Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100005539/qa0272sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100005539/qa0272Isup2.hkl |
CCDC reference: 145636
Crystals of the title compound, [Fe(phen)3](NCS)2·3H2O, were grown from an aqueous solution.
There is a positional disorder of NCS- ion (N8—C38—S2) and one water molecule of crystallization (O5). It was assumed that occupancy factors of two possible combinations (N8—C38—S2 and O5, and N8*—C38*—S2 and O5*) are 50% each, and their positional parameters were refined isotropically. H-atom positional parameters of [Fe(phen)3]2+ were calculated geometrically and fixed with Uiso(H) = 1.2Ueq(parent atom). H atoms of water of crystallization were not introduced. The residual density of 1.27 e Å-3 was located at 0.09 Å from the S2 atom.
Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: TEXSAN.
[Fe(C12H8N2)3](NCS)2·3H2O | Z = 2 |
Mr = 766.67 | Dx = 1.431 Mg m−3 |
Triclinic, P1 | Mo Kα radiation, λ = 0.71073 Å |
a = 12.083 (3) Å | Cell parameters from 25 reflections |
b = 14.234 (4) Å | θ = 14.9–15.0° |
c = 12.050 (2) Å | µ = 0.59 mm−1 |
α = 93.19 (2)° | T = 295 K |
β = 109.53 (1)° | Prismatic, violet |
γ = 111.55 (2)° | 0.6 × 0.5 × 0.5 mm |
V = 1778.7 (8) Å3 |
Rigaku AFC-7R diffractometer | Rint = 0.007 |
θ–2θ scans | θmax = 30.0° |
Absorption correction: ψ scan (North et al., 1968) | h = 0→16 |
Tmin = 0.658, Tmax = 0.744 | k = −20→20 |
10804 measured reflections | l = −16→16 |
10354 independent reflections | 3 standard reflections every 150 reflections |
8387 reflections with I > 2σ(I) | intensity decay: none |
Refinement on F2 | H-atom parameters not refined |
R[F2 > 2σ(F2)] = 0.062 | w = 1/[σ2(Fo2) + (0.1141P)2 + 1.4911P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.201 | (Δ/σ)max = 0.001 |
S = 1.03 | Δρmax = 1.27 e Å−3 |
8387 reflections | Δρmin = −1.55 e Å−3 |
461 parameters |
[Fe(C12H8N2)3](NCS)2·3H2O | γ = 111.55 (2)° |
Mr = 766.67 | V = 1778.7 (8) Å3 |
Triclinic, P1 | Z = 2 |
a = 12.083 (3) Å | Mo Kα radiation |
b = 14.234 (4) Å | µ = 0.59 mm−1 |
c = 12.050 (2) Å | T = 295 K |
α = 93.19 (2)° | 0.6 × 0.5 × 0.5 mm |
β = 109.53 (1)° |
Rigaku AFC-7R diffractometer | 8387 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.007 |
Tmin = 0.658, Tmax = 0.744 | 3 standard reflections every 150 reflections |
10804 measured reflections | intensity decay: none |
10354 independent reflections |
R[F2 > 2σ(F2)] = 0.062 | 461 parameters |
wR(F2) = 0.201 | H-atom parameters not refined |
S = 1.03 | Δρmax = 1.27 e Å−3 |
8387 reflections | Δρmin = −1.55 e Å−3 |
Refinement. Refinement using reflections with F2 > 0.0 σ(F2). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt). |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Fe1 | 0.93955 (3) | 0.21150 (2) | 0.25216 (3) | 0.0334 (1) | |
S1 | 0.6416 (1) | 0.12515 (9) | 0.5754 (1) | 0.0760 (3) | |
S2 | 0.3762 (4) | 0.3022 (3) | 0.7060 (4) | 0.20388 (2)* | |
O3 | 0.0083 (3) | 0.4281 (3) | 0.9214 (3) | 0.0875 (9) | |
O4 | 0.2062 (4) | 0.3535 (3) | 0.9860 (4) | 0.105 (1) | |
O5 | 0.2032 (4) | 0.1930 (3) | 0.7542 (4) | 0.03943 (1)* | 0.50 |
O5* | 0.5474 (8) | 0.5341 (7) | 0.9069 (8) | 0.09300 (3)* | 0.50 |
N1 | 1.0555 (2) | 0.1466 (2) | 0.3327 (2) | 0.0408 (4) | |
N2 | 1.1026 (2) | 0.3249 (2) | 0.2679 (2) | 0.0380 (4) | |
N3 | 0.9486 (2) | 0.2783 (2) | 0.4053 (2) | 0.0366 (4) | |
N4 | 0.8378 (2) | 0.2899 (2) | 0.1828 (2) | 0.0383 (4) | |
N5 | 0.7775 (2) | 0.0928 (2) | 0.2301 (2) | 0.0403 (4) | |
N6 | 0.9115 (2) | 0.1386 (2) | 0.0946 (2) | 0.0403 (4) | |
N7 | 0.7676 (4) | 0.2661 (3) | 0.7916 (3) | 0.092 (1) | |
N8 | 0.5282 (8) | 0.4907 (7) | 0.8999 (7) | 0.07058 (2)* | 0.50 |
N8* | 0.1952 (7) | 0.1990 (6) | 0.7866 (7) | 0.06293 (2)* | 0.50 |
C1 | 1.1821 (3) | 0.2085 (2) | 0.3605 (2) | 0.0445 (5) | |
C2 | 1.2074 (3) | 0.3058 (2) | 0.3264 (2) | 0.0436 (5) | |
C3 | 1.0286 (4) | 0.0534 (2) | 0.3601 (3) | 0.0533 (7) | |
C4 | 1.1244 (5) | 0.0196 (3) | 0.4164 (4) | 0.069 (1) | |
C5 | 1.2510 (5) | 0.0827 (4) | 0.4472 (4) | 0.074 (1) | |
C6 | 1.2838 (3) | 0.1805 (3) | 0.4187 (3) | 0.0604 (8) | |
C7 | 1.4120 (4) | 0.2520 (5) | 0.4421 (4) | 0.082 (1) | |
C8 | 1.4358 (3) | 0.3451 (4) | 0.4090 (4) | 0.080 (1) | |
C9 | 1.3344 (3) | 0.3759 (3) | 0.3504 (3) | 0.0586 (8) | |
C10 | 1.3520 (3) | 0.4708 (3) | 0.3140 (3) | 0.0656 (9) | |
C11 | 1.2468 (4) | 0.4891 (2) | 0.2558 (3) | 0.0595 (8) | |
C12 | 1.1237 (3) | 0.4148 (2) | 0.2330 (3) | 0.0466 (6) | |
C13 | 0.8797 (2) | 0.3372 (2) | 0.3883 (2) | 0.0384 (5) | |
C14 | 0.8203 (2) | 0.3445 (2) | 0.2671 (2) | 0.0393 (5) | |
C15 | 1.0063 (3) | 0.2712 (2) | 0.5178 (2) | 0.0452 (6) | |
C16 | 0.9959 (3) | 0.3192 (3) | 0.6161 (2) | 0.0537 (7) | |
C17 | 0.9257 (3) | 0.3772 (3) | 0.5989 (3) | 0.0535 (7) | |
C18 | 0.8657 (3) | 0.3887 (2) | 0.4820 (3) | 0.0464 (6) | |
C19 | 0.7925 (3) | 0.4500 (3) | 0.4519 (3) | 0.0580 (8) | |
C20 | 0.7381 (3) | 0.4583 (3) | 0.3368 (4) | 0.0593 (8) | |
C21 | 0.7510 (3) | 0.4054 (2) | 0.2405 (3) | 0.0483 (6) | |
C22 | 0.6984 (3) | 0.4109 (3) | 0.1186 (3) | 0.0592 (8) | |
C23 | 0.7172 (3) | 0.3570 (3) | 0.0341 (3) | 0.0546 (7) | |
C24 | 0.7865 (3) | 0.2973 (2) | 0.0685 (2) | 0.0450 (5) | |
C25 | 0.7279 (3) | 0.0257 (2) | 0.1231 (2) | 0.0465 (6) | |
C26 | 0.8023 (3) | 0.0499 (2) | 0.0506 (2) | 0.0462 (6) | |
C27 | 0.7086 (3) | 0.0731 (2) | 0.2991 (3) | 0.0497 (6) | |
C28 | 0.5906 (3) | −0.0116 (3) | 0.2661 (3) | 0.0625 (8) | |
C29 | 0.5423 (3) | −0.0805 (3) | 0.1608 (4) | 0.072 (1) | |
C30 | 0.6112 (4) | −0.0624 (3) | 0.0837 (3) | 0.0649 (9) | |
C31 | 0.5716 (5) | −0.1274 (4) | −0.0294 (4) | 0.098 (2) | |
C32 | 0.6421 (5) | −0.1050 (4) | −0.0970 (4) | 0.101 (2) | |
C33 | 0.7605 (4) | −0.0149 (3) | −0.0602 (3) | 0.0684 (10) | |
C34 | 0.8402 (5) | 0.0136 (3) | −0.1263 (4) | 0.081 (1) | |
C35 | 0.9491 (4) | 0.1017 (3) | −0.0821 (3) | 0.071 (1) | |
C36 | 0.9836 (3) | 0.1631 (2) | 0.0290 (3) | 0.0515 (6) | |
C37 | 0.7167 (3) | 0.2075 (3) | 0.7027 (3) | 0.0548 (7) | |
C38 | 0.454 (2) | 0.402 (2) | 0.817 (2) | 0.16803 (9)* | 0.50 |
C38* | 0.269 (1) | 0.2452 (8) | 0.7574 (9) | 0.08233 (3)* | 0.50 |
H3 | 0.9405 | 0.0081 | 0.3389 | 0.0643* | |
H4 | 1.1007 | −0.0480 | 0.4334 | 0.0793* | |
H5 | 1.3151 | 0.0588 | 0.4862 | 0.0895* | |
H7 | 1.4841 | 0.2354 | 0.4789 | 0.0970* | |
H8 | 1.5227 | 0.3920 | 0.4259 | 0.0903* | |
H10 | 1.4368 | 0.5229 | 0.3315 | 0.0764* | |
H11 | 1.2575 | 0.5527 | 0.2291 | 0.0724* | |
H12 | 1.0505 | 0.4284 | 0.1907 | 0.0568* | |
H15 | 1.0575 | 0.2319 | 0.5315 | 0.0547* | |
H16 | 1.0372 | 0.3105 | 0.6951 | 0.0636* | |
H17 | 0.9179 | 0.4107 | 0.6645 | 0.0639* | |
H19 | 0.7818 | 0.4855 | 0.5145 | 0.0684* | |
H20 | 0.6898 | 0.4995 | 0.3200 | 0.0711* | |
H22 | 0.6507 | 0.4515 | 0.0943 | 0.0710* | |
H23 | 0.6823 | 0.3602 | −0.0486 | 0.0658* | |
H24 | 0.7982 | 0.2594 | 0.0079 | 0.0526* | |
H27 | 0.7414 | 0.1188 | 0.3736 | 0.0600* | |
H28 | 0.5442 | −0.0204 | 0.3171 | 0.0744* | |
H29 | 0.4636 | −0.1403 | 0.1393 | 0.0855* | |
H31 | 0.4951 | −0.1900 | −0.0545 | 0.1179* | |
H32 | 0.6116 | −0.1471 | −0.1746 | 0.1129* | |
H34 | 0.8158 | −0.0284 | −0.2031 | 0.0959* | |
H35 | 1.0058 | 0.1223 | −0.1258 | 0.0828* | |
H36 | 1.0604 | 0.2242 | 0.0587 | 0.0613* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0364 (2) | 0.0330 (2) | 0.0294 (2) | 0.0100 (1) | 0.0155 (1) | 0.0061 (1) |
S1 | 0.0644 (5) | 0.0778 (6) | 0.0698 (6) | 0.0178 (5) | 0.0243 (5) | −0.0161 (5) |
O3 | 0.080 (2) | 0.080 (2) | 0.083 (2) | 0.017 (2) | 0.027 (2) | 0.003 (2) |
O4 | 0.106 (3) | 0.089 (2) | 0.122 (3) | 0.025 (2) | 0.061 (2) | 0.019 (2) |
N1 | 0.049 (1) | 0.043 (1) | 0.0355 (10) | 0.0197 (9) | 0.0196 (9) | 0.0098 (8) |
N2 | 0.0400 (10) | 0.0366 (9) | 0.0340 (9) | 0.0088 (8) | 0.0181 (8) | 0.0044 (7) |
N3 | 0.0401 (10) | 0.0366 (9) | 0.0314 (9) | 0.0113 (8) | 0.0166 (8) | 0.0058 (7) |
N4 | 0.0389 (10) | 0.041 (1) | 0.0342 (9) | 0.0131 (8) | 0.0161 (8) | 0.0091 (8) |
N5 | 0.040 (1) | 0.041 (1) | 0.0355 (10) | 0.0094 (8) | 0.0161 (8) | 0.0086 (8) |
N6 | 0.048 (1) | 0.038 (1) | 0.0348 (10) | 0.0137 (9) | 0.0211 (9) | 0.0054 (8) |
N7 | 0.102 (3) | 0.089 (3) | 0.059 (2) | 0.016 (2) | 0.031 (2) | −0.004 (2) |
C1 | 0.044 (1) | 0.055 (1) | 0.036 (1) | 0.021 (1) | 0.0156 (10) | 0.007 (1) |
C2 | 0.038 (1) | 0.049 (1) | 0.036 (1) | 0.010 (1) | 0.0153 (10) | 0.0005 (10) |
C3 | 0.070 (2) | 0.048 (1) | 0.051 (2) | 0.027 (1) | 0.030 (1) | 0.018 (1) |
C4 | 0.104 (3) | 0.069 (2) | 0.062 (2) | 0.055 (2) | 0.042 (2) | 0.033 (2) |
C5 | 0.088 (3) | 0.105 (3) | 0.057 (2) | 0.067 (3) | 0.028 (2) | 0.031 (2) |
C6 | 0.058 (2) | 0.082 (2) | 0.048 (2) | 0.040 (2) | 0.016 (1) | 0.014 (2) |
C7 | 0.047 (2) | 0.124 (4) | 0.072 (2) | 0.041 (2) | 0.013 (2) | 0.016 (2) |
C8 | 0.038 (2) | 0.108 (3) | 0.075 (3) | 0.017 (2) | 0.016 (2) | 0.008 (2) |
C9 | 0.040 (1) | 0.070 (2) | 0.050 (2) | 0.006 (1) | 0.019 (1) | −0.001 (1) |
C10 | 0.052 (2) | 0.062 (2) | 0.059 (2) | −0.008 (1) | 0.031 (1) | −0.004 (1) |
C11 | 0.069 (2) | 0.043 (1) | 0.056 (2) | 0.002 (1) | 0.036 (2) | 0.005 (1) |
C12 | 0.056 (2) | 0.037 (1) | 0.045 (1) | 0.011 (1) | 0.027 (1) | 0.008 (1) |
C13 | 0.037 (1) | 0.039 (1) | 0.037 (1) | 0.0084 (9) | 0.0196 (9) | 0.0044 (9) |
C14 | 0.037 (1) | 0.041 (1) | 0.041 (1) | 0.0121 (9) | 0.0192 (9) | 0.0089 (9) |
C15 | 0.052 (1) | 0.047 (1) | 0.033 (1) | 0.015 (1) | 0.017 (1) | 0.0081 (10) |
C16 | 0.066 (2) | 0.057 (2) | 0.031 (1) | 0.016 (1) | 0.021 (1) | 0.006 (1) |
C17 | 0.063 (2) | 0.056 (2) | 0.041 (1) | 0.015 (1) | 0.030 (1) | 0.002 (1) |
C18 | 0.045 (1) | 0.045 (1) | 0.047 (1) | 0.009 (1) | 0.027 (1) | 0.002 (1) |
C19 | 0.060 (2) | 0.060 (2) | 0.068 (2) | 0.026 (1) | 0.038 (2) | 0.005 (1) |
C20 | 0.056 (2) | 0.064 (2) | 0.074 (2) | 0.033 (2) | 0.035 (2) | 0.012 (2) |
C21 | 0.043 (1) | 0.052 (1) | 0.057 (2) | 0.021 (1) | 0.026 (1) | 0.016 (1) |
C22 | 0.055 (2) | 0.070 (2) | 0.068 (2) | 0.037 (2) | 0.027 (2) | 0.032 (2) |
C23 | 0.051 (2) | 0.065 (2) | 0.049 (2) | 0.024 (1) | 0.018 (1) | 0.026 (1) |
C24 | 0.044 (1) | 0.053 (1) | 0.036 (1) | 0.017 (1) | 0.016 (1) | 0.013 (1) |
C25 | 0.045 (1) | 0.043 (1) | 0.039 (1) | 0.006 (1) | 0.015 (1) | 0.005 (1) |
C26 | 0.052 (1) | 0.042 (1) | 0.037 (1) | 0.010 (1) | 0.019 (1) | 0.0021 (10) |
C27 | 0.047 (1) | 0.056 (2) | 0.042 (1) | 0.011 (1) | 0.023 (1) | 0.013 (1) |
C28 | 0.048 (2) | 0.071 (2) | 0.058 (2) | 0.005 (1) | 0.028 (1) | 0.016 (2) |
C29 | 0.049 (2) | 0.070 (2) | 0.065 (2) | −0.011 (2) | 0.024 (2) | 0.007 (2) |
C30 | 0.056 (2) | 0.057 (2) | 0.053 (2) | −0.005 (1) | 0.019 (1) | −0.001 (1) |
C31 | 0.085 (3) | 0.075 (3) | 0.071 (3) | −0.027 (2) | 0.027 (2) | −0.023 (2) |
C32 | 0.102 (3) | 0.079 (3) | 0.066 (2) | −0.019 (2) | 0.036 (2) | −0.033 (2) |
C33 | 0.078 (2) | 0.058 (2) | 0.047 (2) | 0.004 (2) | 0.026 (2) | −0.010 (1) |
C34 | 0.103 (3) | 0.070 (2) | 0.055 (2) | 0.011 (2) | 0.043 (2) | −0.012 (2) |
C35 | 0.089 (3) | 0.069 (2) | 0.058 (2) | 0.018 (2) | 0.050 (2) | 0.001 (2) |
C36 | 0.062 (2) | 0.049 (1) | 0.047 (1) | 0.016 (1) | 0.033 (1) | 0.007 (1) |
C37 | 0.055 (2) | 0.054 (2) | 0.054 (2) | 0.016 (1) | 0.026 (1) | 0.012 (1) |
Fe1—N1 | 1.974 (3) | C11—H11 | 0.956 |
Fe1—N2 | 1.976 (2) | C12—H12 | 0.957 |
Fe1—N3 | 1.978 (2) | C13—C14 | 1.425 (4) |
Fe1—N4 | 1.969 (3) | C13—C18 | 1.403 (5) |
Fe1—N5 | 1.982 (2) | C14—C21 | 1.393 (5) |
Fe1—N6 | 1.973 (2) | C15—C16 | 1.400 (5) |
S1—C37 | 1.624 (3) | C15—H15 | 0.959 |
S2—C38 | 1.63 (2) | C16—C17 | 1.364 (6) |
S2—C38* | 1.60 (1) | C16—H16 | 0.955 |
N1—C1 | 1.365 (4) | C17—C18 | 1.401 (4) |
N1—C3 | 1.334 (4) | C17—H17 | 0.949 |
N2—C2 | 1.360 (4) | C18—C19 | 1.436 (6) |
N2—C12 | 1.331 (4) | C19—C20 | 1.355 (5) |
N3—C13 | 1.362 (4) | C19—H19 | 0.955 |
N3—C15 | 1.331 (3) | C20—C21 | 1.431 (6) |
N4—C14 | 1.363 (4) | C20—H20 | 0.955 |
N4—C24 | 1.337 (4) | C21—C22 | 1.411 (5) |
N5—C25 | 1.364 (3) | C22—C23 | 1.369 (6) |
N5—C27 | 1.334 (5) | C22—H22 | 0.951 |
N6—C26 | 1.360 (3) | C23—C24 | 1.387 (6) |
N6—C36 | 1.331 (5) | C23—H23 | 0.956 |
N7—C37 | 1.142 (5) | C24—H24 | 0.960 |
N8—C38 | 1.35 (2) | C25—C26 | 1.422 (5) |
N8*—C38* | 1.07 (1) | C25—C30 | 1.405 (4) |
C1—C2 | 1.420 (4) | C26—C33 | 1.399 (5) |
C1—C6 | 1.406 (6) | C27—C28 | 1.396 (4) |
C2—C9 | 1.407 (4) | C27—H27 | 0.945 |
C3—C4 | 1.397 (7) | C28—C29 | 1.364 (5) |
C3—H3 | 0.954 | C28—H28 | 0.946 |
C4—C5 | 1.364 (7) | C29—C30 | 1.417 (7) |
C4—H4 | 0.952 | C29—H29 | 0.955 |
C5—C6 | 1.397 (7) | C30—C31 | 1.428 (6) |
C5—H5 | 0.951 | C31—C32 | 1.336 (9) |
C6—C7 | 1.426 (5) | C31—H31 | 0.958 |
C7—C8 | 1.362 (9) | C32—C33 | 1.432 (6) |
C7—H7 | 0.957 | C32—H32 | 0.956 |
C8—C9 | 1.429 (7) | C33—C34 | 1.410 (8) |
C8—H8 | 0.957 | C34—C35 | 1.354 (5) |
C9—C10 | 1.407 (6) | C34—H34 | 0.963 |
C10—C11 | 1.358 (6) | C35—C36 | 1.400 (5) |
C10—H10 | 0.961 | C35—H35 | 0.971 |
C11—C12 | 1.395 (4) | C36—H36 | 0.946 |
N1—Fe1—N2 | 82.8 (1) | N4—C14—C13 | 115.6 (3) |
N1—Fe1—N3 | 93.6 (1) | N4—C14—C21 | 123.9 (3) |
N1—Fe1—N4 | 174.05 (7) | C13—C14—C21 | 120.5 (3) |
N1—Fe1—N5 | 95.9 (1) | N3—C15—C16 | 122.7 (3) |
N1—Fe1—N6 | 89.7 (1) | N3—C15—H15 | 118.2 |
N2—Fe1—N3 | 90.74 (9) | C16—C15—H15 | 119.1 |
N2—Fe1—N4 | 92.46 (10) | C15—C16—C17 | 120.1 (3) |
N2—Fe1—N5 | 176.8 (1) | C15—C16—H16 | 119.6 |
N2—Fe1—N6 | 94.35 (10) | C17—C16—H16 | 120.3 |
N3—Fe1—N4 | 82.8 (1) | C16—C17—C18 | 119.1 (3) |
N3—Fe1—N5 | 92.27 (10) | C16—C17—H17 | 121.3 |
N3—Fe1—N6 | 174.25 (10) | C18—C17—H17 | 119.7 |
N4—Fe1—N5 | 89.03 (10) | C13—C18—C17 | 117.3 (3) |
N4—Fe1—N6 | 94.3 (1) | C13—C18—C19 | 117.9 (3) |
N5—Fe1—N6 | 82.69 (10) | C17—C18—C19 | 124.7 (4) |
Fe1—N1—C1 | 112.7 (2) | C18—C19—C20 | 121.6 (4) |
Fe1—N1—C3 | 130.3 (2) | C18—C19—H19 | 119.1 |
C1—N1—C3 | 117.0 (3) | C20—C19—H19 | 119.3 |
Fe1—N2—C2 | 112.5 (2) | C19—C20—C21 | 120.9 (4) |
Fe1—N2—C12 | 130.2 (2) | C19—C20—H20 | 119.3 |
C2—N2—C12 | 117.3 (2) | C21—C20—H20 | 119.8 |
Fe1—N3—C13 | 112.5 (2) | C14—C21—C20 | 118.7 (3) |
Fe1—N3—C15 | 130.3 (2) | C14—C21—C22 | 116.9 (4) |
C13—N3—C15 | 117.2 (3) | C20—C21—C22 | 124.4 (4) |
Fe1—N4—C14 | 113.0 (2) | C21—C22—C23 | 119.2 (4) |
Fe1—N4—C24 | 129.7 (2) | C21—C22—H22 | 121.3 |
C14—N4—C24 | 117.3 (3) | C23—C22—H22 | 119.5 |
Fe1—N5—C25 | 112.6 (2) | C22—C23—C24 | 120.1 (3) |
Fe1—N5—C27 | 130.2 (2) | C22—C23—H23 | 119.9 |
C25—N5—C27 | 117.0 (2) | C24—C23—H23 | 120.0 |
Fe1—N6—C26 | 112.9 (2) | N4—C24—C23 | 122.6 (3) |
Fe1—N6—C36 | 129.6 (2) | N4—C24—H24 | 118.4 |
C26—N6—C36 | 117.6 (2) | C23—C24—H24 | 119.0 |
N1—C1—C2 | 115.7 (3) | N5—C25—C26 | 115.7 (2) |
N1—C1—C6 | 123.8 (3) | N5—C25—C30 | 123.8 (3) |
C2—C1—C6 | 120.4 (3) | C26—C25—C30 | 120.5 (3) |
N2—C2—C1 | 116.2 (2) | N6—C26—C25 | 116.1 (2) |
N2—C2—C9 | 123.1 (3) | N6—C26—C33 | 123.8 (3) |
C1—C2—C9 | 120.7 (3) | C25—C26—C33 | 120.0 (3) |
N1—C3—C4 | 122.4 (3) | N5—C27—C28 | 123.0 (3) |
N1—C3—H3 | 118.4 | N5—C27—H27 | 118.3 |
C4—C3—H3 | 119.2 | C28—C27—H27 | 118.7 |
C3—C4—C5 | 120.4 (4) | C27—C28—C29 | 120.2 (4) |
C3—C4—H4 | 119.5 | C27—C28—H28 | 119.5 |
C5—C4—H4 | 120.1 | C29—C28—H28 | 120.4 |
C4—C5—C6 | 119.3 (5) | C28—C29—C30 | 119.0 (3) |
C4—C5—H5 | 119.4 | C28—C29—H29 | 120.7 |
C6—C5—H5 | 121.3 | C30—C29—H29 | 120.4 |
C1—C6—C5 | 117.0 (3) | C25—C30—C29 | 117.0 (3) |
C1—C6—C7 | 118.3 (4) | C25—C30—C31 | 118.1 (4) |
C5—C6—C7 | 124.6 (5) | C29—C30—C31 | 124.9 (3) |
C6—C7—C8 | 121.1 (5) | C30—C31—C32 | 121.3 (4) |
C6—C7—H7 | 121.3 | C30—C31—H31 | 118.6 |
C8—C7—H7 | 117.6 | C32—C31—H31 | 119.9 |
C7—C8—C9 | 121.8 (4) | C31—C32—C33 | 121.9 (4) |
C7—C8—H8 | 119.6 | C31—C32—H32 | 120.2 |
C9—C8—H8 | 118.6 | C33—C32—H32 | 117.8 |
C2—C9—C8 | 117.6 (4) | C26—C33—C32 | 118.1 (4) |
C2—C9—C10 | 117.6 (3) | C26—C33—C34 | 116.7 (3) |
C8—C9—C10 | 124.8 (3) | C32—C33—C34 | 125.1 (4) |
C9—C10—C11 | 118.9 (3) | C33—C34—C35 | 119.4 (4) |
C9—C10—H10 | 121.2 | C33—C34—H34 | 120.1 |
C11—C10—H10 | 120.0 | C35—C34—H34 | 120.5 |
C10—C11—C12 | 120.2 (3) | C34—C35—C36 | 120.4 (5) |
C10—C11—H11 | 119.6 | C34—C35—H35 | 120.7 |
C12—C11—H11 | 120.2 | C36—C35—H35 | 118.9 |
N2—C12—C11 | 123.0 (3) | N6—C36—C35 | 122.1 (3) |
N2—C12—H12 | 117.8 | N6—C36—H36 | 118.6 |
C11—C12—H12 | 119.2 | C35—C36—H36 | 119.3 |
N3—C13—C14 | 116.0 (3) | S1—C37—N7 | 178.6 (5) |
N3—C13—C18 | 123.6 (2) | S2—C38—N8 | 172 (2) |
C14—C13—C18 | 120.4 (3) | S2—C38*—N8* | 173 (1) |
Experimental details
Crystal data | |
Chemical formula | [Fe(C12H8N2)3](NCS)2·3H2O |
Mr | 766.67 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 295 |
a, b, c (Å) | 12.083 (3), 14.234 (4), 12.050 (2) |
α, β, γ (°) | 93.19 (2), 109.53 (1), 111.55 (2) |
V (Å3) | 1778.7 (8) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.59 |
Crystal size (mm) | 0.6 × 0.5 × 0.5 |
Data collection | |
Diffractometer | Rigaku AFC-7R diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.658, 0.744 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10804, 10354, 8387 |
Rint | 0.007 |
(sin θ/λ)max (Å−1) | 0.703 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.062, 0.201, 1.03 |
No. of reflections | 8387 |
No. of parameters | 461 |
No. of restraints | ? |
H-atom treatment | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 1.27, −1.55 |
Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993), MSC/AFC Diffractometer Control Software, TEXSAN (Molecular Structure Corporation, 1999), SIR92 (Altomare et al., 1994), SHELXL97 (Sheldrick, 1997), TEXSAN.
Fe1—N1 | 1.974 (3) | Fe1—N4 | 1.969 (3) |
Fe1—N2 | 1.976 (2) | Fe1—N5 | 1.982 (2) |
Fe1—N3 | 1.978 (2) | Fe1—N6 | 1.973 (2) |
N1—Fe1—N2 | 82.8 (1) | N2—Fe1—N6 | 94.35 (10) |
N1—Fe1—N3 | 93.6 (1) | N3—Fe1—N4 | 82.8 (1) |
N1—Fe1—N4 | 174.05 (7) | N3—Fe1—N5 | 92.27 (10) |
N1—Fe1—N5 | 95.9 (1) | N3—Fe1—N6 | 174.25 (10) |
N1—Fe1—N6 | 89.7 (1) | N4—Fe1—N5 | 89.03 (10) |
N2—Fe1—N3 | 90.74 (9) | N4—Fe1—N6 | 94.3 (1) |
N2—Fe1—N4 | 92.46 (10) | N5—Fe1—N6 | 82.69 (10) |
N2—Fe1—N5 | 176.8 (1) |
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The October 1999 release of the Cambridge Structural Database (Allen & Kennard, 1993) contains 12 crystal structures which involve the title complex cation, i.e. [Fe(phen)3]2+. Among them, those of the simple inorganic counter-ions are [Fe(phen)3]I2·H2O·C6H5NO2 (Fujiwara et al., 1984), [Fe(phen)3]I2·2H2O (Johansson et al., 1978) and [Fe(phen)3](ClO4)2·0.5H2O (Koh et al., 1978).
Mechanochemical effects on the molecular structures, chemical states and magnetic properties have been investigated for the title compound, (I), by Tsuchiya et al. (1996).