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research papers
E. Dova, A. F. Stassen, R. A. J. Driessen, E. Sonneveld, K. Goubitz, R. Peschar, J. G. Haasnoot, J. Reedijk and H. Schenk
The structure of the coordination compound [Fe(teec)6](BF4)2, hexa[1-(2-chloroethyl)tetrazole]iron(II) di(borotetrafluoride), has been determined using the grid-search techniques of the program suite MRIA. A Guinier-camera data set was used to determine the unit cell, the space group and to position the initial model. A high-resolution synchrotron powder data set was used to position a more detailed model using torsion-angle variation and to refine the structure leading to Rp = 0.0689, Rw = 0.0805 and GoF = 1.38. The crystal structure at room temperature shows the existence of two symmetry-equivalent iron(II) ions in the high-spin state.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010876810100828X/na0120sup1.cif | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S010876810100828X/na0120sup2.rtv |
CCDC reference: 170338
Figures top
| View of the title compound with the atom numbering scheme. Displacement ellipsoids for non-H atoms are drawn at the 50% probability level. |
(stassen) top
Crystal data top
C18H30Cl6FeN24·2(BF4) | V = 2315.5 (3) Å3 |
Mr = 1024.83 | Z = 2 |
Monoclinic, P21/c | F(000) = 1032 |
Hall symbol: -P 2ybc | Dx = 1.470 Mg m−3 |
a = 12.1966 (11) Å | ?? Kα radiation, λ = 0.99542 Å |
b = 17.9677 (13) Å | T = 0 K |
c = 10.5667 (8) Å | × × mm |
β = 90.555 (5)° |
Crystal data top
C18H30Cl6FeN24·2(BF4) | β = 90.555 (5)° |
Mr = 1024.83 | V = 2315.5 (3) Å3 |
Monoclinic, P21/c | Z = 2 |
a = 12.1966 (11) Å | ?? Kα radiation, λ = 0.99542 Å |
b = 17.9677 (13) Å | T = 0 K |
c = 10.5667 (8) Å | × × mm |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Fe | 0.00000 | 0.50000 | 0.50000 | 0.049 (8)* | |
Cl1 | 0.3742 (16) | 0.7360 (11) | 0.4318 (17) | 0.135 (8)* | |
Cl2 | 0.3820 (17) | 0.4423 (11) | 0.8872 (18) | 0.1354* | |
Cl3 | 0.3944 (16) | 0.3536 (10) | 0.224 (2) | 0.1354* | |
N1A | 0.188 (2) | 0.6619 (9) | 0.2947 (18) | 0.0507* | |
N1B | 0.179 (2) | 0.5307 (12) | 0.8490 (13) | 0.0507* | |
N1C | 0.194 (2) | 0.3143 (9) | 0.375 (2) | 0.0507* | |
N2A | 0.224 (2) | 0.6015 (8) | 0.2437 (17) | 0.0507* | |
N2B | 0.212 (2) | 0.5873 (10) | 0.7853 (13) | 0.0507* | |
N2C | 0.231 (2) | 0.3198 (9) | 0.4948 (16) | 0.0507* | |
N3A | 0.175 (2) | 0.5467 (7) | 0.2963 (14) | 0.0507* | |
N3B | 0.167 (2) | 0.5857 (8) | 0.6761 (11) | 0.0507* | |
N3C | 0.177 (2) | 0.3732 (7) | 0.5466 (13) | 0.0507* | |
N4A | 0.1038 (17) | 0.5725 (7) | 0.3836 (14) | 0.0507* | |
N4B | 0.1021 (17) | 0.5274 (9) | 0.6687 (12) | 0.0507* | |
N4C | 0.1065 (17) | 0.4038 (8) | 0.4604 (15) | 0.0507* | |
C1A | 0.1112 (19) | 0.6440 (9) | 0.3786 (17) | 0.0507* | |
C1B | 0.1075 (19) | 0.4932 (11) | 0.7773 (12) | 0.0507* | |
C1C | 0.1174 (18) | 0.3651 (8) | 0.3553 (18) | 0.0507* | |
C2A | 0.221 (2) | 0.7373 (13) | 0.249 (3) | 0.0507* | |
C2B | 0.208 (2) | 0.5173 (18) | 0.9849 (17) | 0.0507* | |
C2C | 0.233 (2) | 0.2547 (11) | 0.290 (3) | 0.0507* | |
C3A | 0.341 (2) | 0.7496 (15) | 0.270 (3) | 0.0507* | |
C3B | 0.335 (2) | 0.5073 (19) | 0.994 (2) | 0.0507* | |
C3C | 0.358 (2) | 0.2599 (15) | 0.277 (3) | 0.0507* | |
F1 | 0.10593 | 0.15933 | 0.55844 | 0.0507* | |
F2 | 0.04371 | 0.17048 | 0.37391 | 0.0507* | |
F3 | −0.02864 | 0.09152 | 0.51076 | 0.0507* | |
F4 | −0.04674 | 0.21288 | 0.53886 | 0.0507* | |
B | 0.00913 | 0.15841 | 0.48901 | 0.0507* | |
H1A | 0.0608 (17) | 0.6823 (8) | 0.4334 (19) | 0.0507* | |
H1B | 0.0625 (18) | 0.4439 (12) | 0.8046 (12) | 0.0507* | |
H1C | 0.0736 (18) | 0.3746 (9) | 0.2687 (17) | 0.0507* | |
H21A | 0.172 (2) | 0.7799 (10) | 0.302 (3) | 0.0507* | |
H21B | 0.170 (3) | 0.466 (2) | 1.0170 (17) | 0.0507* | |
H21C | 0.194 (3) | 0.2609 (15) | 0.199 (3) | 0.0507* | |
H22A | 0.198 (3) | 0.7435 (17) | 0.150 (3) | 0.0507* | |
H22B | 0.182 (3) | 0.563 (2) | 1.042 (2) | 0.0507* | |
H22C | 0.214 (3) | 0.2011 (11) | 0.330 (4) | 0.0507* | |
H31A | 0.385 (2) | 0.7146 (19) | 0.207 (4) | 0.0507* | |
H31B | 0.370 (3) | 0.563 (2) | 0.982 (3) | 0.0507* | |
H31C | 0.397 (2) | 0.245 (2) | 0.361 (3) | 0.0507* | |
H32A | 0.357 (3) | 0.8085 (16) | 0.247 (5) | 0.0507* | |
H32B | 0.351 (3) | 0.491 (3) | 1.094 (3) | 0.0507* | |
H32C | 0.380 (3) | 0.221 (2) | 0.199 (4) | 0.0507* |
Geometric parameters (Å, º) top
Fe—N4A | 2.201 (16) | N3B—N4B | 1.31 (3) |
Fe—N4B | 2.220 (16) | N3C—N4C | 1.36 (3) |
Fe—N4C | 2.205 (17) | N4A—C1A | 1.29 (2) |
Cl1—C3A | 1.77 (4) | N4B—C1B | 1.30 (2) |
Cl2—C3B | 1.73 (3) | N4C—C1C | 1.32 (2) |
Cl3—C3C | 1.83 (3) | C2A—C3A | 1.49 (3) |
F1—B | 1.3841 | C2B—C3B | 1.56 (3) |
F2—B | 1.3092 | C2C—C3C | 1.53 (3) |
F3—B | 1.3082 | C1A—H1A | 1.09 (3) |
F4—B | 1.3064 | C1B—H1B | 1.08 (3) |
N1A—N2A | 1.29 (2) | C1C—H1C | 1.07 (3) |
N1A—C2A | 1.49 (3) | C2A—H22A | 1.09 (4) |
N1A—C1A | 1.34 (3) | C2A—H21A | 1.12 (4) |
N1B—N2B | 1.29 (3) | C2B—H22B | 1.07 (4) |
N1B—C1B | 1.33 (3) | C2B—H21B | 1.09 (5) |
N1B—C2B | 1.50 (2) | C2C—H21C | 1.07 (4) |
N1C—C2C | 1.48 (3) | C2C—H22C | 1.08 (3) |
N1C—C1C | 1.32 (3) | C3A—H31A | 1.06 (5) |
N1C—N2C | 1.34 (3) | C3A—H32A | 1.10 (4) |
N2A—N3A | 1.28 (2) | C3B—H32B | 1.11 (4) |
N2B—N3B | 1.27 (2) | C3B—H31B | 1.10 (5) |
N2C—N3C | 1.29 (3) | C3C—H31C | 1.04 (4) |
N3A—N4A | 1.35 (3) | C3C—H32C | 1.12 (5) |
Cl1···N1A | 2.99 (3) | N2C···H31C | 2.82 (4) |
Cl1···C1A | 3.65 (3) | N3A···H22Bii | 2.71 (3) |
Cl1···C3Ai | 3.61 (4) | N3B···H21Ai | 2.76 (3) |
Cl2···C1B | 3.65 (3) | N3C···H21Ciii | 2.90 (3) |
Cl2···N1B | 2.97 (3) | N4A···H1Bvii | 2.84 (3) |
Cl2···N2B | 3.49 (3) | N4B···H1Cvii | 2.86 (3) |
Cl3···N1C | 3.02 (3) | N4C···H1Avii | 2.80 (3) |
Cl1···H31Ai | 3.04 (5) | C1A···F2ix | 3.2890 |
Cl3···H32Bii | 2.87 (5) | C1A···F4vii | 2.8293 |
F1···C2Ciii | 3.2713 | C1A···N3B | 3.38 (2) |
F1···C1Ciii | 3.1691 | C1A···Cl1 | 3.65 (3) |
F2···C2C | 2.9062 | C1B···F3viii | 3.0171 |
F2···N1C | 3.1682 | C1B···Cl2 | 3.65 (3) |
F2···C1Biv | 3.2112 | C1B···N3C | 3.37 (2) |
F2···C1Av | 3.2890 | C1B···F3iii | 3.3525 |
F3···N1Bvi | 2.6088 | C1B···F2iii | 3.2112 |
F3···C2Bvi | 2.5628 | C1C···N3A | 3.40 (2) |
F3···N2Bvi | 3.1216 | C1C···F1iv | 3.1691 |
F3···C1Bvi | 3.0171 | C2A···N2Bx | 3.18 (3) |
F3···C1Biv | 3.3525 | C2A···N3Bx | 3.34 (3) |
F4···C2Avii | 3.2305 | C2A···F4vii | 3.2305 |
F4···C1Avii | 2.8293 | C2B···F3viii | 2.5628 |
F1···H21Ciii | 2.3201 | C2B···N3Axi | 3.36 (2) |
F1···H21Biv | 2.4250 | C2B···N2Axi | 3.13 (3) |
F1···H1Ciii | 2.3410 | C2C···F2 | 2.9062 |
F1···H22C | 2.8617 | C2C···N2Civ | 3.39 (3) |
F2···H1Biv | 2.1944 | C2C···F1iv | 3.2713 |
F2···H22C | 2.2023 | C3A···N2Bx | 3.33 (3) |
F3···H21Bvi | 2.8522 | C3A···Cl1x | 3.61 (4) |
F3···H1Biv | 2.5364 | C3B···N2Axi | 3.42 (3) |
F3···H21Biv | 2.6342 | B···H21Biv | 2.9871 |
F3···H22Bvi | 2.0130 | B···H22Bvi | 2.9095 |
F4···H22Av | 2.7600 | B···H1Biv | 2.7612 |
F4···H21Avii | 2.2866 | H1A···F4vii | 1.9140 |
F4···H1Avii | 1.9140 | H1A···N4Cvii | 2.80 (3) |
N1A···Cl1 | 2.99 (3) | H1B···N4Avii | 2.84 (3) |
N1B···Cl2 | 2.97 (3) | H1B···F2iii | 2.1944 |
N1B···F3viii | 2.6088 | H1B···Biii | 2.7612 |
N1C···F2 | 3.1682 | H1B···F3iii | 2.5364 |
N1C···Cl3 | 3.02 (3) | H1C···F1iv | 2.3410 |
N2A···C3Bii | 3.42 (3) | H1C···N4Bvii | 2.86 (3) |
N2A···C2Bii | 3.13 (3) | H21A···N2Bx | 2.44 (3) |
N2B···Cl2 | 3.49 (3) | H21A···N3Bx | 2.76 (3) |
N2B···F3viii | 3.1216 | H21A···F4vii | 2.2866 |
N2B···C2Ai | 3.18 (3) | H21B···Biii | 2.9871 |
N2B···C3Ai | 3.33 (3) | H21B···F3iii | 2.6342 |
N2C···C2Ciii | 3.39 (3) | H21B···F3viii | 2.8522 |
N3A···N4C | 3.21 (2) | H21B···F1iii | 2.4250 |
N3A···C2Bii | 3.36 (2) | H21C···F1iv | 2.3201 |
N3A···C1C | 3.40 (2) | H21C···N3Civ | 2.90 (3) |
N3B···C2Ai | 3.34 (3) | H21C···N2Civ | 2.64 (3) |
N3B···C1A | 3.38 (2) | H22A···F4ix | 2.7600 |
N3B···N4A | 3.19 (2) | H22B···F3viii | 2.0130 |
N3C···N4B | 3.19 (2) | H22B···Bviii | 2.9095 |
N3C···C1B | 3.37 (2) | H22B···N2Axi | 2.29 (3) |
N4A···N3B | 3.19 (2) | H22B···N3Axi | 2.71 (3) |
N4B···N3C | 3.19 (2) | H22C···F2 | 2.2023 |
N4C···N3A | 3.21 (2) | H22C···F1 | 2.8617 |
N2A···H31A | 2.85 (4) | H31A···N2A | 2.85 (4) |
N2A···H22Bii | 2.29 (3) | H31A···Cl1x | 3.04 (5) |
N2B···H21Ai | 2.44 (3) | H31B···N2B | 2.85 (4) |
N2B···H32Ai | 2.61 (4) | H31C···N2C | 2.82 (4) |
N2B···H31B | 2.85 (4) | H32A···N2Bx | 2.61 (4) |
N2C···H21Ciii | 2.64 (3) | H32B···Cl3xi | 2.87 (5) |
N2C···H32Ciii | 2.90 (4) | H32C···N2Civ | 2.90 (4) |
N4A—Fe—N4B | 89.8 (6) | Cl1—C3A—C2A | 110 (2) |
N4A—Fe—N4C | 90.8 (6) | Cl2—C3B—C2B | 111.9 (19) |
N4A—Fe—N4Avii | 180.00 | Cl3—C3C—C2C | 109.1 (18) |
N4A—Fe—N4Bvii | 90.2 (6) | N1A—C1A—H1A | 127.0 (18) |
N4A—Fe—N4Cvii | 89.2 (6) | N4A—C1A—H1A | 124 (2) |
N4B—Fe—N4C | 90.0 (6) | N1B—C1B—H1B | 126.4 (16) |
N4Avii—Fe—N4B | 90.2 (6) | N4B—C1B—H1B | 126.8 (19) |
N4B—Fe—N4Bvii | 180.00 | N1C—C1C—H1C | 126 (2) |
N4B—Fe—N4Cvii | 90.0 (6) | N4C—C1C—H1C | 126 (2) |
N4Avii—Fe—N4C | 89.2 (6) | N1A—C2A—H21A | 108 (2) |
N4Bvii—Fe—N4C | 90.0 (6) | N1A—C2A—H22A | 110 (3) |
N4C—Fe—N4Cvii | 180.00 | C3A—C2A—H21A | 110 (3) |
N4Avii—Fe—N4Bvii | 89.8 (6) | C3A—C2A—H22A | 112 (3) |
N4Avii—Fe—N4Cvii | 90.8 (6) | H21A—C2A—H22A | 106 (3) |
N4Bvii—Fe—N4Cvii | 90.0 (6) | N1B—C2B—H21B | 110 (2) |
N2A—N1A—C1A | 108.6 (17) | N1B—C2B—H22B | 110 (3) |
N2A—N1A—C2A | 122 (2) | C3B—C2B—H21B | 108 (3) |
C1A—N1A—C2A | 128.7 (19) | C3B—C2B—H22B | 111 (3) |
N2B—N1B—C1B | 108.0 (15) | H21B—C2B—H22B | 110 (3) |
N2B—N1B—C2B | 124 (2) | N1C—C2C—H21C | 109 (2) |
C1B—N1B—C2B | 128 (2) | N1C—C2C—H22C | 110 (3) |
N2C—N1C—C1C | 109.2 (18) | C3C—C2C—H21C | 110 (3) |
N2C—N1C—C2C | 121 (2) | C3C—C2C—H22C | 108 (3) |
C1C—N1C—C2C | 129 (2) | H21C—C2C—H22C | 110 (3) |
N1A—N2A—N3A | 107.6 (19) | Cl1—C3A—H31A | 114 (3) |
N1B—N2B—N3B | 108.8 (19) | Cl1—C3A—H32A | 108 (3) |
N1C—N2C—N3C | 106.7 (18) | C2A—C3A—H31A | 109 (3) |
N2A—N3A—N4A | 109.7 (14) | C2A—C3A—H32A | 107 (3) |
N2B—N3B—N4B | 109.0 (14) | H31A—C3A—H32A | 110 (4) |
N2C—N3C—N4C | 109.8 (15) | Cl2—C3B—H31B | 114 (2) |
Fe—N4A—N3A | 123.6 (10) | Cl2—C3B—H32B | 113 (3) |
Fe—N4A—C1A | 130.8 (15) | C2B—C3B—H31B | 106 (3) |
N3A—N4A—C1A | 105.5 (16) | C2B—C3B—H32B | 105 (3) |
Fe—N4B—N3B | 123.9 (10) | H31B—C3B—H32B | 107 (4) |
Fe—N4B—C1B | 128.7 (15) | Cl3—C3C—H31C | 113 (3) |
N3B—N4B—C1B | 107.3 (15) | Cl3—C3C—H32C | 107 (3) |
Fe—N4C—N3C | 124.0 (11) | C2C—C3C—H31C | 111 (3) |
Fe—N4C—C1C | 129.6 (14) | C2C—C3C—H32C | 106 (3) |
N3C—N4C—C1C | 106.4 (16) | H31C—C3C—H32C | 111 (4) |
N1A—C1A—N4A | 108.5 (17) | F1—B—F2 | 102.10 |
N1B—C1B—N4B | 106.8 (18) | F1—B—F3 | 102.59 |
N1C—C1C—N4C | 108.0 (18) | F1—B—F4 | 102.87 |
N1A—C2A—C3A | 111 (2) | F2—B—F3 | 115.63 |
N1B—C2B—C3B | 107.6 (18) | F2—B—F4 | 115.11 |
N1C—C2C—C3C | 110 (2) | F3—B—F4 | 115.57 |
N4B—Fe—N4A—N3A | 108.7 (17) | C1B—N1B—N2B—N3B | −2 (3) |
N4B—Fe—N4A—C1A | −73 (2) | C2B—N1B—N2B—N3B | −175 (2) |
N4C—Fe—N4A—N3A | 18.7 (17) | N2B—N1B—C1B—N4B | 2 (3) |
N4C—Fe—N4A—C1A | −162.7 (19) | C2B—N1B—C1B—N4B | 175 (2) |
N4Bvii—Fe—N4A—N3A | −71.3 (17) | N2B—N1B—C2B—C3B | −63 (3) |
N4Bvii—Fe—N4A—C1A | 107 (2) | C1B—N1B—C2B—C3B | 125 (3) |
N4Cvii—Fe—N4A—N3A | −161.3 (17) | C1C—N1C—N2C—N3C | 0 (3) |
N4Cvii—Fe—N4A—C1A | 17.3 (19) | C2C—N1C—N2C—N3C | −176 (2) |
N4A—Fe—N4B—N3B | 18.9 (17) | N2C—N1C—C1C—N4C | 1 (2) |
N4A—Fe—N4B—C1B | −163.9 (19) | C2C—N1C—C1C—N4C | 177 (2) |
N4C—Fe—N4B—N3B | 109.8 (17) | N2C—N1C—C2C—C3C | −59 (3) |
N4C—Fe—N4B—C1B | −73.1 (19) | C1C—N1C—C2C—C3C | 126 (3) |
N4Avii—Fe—N4B—N3B | −161.1 (17) | N1A—N2A—N3A—N4A | 1 (3) |
N4Avii—Fe—N4B—C1B | 16.1 (19) | N1B—N2B—N3B—N4B | 1 (3) |
N4Cvii—Fe—N4B—N3B | −70.2 (17) | N1C—N2C—N3C—N4C | −1 (2) |
N4Cvii—Fe—N4B—C1B | 106.9 (19) | N2A—N3A—N4A—Fe | −179.9 (15) |
N4A—Fe—N4C—N3C | 106.9 (16) | N2A—N3A—N4A—C1A | 1 (2) |
N4A—Fe—N4C—C1C | −72.5 (18) | N2B—N3B—N4B—Fe | 178.2 (15) |
N4B—Fe—N4C—N3C | 17.1 (16) | N2B—N3B—N4B—C1B | 1 (3) |
N4B—Fe—N4C—C1C | −162.3 (18) | N2C—N3C—N4C—Fe | −177.5 (14) |
N4Avii—Fe—N4C—N3C | −73.1 (16) | N2C—N3C—N4C—C1C | 2 (2) |
N4Avii—Fe—N4C—C1C | 107.5 (18) | Fe—N4A—C1A—N1A | 178.7 (15) |
N4Bvii—Fe—N4C—N3C | −162.9 (16) | N3A—N4A—C1A—N1A | −3 (2) |
N4Bvii—Fe—N4C—C1C | 17.7 (18) | Fe—N4B—C1B—N1B | −179.2 (15) |
C1A—N1A—N2A—N3A | −2 (3) | N3B—N4B—C1B—N1B | −2 (2) |
C2A—N1A—N2A—N3A | −175 (2) | Fe—N4C—C1C—N1C | 177.6 (15) |
N2A—N1A—C1A—N4A | 3 (3) | N3C—N4C—C1C—N1C | −2 (2) |
C2A—N1A—C1A—N4A | 175 (2) | N1A—C2A—C3A—Cl1 | −56 (3) |
N2A—N1A—C2A—C3A | −65 (3) | N1B—C2B—C3B—Cl2 | −51 (3) |
C1A—N1A—C2A—C3A | 124 (3) | N1C—C2C—C3C—Cl3 | −55 (3) |
Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) x, y, z−1; (iii) x, −y+1/2, z+1/2; (iv) x, −y+1/2, z−1/2; (v) −x, y−1/2, −z+1/2; (vi) −x, y−1/2, −z+3/2; (vii) −x, −y+1, −z+1; (viii) −x, y+1/2, −z+3/2; (ix) −x, y+1/2, −z+1/2; (x) x, −y+3/2, z−1/2; (xi) x, y, z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C1A—H1A···F4vii | 1.09 (3) | 1.9140 | 2.8293 | 138.82 |
C1B—H1B···F2iii | 1.08 (3) | 2.1944 | 3.2112 | 155.50 |
C1B—H1B···F3iii | 1.08 (3) | 2.5364 | 3.3525 | 131.43 |
C1C—H1C···F1iv | 1.07 (3) | 2.3410 | 3.1691 | 133.12 |
C2A—H21A···F4vii | 1.12 (4) | 2.2866 | 3.2305 | 140.12 |
C2A—H21A···N2Bx | 1.12 (4) | 2.44 (3) | 3.18 (3) | 121 (2) |
C2B—H21B···F1iii | 1.09 (5) | 2.4250 | 3.4993 | 169.28 |
C2C—H21C···F1iv | 1.07 (4) | 2.3201 | 3.2713 | 146.63 |
C2B—H22B···N2Axi | 1.07 (4) | 2.29 (3) | 3.13 (3) | 134 (3) |
C2B—H22B···F3viii | 1.07 (4) | 2.0130 | 2.5628 | 108.61 |
C2C—H22C···F2 | 1.08 (3) | 2.2023 | 2.9062 | 120.84 |
C3A—H32A···N2Bx | 1.10 (4) | 2.61 (4) | 3.33 (3) | 122 (3) |
Symmetry codes: (iii) x, −y+1/2, z+1/2; (iv) x, −y+1/2, z−1/2; (vii) −x, −y+1, −z+1; (viii) −x, y+1/2, −z+3/2; (x) x, −y+3/2, z−1/2; (xi) x, y, z+1. |
Experimental details
Crystal data | |
Chemical formula | C18H30Cl6FeN24·2(BF4) |
Mr | 1024.83 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 0 |
a, b, c (Å) | 12.1966 (11), 17.9677 (13), 10.5667 (8) |
β (°) | 90.555 (5) |
V (Å3) | 2315.5 (3) |
Z | 2 |
Radiation type | ?? Kα, λ = 0.99542 Å |
µ (mm−1) | ? |
Crystal size (mm) | × × |
Data collection | |
Diffractometer | ? |
Absorption correction | – |
No. of measured, independent and observed (?) reflections | ?, ?, ? |
Rint | ? |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | ?, ?, ? |
No. of reflections | ? |
No. of parameters | ? |
H-atom treatment | See text |
Δρmax, Δρmin (e Å−3) | ?, ? |
Computer programs: PLATON (Spek, 1990).
Selected geometric parameters (Å, º) top
Fe—N4A | 2.201 (16) | N1B—C1B | 1.33 (3) |
Fe—N4B | 2.220 (16) | N1B—C2B | 1.50 (2) |
Fe—N4C | 2.205 (17) | N1C—C2C | 1.48 (3) |
Cl1—C3A | 1.77 (4) | N1C—C1C | 1.32 (3) |
Cl2—C3B | 1.73 (3) | N1C—N2C | 1.34 (3) |
Cl3—C3C | 1.83 (3) | N2A—N3A | 1.28 (2) |
F1—B | 1.3841 | N2B—N3B | 1.27 (2) |
F2—B | 1.3092 | N2C—N3C | 1.29 (3) |
F3—B | 1.3082 | N3A—N4A | 1.35 (3) |
F4—B | 1.3064 | N3B—N4B | 1.31 (3) |
N1A—N2A | 1.29 (2) | N3C—N4C | 1.36 (3) |
N1A—C2A | 1.49 (3) | N4A—C1A | 1.29 (2) |
N1A—C1A | 1.34 (3) | N4B—C1B | 1.30 (2) |
N1B—N2B | 1.29 (3) | N4C—C1C | 1.32 (2) |
N4A—Fe—N4B | 89.8 (6) | N2A—N3A—N4A | 109.7 (14) |
N4A—Fe—N4C | 90.8 (6) | N2B—N3B—N4B | 109.0 (14) |
N4A—Fe—N4Ai | 180.00 | N2C—N3C—N4C | 109.8 (15) |
N4A—Fe—N4Bi | 90.2 (6) | Fe—N4A—N3A | 123.6 (10) |
N4A—Fe—N4Ci | 89.2 (6) | Fe—N4A—C1A | 130.8 (15) |
N4B—Fe—N4C | 90.0 (6) | N3A—N4A—C1A | 105.5 (16) |
N4Ai—Fe—N4B | 90.2 (6) | Fe—N4B—N3B | 123.9 (10) |
N4B—Fe—N4Bi | 180.00 | Fe—N4B—C1B | 128.7 (15) |
N4B—Fe—N4Ci | 90.0 (6) | N3B—N4B—C1B | 107.3 (15) |
N4Ai—Fe—N4C | 89.2 (6) | Fe—N4C—N3C | 124.0 (11) |
N4Bi—Fe—N4C | 90.0 (6) | Fe—N4C—C1C | 129.6 (14) |
N4C—Fe—N4Ci | 180.00 | N3C—N4C—C1C | 106.4 (16) |
N4Ai—Fe—N4Bi | 89.8 (6) | N1A—C1A—N4A | 108.5 (17) |
N4Ai—Fe—N4Ci | 90.8 (6) | N1B—C1B—N4B | 106.8 (18) |
N4Bi—Fe—N4Ci | 90.0 (6) | N1C—C1C—N4C | 108.0 (18) |
N2A—N1A—C1A | 108.6 (17) | N1A—C2A—C3A | 111 (2) |
N2A—N1A—C2A | 122 (2) | N1B—C2B—C3B | 107.6 (18) |
C1A—N1A—C2A | 128.7 (19) | N1C—C2C—C3C | 110 (2) |
N2B—N1B—C1B | 108.0 (15) | Cl1—C3A—C2A | 110 (2) |
N2B—N1B—C2B | 124 (2) | Cl2—C3B—C2B | 111.9 (19) |
C1B—N1B—C2B | 128 (2) | Cl3—C3C—C2C | 109.1 (18) |
N2C—N1C—C1C | 109.2 (18) | F1—B—F2 | 102.10 |
N2C—N1C—C2C | 121 (2) | F1—B—F3 | 102.59 |
C1C—N1C—C2C | 129 (2) | F1—B—F4 | 102.87 |
N1A—N2A—N3A | 107.6 (19) | F2—B—F3 | 115.63 |
N1B—N2B—N3B | 108.8 (19) | F2—B—F4 | 115.11 |
N1C—N2C—N3C | 106.7 (18) | F3—B—F4 | 115.57 |
Symmetry code: (i) −x, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C1A—H1A···F4i | 1.09 (3) | 1.9140 | 2.8293 | 138.82 |
C1B—H1B···F2ii | 1.08 (3) | 2.1944 | 3.2112 | 155.50 |
C1B—H1B···F3ii | 1.08 (3) | 2.5364 | 3.3525 | 131.43 |
C1C—H1C···F1iii | 1.07 (3) | 2.3410 | 3.1691 | 133.12 |
C2A—H21A···F4i | 1.12 (4) | 2.2866 | 3.2305 | 140.12 |
C2A—H21A···N2Biv | 1.12 (4) | 2.44 (3) | 3.18 (3) | 121 (2) |
C2B—H21B···F1ii | 1.09 (5) | 2.4250 | 3.4993 | 169.28 |
C2C—H21C···F1iii | 1.07 (4) | 2.3201 | 3.2713 | 146.63 |
C2B—H22B···N2Av | 1.07 (4) | 2.29 (3) | 3.13 (3) | 134 (3) |
C2B—H22B···F3vi | 1.07 (4) | 2.0130 | 2.5628 | 108.61 |
C2C—H22C···F2 | 1.08 (3) | 2.2023 | 2.9062 | 120.84 |
C3A—H32A···N2Biv | 1.10 (4) | 2.61 (4) | 3.33 (3) | 122 (3) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) x, −y+1/2, z+1/2; (iii) x, −y+1/2, z−1/2; (iv) x, −y+3/2, z−1/2; (v) x, y, z+1; (vi) −x, y+1/2, −z+3/2. |
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