (7)
C16—C17—C18118.9 (2)N3—Fe1—O288.49 (7)
C18—C17—H17120.5N4—Fe1—N390.14 (7)
C13—C18—H18119.4N4—Fe1—O191.64 (7)
C17—C18—C13121.3 (2)N4—Fe1—O288.74 (7)
C17—C18—H18119.4O1—Fe1—O2178.54 (7)
C12—C19—C20125.2 (2)C45—C44—H44117.0
N4—C19—C12125.5 (2)O9—C44—H44117.0
N4—C19—C20109.34 (19)O9—C44—C45125.9 (3)
C19—C20—H20126.3C46—C45—C44120.6 (2)
C21—C20—C19107.4 (2)C50—C45—C44119.2 (2)
C21—C20—H20126.3C50—C45—C46120.2 (2)
C20—C21—H21126.2C45—C46—H46120.5
C20—C21—C22107.5 (2)C47—C46—C45119.0 (2)
C22—C21—H21126.2C47—C46—H46120.5
C23—C22—C21125.1 (2)C46—C47—C48120.7 (2)
N4—C22—C21109.11 (19)O8—C47—C46125.5 (2)
N4—C22—C23125.8 (2)O8—C47—C48113.8 (2)
C22—C23—C24117.35 (19)C49—C48—C47119.9 (2)
C22—C23—C30125.5 (2)O7—C48—C47116.2 (2)
C30—C23—C24117.06 (19)O7—C48—C49123.9 (2)
C25—C24—C23122.1 (2)C48—C49—H49120.4
C25—C24—C29119.0 (2)C50—C49—C48119.3 (2)
C29—C24—C23118.90 (19)C50—C49—H49120.4
C24—C25—H25119.5C45—C50—C49121.0 (2)
C24—C25—C26121.0 (2)C45—C50—H50119.5
C26—C25—H25119.5C49—C50—H50119.5
C25—C26—H26120.8H51A—C51—H51B109.5
C27—C26—C25118.5 (2)H51A—C51—H51C109.5
C27—C26—H26120.8H51B—C51—H51C109.5
C26—C27—Cl3119.78 (18)O8—C51—H51A109.5
C28—C27—C26121.9 (2)O8—C51—H51B109.5
C28—C27—Cl3118.34 (18)O8—C51—H51C109.5
C27—C28—H28120.5C48—O7—H7A109.5
C27—C28—C29119.0 (2)C47—O8—C51117.1 (2)
C29—C28—H28120.5F1_1—C52—S0AA107.0 (3)
C24—C29—H29119.7F1_1—C52—F2_1102.0 (3)
C28—C29—C24120.7 (2)F2_1—C52—S0AA106.9 (2)
C28—C29—H29119.7F3_1—C52—S0AA120.7 (3)
C23—C30—C31125.3 (2)F3_1—C52—F1_1112.0 (3)
N3—C30—C23125.4 (2)F3_1—C52—F2_1106.5 (3)
N3—C30—C31109.31 (19)F1A_2—C52—S0AA115.5 (3)
C30—C31—H31126.3F1A_2—C52—F3A_2105.1 (4)
C32—C31—C30107.4 (2)F2A_2—C52—S0AA113.6 (3)
C32—C31—H31126.3F2A_2—C52—F1A_2111.6 (4)
C31—C32—H32126.4F2A_2—C52—F3A_2105.3 (3)
C31—C32—C33107.3 (2)F3A_2—C52—S0AA104.6 (3)
C33—C32—H32126.4O3—S0AA—C52104.66 (12)
C34—C33—C32125.4 (2)O4—S0AA—C52104.07 (14)
N3—C33—C32109.33 (19)O4—S0AA—O3115.50 (12)
N3—C33—C34125.22 (19)O5—S0AA—C52102.84 (14)
C33—C34—C35119.17 (19)O5—S0AA—O3114.19 (12)
C33—C34—C40125.4 (2)O5—S0AA—O4113.65 (12)
C40—C34—C35115.39 (19)H6A—O6—H6B109.5
C36—C35—C34121.8 (2)H10A—O10—H10B109.4
C36—C35—C39118.8 (2)H10C—O10B—H10D109.5
C39—C35—C34119.2 (2)
D—H···AD—HH···AD···AD—H···A
O1—H1A···O10Bi0.891.742.626 (8)171
O1—H1B···O90.891.962.747 (2)146
O2—H2A···O3ii0.881.832.705 (2)171
O6—H6A···O7iii0.872.453.064 (3)128
O6—H6A···O8iii0.872.112.946 (3)162
O6—H6B···O4iv0.871.932.790 (3)168
O7—H7A···O6v0.841.772.596 (3)167
O10—H10A···O7vi0.872.072.92 (3)165
O10B—H10C···O5vii0.871.922.786 (7)177
O10B—H10D···O7vi0.872.022.876 (5)166
C10—H10···Cl3viii0.952.763.659 (2)159
C14—H14···O5ix0.952.383.297 (3)162
C31—H31···Cl2i0.952.823.739 (2)163
C4EA—H4EA···Cg4x0.952.663.5054149
C17—H17···Cg2ii0.952.763.5715144
C20—H20···Cg13ii0.952.823.5054130
C28—H28···Cg3xi0.952.793.6574152
C37—H37···Cg10xii0.952.763.6107149
Table 1

Hydrogen-bond geometry (Å, °)

Cg2, Cg3, Cg4, Cg10 and Cg13 are the centroids of the N2/C40–C43, N3/C30–C33, N4/C19–C22, C2–C7 and C45–C50 rings, respectively.

D—H⋯A D—HH⋯A D⋯A D—H⋯A
O1—H1A⋯O10B i 0.891.742.626 (8)171
O1—H1B⋯O90.891.962.747 (2)146
O2—H2A⋯O3ii 0.881.832.705 (2)171
O6—H6A⋯O7iii 0.872.453.064 (3)128
O6—H6A⋯O8iii 0.872.112.946 (3)162
O6—H6B⋯O4iv 0.871.932.790 (3)168
O7—H7A⋯O6v 0.841.772.596 (3)167
O10—H10A⋯O7vi 0.872.072.92 (3)165
O10B—H10C⋯O5vii 0.871.922.786 (7)177
O10B—H10D⋯O7vi 0.872.022.876 (5)166
C10—H10⋯Cl3viii 0.952.763.659 (2)159
C14—H14⋯O5ix 0.952.383.297 (3)162
C31—H31⋯Cl2i 0.952.823.739 (2)163
C4EA—H4EA⋯Cg4x 0.952.663.5054149
C17—H17⋯Cg2ii 0.952.763.5715144
C20—H20⋯Cg13ii 0.952.823.5054130
C28—H28⋯Cg3xi 0.952.793.6574152
C37—H37⋯Cg10xii 0.952.763.6107149

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) ; (x) ; (xi) ; (xii) .

  5 in total

1.  The Cambridge Structural Database: a quarter of a million crystal structures and rising.

Authors:  Frank H Allen
Journal:  Acta Crystallogr B       Date:  2002-05-29

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

3.  Nitrosylation in a crystal: remarkable movements of iron porphyrins upon binding of nitric oxide.

Authors:  Nan Xu; Douglas R Powell; George B Richter-Addo
Journal:  Angew Chem Int Ed Engl       Date:  2011-09-12       Impact factor: 15.336

4.  Structure of monoclinic chloro(meso-tetraphenylporphyrinato)iron(III).

Authors:  W R Scheidt; M G Finnegan
Journal:  Acta Crystallogr C       Date:  1989-08-15       Impact factor: 1.172

5.  (Cryptand-222)potassium(+) (hydrogensulfido)[5,10,15,20-tetra-kis(2-pival-amido-phen-yl)porphyrinato]ferrate(II).

Authors:  Mondher Dhifet; Mohamed Salah Belkhiria; Jean-Claude Daran; Habib Nasri
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-07-22
  5 in total
  1 in total

1.  Crystal structure of di-aqua-[5,10,15,20-tetra-kis-(4-meth-oxy-phen-yl)porphyrinato-κ(4) N]iron(III) di-aqua-(18-crown-6)potassium bis-(tri-fluoro-methane-sulfonate)-18-crown-6 (1/2).

Authors:  Leila Ben Haj Hassen; Zouhour Denden; Yoann Rousselin; Habib Nasri
Journal:  Acta Crystallogr E Crystallogr Commun       Date:  2015-11-11
  1 in total

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