The effect of pressure (up to 0.17 GPa) on the spin-crossover compound {Fe(pmd)2[Ag(CN)2]2}n [orthorhombic isomer (II), pmd = pyrimidine] has been investigated by temperature- and pressure-dependent neutron Laue diffraction and magnetometry. The cooperative high-spin ↔ low-spin transition, centred at ca 180 K at ambient pressure, is shifted to higher temperatures as pressure is applied, showing a moderate sensitivity of the compound to pressure, since the spin transition is displaced by ca 140 K GPa−1. The space-group symmetry (orthorhombic Pccn) remains unchanged over the pressure–temperature (P–T) range studied. The main structural consequence of the high-spin to low-spin transition is the contraction of the distorted octahedral [FeN6] chromophores, being more marked in the axial positions (occupied by the pmd units), than in the equatorial positions (occupied by four [Ag(CN)2]− bridging ligands).
Supporting information
| Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614003023/xk5013sup1.cif Contains datablocks fepmd1, fepmd2, fepmd3, fepmd4, fepmd5, fepmd6, fepmd7, fepmd8, fepmd9, fepmd10, fepmd11, fepmd12, fepmd13 |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520614003023/xk5013fepmd1sup2.hkl Contains datablock fepmdb |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520614003023/xk5013fepmd2sup3.hkl Contains datablock fepmdj |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520614003023/xk5013fepmd3sup4.hkl Contains datablock shelxl |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520614003023/xk5013fepmd4sup5.hkl Contains datablock fepmdf |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520614003023/xk5013fepmd5sup6.hkl Contains datablock fepmda |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520614003023/xk5013fepmd6sup7.hkl Contains datablock fepmdk |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520614003023/xk5013fepmd7sup8.hkl Contains datablock fepmdm |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520614003023/xk5013fepmd8sup9.hkl Contains datablock fepmdn |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520614003023/xk5013fepmd9sup10.hkl Contains datablock fepmdi |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520614003023/xk5013fepmd10sup11.hkl Contains datablock fepmdl |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520614003023/xk5013fepmd11sup12.hkl Contains datablock fepmdc |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520614003023/xk5013fepmd12sup13.hkl Contains datablock fepmdo |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520614003023/xk5013fepmd13sup14.hkl Contains datablock fepmde |
| Portable Document Format (PDF) file https://doi.org/10.1107/S2052520614003023/xk5013sup15.pdf Neutron Laue diffraction pattern obtained at 0.11 GPa and 187K, showing the coexistence of both LS and HS phases |
CCDC references: 986124; 986125; 986126; 986127; 986128; 986129; 986130; 986131; 986132; 986133; 986134; 986135; 986136
For all compounds, cell refinement: NEWLAUEGEN (J. Campbell et al., 1998); data reduction: ARGONNE-BOXES(C. Wilkinson et al.,1988)& LAUENORM (J. W. Campbell et al.,1986; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
Crystal data top
C12H8Ag2FeN8 | Z = 4 |
Mr = 535.83 | F(000) = 584 |
Orthorhombic, Pccn | Dx = 2.219 Mg m−3 |
Hall symbol: -P 2ab 2ac | Neutron radiation, λ = 0.90-3.00 Å |
a = 14.895 (3) Å | µ = 0.08 mm−1 |
b = 8.106 (3) Å | T = 150 K |
c = 13.285 (3) Å | Prism, orange-yellow |
V = 1604.0 (8) Å3 | 1.0 × 0.6 × 0.5 mm |
Data collection top
ILL-VIVALDI Laue single xtal diffractometer | Rint = 0.197 |
Radiation source: ILL neutron source | θmax = 36.5°, θmin = 4.0° |
7581 measured reflections | h = −12→20 |
1543 independent reflections | k = −10→10 |
1236 reflections with I > 2σ(I) | l = −17→15 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.083 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.149 | All H-atom parameters refined |
S = 1.24 | w = 1/[σ2(Fo2) + (0.0554P)2] where P = (Fo2 + 2Fc2)/3 |
1543 reflections | (Δ/σ)max < 0.001 |
142 parameters | Δρmax = 0.86 e Å−3 |
0 restraints | Δρmin = −0.88 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
C1 | 0.6287 (2) | 0.5259 (4) | 0.9526 (2) | 0.0236 (7) | |
C2 | 0.58924 (18) | 0.4495 (4) | 0.87013 (19) | 0.0211 (6) | |
C3 | 0.58671 (16) | 0.3118 (4) | 1.05253 (18) | 0.0167 (6) | |
C4 | 0.54938 (17) | 0.2976 (4) | 0.88628 (18) | 0.0173 (6) | |
C5 | 0.32911 (16) | 0.0733 (4) | 0.87685 (18) | 0.0170 (6) | |
C6 | 0.38886 (16) | 0.0845 (3) | 1.18864 (18) | 0.0170 (6) | |
Ag1 | 0.29509 (17) | 0.0881 (4) | 1.3042 (2) | 0.0169 (7) | |
Fe1 | 0.5000 | 0.0000 | 1.0000 | 0.0093 (6) | |
N1 | 0.54892 (13) | 0.2265 (2) | 0.97754 (14) | 0.0140 (4) | |
N2 | 0.62570 (14) | 0.4583 (3) | 1.04394 (15) | 0.0213 (5) | |
N3 | 0.43592 (11) | 0.0670 (3) | 1.11982 (12) | 0.0153 (4) | |
N4 | 0.39526 (10) | 0.0526 (3) | 0.92123 (13) | 0.0147 (4) | |
H1 | 0.6612 (5) | 0.6447 (11) | 0.9459 (5) | 0.0508 (19) | |
H2 | 0.5904 (5) | 0.5047 (9) | 0.7960 (5) | 0.0442 (18) | |
H3 | 0.5857 (5) | 0.2556 (8) | 1.1264 (4) | 0.0356 (16) | |
H4 | 0.5169 (5) | 0.2308 (8) | 0.8255 (4) | 0.0350 (15) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0283 (14) | 0.0241 (19) | 0.0182 (14) | −0.0075 (13) | −0.0007 (11) | 0.0009 (12) |
C2 | 0.0294 (13) | 0.0198 (17) | 0.0141 (13) | −0.0049 (12) | 0.0009 (9) | 0.0051 (12) |
C3 | 0.0182 (11) | 0.0202 (17) | 0.0117 (11) | −0.0050 (11) | 0.0001 (8) | −0.0009 (10) |
C4 | 0.0199 (11) | 0.0205 (16) | 0.0115 (11) | −0.0017 (11) | −0.0002 (9) | 0.0020 (10) |
C5 | 0.0139 (11) | 0.0239 (17) | 0.0133 (11) | −0.0002 (11) | −0.0042 (8) | 0.0000 (10) |
C6 | 0.0156 (11) | 0.0245 (17) | 0.0109 (11) | −0.0004 (11) | 0.0061 (8) | 0.0000 (10) |
Ag1 | 0.0143 (12) | 0.0216 (19) | 0.0150 (12) | 0.0040 (11) | 0.0082 (9) | 0.0018 (11) |
Fe1 | 0.0074 (12) | 0.0144 (18) | 0.0060 (13) | 0.0007 (8) | 0.0009 (7) | −0.0008 (8) |
N1 | 0.0135 (8) | 0.0176 (11) | 0.0109 (7) | −0.0004 (7) | 0.0002 (7) | −0.0003 (7) |
N2 | 0.0253 (9) | 0.0217 (12) | 0.0170 (10) | −0.0080 (9) | −0.0010 (7) | −0.0020 (8) |
N3 | 0.0135 (8) | 0.0216 (12) | 0.0108 (8) | 0.0018 (8) | 0.0040 (6) | −0.0008 (7) |
N4 | 0.0114 (7) | 0.0201 (11) | 0.0126 (8) | 0.0003 (8) | −0.0026 (6) | 0.0013 (8) |
H1 | 0.064 (4) | 0.049 (5) | 0.039 (4) | −0.024 (4) | −0.002 (3) | 0.006 (3) |
H2 | 0.065 (4) | 0.047 (5) | 0.021 (3) | −0.008 (3) | −0.001 (3) | 0.012 (3) |
H3 | 0.054 (4) | 0.037 (4) | 0.016 (3) | −0.015 (3) | −0.002 (2) | 0.003 (2) |
H4 | 0.045 (3) | 0.040 (4) | 0.020 (3) | −0.013 (3) | −0.010 (2) | 0.002 (2) |
Geometric parameters (Å, º) top
C1—N2 | 1.332 (4) | C6—N3 | 1.161 (3) |
C1—C2 | 1.389 (4) | C6—Ag1 | 2.075 (3) |
C1—H1 | 1.081 (9) | Ag1—C5ii | 2.090 (3) |
C2—C4 | 1.384 (4) | Ag1—N2iii | 2.563 (3) |
C2—H2 | 1.081 (7) | Ag1—Ag1iv | 2.949 (6) |
C3—N2 | 1.327 (4) | Fe1—N4v | 1.9263 (16) |
C3—N1 | 1.337 (3) | Fe1—N4 | 1.9263 (16) |
C3—H3 | 1.082 (6) | Fe1—N3v | 1.9339 (17) |
C4—N1 | 1.342 (3) | Fe1—N3 | 1.9339 (17) |
C4—H4 | 1.086 (6) | Fe1—N1 | 1.998 (2) |
C5—N4 | 1.161 (3) | Fe1—N1v | 1.998 (2) |
C5—Ag1i | 2.090 (3) | N2—Ag1vi | 2.563 (4) |
| | | |
N2—C1—C2 | 121.4 (3) | N4—Fe1—N3v | 90.84 (7) |
N2—C1—H1 | 117.2 (5) | N4v—Fe1—N3 | 90.84 (7) |
C2—C1—H1 | 121.4 (5) | N4—Fe1—N3 | 89.16 (7) |
C4—C2—C1 | 117.1 (3) | N3v—Fe1—N3 | 180.0 |
C4—C2—H2 | 121.1 (5) | N4v—Fe1—N1 | 89.38 (8) |
C1—C2—H2 | 121.8 (5) | N4—Fe1—N1 | 90.62 (8) |
N2—C3—N1 | 125.7 (2) | N3v—Fe1—N1 | 87.43 (9) |
N2—C3—H3 | 117.4 (4) | N3—Fe1—N1 | 92.57 (9) |
N1—C3—H3 | 116.9 (4) | N4v—Fe1—N1v | 90.62 (8) |
N1—C4—C2 | 121.6 (2) | N4—Fe1—N1v | 89.38 (8) |
N1—C4—H4 | 117.1 (4) | N3v—Fe1—N1v | 92.57 (9) |
C2—C4—H4 | 121.3 (4) | N3—Fe1—N1v | 87.43 (9) |
N4—C5—Ag1i | 174.0 (3) | N1—Fe1—N1v | 180.0 |
N3—C6—Ag1 | 172.1 (2) | C3—N1—C4 | 116.7 (2) |
C6—Ag1—C5ii | 159.47 (18) | C3—N1—Fe1 | 121.16 (17) |
C6—Ag1—N2iii | 105.47 (13) | C4—N1—Fe1 | 122.08 (18) |
C5ii—Ag1—N2iii | 91.16 (13) | C3—N2—C1 | 117.5 (2) |
C6—Ag1—Ag1iv | 108.60 (15) | C3—N2—Ag1vi | 120.06 (17) |
C5ii—Ag1—Ag1iv | 69.38 (13) | C1—N2—Ag1vi | 122.2 (2) |
N2iii—Ag1—Ag1iv | 125.10 (10) | C6—N3—Fe1 | 168.7 (2) |
N4v—Fe1—N4 | 180.0 | C5—N4—Fe1 | 174.7 (2) |
N4v—Fe1—N3v | 89.16 (7) | | |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) −x+1/2, y, z+1/2; (iii) −x+1, y−1/2, −z+5/2; (iv) −x+1/2, −y+1/2, z; (v) −x+1, −y, −z+2; (vi) −x+1, y+1/2, −z+5/2. |
Crystal data top
C12H8Ag2FeN8 | Z = 4 |
Mr = 535.83 | F(000) = 584 |
Orthorhombic, Pccn | Dx = 2.214 Mg m−3 |
Hall symbol: -P 2ab 2ac | Neutron radiation, λ = 0.90-3.00 Å |
a = 14.895 (3) Å | µ = 0.08 mm−1 |
b = 8.122 (3) Å | T = 187 K |
c = 13.288 (3) Å | Prism, orange-yellow |
V = 1607.5 (8) Å3 | 1.0 × 0.6 × 0.5 mm |
Data collection top
ILL-VIVALDI Laue single xtal diffractometer | Rint = 0.321 |
Radiation source: ILL neutron source | θmax = 33.4°, θmin = 4.0° |
5504 measured reflections | h = −11→18 |
1210 independent reflections | k = −9→9 |
943 reflections with I > 2σ(I) | l = −16→14 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.166 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.281 | All H-atom parameters refined |
S = 1.35 | w = 1/[σ2(Fo2) + (0.P)2 + 81.4399P] where P = (Fo2 + 2Fc2)/3 |
1210 reflections | (Δ/σ)max < 0.001 |
142 parameters | Δρmax = 0.90 e Å−3 |
0 restraints | Δρmin = −0.99 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
N3 | 0.6051 (3) | 0.0535 (8) | 0.0788 (4) | 0.0191 (12) | |
N4 | 0.5645 (3) | 0.0687 (8) | −0.1195 (3) | 0.0206 (12) | |
N2 | 0.3744 (4) | 0.4577 (8) | −0.0440 (4) | 0.0257 (13) | |
N1 | 0.4508 (4) | 0.2253 (8) | 0.0221 (4) | 0.0199 (12) | |
C1 | 0.6111 (5) | 0.0859 (11) | −0.1884 (5) | 0.0236 (18) | |
Ag1 | 0.7051 (5) | 0.0867 (12) | −0.3038 (5) | 0.023 (2) | |
C2 | 0.6701 (4) | 0.0727 (11) | 0.1235 (5) | 0.0206 (17) | |
C5 | 0.4107 (5) | 0.4508 (11) | 0.1288 (5) | 0.0251 (18) | |
C3 | 0.4130 (4) | 0.3123 (10) | −0.0526 (5) | 0.0173 (16) | |
Fe1 | 0.5000 | 0.0000 | 0.0000 | 0.015 (2) | |
C6 | 0.4503 (5) | 0.2987 (11) | 0.1134 (5) | 0.0218 (17) | |
C4 | 0.3707 (7) | 0.5234 (12) | 0.0472 (6) | 0.031 (2) | |
H5 | 0.4082 (16) | 0.505 (3) | 0.2026 (12) | 0.058 (6) | |
H3 | 0.4147 (13) | 0.2541 (18) | −0.1261 (11) | 0.034 (4) | |
H6 | 0.4838 (13) | 0.234 (2) | 0.1740 (13) | 0.043 (5) | |
H4 | 0.3383 (15) | 0.645 (3) | 0.0523 (16) | 0.064 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
N3 | 0.015 (2) | 0.027 (3) | 0.015 (2) | −0.004 (2) | −0.0018 (18) | −0.001 (2) |
N4 | 0.019 (2) | 0.028 (4) | 0.015 (2) | 0.001 (2) | 0.0045 (19) | 0.003 (2) |
N2 | 0.035 (3) | 0.021 (3) | 0.021 (3) | 0.006 (3) | −0.002 (2) | 0.002 (2) |
N1 | 0.017 (3) | 0.029 (4) | 0.0138 (19) | 0.003 (2) | −0.0008 (19) | −0.001 (2) |
C1 | 0.023 (3) | 0.033 (5) | 0.014 (3) | 0.000 (3) | 0.005 (3) | 0.005 (3) |
Ag1 | 0.013 (3) | 0.037 (6) | 0.018 (3) | −0.004 (3) | 0.011 (3) | −0.004 (4) |
C2 | 0.018 (3) | 0.024 (5) | 0.020 (3) | 0.000 (3) | −0.004 (3) | 0.003 (3) |
C5 | 0.037 (4) | 0.018 (5) | 0.020 (4) | 0.007 (4) | 0.001 (3) | −0.003 (3) |
C3 | 0.024 (3) | 0.013 (4) | 0.016 (3) | 0.007 (3) | −0.004 (2) | −0.001 (3) |
Fe1 | 0.010 (4) | 0.026 (6) | 0.008 (3) | 0.002 (2) | 0.000 (2) | 0.000 (2) |
C6 | 0.030 (4) | 0.022 (5) | 0.014 (3) | −0.003 (3) | 0.003 (3) | −0.003 (3) |
C4 | 0.042 (5) | 0.029 (6) | 0.023 (4) | 0.010 (4) | 0.001 (4) | −0.001 (3) |
H5 | 0.079 (14) | 0.078 (18) | 0.016 (8) | 0.017 (11) | 0.002 (8) | −0.004 (8) |
H3 | 0.072 (12) | 0.015 (9) | 0.014 (7) | 0.011 (7) | 0.008 (6) | −0.001 (5) |
H6 | 0.046 (9) | 0.052 (14) | 0.030 (9) | 0.007 (8) | −0.016 (7) | −0.006 (7) |
H4 | 0.072 (13) | 0.056 (15) | 0.063 (12) | 0.055 (13) | 0.009 (10) | 0.005 (10) |
Geometric parameters (Å, º) top
N3—C2 | 1.148 (8) | Ag1—N2iii | 2.568 (9) |
N3—Fe1 | 1.932 (5) | Ag1—Ag1iv | 2.970 (18) |
N4—C1 | 1.157 (8) | C2—Ag1v | 2.097 (10) |
N4—Fe1 | 1.939 (4) | C5—C4 | 1.371 (12) |
N2—C3 | 1.318 (10) | C5—C6 | 1.384 (12) |
N2—C4 | 1.325 (12) | C5—H5 | 1.073 (19) |
N2—Ag1i | 2.568 (9) | C3—H3 | 1.085 (15) |
N1—C3 | 1.344 (9) | Fe1—N3vi | 1.932 (5) |
N1—C6 | 1.351 (9) | Fe1—N4vi | 1.939 (4) |
N1—Fe1 | 1.992 (6) | Fe1—N1vi | 1.992 (6) |
C1—Ag1 | 2.077 (9) | C6—H6 | 1.083 (19) |
Ag1—C2ii | 2.097 (10) | C4—H4 | 1.10 (2) |
| | | |
C2—N3—Fe1 | 174.4 (6) | N3vi—Fe1—N3 | 180.0 (3) |
C1—N4—Fe1 | 168.6 (6) | N3vi—Fe1—N4vi | 88.7 (2) |
C3—N2—C4 | 117.3 (7) | N3—Fe1—N4vi | 91.3 (2) |
C3—N2—Ag1i | 119.9 (5) | N3vi—Fe1—N4 | 91.3 (2) |
C4—N2—Ag1i | 122.4 (6) | N3—Fe1—N4 | 88.7 (2) |
C3—N1—C6 | 115.4 (6) | N4vi—Fe1—N4 | 180.0 (4) |
C3—N1—Fe1 | 121.9 (5) | N3vi—Fe1—N1 | 89.4 (2) |
C6—N1—Fe1 | 122.7 (5) | N3—Fe1—N1 | 90.6 (2) |
N4—C1—Ag1 | 171.5 (7) | N4vi—Fe1—N1 | 87.8 (2) |
C1—Ag1—C2ii | 159.6 (5) | N4—Fe1—N1 | 92.2 (2) |
C1—Ag1—N2iii | 105.6 (4) | N3vi—Fe1—N1vi | 90.6 (2) |
C2ii—Ag1—N2iii | 91.4 (4) | N3—Fe1—N1vi | 89.4 (2) |
C1—Ag1—Ag1iv | 107.8 (4) | N4vi—Fe1—N1vi | 92.2 (2) |
C2ii—Ag1—Ag1iv | 69.5 (4) | N4—Fe1—N1vi | 87.8 (2) |
N2iii—Ag1—Ag1iv | 124.9 (3) | N1—Fe1—N1vi | 180.0 (3) |
N3—C2—Ag1v | 173.8 (7) | N1—C6—C5 | 122.0 (7) |
C4—C5—C6 | 116.8 (7) | N1—C6—H6 | 116.9 (12) |
C4—C5—H5 | 122.2 (14) | C5—C6—H6 | 121.1 (12) |
C6—C5—H5 | 120.9 (14) | N2—C4—C5 | 122.2 (9) |
N2—C3—N1 | 126.2 (6) | N2—C4—H4 | 115.9 (14) |
N2—C3—H3 | 118.7 (10) | C5—C4—H4 | 121.8 (14) |
N1—C3—H3 | 115.2 (10) | | |
Symmetry codes: (i) −x+1, y+1/2, −z−1/2; (ii) −x+3/2, y, z−1/2; (iii) −x+1, y−1/2, −z−1/2; (iv) −x+3/2, −y+1/2, z; (v) −x+3/2, y, z+1/2; (vi) −x+1, −y, −z. |
Crystal data top
C12H8Ag2FeN8 | Z = 4 |
Mr = 535.83 | F(000) = 584 |
Orthorhombic, Pccn | Dx = 2.010 Mg m−3 |
Hall symbol: -P 2ab 2ac | Neutron radiation, λ = 0.95-2.50 Å |
a = 15.782 (3) Å | µ = 0.09 mm−1 |
b = 8.424 (3) Å | T = 210 K |
c = 13.320 (3) Å | Prism, orange-yellow |
V = 1770.9 (8) Å3 | 1.0 × 0.6 × 0.5 mm |
Data collection top
ILL-VIVALDI Laue single xtal diffractometer | Rint = 0.259 |
Radiation source: ILL neutron source | θmax = 29.3°, θmin = 4.0° |
2295 measured reflections | h = −17→7 |
686 independent reflections | k = −8→7 |
510 reflections with I > 2σ(I) | l = −14→13 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.158 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.261 | All H-atom parameters refined |
S = 1.39 | w = 1/[σ2(Fo2) + (0.0838P)2] where P = (Fo2 + 2Fc2)/3 |
686 reflections | (Δ/σ)max < 0.001 |
136 parameters | Δρmax = 0.66 e Å−3 |
0 restraints | Δρmin = −0.75 e Å−3 |
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. Restrains used in the refinement EADP C4 H4 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 | x | y | z | Uiso*/Ueq | |
C1 | 0.6281 (10) | 0.538 (2) | 0.9512 (11) | 0.046 (4) | |
C2 | 0.5878 (9) | 0.468 (2) | 0.8682 (10) | 0.040 (4) | |
C3 | 0.5949 (7) | 0.3249 (19) | 1.0486 (9) | 0.033 (3) | |
C4 | 0.5498 (11) | 0.321 (2) | 0.8856 (10) | 0.043 (3) | |
C5 | 0.3257 (8) | 0.0732 (17) | 0.8752 (8) | 0.036 (3) | |
C6 | 0.3852 (7) | 0.0778 (19) | 1.1965 (8) | 0.032 (3) | |
Ag1 | 0.2901 (7) | 0.0853 (18) | 1.3049 (8) | 0.029 (4) | |
Fe1 | 0.5000 | 0.0000 | 1.0000 | 0.031 (4) | |
N1 | 0.5521 (7) | 0.2460 (11) | 0.9760 (6) | 0.036 (3) | |
N2 | 0.6296 (6) | 0.4686 (14) | 1.0395 (7) | 0.040 (3) | |
N3 | 0.4350 (6) | 0.0713 (14) | 1.1341 (6) | 0.038 (3) | |
N4 | 0.3908 (6) | 0.0611 (16) | 0.9142 (6) | 0.041 (3) | |
H1 | 0.660 (3) | 0.658 (5) | 0.944 (3) | 0.090 (12) | |
H2 | 0.583 (2) | 0.530 (4) | 0.794 (3) | 0.079 (10) | |
H3 | 0.5944 (16) | 0.259 (4) | 1.123 (2) | 0.058 (9) | |
H4 | 0.515 (2) | 0.258 (3) | 0.830 (2) | 0.043 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.049 (9) | 0.051 (12) | 0.038 (9) | −0.009 (9) | −0.006 (7) | −0.005 (9) |
C2 | 0.040 (8) | 0.050 (12) | 0.029 (8) | 0.002 (7) | −0.012 (6) | 0.005 (7) |
C3 | 0.039 (7) | 0.048 (11) | 0.012 (7) | −0.016 (8) | −0.010 (5) | 0.000 (8) |
C4 | 0.057 (8) | 0.041 (10) | 0.032 (6) | 0.003 (7) | −0.003 (7) | 0.018 (7) |
C5 | 0.016 (6) | 0.056 (11) | 0.036 (7) | 0.002 (7) | −0.013 (5) | −0.006 (7) |
C6 | 0.028 (7) | 0.048 (11) | 0.019 (6) | 0.005 (6) | 0.013 (5) | 0.002 (6) |
Ag1 | 0.017 (6) | 0.037 (12) | 0.033 (7) | 0.000 (7) | 0.011 (5) | 0.018 (6) |
Fe1 | 0.041 (9) | 0.035 (13) | 0.015 (7) | 0.009 (6) | −0.005 (5) | −0.005 (4) |
N1 | 0.039 (6) | 0.053 (8) | 0.017 (4) | −0.002 (5) | 0.001 (5) | 0.005 (4) |
N2 | 0.031 (5) | 0.053 (8) | 0.036 (6) | −0.008 (5) | 0.007 (4) | −0.007 (5) |
N3 | 0.030 (5) | 0.061 (8) | 0.023 (5) | −0.004 (6) | 0.007 (4) | 0.000 (4) |
N4 | 0.037 (6) | 0.051 (8) | 0.036 (6) | 0.006 (6) | −0.001 (5) | 0.006 (6) |
H1 | 0.12 (3) | 0.05 (3) | 0.10 (3) | −0.04 (3) | 0.01 (2) | 0.00 (2) |
H2 | 0.10 (3) | 0.07 (3) | 0.07 (2) | −0.013 (19) | 0.000 (19) | 0.007 (18) |
H3 | 0.033 (16) | 0.08 (3) | 0.06 (2) | −0.024 (14) | −0.007 (13) | 0.003 (16) |
H4 | 0.057 (8) | 0.041 (10) | 0.032 (6) | 0.003 (7) | −0.003 (7) | 0.018 (7) |
Geometric parameters (Å, º) top
C1—N2 | 1.31 (2) | C6—N3 | 1.146 (12) |
C1—C2 | 1.40 (2) | C6—Ag1 | 2.083 (15) |
C1—H1 | 1.14 (5) | Ag1—C5ii | 2.056 (17) |
C2—C4 | 1.40 (2) | Ag1—N2iii | 2.621 (15) |
C2—H2 | 1.12 (5) | Ag1—Ag1iv | 3.05 (3) |
C3—N2 | 1.334 (17) | Fe1—N4 | 2.130 (10) |
C3—N1 | 1.353 (17) | Fe1—N4v | 2.130 (10) |
C3—H3 | 1.13 (4) | Fe1—N3 | 2.145 (9) |
C4—N1 | 1.359 (16) | Fe1—N3v | 2.145 (9) |
C4—H4 | 1.06 (5) | Fe1—N1v | 2.252 (10) |
C5—N4 | 1.157 (14) | Fe1—N1 | 2.252 (10) |
C5—Ag1i | 2.056 (17) | N2—Ag1vi | 2.621 (15) |
| | | |
N2—C1—C2 | 122.1 (16) | N4v—Fe1—N3 | 90.4 (3) |
N2—C1—H1 | 117 (2) | N4—Fe1—N3v | 90.4 (3) |
C2—C1—H1 | 120 (2) | N4v—Fe1—N3v | 89.6 (3) |
C1—C2—C4 | 115.6 (15) | N3—Fe1—N3v | 180.000 (2) |
C1—C2—H2 | 122 (2) | N4—Fe1—N1v | 90.2 (4) |
C4—C2—H2 | 122 (2) | N4v—Fe1—N1v | 89.8 (4) |
N2—C3—N1 | 125.8 (12) | N3—Fe1—N1v | 88.0 (4) |
N2—C3—H3 | 121.8 (17) | N3v—Fe1—N1v | 92.0 (4) |
N1—C3—H3 | 112.3 (18) | N4—Fe1—N1 | 89.8 (4) |
N1—C4—C2 | 123.1 (15) | N4v—Fe1—N1 | 90.2 (4) |
N1—C4—H4 | 113.9 (18) | N3—Fe1—N1 | 92.0 (4) |
C2—C4—H4 | 123.0 (16) | N3v—Fe1—N1 | 88.0 (4) |
N4—C5—Ag1i | 177.7 (14) | N1v—Fe1—N1 | 180.0000 (10) |
N3—C6—Ag1 | 177.0 (11) | C3—N1—C4 | 114.8 (13) |
C5ii—Ag1—C6 | 162.7 (8) | C3—N1—Fe1 | 122.2 (9) |
C5ii—Ag1—N2iii | 92.9 (6) | C4—N1—Fe1 | 122.8 (10) |
C6—Ag1—N2iii | 100.9 (6) | C1—N2—C3 | 118.4 (12) |
C5ii—Ag1—Ag1iv | 71.1 (6) | C1—N2—Ag1vi | 123.5 (11) |
C6—Ag1—Ag1iv | 109.1 (7) | C3—N2—Ag1vi | 117.8 (8) |
N2iii—Ag1—Ag1iv | 122.8 (5) | C6—N3—Fe1 | 161.1 (11) |
N4—Fe1—N4v | 180.000 (3) | C5—N4—Fe1 | 168.9 (12) |
N4—Fe1—N3 | 89.6 (3) | | |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) −x+1/2, y, z+1/2; (iii) −x+1, y−1/2, −z+5/2; (iv) −x+1/2, −y+1/2, z; (v) −x+1, −y, −z+2; (vi) −x+1, y+1/2, −z+5/2. |
Crystal data top
C12H8Ag2FeN8 | Z = 4 |
Mr = 535.83 | F(000) = 584 |
Orthorhombic, Pccn | Dx = 2.056 Mg m−3 |
Hall symbol: -P 2ab 2ac | Neutron radiation, λ = 0.90-3.00 Å |
a = 15.782 (3) Å | µ = 0.09 mm−1 |
b = 8.235 (3) Å | T = 240 K |
c = 13.319 (3) Å | Prism, orange-yellow |
V = 1731.0 (8) Å3 | 1.0 × 0.6 × 0.5 mm |
Data collection top
ILL-VIVALDI Laue single xtal diffractometer | Rint = 0.267 |
Radiation source: ILL neutron source | θmax = 29.3°, θmin = 4.0° |
3616 measured reflections | h = −17→11 |
788 independent reflections | k = −8→8 |
641 reflections with I > 2σ(I) | l = −14→13 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.128 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.207 | All H-atom parameters refined |
S = 1.28 | w = 1/[σ2(Fo2) + (0.0724P)2 + 8.3726P] where P = (Fo2 + 2Fc2)/3 |
788 reflections | (Δ/σ)max < 0.001 |
142 parameters | Δρmax = 0.62 e Å−3 |
0 restraints | Δρmin = −0.58 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
C1 | 0.6297 (6) | 0.5398 (14) | 0.9508 (7) | 0.045 (2) | |
C2 | 0.5869 (6) | 0.4671 (12) | 0.8703 (7) | 0.041 (2) | |
C3 | 0.5932 (5) | 0.3246 (11) | 1.0485 (6) | 0.034 (2) | |
C4 | 0.5496 (5) | 0.3200 (12) | 0.8861 (7) | 0.041 (2) | |
C5 | 0.3268 (5) | 0.0757 (10) | 0.8742 (5) | 0.0335 (19) | |
C6 | 0.3858 (4) | 0.0805 (11) | 1.1973 (5) | 0.032 (2) | |
Ag1 | 0.2915 (4) | 0.0843 (11) | 1.3041 (6) | 0.034 (2) | |
Fe1 | 0.5000 | 0.0000 | 1.0000 | 0.022 (2) | |
N1 | 0.5530 (4) | 0.2461 (7) | 0.9759 (4) | 0.0312 (15) | |
N2 | 0.6307 (4) | 0.4688 (9) | 1.0403 (5) | 0.0429 (17) | |
N3 | 0.4359 (3) | 0.0709 (8) | 1.1342 (4) | 0.0364 (16) | |
N4 | 0.3907 (3) | 0.0604 (8) | 0.9147 (4) | 0.0352 (15) | |
H1 | 0.6609 (16) | 0.655 (3) | 0.9432 (16) | 0.084 (7) | |
H2 | 0.5845 (15) | 0.528 (3) | 0.793 (2) | 0.088 (7) | |
H3 | 0.5947 (13) | 0.265 (2) | 1.1221 (14) | 0.070 (6) | |
H4 | 0.5157 (14) | 0.258 (2) | 0.8279 (15) | 0.060 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.059 (6) | 0.030 (6) | 0.047 (6) | −0.010 (5) | 0.000 (4) | 0.004 (5) |
C2 | 0.064 (6) | 0.023 (5) | 0.035 (6) | −0.010 (4) | −0.004 (4) | 0.008 (4) |
C3 | 0.042 (4) | 0.040 (6) | 0.020 (5) | −0.012 (4) | −0.010 (3) | 0.002 (5) |
C4 | 0.053 (5) | 0.039 (6) | 0.032 (5) | 0.002 (5) | −0.002 (4) | 0.000 (5) |
C5 | 0.030 (4) | 0.038 (6) | 0.033 (4) | 0.002 (4) | −0.010 (3) | 0.001 (4) |
C6 | 0.030 (4) | 0.043 (6) | 0.024 (4) | 0.007 (3) | 0.010 (3) | 0.000 (3) |
Ag1 | 0.025 (4) | 0.041 (7) | 0.036 (5) | 0.005 (4) | 0.008 (3) | 0.009 (4) |
Fe1 | 0.021 (5) | 0.031 (7) | 0.015 (4) | 0.000 (3) | 0.002 (2) | 0.005 (3) |
N1 | 0.036 (3) | 0.037 (4) | 0.021 (3) | −0.007 (3) | −0.003 (2) | 0.005 (2) |
N2 | 0.050 (4) | 0.039 (4) | 0.039 (4) | −0.014 (3) | −0.003 (3) | −0.006 (3) |
N3 | 0.031 (3) | 0.050 (5) | 0.027 (3) | 0.001 (3) | 0.009 (2) | −0.003 (3) |
N4 | 0.034 (3) | 0.040 (4) | 0.032 (3) | 0.000 (3) | −0.004 (3) | 0.004 (3) |
H1 | 0.131 (19) | 0.064 (17) | 0.058 (14) | −0.040 (16) | 0.015 (11) | −0.006 (11) |
H2 | 0.108 (17) | 0.077 (16) | 0.079 (17) | −0.015 (12) | −0.005 (13) | 0.036 (14) |
H3 | 0.105 (16) | 0.079 (16) | 0.025 (10) | −0.025 (11) | −0.016 (8) | 0.021 (9) |
H4 | 0.113 (15) | 0.029 (12) | 0.038 (11) | −0.014 (9) | −0.029 (10) | 0.018 (8) |
Geometric parameters (Å, º) top
C1—N2 | 1.328 (13) | C6—N3 | 1.157 (8) |
C1—C2 | 1.402 (13) | C6—Ag1 | 2.059 (10) |
C1—H1 | 1.07 (3) | Ag1—C5ii | 2.088 (10) |
C2—C4 | 1.364 (14) | Ag1—N2iii | 2.590 (10) |
C2—H2 | 1.15 (3) | Ag1—Ag1iv | 3.026 (18) |
C3—N1 | 1.325 (10) | Fe1—N4v | 2.125 (6) |
C3—N2 | 1.331 (10) | Fe1—N4 | 2.125 (6) |
C3—H3 | 1.10 (2) | Fe1—N3v | 2.135 (5) |
C4—N1 | 1.342 (11) | Fe1—N3 | 2.135 (5) |
C4—H4 | 1.07 (3) | Fe1—N1v | 2.216 (5) |
C5—N4 | 1.150 (9) | Fe1—N1 | 2.216 (5) |
C5—Ag1i | 2.088 (10) | N2—Ag1vi | 2.590 (10) |
| | | |
N2—C1—C2 | 120.3 (10) | N4—Fe1—N3v | 90.07 (19) |
N2—C1—H1 | 117.9 (15) | N4v—Fe1—N3 | 90.07 (19) |
C2—C1—H1 | 121.7 (15) | N4—Fe1—N3 | 89.93 (19) |
C4—C2—C1 | 118.0 (9) | N3v—Fe1—N3 | 180.0000 (10) |
C4—C2—H2 | 120.9 (15) | N4v—Fe1—N1v | 90.9 (2) |
C1—C2—H2 | 121.2 (15) | N4—Fe1—N1v | 89.1 (2) |
N1—C3—N2 | 126.1 (7) | N3v—Fe1—N1v | 92.9 (2) |
N1—C3—H3 | 116.4 (12) | N3—Fe1—N1v | 87.1 (2) |
N2—C3—H3 | 117.6 (12) | N4v—Fe1—N1 | 89.1 (2) |
N1—C4—C2 | 121.5 (9) | N4—Fe1—N1 | 90.9 (2) |
N1—C4—H4 | 116.7 (12) | N3v—Fe1—N1 | 87.1 (2) |
C2—C4—H4 | 121.7 (11) | N3—Fe1—N1 | 92.9 (2) |
N4—C5—Ag1i | 175.3 (8) | N1v—Fe1—N1 | 180.0000 (10) |
N3—C6—Ag1 | 175.7 (8) | C3—N1—C4 | 116.6 (7) |
C6—Ag1—C5ii | 162.6 (5) | C3—N1—Fe1 | 121.4 (5) |
C6—Ag1—N2iii | 101.8 (4) | C4—N1—Fe1 | 121.9 (6) |
C5ii—Ag1—N2iii | 93.1 (4) | C1—N2—C3 | 117.4 (8) |
C6—Ag1—Ag1iv | 109.1 (4) | C1—N2—Ag1vi | 124.2 (7) |
C5ii—Ag1—Ag1iv | 69.1 (3) | C3—N2—Ag1vi | 118.3 (5) |
N2iii—Ag1—Ag1iv | 122.5 (3) | C6—N3—Fe1 | 161.9 (6) |
N4v—Fe1—N4 | 180.0000 (10) | C5—N4—Fe1 | 171.2 (7) |
N4v—Fe1—N3v | 89.93 (19) | | |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) −x+1/2, y, z+1/2; (iii) −x+1, y−1/2, −z+5/2; (iv) −x+1/2, −y+1/2, z; (v) −x+1, −y, −z+2; (vi) −x+1, y+1/2, −z+5/2. |
Crystal data top
C12H8Ag2FeN8 | Z = 4 |
Mr = 535.83 | F(000) = 584 |
Orthorhombic, Pccn | Dx = 2.048 Mg m−3 |
Hall symbol: -P 2ab 2ac | Neutron radiation, λ = 0.90-3.00 Å |
a = 15.780 (3) Å | µ = 0.08 mm−1 |
b = 8.250 (3) Å | T = 260 K |
c = 13.350 (3) Å | Prism, orange-yellow |
V = 1738.0 (8) Å3 | 1.0 × 0.6 × 0.5 mm |
Data collection top
ILL-VIVALDI Laue single xtal diffractometer | Rint = 0.185 |
Radiation source: ILL neutron source | θmax = 30.0°, θmin = 3.1° |
5945 measured reflections | h = −11→19 |
1291 independent reflections | k = −10→8 |
978 reflections with I > 2σ(I) | l = −14→16 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.079 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.155 | All H-atom parameters refined |
S = 1.16 | w = 1/[σ2(Fo2) + (0.0716P)2] where P = (Fo2 + 2Fc2)/3 |
1291 reflections | (Δ/σ)max < 0.001 |
142 parameters | Δρmax = 0.51 e Å−3 |
0 restraints | Δρmin = −0.56 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
C1 | 0.6286 (3) | 0.5387 (5) | 0.9507 (3) | 0.0471 (9) | |
C2 | 0.5875 (2) | 0.4688 (5) | 0.8702 (3) | 0.0480 (10) | |
C3 | 0.59351 (19) | 0.3249 (4) | 1.0487 (2) | 0.0374 (8) | |
C4 | 0.5498 (2) | 0.3205 (4) | 0.8869 (3) | 0.0384 (8) | |
C5 | 0.32727 (16) | 0.0750 (4) | 0.8729 (2) | 0.0356 (8) | |
C6 | 0.38492 (18) | 0.0786 (4) | 1.1965 (2) | 0.0358 (8) | |
Ag1 | 0.29081 (19) | 0.0830 (4) | 1.3049 (3) | 0.0372 (9) | |
Fe1 | 0.5000 | 0.0000 | 1.0000 | 0.0231 (8) | |
N1 | 0.55374 (14) | 0.2462 (3) | 0.97579 (19) | 0.0322 (6) | |
N2 | 0.63144 (17) | 0.4672 (3) | 1.0406 (2) | 0.0452 (7) | |
N3 | 0.43561 (13) | 0.0713 (3) | 1.13422 (17) | 0.0375 (6) | |
N4 | 0.39103 (12) | 0.0615 (3) | 0.91522 (17) | 0.0353 (6) | |
H1 | 0.6603 (6) | 0.6569 (12) | 0.9466 (8) | 0.085 (3) | |
H2 | 0.5851 (7) | 0.5267 (12) | 0.7998 (9) | 0.085 (3) | |
H3 | 0.5952 (6) | 0.2641 (10) | 1.1219 (6) | 0.070 (3) | |
H4 | 0.5149 (6) | 0.2582 (9) | 0.8289 (7) | 0.067 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.057 (2) | 0.042 (2) | 0.042 (2) | −0.0141 (18) | 0.0019 (16) | 0.0039 (19) |
C2 | 0.058 (2) | 0.048 (2) | 0.038 (2) | −0.0088 (17) | 0.0010 (16) | 0.0085 (19) |
C3 | 0.0419 (16) | 0.043 (2) | 0.028 (2) | −0.0089 (15) | −0.0037 (13) | 0.0024 (16) |
C4 | 0.0452 (17) | 0.041 (2) | 0.0287 (18) | −0.0040 (15) | −0.0033 (14) | 0.0037 (16) |
C5 | 0.0246 (14) | 0.051 (2) | 0.0317 (18) | 0.0005 (14) | −0.0081 (11) | 0.0043 (15) |
C6 | 0.0302 (14) | 0.045 (2) | 0.0322 (19) | 0.0034 (14) | 0.0110 (12) | −0.0023 (14) |
Ag1 | 0.0292 (15) | 0.044 (2) | 0.039 (2) | 0.0074 (15) | 0.0145 (14) | 0.0045 (17) |
Fe1 | 0.0148 (13) | 0.035 (2) | 0.020 (2) | −0.0013 (10) | 0.0016 (8) | 0.0005 (11) |
N1 | 0.0310 (11) | 0.0395 (16) | 0.0261 (11) | −0.0050 (8) | −0.0015 (10) | 0.0005 (10) |
N2 | 0.0512 (15) | 0.0466 (16) | 0.0377 (17) | −0.0155 (12) | −0.0040 (11) | −0.0013 (12) |
N3 | 0.0326 (11) | 0.0504 (17) | 0.0295 (13) | 0.0019 (11) | 0.0114 (9) | −0.0019 (11) |
N4 | 0.0230 (10) | 0.0483 (15) | 0.0345 (13) | 0.0021 (10) | −0.0084 (9) | 0.0038 (11) |
H1 | 0.102 (6) | 0.066 (6) | 0.086 (7) | −0.039 (6) | −0.001 (5) | 0.009 (5) |
H2 | 0.115 (8) | 0.079 (7) | 0.062 (7) | −0.011 (5) | 0.001 (5) | 0.022 (5) |
H3 | 0.109 (7) | 0.071 (6) | 0.030 (4) | −0.031 (5) | −0.014 (4) | 0.017 (4) |
H4 | 0.088 (5) | 0.062 (6) | 0.050 (5) | −0.024 (4) | −0.026 (4) | 0.004 (4) |
Geometric parameters (Å, º) top
C1—N2 | 1.338 (5) | C6—N3 | 1.156 (4) |
C1—C2 | 1.382 (6) | C6—Ag1 | 2.073 (4) |
C1—H1 | 1.097 (10) | Ag1—C5ii | 2.074 (4) |
C2—C4 | 1.378 (6) | Ag1—N2iii | 2.583 (4) |
C2—H2 | 1.055 (13) | Ag1—Ag1iv | 3.042 (7) |
C3—N2 | 1.323 (4) | Fe1—N4v | 2.120 (2) |
C3—N1 | 1.328 (4) | Fe1—N4 | 2.120 (2) |
C3—H3 | 1.098 (9) | Fe1—N3v | 2.142 (2) |
C4—N1 | 1.337 (4) | Fe1—N3 | 2.142 (2) |
C4—H4 | 1.080 (9) | Fe1—N1 | 2.225 (2) |
C5—N4 | 1.159 (3) | Fe1—N1v | 2.225 (2) |
C5—Ag1i | 2.074 (4) | N2—Ag1vi | 2.583 (4) |
| | | |
N2—C1—C2 | 121.9 (4) | N4—Fe1—N3v | 90.22 (9) |
N2—C1—H1 | 115.0 (7) | N4v—Fe1—N3 | 90.22 (9) |
C2—C1—H1 | 123.1 (7) | N4—Fe1—N3 | 89.78 (9) |
C4—C2—C1 | 116.6 (4) | N3v—Fe1—N3 | 180.0000 (10) |
C4—C2—H2 | 122.0 (7) | N4v—Fe1—N1 | 89.25 (9) |
C1—C2—H2 | 121.4 (7) | N4—Fe1—N1 | 90.75 (9) |
N2—C3—N1 | 126.0 (3) | N3v—Fe1—N1 | 87.04 (10) |
N2—C3—H3 | 117.9 (5) | N3—Fe1—N1 | 92.96 (10) |
N1—C3—H3 | 116.1 (5) | N4v—Fe1—N1v | 90.75 (9) |
N1—C4—C2 | 122.0 (3) | N4—Fe1—N1v | 89.25 (9) |
N1—C4—H4 | 116.2 (5) | N3v—Fe1—N1v | 92.96 (10) |
C2—C4—H4 | 121.8 (5) | N3—Fe1—N1v | 87.04 (10) |
N4—C5—Ag1i | 175.0 (3) | N1—Fe1—N1v | 180.0 |
N3—C6—Ag1 | 177.3 (3) | C3—N1—C4 | 116.7 (3) |
C6—Ag1—C5ii | 161.5 (2) | C3—N1—Fe1 | 121.3 (2) |
C6—Ag1—N2iii | 102.16 (15) | C4—N1—Fe1 | 122.0 (2) |
C5ii—Ag1—N2iii | 93.74 (16) | C3—N2—C1 | 116.8 (3) |
C6—Ag1—Ag1iv | 108.60 (17) | C3—N2—Ag1vi | 118.5 (2) |
C5ii—Ag1—Ag1iv | 69.41 (15) | C1—N2—Ag1vi | 124.7 (3) |
N2iii—Ag1—Ag1iv | 122.41 (12) | C6—N3—Fe1 | 160.9 (2) |
N4v—Fe1—N4 | 180.0 | C5—N4—Fe1 | 170.8 (3) |
N4v—Fe1—N3v | 89.78 (9) | | |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) −x+1/2, y, z+1/2; (iii) −x+1, y−1/2, −z+5/2; (iv) −x+1/2, −y+1/2, z; (v) −x+1, −y, −z+2; (vi) −x+1, y+1/2, −z+5/2. |
Crystal data top
C12H8Ag2FeN8 | Z = 4 |
Mr = 535.83 | F(000) = 584 |
Orthorhombic, Pccn | Dx = 2.214 Mg m−3 |
Hall symbol: -P 2ab 2ac | Neutron radiation, λ = 0.90-3.00 Å |
a = 14.895 (3) Å | µ = 0.09 mm−1 |
b = 8.125 (3) Å | T = 200 K |
c = 13.286 (3) Å | Prism, orange-yellow |
V = 1607.9 (8) Å3 | 1.0 × 0.6 × 0.5 mm |
Data collection top
ILL-VIVALDI Laue single xtal diffractometer | Rint = 0.366 |
Radiation source: ILL neutron source | θmax = 30.9°, θmin = 4.0° |
4785 measured reflections | h = −11→17 |
991 independent reflections | k = −9→9 |
735 reflections with I > 2σ(I) | l = −15→14 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.172 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.337 | All H-atom parameters refined |
S = 1.36 | w = 1/[σ2(Fo2) + (0.1301P)2 + 25.1243P] where P = (Fo2 + 2Fc2)/3 |
991 reflections | (Δ/σ)max < 0.001 |
142 parameters | Δρmax = 1.05 e Å−3 |
0 restraints | Δρmin = −0.88 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
N3 | 0.6048 (4) | 0.0531 (11) | 0.0781 (5) | 0.0229 (18) | |
N4 | 0.5640 (4) | 0.0670 (10) | −0.1198 (4) | 0.0234 (18) | |
N2 | 0.3751 (5) | 0.4576 (12) | −0.0434 (5) | 0.030 (2) | |
N1 | 0.4508 (5) | 0.2259 (10) | 0.0222 (5) | 0.0226 (19) | |
C1 | 0.6111 (6) | 0.0859 (13) | −0.1884 (7) | 0.024 (2) | |
Ag1 | 0.7059 (7) | 0.0869 (15) | −0.3036 (7) | 0.025 (3) | |
C2 | 0.6704 (6) | 0.0729 (14) | 0.1241 (6) | 0.024 (2) | |
C5 | 0.4107 (7) | 0.4509 (15) | 0.1293 (8) | 0.029 (3) | |
C3 | 0.4125 (6) | 0.3112 (14) | −0.0531 (6) | 0.021 (2) | |
Fe1 | 0.5000 | 0.0000 | 0.0000 | 0.016 (3) | |
C6 | 0.4513 (6) | 0.2986 (15) | 0.1133 (7) | 0.025 (3) | |
C4 | 0.3704 (9) | 0.5225 (18) | 0.0466 (8) | 0.037 (3) | |
H5 | 0.4070 (17) | 0.503 (3) | 0.2006 (16) | 0.049 (7) | |
H3 | 0.4167 (14) | 0.257 (2) | −0.1281 (14) | 0.035 (6) | |
H6 | 0.4848 (16) | 0.236 (2) | 0.1755 (16) | 0.040 (6) | |
H4 | 0.3363 (18) | 0.641 (4) | 0.0529 (16) | 0.067 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
N3 | 0.017 (3) | 0.032 (5) | 0.020 (4) | 0.002 (3) | −0.003 (3) | −0.003 (3) |
N4 | 0.024 (3) | 0.032 (5) | 0.014 (3) | −0.005 (3) | 0.006 (3) | 0.005 (3) |
N2 | 0.040 (4) | 0.038 (5) | 0.013 (4) | 0.012 (4) | −0.002 (3) | 0.007 (3) |
N1 | 0.026 (4) | 0.032 (5) | 0.010 (3) | 0.002 (3) | 0.000 (3) | −0.001 (3) |
C1 | 0.028 (5) | 0.033 (7) | 0.012 (4) | −0.002 (4) | 0.008 (4) | 0.008 (4) |
Ag1 | 0.022 (5) | 0.039 (9) | 0.014 (5) | −0.002 (5) | 0.006 (4) | −0.006 (5) |
C2 | 0.025 (5) | 0.033 (7) | 0.013 (4) | 0.011 (4) | −0.001 (4) | 0.005 (4) |
C5 | 0.045 (6) | 0.024 (7) | 0.018 (6) | 0.007 (5) | 0.000 (4) | −0.005 (5) |
C3 | 0.030 (5) | 0.020 (7) | 0.015 (6) | 0.011 (5) | −0.001 (4) | 0.001 (4) |
Fe1 | 0.015 (5) | 0.015 (8) | 0.017 (5) | 0.008 (4) | −0.005 (3) | 0.000 (3) |
C6 | 0.030 (5) | 0.031 (7) | 0.014 (5) | 0.007 (5) | −0.001 (4) | −0.007 (5) |
C4 | 0.051 (8) | 0.044 (9) | 0.016 (6) | 0.006 (6) | −0.007 (5) | −0.001 (5) |
H5 | 0.068 (15) | 0.06 (2) | 0.019 (12) | 0.014 (12) | 0.010 (9) | −0.005 (10) |
H3 | 0.061 (14) | 0.038 (15) | 0.007 (10) | 0.012 (10) | −0.004 (8) | 0.003 (7) |
H6 | 0.071 (15) | 0.019 (15) | 0.031 (13) | 0.022 (10) | −0.013 (10) | 0.003 (8) |
H4 | 0.080 (17) | 0.09 (2) | 0.035 (13) | 0.057 (18) | 0.002 (11) | −0.023 (12) |
Geometric parameters (Å, º) top
N3—C2 | 1.165 (11) | Ag1—N2iii | 2.587 (12) |
N3—Fe1 | 1.923 (6) | Ag1—Ag1iv | 2.96 (2) |
N4—C1 | 1.160 (11) | C2—Ag1v | 2.080 (13) |
N4—Fe1 | 1.934 (6) | C5—C4 | 1.381 (16) |
N2—C4 | 1.309 (16) | C5—C6 | 1.393 (16) |
N2—C3 | 1.320 (14) | C5—H5 | 1.04 (3) |
N2—Ag1i | 2.587 (12) | C3—H3 | 1.09 (2) |
N1—C3 | 1.344 (12) | Fe1—N3vi | 1.923 (6) |
N1—C6 | 1.347 (12) | Fe1—N4vi | 1.934 (6) |
N1—Fe1 | 1.998 (8) | Fe1—N1vi | 1.998 (8) |
C1—Ag1 | 2.083 (12) | C6—H6 | 1.09 (2) |
Ag1—C2ii | 2.080 (13) | C4—H4 | 1.09 (4) |
| | | |
C2—N3—Fe1 | 174.7 (8) | N3—Fe1—N3vi | 180.0 (4) |
C1—N4—Fe1 | 169.1 (8) | N3—Fe1—N4 | 88.9 (3) |
C4—N2—C3 | 118.4 (9) | N3vi—Fe1—N4 | 91.1 (3) |
C4—N2—Ag1i | 121.9 (9) | N3—Fe1—N4vi | 91.1 (3) |
C3—N2—Ag1i | 119.1 (6) | N3vi—Fe1—N4vi | 88.9 (3) |
C3—N1—C6 | 116.4 (9) | N4—Fe1—N4vi | 180.0 (6) |
C3—N1—Fe1 | 121.3 (6) | N3—Fe1—N1 | 90.7 (3) |
C6—N1—Fe1 | 122.3 (7) | N3vi—Fe1—N1 | 89.3 (3) |
N4—C1—Ag1 | 171.0 (9) | N4—Fe1—N1 | 92.5 (3) |
C2ii—Ag1—C1 | 160.0 (6) | N4vi—Fe1—N1 | 87.5 (3) |
C2ii—Ag1—N2iii | 91.6 (4) | N3—Fe1—N1vi | 89.3 (3) |
C1—Ag1—N2iii | 105.1 (5) | N3vi—Fe1—N1vi | 90.7 (3) |
C2ii—Ag1—Ag1iv | 69.9 (5) | N4—Fe1—N1vi | 87.5 (3) |
C1—Ag1—Ag1iv | 107.7 (5) | N4vi—Fe1—N1vi | 92.5 (3) |
N2iii—Ag1—Ag1iv | 124.8 (4) | N1—Fe1—N1vi | 180.0 (5) |
N3—C2—Ag1v | 173.5 (9) | N1—C6—C5 | 121.6 (9) |
C4—C5—C6 | 116.2 (10) | N1—C6—H6 | 118.5 (14) |
C4—C5—H5 | 121.9 (17) | C5—C6—H6 | 119.9 (13) |
C6—C5—H5 | 121.7 (16) | N2—C4—C5 | 122.2 (13) |
N2—C3—N1 | 124.9 (8) | N2—C4—H4 | 116.8 (16) |
N2—C3—H3 | 118.6 (13) | C5—C4—H4 | 120.8 (16) |
N1—C3—H3 | 116.5 (14) | | |
Symmetry codes: (i) −x+1, y+1/2, −z−1/2; (ii) −x+3/2, y, z−1/2; (iii) −x+1, y−1/2, −z−1/2; (iv) −x+3/2, −y+1/2, z; (v) −x+3/2, y, z+1/2; (vi) −x+1, −y, −z. |
Crystal data top
C12H8Ag2FeN8 | Z = 4 |
Mr = 535.83 | F(000) = 584 |
Orthorhombic, Pccn | Dx = 2.055 Mg m−3 |
Hall symbol: -P 2ab 2ac | Neutron radiation, λ = 0.90-3.00 Å |
a = 15.782 (3) Å | µ = 0.09 mm−1 |
b = 8.235 (3) Å | T = 250 K |
c = 13.325 (3) Å | Prism, orange-yellow |
V = 1731.8 (8) Å3 | 1.0 × 0.6 × 0.5 mm |
Data collection top
ILL-VIVALDI Laue single xtal diffractometer | Rint = 0.378 |
Radiation source: ILL neutron source | θmax = 31.1°, θmin = 4.3° |
2764 measured reflections | h = −17→10 |
661 independent reflections | k = −8→8 |
600 reflections with I > 2σ(I) | l = −14→13 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.192 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.346 | All H-atom parameters refined |
S = 1.54 | w = 1/[σ2(Fo2) + (0.0553P)2 + 130.1284P] where P = (Fo2 + 2Fc2)/3 |
661 reflections | (Δ/σ)max < 0.001 |
142 parameters | Δρmax = 0.79 e Å−3 |
0 restraints | Δρmin = −0.75 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
C1 | 0.6307 (15) | 0.545 (3) | 0.9491 (15) | 0.048 (5) | |
C2 | 0.5871 (11) | 0.470 (2) | 0.8693 (15) | 0.037 (5) | |
C3 | 0.5949 (10) | 0.325 (2) | 1.0500 (11) | 0.037 (5) | |
C4 | 0.5489 (12) | 0.320 (3) | 0.8849 (15) | 0.041 (5) | |
C5 | 0.3278 (10) | 0.077 (2) | 0.8743 (11) | 0.034 (4) | |
C6 | 0.3878 (10) | 0.083 (2) | 1.1957 (10) | 0.031 (4) | |
Ag1 | 0.2901 (11) | 0.087 (2) | 1.3045 (11) | 0.031 (5) | |
Fe1 | 0.5000 | 0.0000 | 1.0000 | 0.019 (5) | |
N1 | 0.5525 (8) | 0.2448 (13) | 0.9752 (9) | 0.026 (3) | |
N2 | 0.6311 (9) | 0.4681 (17) | 1.0401 (9) | 0.041 (4) | |
N3 | 0.4369 (7) | 0.0673 (17) | 1.1340 (8) | 0.035 (3) | |
N4 | 0.3907 (8) | 0.0590 (17) | 0.9138 (8) | 0.035 (3) | |
H1 | 0.660 (3) | 0.650 (8) | 0.946 (3) | 0.089 (18) | |
H2 | 0.593 (3) | 0.521 (6) | 0.794 (4) | 0.083 (14) | |
H3 | 0.592 (2) | 0.264 (5) | 1.123 (3) | 0.059 (11) | |
H4 | 0.518 (3) | 0.261 (4) | 0.828 (3) | 0.049 (10) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.062 (14) | 0.046 (13) | 0.037 (12) | −0.017 (12) | 0.001 (10) | 0.005 (12) |
C2 | 0.041 (11) | 0.029 (11) | 0.040 (13) | −0.009 (9) | −0.002 (8) | 0.018 (8) |
C3 | 0.042 (10) | 0.056 (13) | 0.013 (10) | −0.029 (10) | −0.015 (6) | 0.010 (8) |
C4 | 0.033 (10) | 0.059 (15) | 0.030 (10) | 0.020 (10) | 0.005 (8) | 0.016 (11) |
C5 | 0.021 (8) | 0.042 (12) | 0.037 (9) | 0.011 (8) | −0.018 (7) | −0.002 (8) |
C6 | 0.037 (9) | 0.035 (11) | 0.020 (8) | 0.003 (8) | 0.002 (7) | −0.002 (7) |
Ag1 | 0.030 (9) | 0.040 (14) | 0.024 (8) | 0.007 (8) | 0.004 (7) | 0.009 (8) |
Fe1 | 0.032 (11) | 0.019 (13) | 0.006 (8) | −0.004 (6) | 0.006 (5) | −0.002 (5) |
N1 | 0.025 (6) | 0.030 (7) | 0.024 (5) | −0.009 (5) | 0.000 (5) | −0.001 (5) |
N2 | 0.048 (8) | 0.042 (9) | 0.032 (8) | −0.013 (7) | 0.005 (6) | −0.011 (6) |
N3 | 0.025 (6) | 0.055 (9) | 0.024 (7) | −0.005 (7) | 0.021 (5) | −0.007 (5) |
N4 | 0.030 (7) | 0.042 (8) | 0.032 (7) | 0.001 (7) | −0.008 (5) | 0.013 (6) |
H1 | 0.12 (4) | 0.10 (4) | 0.04 (3) | −0.07 (4) | 0.02 (2) | 0.00 (3) |
H2 | 0.09 (3) | 0.10 (4) | 0.06 (3) | −0.01 (3) | 0.01 (2) | 0.01 (3) |
H3 | 0.06 (3) | 0.08 (3) | 0.03 (2) | −0.01 (2) | −0.020 (16) | 0.013 (19) |
H4 | 0.09 (3) | 0.012 (19) | 0.04 (2) | −0.019 (18) | −0.02 (2) | 0.016 (15) |
Geometric parameters (Å, º) top
C1—N2 | 1.37 (3) | C6—N3 | 1.137 (18) |
C1—C2 | 1.41 (3) | C6—Ag1 | 2.12 (2) |
C1—H1 | 0.98 (8) | Ag1—C5ii | 2.08 (2) |
C2—C4 | 1.39 (3) | Ag1—N2iii | 2.61 (2) |
C2—H2 | 1.09 (6) | Ag1—Ag1iv | 2.97 (4) |
C3—N2 | 1.32 (2) | Fe1—N3v | 2.119 (10) |
C3—N1 | 1.37 (2) | Fe1—N3 | 2.119 (10) |
C3—H3 | 1.10 (4) | Fe1—N4v | 2.128 (11) |
C4—N1 | 1.35 (2) | Fe1—N4 | 2.128 (11) |
C4—H4 | 1.02 (6) | Fe1—N1v | 2.205 (11) |
C5—N4 | 1.135 (18) | Fe1—N1 | 2.205 (11) |
C5—Ag1i | 2.08 (2) | N2—Ag1vi | 2.61 (2) |
| | | |
N2—C1—C2 | 118 (2) | N3—Fe1—N4v | 89.2 (4) |
N2—C1—H1 | 116 (3) | N3v—Fe1—N4 | 89.2 (4) |
C2—C1—H1 | 126 (3) | N3—Fe1—N4 | 90.8 (4) |
C4—C2—C1 | 119.1 (18) | N4v—Fe1—N4 | 180.000 (2) |
C4—C2—H2 | 121 (3) | N3v—Fe1—N1v | 93.6 (5) |
C1—C2—H2 | 119 (3) | N3—Fe1—N1v | 86.4 (5) |
N2—C3—N1 | 124.7 (14) | N4v—Fe1—N1v | 90.8 (5) |
N2—C3—H3 | 121 (2) | N4—Fe1—N1v | 89.2 (5) |
N1—C3—H3 | 114 (2) | N3v—Fe1—N1 | 86.4 (5) |
N1—C4—C2 | 121 (2) | N3—Fe1—N1 | 93.6 (5) |
N1—C4—H4 | 118 (3) | N4v—Fe1—N1 | 89.2 (5) |
C2—C4—H4 | 121 (2) | N4—Fe1—N1 | 90.8 (5) |
N4—C5—Ag1i | 174.4 (17) | N1v—Fe1—N1 | 180.0000 (10) |
N3—C6—Ag1 | 173.5 (16) | C4—N1—C3 | 116.6 (16) |
C5ii—Ag1—C6 | 163.1 (10) | C4—N1—Fe1 | 122.3 (14) |
C5ii—Ag1—N2iii | 93.3 (8) | C3—N1—Fe1 | 121.0 (10) |
C6—Ag1—N2iii | 101.0 (8) | C3—N2—C1 | 120.1 (17) |
C5ii—Ag1—Ag1iv | 69.7 (8) | C3—N2—Ag1vi | 117.6 (11) |
C6—Ag1—Ag1iv | 109.0 (9) | C1—N2—Ag1vi | 122.2 (15) |
N2iii—Ag1—Ag1iv | 122.9 (6) | C6—N3—Fe1 | 163.5 (12) |
N3v—Fe1—N3 | 180.000 (3) | C5—N4—Fe1 | 172.1 (13) |
N3v—Fe1—N4v | 90.8 (4) | | |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) −x+1/2, y, z+1/2; (iii) −x+1, y−1/2, −z+5/2; (iv) −x+1/2, −y+1/2, z; (v) −x+1, −y, −z+2; (vi) −x+1, y+1/2, −z+5/2. |
Crystal data top
C12H8Ag2FeN8 | Z = 4 |
Mr = 535.83 | F(000) = 584 |
Orthorhombic, Pccn | Dx = 2.045 Mg m−3 |
Hall symbol: -P 2ab 2ac | Neutron radiation, λ = 0.90-3.00 Å |
a = 15.782 (3) Å | µ = 0.09 mm−1 |
b = 8.262 (3) Å | T = 280 K |
c = 13.350 (3) Å | Prism, orange-yellow |
V = 1740.7 (8) Å3 | 1.0 × 0.6 × 0.5 mm |
Data collection top
ILL-VIVALDI Laue single xtal diffractometer | Rint = 0.300 |
Radiation source: ILL neutron source | θmax = 28.6°, θmin = 3.9° |
3564 measured reflections | h = −17→11 |
797 independent reflections | k = −8→8 |
674 reflections with I > 2σ(I) | l = −14→13 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.169 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.259 | All H-atom parameters refined |
S = 1.51 | w = 1/[σ2(Fo2) + (0.0661P)2 + 21.984P] where P = (Fo2 + 2Fc2)/3 |
797 reflections | (Δ/σ)max < 0.001 |
142 parameters | Δρmax = 0.70 e Å−3 |
0 restraints | Δρmin = −0.57 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
C1 | 0.6308 (9) | 0.5371 (17) | 0.9510 (9) | 0.055 (3) | |
C2 | 0.5872 (7) | 0.4672 (15) | 0.8704 (9) | 0.049 (3) | |
C3 | 0.5940 (6) | 0.3236 (14) | 1.0490 (7) | 0.041 (3) | |
C4 | 0.5495 (7) | 0.3195 (15) | 0.8862 (8) | 0.045 (3) | |
C5 | 0.3278 (6) | 0.0762 (13) | 0.8728 (6) | 0.041 (3) | |
C6 | 0.3858 (6) | 0.0792 (13) | 1.1962 (6) | 0.036 (2) | |
Ag1 | 0.2906 (6) | 0.0842 (14) | 1.3043 (7) | 0.041 (3) | |
Fe1 | 0.5000 | 0.0000 | 1.0000 | 0.026 (3) | |
N1 | 0.5530 (5) | 0.2461 (8) | 0.9762 (5) | 0.0345 (18) | |
N2 | 0.6312 (5) | 0.4680 (10) | 1.0409 (6) | 0.049 (2) | |
N3 | 0.4353 (4) | 0.0700 (10) | 1.1338 (5) | 0.042 (2) | |
N4 | 0.3909 (4) | 0.0606 (10) | 0.9147 (5) | 0.0411 (19) | |
H1 | 0.661 (2) | 0.656 (4) | 0.944 (2) | 0.100 (10) | |
H2 | 0.589 (2) | 0.527 (4) | 0.796 (2) | 0.103 (10) | |
H3 | 0.5930 (16) | 0.265 (3) | 1.1205 (19) | 0.074 (8) | |
H4 | 0.5158 (18) | 0.259 (3) | 0.8274 (19) | 0.067 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.069 (8) | 0.042 (7) | 0.053 (8) | −0.021 (7) | 0.002 (6) | 0.008 (7) |
C2 | 0.057 (7) | 0.050 (8) | 0.041 (7) | −0.013 (6) | −0.002 (5) | 0.011 (5) |
C3 | 0.046 (6) | 0.051 (8) | 0.027 (6) | −0.021 (6) | −0.004 (4) | 0.000 (6) |
C4 | 0.048 (6) | 0.052 (8) | 0.034 (6) | −0.002 (6) | −0.004 (5) | 0.007 (6) |
C5 | 0.030 (5) | 0.053 (7) | 0.039 (5) | 0.004 (5) | −0.011 (4) | 0.003 (5) |
C6 | 0.035 (5) | 0.043 (7) | 0.031 (5) | 0.004 (4) | 0.011 (4) | −0.004 (4) |
Ag1 | 0.029 (5) | 0.053 (8) | 0.042 (6) | 0.005 (5) | 0.011 (4) | 0.009 (5) |
Fe1 | 0.026 (6) | 0.040 (8) | 0.014 (5) | −0.003 (4) | −0.002 (3) | 0.003 (3) |
N1 | 0.037 (4) | 0.041 (5) | 0.025 (3) | −0.008 (3) | −0.001 (3) | 0.003 (3) |
N2 | 0.055 (5) | 0.049 (5) | 0.042 (5) | −0.014 (4) | −0.001 (4) | −0.004 (4) |
N3 | 0.036 (4) | 0.057 (6) | 0.033 (4) | 0.005 (4) | 0.013 (3) | −0.004 (3) |
N4 | 0.031 (4) | 0.051 (5) | 0.041 (4) | 0.000 (4) | −0.007 (3) | 0.004 (4) |
H1 | 0.13 (3) | 0.11 (2) | 0.064 (17) | −0.07 (2) | 0.005 (14) | 0.016 (15) |
H2 | 0.13 (3) | 0.11 (2) | 0.07 (2) | −0.027 (18) | 0.000 (17) | 0.033 (17) |
H3 | 0.083 (19) | 0.09 (2) | 0.047 (14) | −0.031 (14) | −0.014 (11) | 0.020 (13) |
H4 | 0.110 (19) | 0.043 (16) | 0.048 (14) | −0.007 (12) | −0.033 (13) | 0.017 (10) |
Geometric parameters (Å, º) top
C1—N2 | 1.329 (16) | C6—N3 | 1.145 (10) |
C1—C2 | 1.401 (17) | C6—Ag1 | 2.083 (13) |
C1—H1 | 1.10 (4) | Ag1—C5ii | 2.082 (13) |
C2—C4 | 1.375 (17) | Ag1—N2iii | 2.592 (12) |
C2—H2 | 1.11 (3) | Ag1—Ag1iv | 3.02 (2) |
C3—N1 | 1.332 (12) | Fe1—N4 | 2.124 (7) |
C3—N2 | 1.333 (13) | Fe1—N4v | 2.124 (7) |
C3—H3 | 1.07 (3) | Fe1—N3 | 2.138 (6) |
C4—N1 | 1.346 (13) | Fe1—N3v | 2.138 (6) |
C4—H4 | 1.07 (3) | Fe1—N1v | 2.222 (6) |
C5—N4 | 1.150 (11) | Fe1—N1 | 2.222 (7) |
C5—Ag1i | 2.082 (13) | N2—Ag1vi | 2.592 (12) |
| | | |
N2—C1—C2 | 121.2 (12) | N4v—Fe1—N3 | 90.2 (2) |
N2—C1—H1 | 117.3 (19) | N4—Fe1—N3v | 90.2 (2) |
C2—C1—H1 | 121.3 (18) | N4v—Fe1—N3v | 89.8 (2) |
C4—C2—C1 | 117.4 (11) | N3—Fe1—N3v | 180.0000 (10) |
C4—C2—H2 | 122.8 (19) | N4—Fe1—N1v | 89.3 (3) |
C1—C2—H2 | 119 (2) | N4v—Fe1—N1v | 90.7 (3) |
N1—C3—N2 | 125.8 (9) | N3—Fe1—N1v | 87.0 (3) |
N1—C3—H3 | 115.3 (16) | N3v—Fe1—N1v | 93.0 (3) |
N2—C3—H3 | 118.8 (15) | N4—Fe1—N1 | 90.7 (3) |
N1—C4—C2 | 121.3 (10) | N4v—Fe1—N1 | 89.3 (3) |
N1—C4—H4 | 117.6 (15) | N3—Fe1—N1 | 93.0 (3) |
C2—C4—H4 | 121.1 (14) | N3v—Fe1—N1 | 87.0 (3) |
N4—C5—Ag1i | 174.3 (9) | N1v—Fe1—N1 | 180.0000 (10) |
N3—C6—Ag1 | 176.0 (9) | C3—N1—C4 | 117.0 (9) |
C5ii—Ag1—C6 | 162.0 (7) | C3—N1—Fe1 | 121.2 (7) |
C5ii—Ag1—N2iii | 93.7 (5) | C4—N1—Fe1 | 121.6 (7) |
C6—Ag1—N2iii | 101.6 (5) | C1—N2—C3 | 117.1 (10) |
C5ii—Ag1—Ag1iv | 69.4 (5) | C1—N2—Ag1vi | 124.3 (8) |
C6—Ag1—Ag1iv | 108.9 (5) | C3—N2—Ag1vi | 118.4 (6) |
N2iii—Ag1—Ag1iv | 122.5 (4) | C6—N3—Fe1 | 162.2 (7) |
N4—Fe1—N4v | 180.000 (2) | C5—N4—Fe1 | 171.8 (8) |
N4—Fe1—N3 | 89.8 (2) | | |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) −x+1/2, y, z+1/2; (iii) −x+1, y−1/2, −z+5/2; (iv) −x+1/2, −y+1/2, z; (v) −x+1, −y, −z+2; (vi) −x+1, y+1/2, −z+5/2. |
Crystal data top
C12H8Ag2FeN8 | Z = 4 |
Mr = 535.83 | F(000) = 584 |
Orthorhombic, Pccn | Dx = 2.060 Mg m−3 |
Hall symbol: -P 2ab 2ac | Neutron radiation, λ = 1.10-2.50 Å |
a = 15.782 (3) Å | µ = 0.09 mm−1 |
b = 8.229 (3) Å | T = 250 K |
c = 13.304 (3) Å | Prism, orange-yellow |
V = 1727.8 (8) Å3 | 1.0 × 0.6 × 0.5 mm |
Data collection top
ILL-VIVALDI Laue single xtal diffractometer | Rint = 0.242 |
Radiation source: ILL neutron source | θmax = 30.0°, θmin = 3.5° |
2910 measured reflections | h = −17→10 |
772 independent reflections | k = −8→8 |
618 reflections with I > 2σ(I) | l = −14→12 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.155 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.194 | All H-atom parameters refined |
S = 1.45 | w = 1/[σ2(Fo2) + (0.016P)2 + 13.6689P] where P = (Fo2 + 2Fc2)/3 |
772 reflections | (Δ/σ)max < 0.001 |
142 parameters | Δρmax = 0.59 e Å−3 |
0 restraints | Δρmin = −0.68 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
C1 | 0.6292 (9) | 0.5383 (17) | 0.9501 (9) | 0.055 (3) | |
C2 | 0.5870 (7) | 0.4697 (14) | 0.8692 (9) | 0.045 (3) | |
C3 | 0.5938 (6) | 0.3268 (13) | 1.0481 (7) | 0.039 (3) | |
C4 | 0.5497 (7) | 0.3208 (16) | 0.8862 (7) | 0.046 (3) | |
C5 | 0.3275 (6) | 0.0737 (13) | 0.8739 (6) | 0.042 (3) | |
C6 | 0.3859 (6) | 0.0801 (13) | 1.1955 (6) | 0.036 (2) | |
Ag1 | 0.2907 (6) | 0.0847 (14) | 1.3034 (7) | 0.038 (3) | |
Fe1 | 0.5000 | 0.0000 | 1.0000 | 0.029 (3) | |
N1 | 0.5529 (5) | 0.2465 (8) | 0.9760 (5) | 0.0340 (18) | |
N2 | 0.6304 (6) | 0.4701 (10) | 1.0393 (5) | 0.047 (2) | |
N3 | 0.4354 (4) | 0.0681 (10) | 1.1341 (5) | 0.044 (2) | |
N4 | 0.3906 (5) | 0.0606 (10) | 0.9141 (4) | 0.043 (2) | |
H1 | 0.6617 (19) | 0.657 (4) | 0.9412 (19) | 0.100 (10) | |
H2 | 0.5879 (17) | 0.522 (3) | 0.798 (2) | 0.087 (8) | |
H3 | 0.5932 (14) | 0.263 (3) | 1.1249 (15) | 0.065 (7) | |
H4 | 0.5128 (17) | 0.257 (2) | 0.8273 (18) | 0.063 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.076 (9) | 0.045 (8) | 0.043 (7) | −0.005 (7) | 0.001 (6) | 0.001 (7) |
C2 | 0.050 (7) | 0.030 (8) | 0.054 (8) | −0.010 (6) | −0.008 (6) | 0.005 (6) |
C3 | 0.052 (6) | 0.044 (8) | 0.021 (6) | −0.018 (6) | −0.003 (4) | 0.011 (5) |
C4 | 0.048 (7) | 0.060 (9) | 0.029 (6) | 0.007 (7) | −0.006 (5) | 0.007 (6) |
C5 | 0.040 (5) | 0.046 (7) | 0.040 (5) | 0.011 (6) | −0.017 (4) | −0.008 (5) |
C6 | 0.038 (5) | 0.045 (7) | 0.025 (5) | −0.007 (5) | 0.014 (4) | −0.008 (4) |
Ag1 | 0.034 (6) | 0.045 (8) | 0.036 (6) | 0.003 (6) | 0.007 (4) | 0.009 (5) |
Fe1 | 0.034 (6) | 0.034 (9) | 0.019 (5) | −0.001 (4) | 0.001 (3) | 0.000 (3) |
N1 | 0.038 (4) | 0.042 (5) | 0.022 (3) | −0.008 (3) | −0.002 (3) | 0.002 (3) |
N2 | 0.057 (5) | 0.047 (6) | 0.037 (5) | −0.016 (4) | 0.006 (4) | −0.005 (4) |
N3 | 0.036 (4) | 0.063 (6) | 0.032 (4) | 0.007 (4) | 0.011 (3) | −0.006 (3) |
N4 | 0.039 (4) | 0.057 (6) | 0.033 (4) | 0.002 (4) | −0.006 (3) | 0.008 (4) |
H1 | 0.14 (3) | 0.10 (2) | 0.061 (17) | −0.06 (2) | 0.013 (14) | 0.015 (15) |
H2 | 0.091 (19) | 0.10 (2) | 0.065 (17) | −0.011 (15) | 0.001 (14) | −0.001 (16) |
H3 | 0.077 (17) | 0.084 (19) | 0.034 (12) | −0.035 (12) | −0.019 (10) | 0.014 (11) |
H4 | 0.11 (2) | 0.033 (17) | 0.044 (13) | 0.010 (12) | −0.021 (12) | 0.001 (10) |
Geometric parameters (Å, º) top
C1—N2 | 1.313 (15) | C6—N3 | 1.136 (9) |
C1—C2 | 1.385 (15) | C6—Ag1 | 2.078 (12) |
C1—H1 | 1.11 (4) | Ag1—C5ii | 2.089 (13) |
C2—C4 | 1.379 (15) | Ag1—N2iii | 2.611 (12) |
C2—H2 | 1.04 (4) | Ag1—Ag1iv | 3.01 (2) |
C3—N2 | 1.318 (12) | Fe1—N3v | 2.129 (6) |
C3—N1 | 1.331 (12) | Fe1—N3 | 2.129 (6) |
C3—H3 | 1.15 (2) | Fe1—N4v | 2.130 (7) |
C4—N1 | 1.343 (11) | Fe1—N4 | 2.130 (7) |
C4—H4 | 1.11 (3) | Fe1—N1 | 2.217 (7) |
C5—N4 | 1.136 (10) | Fe1—N1v | 2.217 (7) |
C5—Ag1i | 2.089 (13) | N2—Ag1vi | 2.611 (12) |
| | | |
N2—C1—C2 | 122.4 (12) | N3—Fe1—N4v | 90.0 (2) |
N2—C1—H1 | 117.7 (17) | N3v—Fe1—N4 | 90.0 (2) |
C2—C1—H1 | 119.9 (16) | N3—Fe1—N4 | 90.0 (2) |
C4—C2—C1 | 116.0 (11) | N4v—Fe1—N4 | 180.0000 (10) |
C4—C2—H2 | 121.7 (18) | N3v—Fe1—N1 | 86.6 (3) |
C1—C2—H2 | 122.1 (18) | N3—Fe1—N1 | 93.4 (3) |
N2—C3—N1 | 126.3 (8) | N4v—Fe1—N1 | 89.2 (3) |
N2—C3—H3 | 119.5 (13) | N4—Fe1—N1 | 90.8 (3) |
N1—C3—H3 | 114.1 (14) | N3v—Fe1—N1v | 93.4 (3) |
N1—C4—C2 | 122.3 (11) | N3—Fe1—N1v | 86.6 (3) |
N1—C4—H4 | 115.6 (15) | N4v—Fe1—N1v | 90.8 (3) |
C2—C4—H4 | 122.1 (13) | N4—Fe1—N1v | 89.2 (3) |
N4—C5—Ag1i | 176.7 (10) | N1—Fe1—N1v | 180.0000 (10) |
N3—C6—Ag1 | 175.3 (9) | C3—N1—C4 | 115.7 (9) |
C6—Ag1—C5ii | 162.6 (6) | C3—N1—Fe1 | 122.2 (6) |
C6—Ag1—N2iii | 101.7 (5) | C4—N1—Fe1 | 122.0 (7) |
C5ii—Ag1—N2iii | 92.9 (4) | C1—N2—C3 | 117.1 (9) |
C6—Ag1—Ag1iv | 109.0 (5) | C1—N2—Ag1vi | 125.2 (8) |
C5ii—Ag1—Ag1iv | 70.0 (5) | C3—N2—Ag1vi | 117.5 (6) |
N2iii—Ag1—Ag1iv | 122.0 (4) | C6—N3—Fe1 | 162.8 (8) |
N3v—Fe1—N3 | 180.000 (2) | C5—N4—Fe1 | 170.4 (9) |
N3v—Fe1—N4v | 90.0 (2) | | |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) −x+1/2, y, z+1/2; (iii) −x+1, y−1/2, −z+5/2; (iv) −x+1/2, −y+1/2, z; (v) −x+1, −y, −z+2; (vi) −x+1, y+1/2, −z+5/2. |
Crystal data top
C12H8Ag2FeN8 | Z = 4 |
Mr = 535.83 | F(000) = 584 |
Orthorhombic, Pccn | Dx = 2.077 Mg m−3 |
Hall symbol: -P 2ab 2ac | Neutron radiation, λ = 0.90-3.00 Å |
a = 15.780 (3) Å | µ = 0.08 mm−1 |
b = 8.200 (3) Å | T = 220 K |
c = 13.240 (3) Å | Prism, orange-yellow |
V = 1713.2 (8) Å3 | 1.0 × 0.6 × 0.5 mm |
Data collection top
ILL-VIVALDI Laue single xtal diffractometer | Rint = 0.357 |
Radiation source: ILL neutron source | θmax = 24.5°, θmin = 3.2° |
3553 measured reflections | h = −7→18 |
973 independent reflections | k = −8→9 |
743 reflections with I > 2σ(I) | l = −15→14 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.167 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.307 | All H-atom parameters refined |
S = 1.40 | w = 1/[σ2(Fo2) + (0.0516P)2 + 58.4407P] where P = (Fo2 + 2Fc2)/3 |
973 reflections | (Δ/σ)max < 0.001 |
142 parameters | Δρmax = 0.69 e Å−3 |
0 restraints | Δρmin = −0.82 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
C1 | 0.6289 (8) | 0.5408 (17) | 0.9490 (9) | 0.044 (3) | |
C2 | 0.5862 (7) | 0.4690 (16) | 0.8683 (8) | 0.040 (3) | |
C3 | 0.5952 (6) | 0.3251 (15) | 1.0484 (7) | 0.033 (3) | |
C4 | 0.5486 (7) | 0.3201 (17) | 0.8839 (8) | 0.039 (3) | |
C5 | 0.3272 (6) | 0.0750 (13) | 0.8738 (7) | 0.032 (2) | |
C6 | 0.3866 (6) | 0.0818 (14) | 1.1971 (6) | 0.031 (2) | |
Ag1 | 0.2919 (6) | 0.0837 (16) | 1.3055 (7) | 0.034 (3) | |
Fe1 | 0.5000 | 0.0000 | 1.0000 | 0.024 (3) | |
N1 | 0.5520 (5) | 0.2464 (9) | 0.9761 (5) | 0.0309 (18) | |
N2 | 0.6309 (5) | 0.4692 (11) | 1.0406 (6) | 0.039 (2) | |
N3 | 0.4365 (4) | 0.0707 (11) | 1.1344 (5) | 0.0347 (19) | |
N4 | 0.3906 (4) | 0.0607 (11) | 0.9153 (5) | 0.0344 (19) | |
H1 | 0.6606 (18) | 0.655 (4) | 0.9430 (19) | 0.075 (9) | |
H2 | 0.584 (2) | 0.527 (4) | 0.794 (2) | 0.085 (9) | |
H3 | 0.5943 (15) | 0.264 (3) | 1.1198 (18) | 0.050 (6) | |
H4 | 0.5158 (18) | 0.258 (3) | 0.8284 (19) | 0.053 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.053 (7) | 0.037 (7) | 0.044 (7) | −0.009 (7) | 0.003 (5) | 0.006 (6) |
C2 | 0.045 (6) | 0.045 (8) | 0.030 (6) | −0.006 (5) | −0.003 (4) | 0.007 (5) |
C3 | 0.027 (5) | 0.043 (8) | 0.027 (6) | −0.017 (5) | −0.007 (4) | −0.002 (5) |
C4 | 0.040 (6) | 0.055 (8) | 0.023 (5) | 0.008 (6) | 0.000 (4) | 0.010 (6) |
C5 | 0.027 (5) | 0.040 (7) | 0.031 (5) | 0.013 (5) | −0.011 (4) | −0.001 (5) |
C6 | 0.032 (5) | 0.040 (7) | 0.022 (4) | 0.010 (4) | 0.006 (4) | −0.001 (4) |
Ag1 | 0.026 (5) | 0.045 (8) | 0.030 (5) | 0.012 (5) | 0.012 (4) | 0.010 (5) |
Fe1 | 0.020 (5) | 0.041 (9) | 0.010 (5) | 0.002 (4) | 0.001 (3) | −0.001 (3) |
N1 | 0.025 (4) | 0.046 (5) | 0.022 (3) | −0.006 (3) | −0.004 (3) | 0.003 (3) |
N2 | 0.043 (5) | 0.043 (5) | 0.029 (4) | −0.007 (4) | −0.001 (3) | −0.001 (3) |
N3 | 0.030 (4) | 0.049 (5) | 0.025 (4) | −0.002 (4) | 0.009 (3) | −0.006 (3) |
N4 | 0.029 (4) | 0.045 (5) | 0.030 (4) | 0.009 (4) | −0.005 (3) | 0.001 (4) |
H1 | 0.089 (19) | 0.08 (2) | 0.060 (15) | −0.057 (18) | 0.017 (13) | −0.004 (13) |
H2 | 0.11 (2) | 0.08 (2) | 0.07 (2) | −0.026 (17) | −0.006 (16) | 0.027 (16) |
H3 | 0.068 (15) | 0.043 (14) | 0.039 (12) | −0.009 (10) | 0.000 (10) | −0.002 (10) |
H4 | 0.084 (17) | 0.028 (15) | 0.046 (14) | −0.020 (11) | −0.009 (12) | 0.009 (10) |
Geometric parameters (Å, º) top
C1—N2 | 1.348 (16) | C6—N3 | 1.148 (11) |
C1—C2 | 1.394 (17) | C6—Ag1 | 2.073 (12) |
C1—H1 | 1.07 (3) | Ag1—C5ii | 2.086 (13) |
C2—C4 | 1.373 (18) | Ag1—N2iii | 2.553 (12) |
C2—H2 | 1.10 (3) | Ag1—Ag1iv | 3.03 (2) |
C3—N2 | 1.313 (14) | Fe1—N4v | 2.118 (7) |
C3—N1 | 1.340 (12) | Fe1—N4 | 2.118 (7) |
C3—H3 | 1.07 (3) | Fe1—N3 | 2.123 (6) |
C4—N1 | 1.363 (13) | Fe1—N3v | 2.123 (6) |
C4—H4 | 1.03 (3) | Fe1—N1 | 2.204 (7) |
C5—N4 | 1.148 (11) | Fe1—N1v | 2.204 (7) |
C5—Ag1i | 2.086 (13) | N2—Ag1vi | 2.553 (12) |
| | | |
N2—C1—C2 | 121.1 (12) | N4—Fe1—N3 | 89.7 (3) |
N2—C1—H1 | 116.1 (19) | N4v—Fe1—N3v | 89.7 (3) |
C2—C1—H1 | 122.8 (19) | N4—Fe1—N3v | 90.3 (3) |
C4—C2—C1 | 118.0 (11) | N3—Fe1—N3v | 180.0000 (10) |
C4—C2—H2 | 120 (2) | N4v—Fe1—N1 | 89.3 (3) |
C1—C2—H2 | 122 (2) | N4—Fe1—N1 | 90.7 (3) |
N2—C3—N1 | 126.6 (9) | N3—Fe1—N1 | 92.6 (3) |
N2—C3—H3 | 119.7 (14) | N3v—Fe1—N1 | 87.4 (3) |
N1—C3—H3 | 113.5 (15) | N4v—Fe1—N1v | 90.7 (3) |
N1—C4—C2 | 120.8 (11) | N4—Fe1—N1v | 89.3 (3) |
N1—C4—H4 | 116.0 (16) | N3—Fe1—N1v | 87.4 (3) |
C2—C4—H4 | 123.2 (15) | N3v—Fe1—N1v | 92.6 (3) |
N4—C5—Ag1i | 175.1 (10) | N1—Fe1—N1v | 180.0000 (10) |
N3—C6—Ag1 | 175.1 (10) | C3—N1—C4 | 116.5 (10) |
C6—Ag1—C5ii | 161.7 (7) | C3—N1—Fe1 | 121.9 (7) |
C6—Ag1—N2iii | 101.9 (5) | C4—N1—Fe1 | 121.4 (7) |
C5ii—Ag1—N2iii | 94.1 (5) | C3—N2—C1 | 116.9 (10) |
C6—Ag1—Ag1iv | 108.8 (6) | C3—N2—Ag1vi | 118.3 (7) |
C5ii—Ag1—Ag1iv | 68.8 (5) | C1—N2—Ag1vi | 124.7 (8) |
N2iii—Ag1—Ag1iv | 122.6 (4) | C6—N3—Fe1 | 162.1 (8) |
N4v—Fe1—N4 | 180.000 (2) | C5—N4—Fe1 | 171.2 (9) |
N4v—Fe1—N3 | 90.3 (3) | | |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) −x+1/2, y, z+1/2; (iii) −x+1, y−1/2, −z+5/2; (iv) −x+1/2, −y+1/2, z; (v) −x+1, −y, −z+2; (vi) −x+1, y+1/2, −z+5/2. |
Crystal data top
C12H8Ag2FeN8 | Z = 4 |
Mr = 535.83 | F(000) = 584 |
Orthorhombic, Pccn | Dx = 2.062 Mg m−3 |
Hall symbol: -P 2ab 2ac | Neutron radiation, λ = 0.90-3.00 Å |
a = 15.7820 (15) Å | µ = 0.08 mm−1 |
b = 8.2250 (15) Å | T = 260 K |
c = 13.2980 (15) Å | Prism, orange-yellow |
V = 1726.2 (4) Å3 | 1.0 × 0.6 × 0.5 mm |
Data collection top
ILL-VIVALDI Laue single xtal diffractometer | Rint = 0.221 |
Radiation source: ILL neutron source | θmax = 27.7°, θmin = 3.6° |
5638 measured reflections | h = −11→18 |
1069 independent reflections | k = −9→9 |
885 reflections with I > 2σ(I) | l = −15→14 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.100 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.161 | All H-atom parameters refined |
S = 1.29 | w = 1/[σ2(Fo2) + (0.0558P)2 + 4.1743P] where P = (Fo2 + 2Fc2)/3 |
1069 reflections | (Δ/σ)max < 0.001 |
142 parameters | Δρmax = 0.60 e Å−3 |
0 restraints | Δρmin = −0.57 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
C1 | 0.6287 (3) | 0.5402 (7) | 0.9506 (4) | 0.0488 (12) | |
C2 | 0.5870 (3) | 0.4695 (7) | 0.8701 (4) | 0.0464 (13) | |
C3 | 0.5938 (3) | 0.3241 (6) | 1.0486 (3) | 0.0373 (11) | |
C4 | 0.5493 (3) | 0.3207 (6) | 0.8867 (3) | 0.0389 (11) | |
C5 | 0.3273 (2) | 0.0757 (6) | 0.8735 (3) | 0.0351 (10) | |
C6 | 0.3856 (2) | 0.0790 (6) | 1.1968 (3) | 0.0338 (10) | |
Ag1 | 0.2911 (2) | 0.0851 (6) | 1.3053 (3) | 0.0371 (12) | |
Fe1 | 0.5000 | 0.0000 | 1.0000 | 0.0236 (11) | |
N1 | 0.55311 (19) | 0.2470 (3) | 0.9755 (2) | 0.0312 (8) | |
N2 | 0.6316 (2) | 0.4678 (5) | 1.0403 (3) | 0.0448 (9) | |
N3 | 0.43573 (17) | 0.0711 (4) | 1.1348 (2) | 0.0371 (8) | |
N4 | 0.39087 (16) | 0.0608 (4) | 0.9150 (2) | 0.0361 (8) | |
H1 | 0.6601 (9) | 0.6579 (16) | 0.9446 (9) | 0.084 (4) | |
H2 | 0.5852 (9) | 0.5243 (16) | 0.7971 (10) | 0.084 (4) | |
H3 | 0.5949 (7) | 0.2650 (14) | 1.1198 (8) | 0.069 (3) | |
H4 | 0.5152 (8) | 0.2584 (13) | 0.8278 (9) | 0.070 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.063 (3) | 0.038 (3) | 0.045 (3) | −0.015 (3) | 0.005 (2) | 0.005 (3) |
C2 | 0.063 (3) | 0.039 (3) | 0.038 (3) | −0.008 (2) | −0.001 (2) | 0.008 (2) |
C3 | 0.046 (2) | 0.036 (3) | 0.030 (3) | −0.011 (2) | −0.0039 (16) | 0.001 (2) |
C4 | 0.048 (2) | 0.040 (3) | 0.029 (2) | −0.005 (2) | −0.0021 (18) | 0.006 (2) |
C5 | 0.0248 (19) | 0.046 (3) | 0.034 (2) | 0.0003 (18) | −0.0078 (15) | 0.0035 (19) |
C6 | 0.0341 (19) | 0.037 (3) | 0.030 (2) | 0.0044 (18) | 0.0092 (16) | −0.0002 (18) |
Ag1 | 0.031 (2) | 0.041 (3) | 0.040 (3) | 0.005 (2) | 0.0146 (18) | 0.008 (2) |
Fe1 | 0.021 (2) | 0.030 (3) | 0.019 (2) | −0.0012 (13) | −0.0007 (11) | 0.0000 (13) |
N1 | 0.0352 (15) | 0.031 (2) | 0.0271 (14) | −0.0049 (11) | −0.0023 (13) | 0.0012 (12) |
N2 | 0.055 (2) | 0.041 (2) | 0.038 (2) | −0.0115 (16) | −0.0017 (15) | −0.0018 (16) |
N3 | 0.0369 (15) | 0.045 (2) | 0.0297 (16) | 0.0026 (15) | 0.0115 (12) | −0.0018 (14) |
N4 | 0.0275 (14) | 0.046 (2) | 0.0352 (17) | 0.0017 (14) | −0.0055 (12) | 0.0034 (15) |
H1 | 0.122 (9) | 0.058 (8) | 0.073 (8) | −0.041 (8) | −0.008 (6) | 0.016 (6) |
H2 | 0.133 (11) | 0.073 (9) | 0.047 (7) | −0.019 (7) | −0.004 (6) | 0.021 (6) |
H3 | 0.108 (8) | 0.071 (8) | 0.028 (5) | −0.032 (6) | −0.012 (5) | 0.008 (5) |
H4 | 0.091 (7) | 0.068 (8) | 0.051 (7) | −0.011 (5) | −0.024 (5) | 0.003 (5) |
Geometric parameters (Å, º) top
C1—N2 | 1.335 (7) | C6—N3 | 1.145 (5) |
C1—C2 | 1.384 (7) | C6—Ag1 | 2.075 (5) |
C1—H1 | 1.091 (15) | Ag1—C5ii | 2.079 (5) |
C2—C4 | 1.379 (7) | Ag1—N2iii | 2.576 (5) |
C2—H2 | 1.071 (14) | Ag1—Ag1iv | 3.006 (9) |
C3—N1 | 1.326 (5) | Fe1—N4v | 2.120 (3) |
C3—N2 | 1.328 (6) | Fe1—N4 | 2.120 (3) |
C3—H3 | 1.065 (12) | Fe1—N3v | 2.141 (3) |
C4—N1 | 1.328 (5) | Fe1—N3 | 2.141 (3) |
C4—H4 | 1.080 (13) | Fe1—N1 | 2.221 (3) |
C5—N4 | 1.152 (4) | Fe1—N1v | 2.221 (3) |
C5—Ag1i | 2.079 (5) | N2—Ag1vi | 2.576 (5) |
| | | |
N2—C1—C2 | 121.3 (5) | N4—Fe1—N3v | 90.16 (11) |
N2—C1—H1 | 116.4 (8) | N4v—Fe1—N3 | 90.16 (11) |
C2—C1—H1 | 122.2 (8) | N4—Fe1—N3 | 89.84 (11) |
C4—C2—C1 | 117.0 (5) | N3v—Fe1—N3 | 180.0000 (10) |
C4—C2—H2 | 120.4 (8) | N4v—Fe1—N1 | 89.28 (12) |
C1—C2—H2 | 122.5 (8) | N4—Fe1—N1 | 90.72 (12) |
N1—C3—N2 | 125.6 (4) | N3v—Fe1—N1 | 87.02 (12) |
N1—C3—H3 | 116.2 (7) | N3—Fe1—N1 | 92.98 (12) |
N2—C3—H3 | 118.2 (7) | N4v—Fe1—N1v | 90.72 (12) |
N1—C4—C2 | 121.8 (4) | N4—Fe1—N1v | 89.28 (12) |
N1—C4—H4 | 116.8 (7) | N3v—Fe1—N1v | 92.98 (12) |
C2—C4—H4 | 121.4 (7) | N3—Fe1—N1v | 87.02 (12) |
N4—C5—Ag1i | 175.1 (4) | N1—Fe1—N1v | 180.0 |
N3—C6—Ag1 | 177.2 (4) | C3—N1—C4 | 117.0 (4) |
C6—Ag1—C5ii | 161.5 (3) | C3—N1—Fe1 | 120.8 (3) |
C6—Ag1—N2iii | 101.8 (2) | C4—N1—Fe1 | 122.0 (3) |
C5ii—Ag1—N2iii | 93.7 (2) | C3—N2—C1 | 117.1 (4) |
C6—Ag1—Ag1iv | 109.4 (2) | C3—N2—Ag1vi | 118.7 (3) |
C5ii—Ag1—Ag1iv | 69.24 (19) | C1—N2—Ag1vi | 124.2 (3) |
N2iii—Ag1—Ag1iv | 122.86 (16) | C6—N3—Fe1 | 161.1 (3) |
N4v—Fe1—N4 | 180.0000 (10) | C5—N4—Fe1 | 171.3 (3) |
N4v—Fe1—N3v | 89.84 (11) | | |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) −x+1/2, y, z+1/2; (iii) −x+1, y−1/2, −z+5/2; (iv) −x+1/2, −y+1/2, z; (v) −x+1, −y, −z+2; (vi) −x+1, y+1/2, −z+5/2. |
Crystal data top
C12H8Ag2FeN8 | Z = 4 |
Mr = 535.83 | F(000) = 584 |
Orthorhombic, Pccn | Dx = 2.054 Mg m−3 |
Hall symbol: -P 2ab 2ac | Neutron radiation, λ = 0.95-2.50 Å |
a = 15.782 (3) Å | µ = 0.09 mm−1 |
b = 8.242 (3) Å | T = 280 K |
c = 13.320 (3) Å | Prism, orange-yellow |
V = 1732.6 (8) Å3 | 1.0 × 0.6 × 0.5 mm |
Data collection top
ILL-VIVALDI Laue single xtal diffractometer | Rint = 0.352 |
Radiation source: ILL neutron source | θmax = 29.3°, θmin = 4.0° |
3459 measured reflections | h = −17→11 |
782 independent reflections | k = −8→8 |
641 reflections with I > 2σ(I) | l = −14→13 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.172 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.293 | All H-atom parameters refined |
S = 1.42 | w = 1/[σ2(Fo2) + (0.0311P)2 + 71.9321P] where P = (Fo2 + 2Fc2)/3 |
782 reflections | (Δ/σ)max < 0.001 |
142 parameters | Δρmax = 0.73 e Å−3 |
0 restraints | Δρmin = −0.58 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
C1 | 0.6283 (10) | 0.537 (2) | 0.9494 (11) | 0.052 (4) | |
C2 | 0.5866 (9) | 0.4672 (18) | 0.8697 (10) | 0.045 (3) | |
C3 | 0.5949 (7) | 0.3248 (16) | 1.0484 (8) | 0.037 (3) | |
C4 | 0.5492 (8) | 0.3209 (19) | 0.8862 (10) | 0.045 (3) | |
C5 | 0.3269 (8) | 0.0766 (17) | 0.8740 (8) | 0.043 (3) | |
C6 | 0.3858 (7) | 0.0805 (16) | 1.1963 (8) | 0.037 (3) | |
Fe1 | 0.5000 | 0.0000 | 1.0000 | 0.029 (3) | |
N1 | 0.5523 (6) | 0.2463 (10) | 0.9759 (7) | 0.036 (2) | |
N2 | 0.6307 (6) | 0.4686 (12) | 1.0403 (7) | 0.045 (3) | |
N3 | 0.4362 (5) | 0.0694 (13) | 1.1344 (6) | 0.041 (2) | |
N4 | 0.3902 (6) | 0.0605 (13) | 0.9146 (6) | 0.042 (2) | |
Ag1 | 0.2901 (8) | 0.0861 (18) | 1.3047 (9) | 0.039 (4) | |
H1 | 0.661 (3) | 0.655 (5) | 0.944 (2) | 0.104 (14) | |
H3 | 0.5933 (19) | 0.263 (4) | 1.122 (2) | 0.071 (9) | |
H2 | 0.589 (2) | 0.525 (5) | 0.794 (3) | 0.085 (10) | |
H4 | 0.514 (2) | 0.255 (3) | 0.829 (2) | 0.066 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.063 (9) | 0.046 (9) | 0.047 (9) | −0.003 (8) | 0.003 (7) | 0.005 (8) |
C2 | 0.058 (8) | 0.041 (8) | 0.036 (8) | −0.014 (7) | −0.003 (6) | 0.005 (6) |
C3 | 0.044 (7) | 0.050 (9) | 0.016 (6) | −0.021 (7) | −0.009 (5) | 0.007 (6) |
C4 | 0.044 (7) | 0.054 (10) | 0.038 (8) | 0.002 (7) | −0.008 (6) | 0.010 (7) |
C5 | 0.031 (6) | 0.055 (9) | 0.044 (6) | 0.004 (6) | −0.020 (6) | −0.002 (6) |
C6 | 0.039 (6) | 0.045 (8) | 0.027 (6) | 0.002 (6) | 0.009 (5) | −0.002 (5) |
Fe1 | 0.039 (8) | 0.035 (9) | 0.014 (6) | −0.001 (5) | 0.005 (4) | 0.005 (4) |
N1 | 0.035 (5) | 0.043 (6) | 0.028 (4) | −0.005 (4) | −0.004 (4) | 0.001 (3) |
N2 | 0.047 (6) | 0.045 (6) | 0.043 (6) | −0.018 (5) | 0.002 (4) | −0.009 (5) |
N3 | 0.033 (5) | 0.065 (7) | 0.026 (5) | 0.001 (5) | 0.011 (4) | −0.005 (4) |
N4 | 0.039 (5) | 0.050 (6) | 0.038 (5) | 0.005 (5) | −0.006 (4) | 0.000 (5) |
Ag1 | 0.029 (6) | 0.055 (11) | 0.032 (7) | 0.006 (6) | 0.011 (5) | 0.017 (6) |
H1 | 0.17 (4) | 0.09 (3) | 0.06 (2) | −0.07 (3) | 0.03 (2) | 0.005 (17) |
H3 | 0.09 (2) | 0.08 (2) | 0.046 (18) | −0.041 (17) | −0.015 (13) | 0.022 (14) |
H2 | 0.08 (2) | 0.10 (3) | 0.08 (2) | −0.008 (17) | −0.001 (18) | 0.03 (2) |
H4 | 0.13 (3) | 0.04 (2) | 0.033 (16) | 0.003 (15) | −0.029 (15) | −0.004 (11) |
Geometric parameters (Å, º) top
C1—N2 | 1.34 (2) | C6—N3 | 1.150 (13) |
C1—C2 | 1.37 (2) | C6—Ag1 | 2.088 (15) |
C1—H1 | 1.11 (5) | Fe1—N3 | 2.132 (8) |
C2—C4 | 1.36 (2) | Fe1—N3ii | 2.132 (8) |
C2—H2 | 1.12 (4) | Fe1—N4 | 2.132 (9) |
C3—N2 | 1.318 (16) | Fe1—N4ii | 2.132 (9) |
C3—N1 | 1.343 (15) | Fe1—N1ii | 2.214 (9) |
C3—H3 | 1.10 (3) | Fe1—N1 | 2.214 (9) |
C4—N1 | 1.346 (16) | N2—Ag1iii | 2.601 (15) |
C4—H4 | 1.09 (4) | Ag1—C5iv | 2.067 (16) |
C5—N4 | 1.144 (14) | Ag1—N2v | 2.601 (14) |
C5—Ag1i | 2.067 (16) | Ag1—Ag1vi | 2.98 (3) |
| | | |
N2—C1—C2 | 122.6 (15) | N4—Fe1—N1ii | 89.4 (4) |
N2—C1—H1 | 114 (2) | N4ii—Fe1—N1ii | 90.6 (4) |
C2—C1—H1 | 123 (2) | N3—Fe1—N1 | 92.9 (4) |
C4—C2—C1 | 116.9 (13) | N3ii—Fe1—N1 | 87.1 (4) |
C4—C2—H2 | 123 (2) | N4—Fe1—N1 | 90.6 (4) |
C1—C2—H2 | 120 (2) | N4ii—Fe1—N1 | 89.4 (4) |
N2—C3—N1 | 126.2 (10) | N1ii—Fe1—N1 | 180.0000 (10) |
N2—C3—H3 | 119.7 (17) | C3—N1—C4 | 115.8 (11) |
N1—C3—H3 | 113.9 (18) | C3—N1—Fe1 | 121.7 (8) |
N1—C4—C2 | 122.3 (13) | C4—N1—Fe1 | 122.3 (9) |
N1—C4—H4 | 114 (2) | C3—N2—C1 | 116.1 (12) |
C2—C4—H4 | 123.2 (18) | C3—N2—Ag1iii | 118.4 (8) |
N4—C5—Ag1i | 175.1 (13) | C1—N2—Ag1iii | 125.3 (10) |
N3—C6—Ag1 | 176.0 (12) | C6—N3—Fe1 | 161.9 (9) |
N3—Fe1—N3ii | 180.000 (2) | C5—N4—Fe1 | 171.6 (11) |
N3—Fe1—N4 | 90.1 (3) | C5iv—Ag1—C6 | 162.5 (8) |
N3ii—Fe1—N4 | 89.9 (3) | C5iv—Ag1—N2v | 93.4 (6) |
N3—Fe1—N4ii | 89.9 (3) | C6—Ag1—N2v | 101.1 (6) |
N3ii—Fe1—N4ii | 90.1 (3) | C5iv—Ag1—Ag1vi | 69.8 (6) |
N4—Fe1—N4ii | 180.000 (2) | C6—Ag1—Ag1vi | 109.1 (7) |
N3—Fe1—N1ii | 87.1 (4) | N2v—Ag1—Ag1vi | 122.8 (5) |
N3ii—Fe1—N1ii | 92.9 (4) | | |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) −x+1, −y, −z+2; (iii) −x+1, y+1/2, −z+5/2; (iv) −x+1/2, y, z+1/2; (v) −x+1, y−1/2, −z+5/2; (vi) −x+1/2, −y+1/2, z. |
Crystal data top
C12H8Ag2FeN8 | Z = 4 |
Mr = 535.83 | F(000) = 584 |
Orthorhombic, Pccn | Dx = 2.055 Mg m−3 |
Hall symbol: -P 2ab 2ac | Neutron radiation, λ = 0.90-3.00 Å |
a = 15.7820 (15) Å | µ = 0.08 mm−1 |
b = 8.2430 (15) Å | T = 290 K |
c = 13.3100 (15) Å | Prism, orange-yellow |
V = 1731.5 (4) Å3 | 1.0 × 0.6 × 0.5 mm |
Data collection top
ILL-VIVALDI Laue single xtal diffractometer | Rint = 0.227 |
Radiation source: ILL neutron source | θmax = 31.5°, θmin = 4.0° |
5485 measured reflections | h = −11→18 |
1068 independent reflections | k = −9→9 |
860 reflections with I > 2σ(I) | l = −15→14 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.114 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.168 | All H-atom parameters refined |
S = 1.30 | w = 1/[σ2(Fo2) + (0.0625P)2 + 3.3037P] where P = (Fo2 + 2Fc2)/3 |
1068 reflections | (Δ/σ)max < 0.001 |
142 parameters | Δρmax = 0.47 e Å−3 |
0 restraints | Δρmin = −0.54 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
C1 | 0.3857 (2) | 0.0795 (6) | 0.1965 (3) | 0.0371 (11) | |
C2 | 0.5935 (3) | 0.3244 (6) | 0.0485 (3) | 0.0400 (12) | |
C3 | 0.5496 (3) | 0.3203 (7) | −0.1137 (3) | 0.0426 (12) | |
C4 | 0.5869 (3) | 0.4685 (7) | −0.1296 (4) | 0.0515 (14) | |
C5 | 0.3274 (2) | 0.0760 (6) | −0.1265 (3) | 0.0390 (11) | |
C6 | 0.6289 (4) | 0.5389 (8) | −0.0496 (4) | 0.0512 (13) | |
Ag1 | 0.2915 (3) | 0.0844 (6) | 0.3051 (3) | 0.0395 (13) | |
Fe1 | 0.5000 | 0.0000 | 0.0000 | 0.0241 (12) | |
N1 | 0.39086 (17) | 0.0610 (5) | −0.0850 (2) | 0.0385 (9) | |
N2 | 0.43564 (18) | 0.0710 (5) | 0.1347 (2) | 0.0402 (9) | |
N3 | 0.6314 (2) | 0.4675 (5) | 0.0405 (3) | 0.0483 (10) | |
N4 | 0.5532 (2) | 0.2458 (4) | −0.0243 (2) | 0.0342 (8) | |
H2 | 0.5953 (8) | 0.2643 (15) | 0.1200 (8) | 0.078 (4) | |
H3 | 0.5138 (8) | 0.2582 (14) | −0.1714 (9) | 0.071 (3) | |
H4 | 0.5851 (10) | 0.5259 (18) | −0.2041 (11) | 0.096 (4) | |
H6 | 0.6611 (10) | 0.6551 (18) | −0.0562 (10) | 0.096 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.039 (2) | 0.042 (3) | 0.031 (2) | 0.004 (2) | 0.0100 (17) | −0.0007 (19) |
C2 | 0.048 (2) | 0.044 (3) | 0.028 (3) | −0.014 (2) | −0.0028 (17) | 0.001 (2) |
C3 | 0.054 (3) | 0.044 (3) | 0.030 (2) | −0.004 (2) | −0.0025 (19) | 0.005 (2) |
C4 | 0.070 (3) | 0.047 (4) | 0.038 (3) | −0.013 (2) | 0.003 (2) | 0.011 (3) |
C5 | 0.030 (2) | 0.053 (3) | 0.035 (2) | 0.001 (2) | −0.0090 (16) | 0.005 (2) |
C6 | 0.067 (3) | 0.037 (3) | 0.050 (3) | −0.014 (3) | 0.002 (2) | 0.008 (3) |
Ag1 | 0.035 (2) | 0.044 (4) | 0.040 (3) | 0.008 (2) | 0.0155 (18) | 0.008 (2) |
Fe1 | 0.021 (2) | 0.031 (4) | 0.020 (2) | −0.0012 (14) | −0.0003 (12) | −0.0017 (14) |
N1 | 0.0286 (15) | 0.050 (2) | 0.0374 (19) | 0.0018 (15) | −0.0084 (13) | 0.0016 (16) |
N2 | 0.0390 (15) | 0.051 (3) | 0.0307 (17) | 0.0029 (16) | 0.0131 (13) | −0.0024 (15) |
N3 | 0.062 (2) | 0.042 (2) | 0.041 (2) | −0.0142 (18) | −0.0026 (16) | −0.0008 (17) |
N4 | 0.0389 (16) | 0.035 (2) | 0.0288 (15) | −0.0049 (13) | −0.0002 (14) | 0.0024 (13) |
H2 | 0.130 (10) | 0.071 (9) | 0.034 (6) | −0.035 (7) | −0.022 (5) | 0.015 (5) |
H3 | 0.104 (8) | 0.062 (9) | 0.048 (7) | −0.018 (6) | −0.021 (6) | 0.007 (5) |
H4 | 0.147 (12) | 0.077 (10) | 0.065 (9) | −0.027 (8) | −0.008 (7) | 0.028 (7) |
H6 | 0.132 (11) | 0.074 (10) | 0.082 (9) | −0.049 (9) | −0.001 (7) | 0.012 (7) |
Geometric parameters (Å, º) top
C1—N2 | 1.142 (5) | C6—N3 | 1.336 (8) |
C1—Ag1 | 2.074 (5) | C6—H6 | 1.088 (17) |
C2—N3 | 1.327 (6) | Ag1—C5ii | 2.088 (5) |
C2—N4 | 1.329 (6) | Ag1—N3iii | 2.576 (6) |
C2—H2 | 1.073 (13) | Ag1—Ag1iv | 3.028 (10) |
C3—N4 | 1.339 (6) | Fe1—N1v | 2.121 (3) |
C3—C4 | 1.372 (8) | Fe1—N1 | 2.121 (3) |
C3—H3 | 1.082 (14) | Fe1—N2v | 2.142 (3) |
C4—C6 | 1.381 (8) | Fe1—N2 | 2.142 (3) |
C4—H4 | 1.100 (16) | Fe1—N4 | 2.217 (3) |
C5—N1 | 1.150 (5) | Fe1—N4v | 2.217 (3) |
C5—Ag1i | 2.088 (5) | N3—Ag1vi | 2.576 (6) |
| | | |
N2—C1—Ag1 | 176.8 (4) | N1—Fe1—N2v | 90.21 (12) |
N3—C2—N4 | 126.2 (4) | N1v—Fe1—N2 | 90.21 (12) |
N3—C2—H2 | 118.1 (7) | N1—Fe1—N2 | 89.79 (12) |
N4—C2—H2 | 115.8 (7) | N2v—Fe1—N2 | 180.00 (15) |
N4—C3—C4 | 121.8 (4) | N1v—Fe1—N4 | 89.27 (13) |
N4—C3—H3 | 115.8 (7) | N1—Fe1—N4 | 90.73 (13) |
C4—C3—H3 | 122.4 (7) | N2v—Fe1—N4 | 87.01 (13) |
C3—C4—C6 | 117.4 (5) | N2—Fe1—N4 | 92.99 (13) |
C3—C4—H4 | 120.7 (9) | N1v—Fe1—N4v | 90.73 (13) |
C6—C4—H4 | 121.8 (9) | N1—Fe1—N4v | 89.27 (13) |
N1—C5—Ag1i | 174.8 (4) | N2v—Fe1—N4v | 92.99 (13) |
N3—C6—C4 | 121.4 (6) | N2—Fe1—N4v | 87.01 (13) |
N3—C6—H6 | 116.4 (9) | N4—Fe1—N4v | 180.0 (2) |
C4—C6—H6 | 122.2 (9) | C5—N1—Fe1 | 171.3 (4) |
C1—Ag1—C5ii | 161.5 (3) | C1—N2—Fe1 | 161.4 (4) |
C1—Ag1—N3iii | 102.1 (2) | C2—N3—C6 | 116.8 (4) |
C5ii—Ag1—N3iii | 93.7 (2) | C2—N3—Ag1vi | 118.7 (3) |
C1—Ag1—Ag1iv | 109.1 (2) | C6—N3—Ag1vi | 124.5 (4) |
C5ii—Ag1—Ag1iv | 69.0 (2) | C2—N4—C3 | 116.4 (4) |
N3iii—Ag1—Ag1iv | 122.78 (17) | C2—N4—Fe1 | 121.3 (3) |
N1v—Fe1—N1 | 180.0 (3) | C3—N4—Fe1 | 122.2 (3) |
N1v—Fe1—N2v | 89.79 (12) | | |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) −x+1/2, y, z+1/2; (iii) −x+1, y−1/2, −z+1/2; (iv) −x+1/2, −y+1/2, z; (v) −x+1, −y, −z; (vi) −x+1, y+1/2, −z+1/2. |