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The photocrystallographic investigation of the light-induced excited spin-state trapping effect in the dinuclear spin-crossover compound {[Fe(bt)(NCS)2]2(bpym)} is reported. In this system, each of the two Fe sites may be either in the high-spin (HS) or in the low-spin (LS) state, so that the molecule corresponds to a three-state system (LS-LS, HS-LS and HS-HS). At low temperature, the laser excitation wavelength controls the photoswitching from the stable LS-LS state to one of the metastable excited states (HS-LS or HS-HS), and also between these two excited states. Significant changes in the crystalline structure associated with the photoinduced change of spin state are detailed here. The low-temperature photoinduced states look similar to the corresponding states observed at thermal equilibrium within the unit-cell thermal contraction.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S002188980605028X/db5014sup1.cif
Contains datablocks LSLS-23K, HSLS-180K, HSHS-250K, photoHSLS-23K, photoHSHS-23K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S002188980605028X/db5014LSLS-23Ksup2.hkl
Contains datablock LSLS-23K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S002188980605028X/db5014photoHSLS-23Ksup3.hkl
Contains datablock photoHSLS-23K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S002188980605028X/db5014photoHSHS-23Ksup4.hkl
Contains datablock photoHSHS-23K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S002188980605028X/db5014HSLS-180Ksup5.hkl
Contains datablock HSLS-180K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S002188980605028X/db5014HSHS-250Ksup6.hkl
Contains datablock HSHS-250K

CCDC references: 644705; 644706; 644707; 644708; 644709

Computing details top

For all compounds, data collection: CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.26; cell refinement: CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26; data reduction: CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26; program(s) used to solve structure: SIR97_(Altomare & al., 1998); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON_(Spek, 1998); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
(LSLS-23K) top
Crystal data top
C12H11FeN6S4V = 796.83 (19) Å3
Mr = 423.36Z = 2
Triclinic, P1F(000) = 430
a = 8.446 (1) ÅDx = 1.764 Mg m3
b = 9.123 (1) ÅMo Kα radiation, λ = 0.71069 Å
c = 11.779 (2) ŵ = 1.48 mm1
α = 72.26 (1)°T = 23 K
β = 80.94 (1)°Block, black
γ = 67.33 (1)°0.1 × 0.1 × 0.1 mm
Data collection top
CCD Saphire 3 Xcalibur
diffractometer
2190 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.054
Graphite monochromatorθmax = 27.0°, θmin = 2.9°
Detector resolution: 19.64 pixels mm-1h = 1010
ω scank = 1111
11525 measured reflectionsl = 1515
3210 independent 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)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.090H-atom parameters constrained
S = 0.92 w = 1/[σ2(Fo2) + (0.0502P)2]
where P = (Fo2 + 2Fc2)/3
3210 reflections(Δ/σ)max < 0.001
208 parametersΔρmax = 0.65 e Å3
0 restraintsΔρmin = 0.47 e Å3
Crystal data top
C12H11FeN6S4γ = 67.33 (1)°
Mr = 423.36V = 796.83 (19) Å3
Triclinic, P1Z = 2
a = 8.446 (1) ÅMo Kα radiation
b = 9.123 (1) ŵ = 1.48 mm1
c = 11.779 (2) ÅT = 23 K
α = 72.26 (1)°0.1 × 0.1 × 0.1 mm
β = 80.94 (1)°
Data collection top
CCD Saphire 3 Xcalibur
diffractometer
2190 reflections with I > 2σ(I)
11525 measured reflectionsRint = 0.054
3210 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0370 restraints
wR(F2) = 0.090H-atom parameters constrained
S = 0.92Δρmax = 0.65 e Å3
3210 reflectionsΔρmin = 0.47 e Å3
208 parameters
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
Fe10.86543 (6)0.21942 (6)0.79761 (5)0.01265 (14)
S10.33539 (11)0.23352 (11)1.00751 (9)0.0199 (2)
S20.74652 (11)0.13248 (12)0.44897 (8)0.0194 (2)
S30.87791 (11)0.71148 (11)0.59855 (9)0.0194 (2)
S41.29047 (12)0.39968 (12)0.63828 (9)0.0223 (2)
N10.6366 (3)0.2317 (3)0.8656 (3)0.0146 (6)
N20.8176 (3)0.1965 (3)0.6503 (3)0.0142 (6)
N30.8007 (4)0.4563 (3)0.7316 (3)0.0144 (6)
N41.0904 (3)0.2310 (4)0.7352 (3)0.0140 (6)
N50.9652 (3)0.0225 (3)0.8622 (3)0.0116 (6)
N61.0855 (3)0.2183 (3)1.0435 (3)0.0118 (6)
C10.5124 (5)0.2328 (4)0.9246 (3)0.0155 (8)
C20.7887 (4)0.1711 (4)0.5659 (3)0.0154 (8)
C30.6328 (4)0.5884 (4)0.7125 (4)0.0193 (8)
H3A0.56220.58270.78590.023*
H3B0.57460.57820.65220.023*
C40.6625 (4)0.7545 (4)0.6710 (3)0.0199 (8)
H4A0.65540.79660.73870.024*
H4B0.57700.83550.61530.024*
C50.9242 (4)0.5063 (4)0.6763 (3)0.0144 (8)
C61.0933 (4)0.3767 (4)0.6835 (3)0.0141 (8)
C71.3935 (4)0.1746 (4)0.6747 (3)0.0192 (8)
H7A1.42240.13770.60250.023*
H7B1.49790.13860.71630.023*
C81.2642 (4)0.1047 (4)0.7543 (3)0.0192 (8)
H8A1.26960.00690.73490.023*
H8B1.29100.07420.83730.023*
C91.0003 (4)0.1468 (4)0.8122 (3)0.0153 (8)
H90.96960.12380.73450.018*
C101.0814 (4)0.3082 (4)0.8754 (3)0.0158 (8)
H101.10880.39360.83990.019*
C111.1213 (4)0.3409 (4)0.9917 (3)0.0150 (8)
H111.17390.44951.03520.018*
C121.0140 (4)0.0674 (4)0.9744 (3)0.0113 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0119 (3)0.0140 (3)0.0120 (3)0.0044 (2)0.0003 (2)0.0039 (2)
S10.0161 (4)0.0187 (5)0.0249 (6)0.0065 (4)0.0053 (4)0.0087 (4)
S20.0170 (5)0.0288 (5)0.0148 (5)0.0090 (4)0.0008 (4)0.0080 (5)
S30.0172 (5)0.0192 (5)0.0220 (6)0.0072 (4)0.0015 (4)0.0047 (4)
S40.0181 (5)0.0235 (5)0.0276 (6)0.0101 (4)0.0023 (4)0.0081 (5)
N10.0117 (15)0.0150 (15)0.0166 (18)0.0043 (12)0.0049 (13)0.0019 (14)
N20.0134 (15)0.0141 (15)0.0150 (18)0.0046 (12)0.0008 (13)0.0038 (14)
N30.0127 (14)0.0169 (16)0.0130 (17)0.0035 (12)0.0046 (12)0.0033 (14)
N40.0118 (14)0.0176 (16)0.0122 (17)0.0027 (12)0.0009 (12)0.0066 (14)
N50.0069 (13)0.0158 (15)0.0135 (17)0.0057 (11)0.0002 (12)0.0041 (14)
N60.0080 (13)0.0132 (15)0.0131 (17)0.0017 (12)0.0019 (12)0.0038 (14)
C10.0192 (19)0.0110 (17)0.016 (2)0.0038 (14)0.0074 (16)0.0025 (17)
C20.0085 (16)0.0121 (17)0.021 (2)0.0037 (14)0.0002 (15)0.0011 (17)
C30.0120 (17)0.0211 (19)0.023 (2)0.0036 (15)0.0054 (15)0.0048 (18)
C40.0172 (18)0.020 (2)0.019 (2)0.0022 (16)0.0030 (16)0.0048 (18)
C50.0170 (18)0.0177 (18)0.009 (2)0.0073 (15)0.0043 (15)0.0005 (16)
C60.0130 (17)0.0210 (19)0.009 (2)0.0075 (15)0.0015 (14)0.0034 (17)
C70.0153 (18)0.0209 (19)0.022 (2)0.0047 (15)0.0018 (16)0.0086 (18)
C80.0133 (18)0.0196 (19)0.027 (2)0.0049 (15)0.0001 (16)0.0118 (18)
C90.0138 (17)0.0201 (19)0.014 (2)0.0070 (15)0.0007 (14)0.0073 (17)
C100.0143 (17)0.0183 (18)0.018 (2)0.0064 (15)0.0016 (15)0.0100 (17)
C110.0119 (17)0.0118 (17)0.021 (2)0.0034 (14)0.0007 (15)0.0060 (17)
C120.0065 (15)0.0147 (17)0.013 (2)0.0040 (13)0.0004 (13)0.0036 (16)
Geometric parameters (Å, º) top
Fe1—N21.930 (3)N6—C121.324 (4)
Fe1—N31.942 (3)N6—C111.346 (4)
Fe1—N11.947 (3)N6—Fe1i1.975 (3)
Fe1—N41.957 (3)C3—C41.549 (5)
Fe1—N6i1.975 (3)C3—H3A0.9700
Fe1—N51.976 (3)C3—H3B0.9700
S1—C11.651 (4)C4—H4A0.9700
S2—C21.642 (4)C4—H4B0.9700
S3—C51.732 (4)C5—C61.457 (5)
S3—C41.832 (4)C7—C81.526 (5)
S4—C61.738 (3)C7—H7A0.9700
S4—C71.834 (4)C7—H7B0.9700
N1—C11.162 (5)C8—H8A0.9700
N2—C21.167 (4)C8—H8B0.9700
N3—C51.301 (4)C9—C101.380 (5)
N3—C31.460 (4)C9—H90.9300
N4—C61.290 (4)C10—C111.378 (5)
N4—C81.475 (4)C10—H100.9300
N5—C121.340 (4)C11—H110.9300
N5—C91.347 (4)C12—C12i1.454 (6)
N2—Fe1—N391.05 (12)H3A—C3—H3B108.5
N2—Fe1—N191.93 (12)C3—C4—S3106.2 (2)
N3—Fe1—N194.37 (12)C3—C4—H4A110.5
N2—Fe1—N492.51 (12)S3—C4—H4A110.5
N3—Fe1—N480.25 (12)C3—C4—H4B110.5
N1—Fe1—N4173.08 (11)S3—C4—H4B110.5
N2—Fe1—N6i173.76 (12)H4A—C4—H4B108.7
N3—Fe1—N6i94.98 (11)N3—C5—C6114.4 (3)
N1—Fe1—N6i86.04 (11)N3—C5—S3119.8 (3)
N4—Fe1—N6i90.08 (11)C6—C5—S3125.7 (3)
N2—Fe1—N591.26 (12)N4—C6—C5113.5 (3)
N3—Fe1—N5171.88 (12)N4—C6—S4118.9 (3)
N1—Fe1—N593.34 (12)C5—C6—S4127.5 (3)
N4—Fe1—N591.86 (12)C8—C7—S4106.5 (2)
N6i—Fe1—N582.98 (11)C8—C7—H7A110.4
C5—S3—C487.81 (17)S4—C7—H7A110.4
C6—S4—C788.96 (17)C8—C7—H7B110.4
C1—N1—Fe1168.3 (3)S4—C7—H7B110.4
C2—N2—Fe1175.0 (3)H7A—C7—H7B108.6
C5—N3—C3111.9 (3)N4—C8—C7108.9 (3)
C5—N3—Fe1115.5 (2)N4—C8—H8A109.9
C3—N3—Fe1131.5 (2)C7—C8—H8A109.9
C6—N4—C8112.4 (3)N4—C8—H8B109.9
C6—N4—Fe1116.0 (2)C7—C8—H8B109.9
C8—N4—Fe1130.7 (2)H8A—C8—H8B108.3
C12—N5—C9115.6 (3)N5—C9—C10120.6 (3)
C12—N5—Fe1112.5 (2)N5—C9—H9119.7
C9—N5—Fe1131.8 (3)C10—C9—H9119.7
C12—N6—C11115.4 (3)C11—C10—C9119.1 (3)
C12—N6—Fe1i112.7 (2)C11—C10—H10120.5
C11—N6—Fe1i131.8 (2)C9—C10—H10120.5
N1—C1—S1179.4 (3)N6—C11—C10121.2 (3)
N2—C2—S2178.8 (3)N6—C11—H11119.4
N3—C3—C4107.7 (3)C10—C11—H11119.4
N3—C3—H3A110.2N6—C12—N5128.2 (3)
C4—C3—H3A110.2N6—C12—C12i116.3 (4)
N3—C3—H3B110.2N5—C12—C12i115.5 (4)
C4—C3—H3B110.2
N2—Fe1—N1—C1162.3 (13)Fe1—N1—C1—S1146 (44)
N3—Fe1—N1—C1106.5 (13)Fe1—N2—C2—S223 (18)
N4—Fe1—N1—C167.7 (19)C5—N3—C3—C419.6 (4)
N6i—Fe1—N1—C111.8 (13)Fe1—N3—C3—C4173.2 (2)
N5—Fe1—N1—C171.0 (14)N3—C3—C4—S326.6 (3)
N3—Fe1—N2—C2164 (3)C5—S3—C4—C321.1 (3)
N1—Fe1—N2—C270 (3)C3—N3—C5—C6175.0 (3)
N4—Fe1—N2—C2115 (3)Fe1—N3—C5—C65.6 (4)
N6i—Fe1—N2—C21 (4)C3—N3—C5—S33.0 (4)
N5—Fe1—N2—C223 (3)Fe1—N3—C5—S3172.34 (16)
N2—Fe1—N3—C589.1 (3)C4—S3—C5—N311.8 (3)
N1—Fe1—N3—C5178.9 (2)C4—S3—C5—C6170.5 (3)
N4—Fe1—N3—C53.2 (2)C8—N4—C6—C5173.1 (3)
N6i—Fe1—N3—C592.5 (2)Fe1—N4—C6—C52.9 (4)
N5—Fe1—N3—C517.4 (10)C8—N4—C6—S43.7 (4)
N2—Fe1—N3—C377.6 (3)Fe1—N4—C6—S4173.96 (15)
N1—Fe1—N3—C314.4 (3)N3—C5—C6—N45.6 (4)
N4—Fe1—N3—C3170.0 (3)S3—C5—C6—N4172.3 (2)
N6i—Fe1—N3—C3100.8 (3)N3—C5—C6—S4170.9 (2)
N5—Fe1—N3—C3175.9 (7)S3—C5—C6—S411.3 (5)
N2—Fe1—N4—C690.6 (2)C7—S4—C6—N48.4 (3)
N3—Fe1—N4—C60.0 (2)C7—S4—C6—C5175.2 (3)
N1—Fe1—N4—C639.3 (11)C6—S4—C7—C816.7 (3)
N6i—Fe1—N4—C695.0 (2)C6—N4—C8—C717.0 (4)
N5—Fe1—N4—C6178.0 (2)Fe1—N4—C8—C7174.6 (2)
N2—Fe1—N4—C8101.2 (3)S4—C7—C8—N421.7 (3)
N3—Fe1—N4—C8168.1 (3)C12—N5—C9—C100.0 (5)
N1—Fe1—N4—C8128.8 (10)Fe1—N5—C9—C10175.8 (2)
N6i—Fe1—N4—C873.1 (3)N5—C9—C10—C112.0 (5)
N5—Fe1—N4—C89.9 (3)C12—N6—C11—C101.4 (5)
N2—Fe1—N5—C12177.5 (2)Fe1i—N6—C11—C10176.4 (2)
N3—Fe1—N5—C1276.1 (9)C9—C10—C11—N61.3 (5)
N1—Fe1—N5—C1285.5 (2)C11—N6—C12—N53.8 (5)
N4—Fe1—N5—C1290.0 (2)Fe1i—N6—C12—N5179.8 (3)
N6i—Fe1—N5—C120.1 (2)C11—N6—C12—C12i175.5 (3)
N2—Fe1—N5—C96.6 (3)Fe1i—N6—C12—C12i0.4 (5)
N3—Fe1—N5—C999.8 (8)C9—N5—C12—N63.2 (5)
N1—Fe1—N5—C998.6 (3)Fe1—N5—C12—N6179.8 (3)
N4—Fe1—N5—C985.9 (3)C9—N5—C12—C12i176.2 (4)
N6i—Fe1—N5—C9175.8 (3)Fe1—N5—C12—C12i0.4 (4)
Symmetry code: (i) x+2, y, z+2.
(HSLS-180K) top
Crystal data top
C12H11FeN6S4V = 834.84 (12) Å3
Mr = 423.36Z = 2
Triclinic, P1F(000) = 430
a = 8.6103 (7) ÅDx = 1.684 Mg m3
b = 9.2628 (8) ÅMo Kα radiation, λ = 0.71069 Å
c = 11.9305 (9) ŵ = 1.41 mm1
α = 72.903 (7)°T = 180 K
β = 80.057 (7)°Block, black
γ = 66.911 (8)°0.1 × 0.1 × 0.1 mm
Data collection top
CCD Saphire 3 Xcalibur
diffractometer
1201 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.095
Graphite monochromatorθmax = 27.0°, θmin = 2.9°
Detector resolution: 19.64 pixels mm-1h = 1010
ω scank = 1111
11132 measured reflectionsl = 1515
3353 independent 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)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.073H-atom parameters constrained
S = 0.62 w = 1/[σ2(Fo2) + (0.0297P)2]
where P = (Fo2 + 2Fc2)/3
3353 reflections(Δ/σ)max < 0.001
208 parametersΔρmax = 0.32 e Å3
0 restraintsΔρmin = 0.31 e Å3
Crystal data top
C12H11FeN6S4γ = 66.911 (8)°
Mr = 423.36V = 834.84 (12) Å3
Triclinic, P1Z = 2
a = 8.6103 (7) ÅMo Kα radiation
b = 9.2628 (8) ŵ = 1.41 mm1
c = 11.9305 (9) ÅT = 180 K
α = 72.903 (7)°0.1 × 0.1 × 0.1 mm
β = 80.057 (7)°
Data collection top
CCD Saphire 3 Xcalibur
diffractometer
1201 reflections with I > 2σ(I)
11132 measured reflectionsRint = 0.095
3353 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0390 restraints
wR(F2) = 0.073H-atom parameters constrained
S = 0.62Δρmax = 0.32 e Å3
3353 reflectionsΔρmin = 0.31 e Å3
208 parameters
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
Fe10.84717 (9)0.22412 (8)0.79538 (5)0.0362 (2)
S10.32617 (18)0.23333 (16)1.01340 (12)0.0620 (4)
S20.74416 (17)0.12773 (17)0.44816 (11)0.0570 (4)
S30.87992 (18)0.71048 (15)0.60031 (10)0.0514 (4)
S41.27526 (18)0.40990 (17)0.63954 (11)0.0591 (4)
N10.6159 (6)0.2454 (4)0.8694 (3)0.0473 (12)
N20.8072 (5)0.1896 (4)0.6479 (3)0.0453 (12)
N30.7915 (5)0.4687 (4)0.7322 (3)0.0379 (10)
N41.0837 (4)0.2388 (5)0.7332 (3)0.0342 (10)
N50.9682 (4)0.0249 (4)0.8633 (3)0.0281 (9)
N61.0951 (4)0.2155 (4)1.0378 (3)0.0297 (9)
C10.4943 (7)0.2407 (5)0.9301 (4)0.0396 (13)
C20.7818 (6)0.1653 (5)0.5640 (4)0.0393 (14)
C30.6329 (6)0.6033 (6)0.7114 (4)0.0587 (15)
H3A0.56120.60450.78370.070*
H3B0.57490.59200.65350.070*
C40.6666 (6)0.7633 (6)0.6667 (4)0.0537 (14)
H4A0.65600.81080.73130.064*
H4B0.58680.84040.60930.064*
C50.9170 (6)0.5124 (5)0.6778 (3)0.0329 (11)
C61.0801 (6)0.3840 (6)0.6856 (4)0.0349 (12)
C71.3822 (6)0.1915 (5)0.6746 (4)0.0519 (14)
H7A1.41890.15410.60310.062*
H7B1.48070.15980.71800.062*
C81.2566 (7)0.1193 (6)0.7482 (4)0.0538 (15)
H8A1.26670.02410.72460.065*
H8B1.28080.08610.83030.065*
C91.0060 (6)0.1466 (6)0.8132 (4)0.0389 (12)
H90.97400.12430.73760.047*
C101.0915 (6)0.3046 (6)0.8708 (4)0.0425 (13)
H101.12000.38830.83420.051*
C111.1340 (6)0.3360 (5)0.9850 (4)0.0374 (12)
H111.19050.44221.02550.045*
C121.0167 (5)0.0651 (5)0.9721 (4)0.0248 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0393 (5)0.0380 (4)0.0302 (4)0.0169 (4)0.0032 (3)0.0061 (3)
S10.0532 (11)0.0549 (9)0.0819 (11)0.0259 (8)0.0184 (8)0.0271 (8)
S20.0447 (10)0.0853 (11)0.0387 (9)0.0247 (8)0.0020 (7)0.0110 (7)
S30.0555 (10)0.0516 (9)0.0498 (9)0.0241 (8)0.0094 (7)0.0067 (7)
S40.0486 (10)0.0738 (10)0.0684 (10)0.0373 (9)0.0127 (7)0.0255 (8)
N10.063 (4)0.047 (3)0.038 (3)0.027 (3)0.008 (2)0.006 (2)
N20.033 (3)0.057 (3)0.037 (3)0.015 (2)0.001 (2)0.003 (2)
N30.029 (3)0.048 (3)0.031 (2)0.004 (2)0.0091 (19)0.0112 (18)
N40.027 (3)0.040 (2)0.040 (2)0.013 (2)0.0064 (19)0.0120 (19)
N50.031 (2)0.041 (2)0.021 (2)0.020 (2)0.0007 (18)0.0120 (19)
N60.028 (2)0.033 (2)0.035 (2)0.0116 (19)0.0035 (17)0.020 (2)
C10.049 (4)0.031 (3)0.040 (3)0.014 (3)0.012 (3)0.005 (2)
C20.021 (3)0.035 (3)0.041 (4)0.004 (2)0.001 (2)0.011 (3)
C30.029 (4)0.075 (4)0.066 (4)0.013 (3)0.002 (3)0.018 (3)
C40.049 (4)0.053 (3)0.043 (3)0.001 (3)0.009 (3)0.009 (3)
C50.034 (3)0.048 (3)0.025 (3)0.021 (3)0.008 (2)0.009 (2)
C60.038 (4)0.054 (3)0.027 (3)0.027 (3)0.002 (2)0.017 (2)
C70.035 (3)0.062 (4)0.063 (3)0.013 (3)0.003 (3)0.030 (3)
C80.040 (4)0.053 (3)0.077 (4)0.018 (3)0.001 (3)0.031 (3)
C90.045 (4)0.059 (4)0.029 (3)0.031 (3)0.004 (2)0.020 (3)
C100.048 (4)0.046 (3)0.046 (4)0.019 (3)0.013 (3)0.035 (3)
C110.039 (3)0.034 (3)0.041 (3)0.012 (2)0.000 (2)0.013 (2)
C120.020 (3)0.029 (3)0.031 (3)0.012 (2)0.000 (2)0.012 (2)
Geometric parameters (Å, º) top
Fe1—N21.985 (4)N6—C121.347 (5)
Fe1—N11.993 (4)N6—C111.342 (5)
Fe1—N32.049 (4)N6—Fe1i2.106 (3)
Fe1—N42.086 (3)C3—C41.543 (6)
Fe1—N52.091 (4)C3—H3A0.9700
Fe1—N6i2.106 (3)C3—H3B0.9700
S1—C11.622 (5)C4—H4A0.9700
S2—C21.631 (6)C4—H4B0.9700
S3—C51.723 (5)C5—C61.437 (6)
S3—C41.806 (5)C7—C81.511 (6)
S4—C61.762 (5)C7—H7A0.9700
S4—C71.814 (5)C7—H7B0.9700
N1—C11.173 (5)C8—H8A0.9700
N2—C21.161 (5)C8—H8B0.9700
N3—C51.303 (5)C9—C101.376 (6)
N3—C31.443 (5)C9—H90.9300
N4—C61.287 (5)C10—C111.390 (6)
N4—C81.468 (5)C10—H100.9300
N5—C121.334 (5)C11—H110.9300
N5—C91.332 (5)C12—C12i1.454 (7)
N2—Fe1—N194.95 (15)H3A—C3—H3B108.2
N2—Fe1—N395.51 (14)C3—C4—S3105.9 (3)
N1—Fe1—N394.78 (16)C3—C4—H4A110.5
N2—Fe1—N494.00 (14)S3—C4—H4A110.5
N1—Fe1—N4168.52 (15)C3—C4—H4B110.5
N3—Fe1—N477.20 (16)S3—C4—H4B110.5
N2—Fe1—N591.56 (15)H4A—C4—H4B108.7
N1—Fe1—N598.33 (14)N3—C5—C6115.1 (4)
N3—Fe1—N5164.51 (14)N3—C5—S3120.1 (4)
N4—Fe1—N588.59 (14)C6—C5—S3124.8 (4)
N2—Fe1—N6i169.79 (15)N4—C6—C5117.1 (4)
N1—Fe1—N6i85.36 (14)N4—C6—S4117.5 (4)
N3—Fe1—N6i94.63 (13)C5—C6—S4125.4 (4)
N4—Fe1—N6i87.10 (12)C8—C7—S4106.9 (3)
N5—Fe1—N6i78.31 (14)C8—C7—H7A110.3
C5—S3—C488.4 (2)S4—C7—H7A110.3
C6—S4—C789.6 (2)C8—C7—H7B110.3
C1—N1—Fe1168.4 (4)S4—C7—H7B110.3
C2—N2—Fe1177.6 (4)H7A—C7—H7B108.6
C5—N3—C3110.5 (4)N4—C8—C7110.1 (4)
C5—N3—Fe1115.8 (3)N4—C8—H8A109.6
C3—N3—Fe1131.9 (3)C7—C8—H8A109.6
C6—N4—C8112.7 (4)N4—C8—H8B109.6
C6—N4—Fe1114.2 (3)C7—C8—H8B109.6
C8—N4—Fe1132.4 (3)H8A—C8—H8B108.2
C12—N5—C9116.3 (4)N5—C9—C10121.6 (4)
C12—N5—Fe1114.1 (3)N5—C9—H9119.2
C9—N5—Fe1129.6 (3)C10—C9—H9119.2
C12—N6—C11115.6 (4)C9—C10—C11118.3 (4)
C12—N6—Fe1i114.6 (3)C9—C10—H10120.8
C11—N6—Fe1i129.6 (3)C11—C10—H10120.8
N1—C1—S1179.6 (4)N6—C11—C10121.1 (4)
N2—C2—S2178.6 (4)N6—C11—H11119.4
N3—C3—C4109.5 (4)C10—C11—H11119.4
N3—C3—H3A109.8N5—C12—N6127.0 (3)
C4—C3—H3A109.8N5—C12—C12i117.9 (5)
N3—C3—H3B109.8N6—C12—C12i115.1 (5)
C4—C3—H3B109.8
N2—Fe1—N1—C1135.8 (18)Fe1—N1—C1—S1104 (79)
N3—Fe1—N1—C1128.2 (18)Fe1—N2—C2—S23 (26)
N4—Fe1—N1—C183 (2)C5—N3—C3—C418.0 (5)
N5—Fe1—N1—C143.5 (18)Fe1—N3—C3—C4178.0 (3)
N6i—Fe1—N1—C133.9 (18)N3—C3—C4—S324.7 (4)
N1—Fe1—N2—C251 (9)C5—S3—C4—C319.2 (3)
N3—Fe1—N2—C2146 (9)C3—N3—C5—C6175.6 (4)
N4—Fe1—N2—C2136 (9)Fe1—N3—C5—C68.8 (4)
N5—Fe1—N2—C248 (9)C3—N3—C5—S32.6 (5)
N6i—Fe1—N2—C240 (10)Fe1—N3—C5—S3169.43 (19)
N2—Fe1—N3—C587.0 (3)C4—S3—C5—N311.0 (4)
N1—Fe1—N3—C5177.6 (3)C4—S3—C5—C6171.0 (4)
N4—Fe1—N3—C55.9 (3)C8—N4—C6—C5173.9 (4)
N5—Fe1—N3—C529.8 (7)Fe1—N4—C6—C52.3 (4)
N6i—Fe1—N3—C591.8 (3)C8—N4—C6—S44.2 (5)
N2—Fe1—N3—C376.3 (4)Fe1—N4—C6—S4175.78 (18)
N1—Fe1—N3—C319.2 (4)N3—C5—C6—N47.4 (5)
N4—Fe1—N3—C3169.1 (4)S3—C5—C6—N4170.7 (3)
N5—Fe1—N3—C3166.9 (5)N3—C5—C6—S4170.5 (3)
N6i—Fe1—N3—C3104.9 (4)S3—C5—C6—S411.4 (5)
N2—Fe1—N4—C693.0 (3)C7—S4—C6—N46.4 (3)
N1—Fe1—N4—C648.1 (9)C7—S4—C6—C5175.7 (4)
N3—Fe1—N4—C61.7 (3)C6—S4—C7—C814.0 (3)
N5—Fe1—N4—C6175.5 (3)C6—N4—C8—C715.3 (5)
N6i—Fe1—N4—C697.1 (3)Fe1—N4—C8—C7175.0 (3)
N2—Fe1—N4—C897.4 (4)S4—C7—C8—N418.9 (5)
N1—Fe1—N4—C8121.4 (8)C12—N5—C9—C100.4 (6)
N3—Fe1—N4—C8167.8 (4)Fe1—N5—C9—C10178.0 (3)
N5—Fe1—N4—C86.0 (4)N5—C9—C10—C111.8 (7)
N6i—Fe1—N4—C872.4 (4)C12—N6—C11—C101.4 (6)
N2—Fe1—N5—C12177.6 (3)Fe1i—N6—C11—C10176.7 (3)
N1—Fe1—N5—C1282.4 (3)C9—C10—C11—N60.9 (6)
N3—Fe1—N5—C1265.1 (6)C9—N5—C12—N62.1 (6)
N4—Fe1—N5—C1288.4 (3)Fe1—N5—C12—N6179.1 (3)
N6i—Fe1—N5—C121.1 (3)C9—N5—C12—C12i177.7 (4)
N2—Fe1—N5—C93.9 (4)Fe1—N5—C12—C12i1.0 (5)
N1—Fe1—N5—C999.1 (4)C11—N6—C12—N53.0 (6)
N3—Fe1—N5—C9113.4 (6)Fe1i—N6—C12—N5179.1 (3)
N4—Fe1—N5—C990.1 (4)C11—N6—C12—C12i176.8 (4)
N6i—Fe1—N5—C9177.4 (4)Fe1i—N6—C12—C12i0.8 (5)
Symmetry code: (i) x+2, y, z+2.
(HSHS-250K) top
Crystal data top
C12H11FeN6S4V = 863.2 (3) Å3
Mr = 423.36Z = 2
Triclinic, P1F(000) = 430
a = 8.727 (1) ÅDx = 1.629 Mg m3
b = 9.385 (2) ÅMo Kα radiation, λ = 0.71069 Å
c = 12.041 (2) ŵ = 1.36 mm1
α = 73.04 (2)°T = 250 K
β = 79.43 (1)°Block, black
γ = 66.60 (2)°0.1 × 0.1 × 0.1 mm
Data collection top
CCD Saphire 3 Xcalibur
diffractometer
1292 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.126
Graphite monochromatorθmax = 27.0°, θmin = 2.6°
Detector resolution: 19.64 pixels mm-1h = 1111
ω scank = 1111
12617 measured reflectionsl = 1515
3452 independent 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)] = 0.055Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.160H-atom parameters constrained
S = 0.84 w = 1/[σ2(Fo2) + (0.0687P)2]
where P = (Fo2 + 2Fc2)/3
3452 reflections(Δ/σ)max = 0.003
208 parametersΔρmax = 0.53 e Å3
0 restraintsΔρmin = 0.33 e Å3
Crystal data top
C12H11FeN6S4γ = 66.60 (2)°
Mr = 423.36V = 863.2 (3) Å3
Triclinic, P1Z = 2
a = 8.727 (1) ÅMo Kα radiation
b = 9.385 (2) ŵ = 1.36 mm1
c = 12.041 (2) ÅT = 250 K
α = 73.04 (2)°0.1 × 0.1 × 0.1 mm
β = 79.43 (1)°
Data collection top
CCD Saphire 3 Xcalibur
diffractometer
1292 reflections with I > 2σ(I)
12617 measured reflectionsRint = 0.126
3452 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0550 restraints
wR(F2) = 0.160H-atom parameters constrained
S = 0.84Δρmax = 0.53 e Å3
3452 reflectionsΔρmin = 0.33 e Å3
208 parameters
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
Fe10.82954 (13)0.23023 (13)0.79407 (9)0.0435 (4)
S10.3097 (3)0.2387 (3)1.0136 (2)0.0893 (9)
S20.7412 (3)0.1261 (3)0.44849 (18)0.0652 (7)
S30.8776 (3)0.7148 (3)0.6037 (2)0.0707 (7)
S41.2594 (3)0.4218 (3)0.6371 (2)0.0774 (8)
N10.5909 (8)0.2619 (8)0.8709 (6)0.062 (2)
N20.7978 (7)0.1896 (8)0.6445 (5)0.0572 (19)
N30.7820 (8)0.4816 (8)0.7313 (5)0.0538 (17)
N41.0779 (7)0.2497 (8)0.7296 (5)0.0442 (16)
N50.9690 (7)0.0246 (7)0.8649 (5)0.0379 (15)
N61.1038 (7)0.2118 (8)1.0309 (5)0.0412 (15)
C10.4760 (10)0.2517 (9)0.9306 (6)0.047 (2)
C20.7757 (8)0.1617 (8)0.5631 (7)0.0432 (19)
C30.6231 (10)0.6167 (11)0.7143 (8)0.074 (3)
H3A0.55470.61960.78740.089*
H3B0.56220.60700.65890.089*
C40.6640 (10)0.7716 (10)0.6675 (8)0.073 (3)
H4A0.65200.82100.73050.088*
H4B0.58800.84750.60940.088*
C50.9041 (11)0.5200 (9)0.6789 (6)0.046 (2)
C61.0720 (9)0.3902 (11)0.6869 (7)0.048 (2)
C71.3721 (10)0.2075 (10)0.6722 (8)0.069 (3)
H7A1.41680.17060.60150.083*
H7B1.46440.18000.71840.083*
C81.2500 (9)0.1304 (10)0.7402 (8)0.066 (3)
H8A1.26110.04110.71020.079*
H8B1.27400.08990.82140.079*
C91.0125 (9)0.1459 (11)0.8129 (6)0.045 (2)
H90.97920.12420.73880.054*
C101.1058 (10)0.3028 (11)0.8670 (7)0.056 (2)
H101.13920.38540.82960.067*
C111.1456 (9)0.3295 (10)0.9768 (7)0.053 (2)
H111.20420.43391.01600.064*
C121.0192 (8)0.0649 (9)0.9725 (6)0.0328 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0390 (7)0.0546 (8)0.0368 (7)0.0214 (6)0.0033 (5)0.0048 (5)
S10.0802 (18)0.094 (2)0.107 (2)0.0549 (17)0.0479 (15)0.0443 (17)
S20.0669 (15)0.0897 (19)0.0475 (13)0.0357 (14)0.0034 (11)0.0196 (12)
S30.0816 (18)0.0727 (19)0.0664 (16)0.0422 (15)0.0126 (13)0.0055 (13)
S40.0667 (16)0.096 (2)0.0899 (19)0.0536 (16)0.0201 (13)0.0347 (15)
N10.058 (5)0.080 (6)0.052 (4)0.038 (4)0.004 (4)0.006 (4)
N20.057 (4)0.081 (6)0.042 (4)0.034 (4)0.007 (3)0.012 (4)
N30.050 (4)0.054 (5)0.054 (4)0.018 (4)0.012 (3)0.004 (3)
N40.036 (4)0.050 (5)0.051 (4)0.015 (4)0.003 (3)0.018 (3)
N50.042 (4)0.042 (4)0.027 (3)0.015 (3)0.001 (3)0.007 (3)
N60.046 (4)0.034 (4)0.045 (4)0.016 (3)0.000 (3)0.013 (3)
C10.051 (5)0.042 (5)0.049 (5)0.021 (5)0.002 (4)0.009 (4)
C20.036 (4)0.034 (5)0.051 (5)0.015 (4)0.010 (4)0.010 (4)
C30.050 (6)0.070 (7)0.082 (7)0.010 (6)0.025 (5)0.007 (5)
C40.056 (6)0.060 (7)0.097 (7)0.006 (5)0.020 (5)0.020 (6)
C50.063 (6)0.046 (6)0.036 (4)0.028 (5)0.015 (4)0.001 (4)
C60.047 (5)0.060 (6)0.049 (5)0.029 (5)0.002 (4)0.019 (4)
C70.044 (5)0.089 (8)0.083 (7)0.025 (5)0.017 (4)0.045 (6)
C80.046 (5)0.076 (7)0.082 (7)0.027 (5)0.008 (5)0.032 (5)
C90.047 (5)0.059 (6)0.028 (4)0.021 (5)0.002 (3)0.006 (4)
C100.063 (6)0.064 (7)0.055 (6)0.025 (5)0.006 (4)0.039 (5)
C110.054 (5)0.044 (6)0.061 (6)0.015 (4)0.002 (4)0.021 (5)
C120.032 (4)0.037 (6)0.032 (4)0.016 (4)0.004 (3)0.011 (3)
Geometric parameters (Å, º) top
Fe1—N22.033 (6)N6—C121.325 (8)
Fe1—N12.060 (7)N6—C111.339 (8)
Fe1—N32.146 (7)N6—Fe1i2.229 (6)
Fe1—N52.192 (6)C3—C41.555 (11)
Fe1—N42.225 (6)C3—H3A0.9700
Fe1—N6i2.229 (6)C3—H3B0.9700
S1—C11.630 (8)C4—H4A0.9700
S2—C21.615 (8)C4—H4B0.9700
S3—C51.730 (8)C5—C61.485 (10)
S3—C41.809 (8)C7—C81.508 (10)
S4—C61.745 (7)C7—H7A0.9700
S4—C71.810 (9)C7—H7B0.9700
N1—C11.141 (8)C8—H8A0.9700
N2—C21.151 (8)C8—H8B0.9700
N3—C51.261 (8)C9—C101.392 (10)
N3—C31.459 (9)C9—H90.9300
N4—C61.252 (9)C10—C111.355 (10)
N4—C81.475 (9)C10—H100.9300
N5—C121.343 (8)C11—H110.9300
N5—C91.348 (9)C12—C12i1.450 (12)
N2—Fe1—N197.4 (2)H3A—C3—H3B108.5
N2—Fe1—N397.9 (2)C3—C4—S3107.5 (5)
N1—Fe1—N394.5 (3)C3—C4—H4A110.2
N2—Fe1—N592.1 (2)S3—C4—H4A110.2
N1—Fe1—N5103.1 (2)C3—C4—H4B110.2
N3—Fe1—N5158.4 (2)S3—C4—H4B110.2
N2—Fe1—N493.9 (2)H4A—C4—H4B108.5
N1—Fe1—N4165.0 (2)N3—C5—C6116.6 (7)
N3—Fe1—N474.2 (3)N3—C5—S3121.6 (7)
N5—Fe1—N486.2 (2)C6—C5—S3121.8 (6)
N2—Fe1—N6i166.3 (2)N4—C6—C5117.5 (7)
N1—Fe1—N6i85.9 (2)N4—C6—S4118.5 (6)
N3—Fe1—N6i95.1 (2)C5—C6—S4124.0 (7)
N5—Fe1—N6i74.2 (2)C8—C7—S4107.4 (5)
N4—Fe1—N6i85.4 (2)C8—C7—H7A110.2
C5—S3—C487.3 (4)S4—C7—H7A110.2
C6—S4—C789.6 (4)C8—C7—H7B110.2
C1—N1—Fe1165.6 (7)S4—C7—H7B110.2
C2—N2—Fe1176.6 (6)H7A—C7—H7B108.5
C5—N3—C3112.0 (7)N4—C8—C7109.3 (7)
C5—N3—Fe1116.6 (6)N4—C8—H8A109.8
C3—N3—Fe1129.7 (5)C7—C8—H8A109.8
C6—N4—C8113.5 (6)N4—C8—H8B109.8
C6—N4—Fe1114.1 (5)C7—C8—H8B109.8
C8—N4—Fe1132.0 (5)H8A—C8—H8B108.3
C12—N5—C9115.8 (6)N5—C9—C10121.9 (6)
C12—N5—Fe1116.3 (5)N5—C9—H9119.0
C9—N5—Fe1127.9 (5)C10—C9—H9119.0
C12—N6—C11116.9 (6)C11—C10—C9116.9 (7)
C12—N6—Fe1i115.2 (4)C11—C10—H10121.6
C11—N6—Fe1i127.7 (6)C9—C10—H10121.6
N1—C1—S1178.9 (7)N6—C11—C10122.6 (8)
N2—C2—S2178.8 (7)N6—C11—H11118.7
N3—C3—C4107.4 (7)C10—C11—H11118.7
N3—C3—H3A110.2N6—C12—N5125.7 (6)
C4—C3—H3A110.2N6—C12—C12i117.6 (8)
N3—C3—H3B110.2N5—C12—C12i116.7 (9)
C4—C3—H3B110.2
N2—Fe1—N1—C1117 (2)Fe1—N1—C1—S1149 (34)
N3—Fe1—N1—C1144 (2)Fe1—N2—C2—S297 (33)
N5—Fe1—N1—C124 (2)C5—N3—C3—C416.1 (9)
N4—Fe1—N1—C1104 (3)Fe1—N3—C3—C4179.7 (5)
N6i—Fe1—N1—C149 (2)N3—C3—C4—S321.6 (8)
N1—Fe1—N2—C244 (10)C5—S3—C4—C316.8 (6)
N3—Fe1—N2—C2139 (10)C3—N3—C5—C6178.0 (6)
N5—Fe1—N2—C260 (10)Fe1—N3—C5—C611.6 (8)
N4—Fe1—N2—C2146 (10)C3—N3—C5—S33.0 (9)
N6i—Fe1—N2—C259 (11)Fe1—N3—C5—S3169.5 (3)
N2—Fe1—N3—C584.4 (5)C4—S3—C5—N39.2 (6)
N1—Fe1—N3—C5177.5 (5)C4—S3—C5—C6169.7 (6)
N5—Fe1—N3—C532.5 (9)C8—N4—C6—C5176.6 (6)
N4—Fe1—N3—C57.4 (5)Fe1—N4—C6—C53.5 (8)
N6i—Fe1—N3—C591.2 (5)C8—N4—C6—S45.0 (8)
N2—Fe1—N3—C379.2 (6)Fe1—N4—C6—S4178.2 (3)
N1—Fe1—N3—C319.0 (7)N3—C5—C6—N410.2 (9)
N5—Fe1—N3—C3163.9 (6)S3—C5—C6—N4170.9 (5)
N4—Fe1—N3—C3171.0 (7)N3—C5—C6—S4171.5 (5)
N6i—Fe1—N3—C3105.2 (6)S3—C5—C6—S47.4 (8)
N2—Fe1—N4—C695.5 (5)C7—S4—C6—N43.0 (6)
N1—Fe1—N4—C643.3 (12)C7—S4—C6—C5175.3 (6)
N3—Fe1—N4—C61.6 (5)C6—S4—C7—C89.4 (6)
N5—Fe1—N4—C6172.6 (5)C6—N4—C8—C712.2 (9)
N6i—Fe1—N4—C698.2 (5)Fe1—N4—C8—C7176.1 (5)
N2—Fe1—N4—C892.9 (6)S4—C7—C8—N413.5 (8)
N1—Fe1—N4—C8128.2 (10)C12—N5—C9—C100.9 (9)
N3—Fe1—N4—C8169.9 (6)Fe1—N5—C9—C10178.2 (5)
N5—Fe1—N4—C81.1 (6)N5—C9—C10—C112.6 (10)
N6i—Fe1—N4—C873.4 (6)C12—N6—C11—C100.5 (10)
N2—Fe1—N5—C12178.4 (5)Fe1i—N6—C11—C10176.2 (5)
N1—Fe1—N5—C1280.3 (5)C9—C10—C11—N62.3 (11)
N3—Fe1—N5—C1263.7 (8)C11—N6—C12—N51.4 (10)
N4—Fe1—N5—C1287.8 (4)Fe1i—N6—C12—N5178.5 (5)
N6i—Fe1—N5—C121.5 (4)C11—N6—C12—C12i176.8 (7)
N2—Fe1—N5—C92.5 (6)Fe1i—N6—C12—C12i0.2 (9)
N1—Fe1—N5—C9100.6 (6)C9—N5—C12—N61.2 (9)
N3—Fe1—N5—C9115.4 (7)Fe1—N5—C12—N6179.6 (5)
N4—Fe1—N5—C991.3 (5)C9—N5—C12—C12i177.1 (6)
N6i—Fe1—N5—C9177.6 (6)Fe1—N5—C12—C12i2.1 (9)
Symmetry code: (i) x+2, y, z+2.
(photoHSLS-23K) top
Crystal data top
C12H11FeN6S4V = 831.4 (3) Å3
Mr = 423.36Z = 2
Triclinic, P1F(000) = 430
a = 8.581 (2) ÅDx = 1.691 Mg m3
b = 9.196 (2) ÅMo Kα radiation, λ = 0.71069 Å
c = 11.948 (3) ŵ = 1.42 mm1
α = 73.34 (2)°T = 23 K
β = 80.53 (2)°Block, black
γ = 67.24 (2)°0.1 × 0.1 × 0.1 mm
Data collection top
CCD Saphire 3 Xcalibur
diffractometer
2278 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.129
Graphite monochromatorθmax = 27.0°, θmin = 2.7°
Detector resolution: 19.64 pixels mm-1h = 1010
ω scank = 1111
10339 measured reflectionsl = 1515
3250 independent 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)] = 0.065Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.153H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0627P)2 + 1.2812P]
where P = (Fo2 + 2Fc2)/3
3250 reflections(Δ/σ)max < 0.001
208 parametersΔρmax = 0.88 e Å3
0 restraintsΔρmin = 0.69 e Å3
Crystal data top
C12H11FeN6S4γ = 67.24 (2)°
Mr = 423.36V = 831.4 (3) Å3
Triclinic, P1Z = 2
a = 8.581 (2) ÅMo Kα radiation
b = 9.196 (2) ŵ = 1.42 mm1
c = 11.948 (3) ÅT = 23 K
α = 73.34 (2)°0.1 × 0.1 × 0.1 mm
β = 80.53 (2)°
Data collection top
CCD Saphire 3 Xcalibur
diffractometer
2278 reflections with I > 2σ(I)
10339 measured reflectionsRint = 0.129
3250 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0650 restraints
wR(F2) = 0.153H-atom parameters constrained
S = 1.09Δρmax = 0.88 e Å3
3250 reflectionsΔρmin = 0.69 e Å3
208 parameters
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
Fe10.84473 (11)0.22374 (10)0.79366 (6)0.0195 (2)
S10.3264 (2)0.22949 (19)1.01892 (13)0.0287 (4)
S20.7446 (2)0.1214 (2)0.44391 (13)0.0301 (4)
S30.88447 (19)0.71196 (19)0.59514 (12)0.0236 (3)
S41.27821 (19)0.4114 (2)0.64131 (12)0.0265 (4)
N10.6092 (7)0.2482 (6)0.8684 (4)0.0288 (12)
N20.8057 (6)0.1854 (6)0.6441 (4)0.0261 (11)
N30.7913 (6)0.4718 (6)0.7283 (4)0.0233 (11)
N41.0879 (6)0.2369 (6)0.7332 (4)0.0176 (10)
N50.9692 (5)0.0282 (6)0.8642 (4)0.0181 (10)
N61.0963 (5)0.2167 (6)1.0378 (4)0.0169 (10)
C10.4914 (8)0.2397 (7)0.9316 (5)0.0234 (13)
C20.7813 (7)0.1602 (7)0.5601 (5)0.0247 (13)
C30.6307 (7)0.6084 (8)0.7044 (5)0.0294 (15)
H3A0.55570.61010.77460.035*
H3B0.57580.59740.64410.035*
C40.6684 (7)0.7667 (8)0.6634 (5)0.0254 (13)
H4A0.66070.81130.72940.030*
H4B0.58830.84700.60740.030*
C50.9192 (7)0.5128 (7)0.6756 (4)0.0186 (12)
C61.0842 (7)0.3829 (7)0.6854 (4)0.0194 (12)
C71.3853 (7)0.1893 (8)0.6740 (5)0.0260 (13)
H7A1.41550.15240.60230.031*
H7B1.48760.15650.71400.031*
C81.2598 (7)0.1170 (8)0.7524 (5)0.0253 (13)
H8A1.27010.01780.73350.030*
H8B1.28370.09090.83390.030*
C91.0096 (7)0.1541 (8)0.8135 (5)0.0229 (13)
H90.97840.13340.73790.028*
C101.0953 (7)0.3108 (8)0.8718 (5)0.0238 (13)
H101.12570.39550.83530.029*
C111.1363 (7)0.3416 (8)0.9862 (5)0.0246 (13)
H111.19130.44791.02750.029*
C121.0186 (6)0.0689 (7)0.9738 (4)0.0151 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0229 (5)0.0213 (5)0.0141 (4)0.0086 (4)0.0045 (3)0.0066 (3)
S10.0277 (9)0.0282 (9)0.0323 (8)0.0097 (8)0.0033 (7)0.0140 (7)
S20.0218 (9)0.0441 (10)0.0232 (7)0.0129 (8)0.0020 (6)0.0069 (7)
S30.0241 (9)0.0282 (8)0.0207 (7)0.0108 (7)0.0017 (6)0.0071 (6)
S40.0215 (8)0.0377 (9)0.0276 (7)0.0166 (8)0.0061 (6)0.0147 (7)
N10.041 (3)0.034 (3)0.019 (2)0.023 (3)0.002 (2)0.004 (2)
N20.022 (3)0.029 (3)0.018 (2)0.004 (2)0.003 (2)0.001 (2)
N30.020 (3)0.034 (3)0.018 (2)0.008 (2)0.0014 (19)0.011 (2)
N40.015 (3)0.026 (3)0.015 (2)0.006 (2)0.0003 (18)0.0112 (19)
N50.012 (2)0.029 (3)0.019 (2)0.008 (2)0.0015 (17)0.013 (2)
N60.007 (2)0.024 (3)0.023 (2)0.006 (2)0.0049 (18)0.014 (2)
C10.036 (4)0.018 (3)0.020 (3)0.011 (3)0.008 (3)0.005 (2)
C20.012 (3)0.025 (3)0.024 (3)0.003 (3)0.005 (2)0.004 (2)
C30.011 (3)0.048 (4)0.033 (3)0.008 (3)0.004 (2)0.018 (3)
C40.012 (3)0.036 (4)0.023 (3)0.000 (3)0.007 (2)0.010 (3)
C50.022 (3)0.025 (3)0.014 (2)0.011 (3)0.004 (2)0.007 (2)
C60.020 (3)0.030 (3)0.016 (2)0.014 (3)0.001 (2)0.011 (2)
C70.017 (3)0.036 (4)0.028 (3)0.007 (3)0.000 (2)0.016 (3)
C80.020 (3)0.033 (4)0.024 (3)0.010 (3)0.003 (2)0.012 (3)
C90.019 (3)0.042 (4)0.019 (3)0.016 (3)0.005 (2)0.020 (3)
C100.019 (3)0.033 (4)0.025 (3)0.009 (3)0.004 (2)0.020 (3)
C110.021 (3)0.027 (3)0.030 (3)0.010 (3)0.005 (2)0.017 (3)
C120.009 (3)0.026 (3)0.016 (2)0.008 (2)0.003 (2)0.013 (2)
Geometric parameters (Å, º) top
Fe1—N22.019 (5)N6—C121.322 (7)
Fe1—N12.026 (5)N6—C111.360 (7)
Fe1—N32.076 (5)N6—Fe1i2.133 (4)
Fe1—N52.117 (5)C3—C41.538 (9)
Fe1—N42.131 (4)C3—H3A0.9700
Fe1—N6i2.133 (4)C3—H3B0.9700
S1—C11.632 (6)C4—H4A0.9700
S2—C21.634 (6)C4—H4B0.9700
S3—C51.740 (6)C5—C61.453 (8)
S3—C41.836 (6)C7—C81.531 (8)
S4—C61.757 (5)C7—H7A0.9700
S4—C71.838 (6)C7—H7B0.9700
N1—C11.172 (7)C8—H8A0.9700
N2—C21.160 (7)C8—H8B0.9700
N3—C51.304 (7)C9—C101.370 (8)
N3—C31.464 (8)C9—H90.9300
N4—C61.290 (7)C10—C111.390 (8)
N4—C81.467 (8)C10—H100.9300
N5—C121.347 (6)C11—H110.9300
N5—C91.360 (7)C12—C12i1.475 (9)
N2—Fe1—N195.78 (19)H3A—C3—H3B108.4
N2—Fe1—N395.48 (18)C3—C4—S3106.1 (4)
N1—Fe1—N394.8 (2)C3—C4—H4A110.5
N2—Fe1—N592.01 (18)S3—C4—H4A110.5
N1—Fe1—N599.18 (19)C3—C4—H4B110.5
N3—Fe1—N5163.35 (18)S3—C4—H4B110.5
N2—Fe1—N494.20 (17)H4A—C4—H4B108.7
N1—Fe1—N4167.72 (17)N3—C5—C6116.0 (5)
N3—Fe1—N477.06 (19)N3—C5—S3119.7 (5)
N5—Fe1—N487.59 (17)C6—C5—S3124.2 (4)
N2—Fe1—N6i169.46 (19)N4—C6—C5117.3 (5)
N1—Fe1—N6i85.03 (17)N4—C6—S4117.9 (4)
N3—Fe1—N6i94.93 (17)C5—C6—S4124.8 (4)
N5—Fe1—N6i77.50 (17)C8—C7—S4106.5 (4)
N4—Fe1—N6i86.47 (15)C8—C7—H7A110.4
C5—S3—C487.5 (3)S4—C7—H7A110.4
C6—S4—C788.8 (3)C8—C7—H7B110.4
C1—N1—Fe1165.8 (5)S4—C7—H7B110.4
C2—N2—Fe1178.1 (5)H7A—C7—H7B108.6
C5—N3—C3111.3 (5)N4—C8—C7108.5 (5)
C5—N3—Fe1115.4 (4)N4—C8—H8A110.0
C3—N3—Fe1131.5 (4)C7—C8—H8A110.0
C6—N4—C8113.3 (5)N4—C8—H8B110.0
C6—N4—Fe1113.6 (4)C7—C8—H8B110.0
C8—N4—Fe1132.2 (4)H8A—C8—H8B108.4
C12—N5—C9115.6 (5)N5—C9—C10121.2 (5)
C12—N5—Fe1115.3 (3)N5—C9—H9119.4
C9—N5—Fe1129.1 (4)C10—C9—H9119.4
C12—N6—C11116.6 (5)C9—C10—C11119.1 (5)
C12—N6—Fe1i114.5 (3)C9—C10—H10120.4
C11—N6—Fe1i128.8 (4)C11—C10—H10120.4
N1—C1—S1179.5 (7)N6—C11—C10120.2 (6)
N2—C2—S2178.5 (5)N6—C11—H11119.9
N3—C3—C4108.2 (5)C10—C11—H11119.9
N3—C3—H3A110.1N6—C12—N5127.2 (4)
C4—C3—H3A110.1N6—C12—C12i117.5 (6)
N3—C3—H3B110.1N5—C12—C12i115.3 (6)
C4—C3—H3B110.1
N2—Fe1—N1—C1131.8 (18)Fe1—N1—C1—S1155 (59)
N3—Fe1—N1—C1132.2 (18)Fe1—N2—C2—S22 (35)
N5—Fe1—N1—C138.8 (18)C5—N3—C3—C420.1 (6)
N4—Fe1—N1—C184 (2)Fe1—N3—C3—C4176.6 (3)
N6i—Fe1—N1—C137.7 (18)N3—C3—C4—S327.6 (5)
N1—Fe1—N2—C247 (15)C5—S3—C4—C321.9 (4)
N3—Fe1—N2—C2143 (15)C3—N3—C5—C6175.2 (4)
N5—Fe1—N2—C252 (15)Fe1—N3—C5—C68.9 (6)
N4—Fe1—N2—C2140 (15)C3—N3—C5—S32.5 (6)
N6i—Fe1—N2—C247 (16)Fe1—N3—C5—S3168.8 (2)
N2—Fe1—N3—C587.2 (4)C4—S3—C5—N312.5 (4)
N1—Fe1—N3—C5176.5 (4)C4—S3—C5—C6169.9 (4)
N5—Fe1—N3—C529.1 (8)C8—N4—C6—C5172.9 (4)
N4—Fe1—N3—C55.9 (4)Fe1—N4—C6—C52.4 (5)
N6i—Fe1—N3—C591.1 (4)C8—N4—C6—S45.1 (6)
N2—Fe1—N3—C375.6 (5)Fe1—N4—C6—S4175.6 (2)
N1—Fe1—N3—C320.7 (5)N3—C5—C6—N47.6 (7)
N5—Fe1—N3—C3168.0 (5)S3—C5—C6—N4170.0 (4)
N4—Fe1—N3—C3168.7 (5)N3—C5—C6—S4170.2 (4)
N6i—Fe1—N3—C3106.1 (5)S3—C5—C6—S412.2 (6)
N2—Fe1—N4—C693.0 (4)C7—S4—C6—N48.1 (4)
N1—Fe1—N4—C651.3 (10)C7—S4—C6—C5174.1 (4)
N3—Fe1—N4—C61.7 (3)C6—S4—C7—C817.4 (4)
N5—Fe1—N4—C6175.2 (4)C6—N4—C8—C718.8 (6)
N6i—Fe1—N4—C697.6 (4)Fe1—N4—C8—C7172.9 (3)
N2—Fe1—N4—C898.7 (4)S4—C7—C8—N423.2 (5)
N1—Fe1—N4—C8117.0 (9)C12—N5—C9—C100.1 (7)
N3—Fe1—N4—C8166.6 (5)Fe1—N5—C9—C10178.2 (4)
N5—Fe1—N4—C86.9 (4)N5—C9—C10—C112.2 (8)
N6i—Fe1—N4—C870.7 (4)C12—N6—C11—C100.1 (7)
N2—Fe1—N5—C12177.7 (4)Fe1i—N6—C11—C10175.9 (4)
N1—Fe1—N5—C1281.5 (4)C9—C10—C11—N62.1 (8)
N3—Fe1—N5—C1265.5 (7)C11—N6—C12—N52.5 (7)
N4—Fe1—N5—C1288.2 (4)Fe1i—N6—C12—N5178.9 (4)
N6i—Fe1—N5—C121.2 (3)C11—N6—C12—C12i177.2 (5)
N2—Fe1—N5—C94.0 (4)Fe1i—N6—C12—C12i0.8 (7)
N1—Fe1—N5—C9100.2 (4)C9—N5—C12—N62.4 (7)
N3—Fe1—N5—C9112.8 (6)Fe1—N5—C12—N6179.1 (4)
N4—Fe1—N5—C990.1 (4)C9—N5—C12—C12i177.3 (5)
N6i—Fe1—N5—C9177.1 (5)Fe1—N5—C12—C12i1.2 (7)
Symmetry code: (i) x+2, y, z+2.
(photoHSHS-23K) top
Crystal data top
C12H11FeN6S4V = 848.0 (3) Å3
Mr = 423.36Z = 2
Triclinic, P1F(000) = 430
a = 8.642 (1) ÅDx = 1.658 Mg m3
b = 9.224 (2) ÅMo Kα radiation, λ = 0.71069 Å
c = 12.050 (3) ŵ = 1.39 mm1
α = 73.63 (2)°T = 23 K
β = 80.29 (1)°Block, black
γ = 67.25 (2)°0.1 × 0.1 × 0.1 mm
Data collection top
CCD Saphire 3 Xcalibur
diffractometer
2433 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.045
Graphite monochromatorθmax = 27.0°, θmin = 2.7°
Detector resolution: 19.64 pixels mm-1h = 1111
ω scank = 1111
10910 measured reflectionsl = 1515
3358 independent 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)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.116H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0666P)2 + 0.2166P]
where P = (Fo2 + 2Fc2)/3
3358 reflections(Δ/σ)max < 0.001
208 parametersΔρmax = 0.84 e Å3
0 restraintsΔρmin = 0.59 e Å3
Crystal data top
C12H11FeN6S4γ = 67.25 (2)°
Mr = 423.36V = 848.0 (3) Å3
Triclinic, P1Z = 2
a = 8.642 (1) ÅMo Kα radiation
b = 9.224 (2) ŵ = 1.39 mm1
c = 12.050 (3) ÅT = 23 K
α = 73.63 (2)°0.1 × 0.1 × 0.1 mm
β = 80.29 (1)°
Data collection top
CCD Saphire 3 Xcalibur
diffractometer
2433 reflections with I > 2σ(I)
10910 measured reflectionsRint = 0.045
3358 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0400 restraints
wR(F2) = 0.116H-atom parameters constrained
S = 1.05Δρmax = 0.84 e Å3
3358 reflectionsΔρmin = 0.59 e Å3
208 parameters
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
Fe10.83324 (7)0.22564 (7)0.79169 (4)0.01562 (16)
S10.31893 (13)0.22796 (13)1.02295 (9)0.0254 (3)
S20.74282 (13)0.11766 (13)0.44124 (8)0.0227 (2)
S30.88667 (13)0.71390 (13)0.59391 (8)0.0227 (2)
S41.27151 (13)0.41835 (13)0.64048 (9)0.0248 (3)
N10.5924 (4)0.2578 (4)0.8680 (3)0.0198 (7)
N20.8011 (4)0.1791 (4)0.6415 (3)0.0191 (7)
N30.7869 (4)0.4809 (4)0.7261 (3)0.0193 (7)
N41.0859 (4)0.2418 (4)0.7318 (3)0.0185 (7)
N50.9712 (4)0.0313 (4)0.8653 (2)0.0159 (7)
N61.1028 (4)0.2152 (4)1.0343 (2)0.0158 (7)
C10.4780 (5)0.2457 (5)0.9322 (3)0.0185 (8)
C20.7782 (5)0.1540 (5)0.5577 (3)0.0175 (8)
C30.6307 (5)0.6180 (5)0.7010 (3)0.0231 (9)
H3A0.55450.62210.77010.028*
H3B0.57690.60660.64120.028*
C40.6703 (5)0.7762 (5)0.6595 (3)0.0231 (9)
H4A0.66240.82220.72440.028*
H4B0.59300.85580.60310.028*
C50.9160 (5)0.5162 (5)0.6747 (3)0.0187 (8)
C61.0815 (5)0.3857 (5)0.6851 (3)0.0191 (9)
C71.3813 (5)0.1983 (5)0.6699 (3)0.0240 (9)
H7A1.40890.16210.59850.029*
H7B1.48430.16700.70720.029*
C81.2589 (5)0.1252 (5)0.7505 (3)0.0238 (9)
H8A1.27130.02430.73370.029*
H8B1.28290.10300.83070.029*
C91.0157 (4)0.1565 (5)0.8145 (3)0.0169 (8)
H90.98490.13650.73980.020*
C101.1053 (5)0.3127 (5)0.8704 (3)0.0198 (8)
H101.13710.39750.83410.024*
C111.1468 (5)0.3395 (5)0.9824 (3)0.0198 (8)
H111.20550.44421.02250.024*
C121.0214 (4)0.0692 (4)0.9729 (3)0.0147 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0129 (3)0.0217 (3)0.0131 (3)0.0065 (3)0.0004 (2)0.0057 (2)
S10.0237 (6)0.0280 (6)0.0267 (5)0.0125 (5)0.0110 (4)0.0128 (4)
S20.0229 (6)0.0339 (6)0.0161 (4)0.0138 (5)0.0010 (4)0.0092 (4)
S30.0225 (6)0.0275 (6)0.0204 (5)0.0119 (5)0.0004 (4)0.0062 (4)
S40.0211 (6)0.0321 (6)0.0271 (5)0.0136 (5)0.0051 (4)0.0142 (4)
N10.0168 (18)0.0254 (19)0.0147 (14)0.0057 (16)0.0026 (13)0.0030 (13)
N20.0161 (18)0.0262 (19)0.0143 (15)0.0071 (16)0.0017 (12)0.0043 (13)
N30.0157 (18)0.0265 (19)0.0163 (15)0.0071 (16)0.0020 (13)0.0058 (13)
N40.0155 (18)0.0270 (19)0.0164 (15)0.0088 (16)0.0010 (12)0.0100 (13)
N50.0124 (17)0.0241 (18)0.0132 (14)0.0082 (15)0.0001 (12)0.0056 (13)
N60.0113 (17)0.0219 (17)0.0151 (14)0.0061 (15)0.0026 (12)0.0075 (13)
C10.020 (2)0.0167 (19)0.0190 (18)0.0043 (18)0.0033 (16)0.0060 (15)
C20.012 (2)0.019 (2)0.0175 (18)0.0044 (17)0.0007 (14)0.0002 (15)
C30.016 (2)0.027 (2)0.026 (2)0.007 (2)0.0022 (16)0.0064 (17)
C40.018 (2)0.026 (2)0.0219 (19)0.005 (2)0.0018 (16)0.0055 (16)
C50.023 (2)0.023 (2)0.0146 (17)0.012 (2)0.0017 (15)0.0063 (15)
C60.018 (2)0.030 (2)0.0135 (17)0.011 (2)0.0013 (15)0.0087 (16)
C70.015 (2)0.030 (2)0.030 (2)0.008 (2)0.0056 (17)0.0171 (18)
C80.019 (2)0.029 (2)0.025 (2)0.008 (2)0.0045 (16)0.0143 (17)
C90.014 (2)0.027 (2)0.0125 (16)0.0086 (19)0.0007 (14)0.0072 (15)
C100.016 (2)0.027 (2)0.0190 (18)0.0071 (19)0.0042 (15)0.0132 (16)
C110.016 (2)0.023 (2)0.0211 (18)0.0079 (18)0.0026 (15)0.0085 (16)
C120.013 (2)0.023 (2)0.0125 (16)0.0086 (18)0.0033 (14)0.0090 (15)
Geometric parameters (Å, º) top
Fe1—N22.058 (3)N6—C121.318 (5)
Fe1—N12.072 (3)N6—C111.355 (5)
Fe1—N32.158 (3)N6—Fe1i2.225 (3)
Fe1—N52.193 (3)C3—C41.554 (5)
Fe1—N6i2.225 (3)C3—H3A0.9700
Fe1—N42.229 (3)C3—H3B0.9700
S1—C11.636 (4)C4—H4A0.9700
S2—C21.632 (4)C4—H4B0.9700
S3—C51.750 (4)C5—C61.468 (6)
S3—C41.838 (4)C7—C81.534 (5)
S4—C61.752 (4)C7—H7A0.9700
S4—C71.834 (4)C7—H7B0.9700
N1—C11.170 (5)C8—H8A0.9700
N2—C21.161 (5)C8—H8B0.9700
N3—C51.292 (5)C9—C101.376 (5)
N3—C31.454 (5)C9—H90.9300
N4—C61.275 (5)C10—C111.384 (5)
N4—C81.475 (5)C10—H100.9300
N5—C121.345 (4)C11—H110.9300
N5—C91.354 (5)C12—C12i1.488 (7)
N2—Fe1—N197.68 (12)H3A—C3—H3B108.3
N2—Fe1—N397.80 (12)C3—C4—S3104.8 (3)
N1—Fe1—N394.80 (12)C3—C4—H4A110.8
N2—Fe1—N592.11 (12)S3—C4—H4A110.8
N1—Fe1—N5102.59 (12)C3—C4—H4B110.8
N3—Fe1—N5158.64 (12)S3—C4—H4B110.8
N2—Fe1—N6i166.95 (12)H4A—C4—H4B108.9
N1—Fe1—N6i85.13 (11)N3—C5—C6117.7 (3)
N3—Fe1—N6i94.64 (12)N3—C5—S3119.3 (3)
N5—Fe1—N6i74.84 (11)C6—C5—S3123.0 (3)
N2—Fe1—N494.58 (11)N4—C6—C5117.7 (3)
N1—Fe1—N4164.96 (13)N4—C6—S4118.8 (3)
N3—Fe1—N474.86 (12)C5—C6—S4123.5 (3)
N5—Fe1—N485.57 (11)C8—C7—S4105.7 (3)
N6i—Fe1—N484.88 (11)C8—C7—H7A110.6
C5—S3—C488.21 (18)S4—C7—H7A110.6
C6—S4—C788.71 (18)C8—C7—H7B110.6
C1—N1—Fe1163.5 (3)S4—C7—H7B110.6
C2—N2—Fe1178.1 (3)H7A—C7—H7B108.7
C5—N3—C3111.7 (3)N4—C8—C7108.6 (3)
C5—N3—Fe1115.1 (3)N4—C8—H8A110.0
C3—N3—Fe1130.8 (2)C7—C8—H8A110.0
C6—N4—C8112.4 (3)N4—C8—H8B110.0
C6—N4—Fe1113.7 (3)C7—C8—H8B110.0
C8—N4—Fe1133.1 (2)H8A—C8—H8B108.4
C12—N5—C9115.8 (3)N5—C9—C10121.8 (3)
C12—N5—Fe1116.4 (2)N5—C9—H9119.1
C9—N5—Fe1127.9 (2)C10—C9—H9119.1
C12—N6—C11117.0 (3)C9—C10—C11117.9 (4)
C12—N6—Fe1i115.4 (2)C9—C10—H10121.1
C11—N6—Fe1i127.5 (3)C11—C10—H10121.1
N1—C1—S1179.5 (4)N6—C11—C10120.9 (4)
N2—C2—S2178.8 (3)N6—C11—H11119.6
N3—C3—C4109.0 (3)C10—C11—H11119.6
N3—C3—H3A109.9N6—C12—N5126.6 (3)
C4—C3—H3A109.9N6—C12—C12i117.6 (4)
N3—C3—H3B109.9N5—C12—C12i115.9 (4)
C4—C3—H3B109.9
N2—Fe1—N1—C1122.3 (11)Fe1—N1—C1—S125 (44)
N3—Fe1—N1—C1139.2 (11)Fe1—N2—C2—S233 (27)
N5—Fe1—N1—C128.4 (11)C5—N3—C3—C420.6 (4)
N6i—Fe1—N1—C144.9 (11)Fe1—N3—C3—C4177.9 (2)
N4—Fe1—N1—C193.4 (12)N3—C3—C4—S327.6 (4)
N1—Fe1—N2—C29 (9)C5—S3—C4—C321.5 (3)
N3—Fe1—N2—C287 (9)C3—N3—C5—C6175.5 (3)
N5—Fe1—N2—C2112 (9)Fe1—N3—C5—C611.0 (4)
N6i—Fe1—N2—C2111 (9)C3—N3—C5—S33.2 (4)
N4—Fe1—N2—C2162 (9)Fe1—N3—C5—S3167.73 (17)
N2—Fe1—N3—C585.1 (3)C4—S3—C5—N312.2 (3)
N1—Fe1—N3—C5176.4 (3)C4—S3—C5—C6169.2 (3)
N5—Fe1—N3—C531.8 (5)C8—N4—C6—C5172.9 (3)
N6i—Fe1—N3—C590.9 (3)Fe1—N4—C6—C51.5 (4)
N4—Fe1—N3—C57.5 (3)C8—N4—C6—S45.5 (4)
N2—Fe1—N3—C375.8 (3)Fe1—N4—C6—S4176.84 (17)
N1—Fe1—N3—C322.7 (3)N3—C5—C6—N48.5 (5)
N5—Fe1—N3—C3167.3 (3)S3—C5—C6—N4170.1 (3)
N6i—Fe1—N3—C3108.2 (3)N3—C5—C6—S4169.7 (3)
N4—Fe1—N3—C3168.4 (3)S3—C5—C6—S411.6 (5)
N2—Fe1—N4—C693.9 (3)C7—S4—C6—N48.8 (3)
N1—Fe1—N4—C650.6 (6)C7—S4—C6—C5172.9 (3)
N3—Fe1—N4—C62.9 (2)C6—S4—C7—C818.8 (3)
N5—Fe1—N4—C6174.3 (3)C6—N4—C8—C720.4 (4)
N6i—Fe1—N4—C699.2 (3)Fe1—N4—C8—C7170.5 (2)
N2—Fe1—N4—C897.1 (3)S4—C7—C8—N425.1 (4)
N1—Fe1—N4—C8118.3 (5)C12—N5—C9—C100.6 (5)
N3—Fe1—N4—C8166.0 (3)Fe1—N5—C9—C10178.9 (2)
N5—Fe1—N4—C85.3 (3)N5—C9—C10—C111.2 (5)
N6i—Fe1—N4—C869.8 (3)C12—N6—C11—C100.8 (5)
N2—Fe1—N5—C12178.5 (2)Fe1i—N6—C11—C10176.3 (2)
N1—Fe1—N5—C1280.2 (3)C9—C10—C11—N61.1 (5)
N3—Fe1—N5—C1263.6 (4)C11—N6—C12—N52.9 (5)
N6i—Fe1—N5—C121.2 (2)Fe1i—N6—C12—N5179.0 (3)
N4—Fe1—N5—C1287.0 (2)C11—N6—C12—C12i177.6 (4)
N2—Fe1—N5—C93.2 (3)Fe1i—N6—C12—C12i1.4 (5)
N1—Fe1—N5—C9101.6 (3)C9—N5—C12—N62.8 (5)
N3—Fe1—N5—C9114.6 (4)Fe1—N5—C12—N6178.7 (3)
N6i—Fe1—N5—C9177.1 (3)C9—N5—C12—C12i177.6 (3)
N4—Fe1—N5—C991.2 (3)Fe1—N5—C12—C12i0.8 (5)
Symmetry code: (i) x+2, y, z+2.

Experimental details

(LSLS-23K)(HSLS-180K)(HSHS-250K)(photoHSLS-23K)
Crystal data
Chemical formulaC12H11FeN6S4C12H11FeN6S4C12H11FeN6S4C12H11FeN6S4
Mr423.36423.36423.36423.36
Crystal system, space groupTriclinic, P1Triclinic, P1Triclinic, P1Triclinic, P1
Temperature (K)2318025023
a, b, c (Å)8.446 (1), 9.123 (1), 11.779 (2)8.6103 (7), 9.2628 (8), 11.9305 (9)8.727 (1), 9.385 (2), 12.041 (2)8.581 (2), 9.196 (2), 11.948 (3)
α, β, γ (°)72.26 (1), 80.94 (1), 67.33 (1)72.903 (7), 80.057 (7), 66.911 (8)73.04 (2), 79.43 (1), 66.60 (2)73.34 (2), 80.53 (2), 67.24 (2)
V3)796.83 (19)834.84 (12)863.2 (3)831.4 (3)
Z2222
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)1.481.411.361.42
Crystal size (mm)0.1 × 0.1 × 0.10.1 × 0.1 × 0.10.1 × 0.1 × 0.10.1 × 0.1 × 0.1
Data collection
DiffractometerCCD Saphire 3 Xcalibur
diffractometer
CCD Saphire 3 Xcalibur
diffractometer
CCD Saphire 3 Xcalibur
diffractometer
CCD Saphire 3 Xcalibur
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
11525, 3210, 2190 11132, 3353, 1201 12617, 3452, 1292 10339, 3250, 2278
Rint0.0540.0950.1260.129
(sin θ/λ)max1)0.6390.6390.6390.639
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.090, 0.92 0.039, 0.073, 0.62 0.055, 0.160, 0.84 0.065, 0.153, 1.09
No. of reflections3210335334523250
No. of parameters208208208208
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.65, 0.470.32, 0.310.53, 0.330.88, 0.69


(photoHSHS-23K)
Crystal data
Chemical formulaC12H11FeN6S4
Mr423.36
Crystal system, space groupTriclinic, P1
Temperature (K)23
a, b, c (Å)8.642 (1), 9.224 (2), 12.050 (3)
α, β, γ (°)73.63 (2), 80.29 (1), 67.25 (2)
V3)848.0 (3)
Z2
Radiation typeMo Kα
µ (mm1)1.39
Crystal size (mm)0.1 × 0.1 × 0.1
Data collection
DiffractometerCCD Saphire 3 Xcalibur
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
10910, 3358, 2433
Rint0.045
(sin θ/λ)max1)0.639
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.040, 0.116, 1.05
No. of reflections3358
No. of parameters208
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.84, 0.59

Computer programs: CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.26, CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26, SIR97_(Altomare & al., 1998), SHELXL97 (Sheldrick, 1997), PLATON_(Spek, 1998).

 

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