In the title compound, [Fe(C
9H
10BN
6)
2][FeCl
4]·C
2H
3N, extensive weak C—H
Cl/N interactions exist between the octahedral [Fe(HBpz
3)
2]
+ cations [HBpz
3− is hydrotris(pyrazolyl)borate], tetrahedral FeCl
4− anions and acetonitrile solvent molecules.
Supporting information
CCDC reference: 283973
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.047
- wR factor = 0.127
- Data-to-parameter ratio = 13.4
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.95
Alert level C
REFLT03_ALERT_3_C Reflection count < 95% complete
From the CIF: _diffrn_reflns_theta_max 25.00
From the CIF: _diffrn_reflns_theta_full 25.00
From the CIF: _reflns_number_total 5080
TEST2: Reflns within _diffrn_reflns_theta_max
Count of symmetry unique reflns 5355
Completeness (_total/calc) 94.86%
PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.95
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C19
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Fe2
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2 .. CL1 .. 2.87 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H17 .. CL2 .. 3.15 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H6 .. CL3 .. 2.99 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H9 .. CL3 .. 3.10 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H4 .. CL4 .. 3.08 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H20C .. CL4 .. 2.95 Ang.
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
14 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
9 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CrystalClear (Rigaku, 2002); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Bis[hydrotris(1-pyrazolyl)borato-
κ3N,
N',
N'']iron(III)
tetrachloroferrate(III) acetonitrile solvate
top
Crystal data top
[Fe(C9H10BN6)2][FeCl4]·C2H3N | F(000) = 1456 |
Mr = 720.63 | Dx = 1.577 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 9.779 (4) Å | Cell parameters from 3568 reflections |
b = 20.122 (8) Å | θ = 3.1–25.0° |
c = 15.667 (6) Å | µ = 1.34 mm−1 |
β = 100.011 (5)° | T = 293 K |
V = 3036 (2) Å3 | Block, red |
Z = 4 | 0.32 × 0.26 × 0.18 mm |
Data collection top
Rigaku Mercury CCD-detector diffractometer | 5080 independent reflections |
Radiation source: rotating anode | 4174 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
ω scans | θmax = 25.0°, θmin = 3.1° |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2002) | h = −11→5 |
Tmin = 0.673, Tmax = 0.794 | k = −23→21 |
9914 measured reflections | l = −18→17 |
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)] = 0.047 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.127 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0689P)2] where P = (Fo2 + 2Fc2)/3 |
5080 reflections | (Δ/σ)max = 0.001 |
379 parameters | Δρmax = 0.67 e Å−3 |
0 restraints | Δρmin = −0.73 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 | |
Fe1 | 0.46838 (5) | 0.74982 (2) | 0.07538 (3) | 0.02420 (15) | |
Fe2 | 0.00331 (5) | 0.42813 (3) | 0.29761 (4) | 0.04142 (18) | |
Cl1 | −0.20656 (10) | 0.44766 (6) | 0.32307 (7) | 0.0641 (3) | |
Cl2 | 0.14725 (11) | 0.42009 (7) | 0.41963 (8) | 0.0726 (4) | |
Cl3 | 0.06386 (11) | 0.51080 (5) | 0.22107 (8) | 0.0592 (3) | |
Cl4 | 0.00150 (12) | 0.33578 (5) | 0.22233 (8) | 0.0669 (3) | |
B1 | 0.4800 (4) | 0.60657 (19) | 0.1472 (3) | 0.0337 (9) | |
H1B | 0.483 (3) | 0.5561 (17) | 0.174 (2) | 0.040 (10)* | |
B2 | 0.4564 (4) | 0.89358 (19) | 0.0060 (2) | 0.0306 (9) | |
H2B | 0.455 (3) | 0.9449 (15) | −0.0170 (19) | 0.028 (8)* | |
N1 | 0.4134 (3) | 0.66944 (12) | 0.00872 (17) | 0.0287 (6) | |
N2 | 0.4212 (3) | 0.60917 (13) | 0.04966 (18) | 0.0315 (6) | |
N3 | 0.3721 (3) | 0.71642 (13) | 0.16531 (17) | 0.0300 (6) | |
N4 | 0.3876 (3) | 0.65190 (13) | 0.19168 (18) | 0.0311 (6) | |
N5 | 0.6343 (3) | 0.70309 (13) | 0.13139 (17) | 0.0293 (6) | |
N6 | 0.6246 (3) | 0.63916 (13) | 0.15946 (17) | 0.0309 (6) | |
N7 | 0.5233 (3) | 0.82934 (12) | 0.14306 (16) | 0.0263 (6) | |
N8 | 0.5128 (3) | 0.89044 (12) | 0.10418 (17) | 0.0277 (6) | |
N9 | 0.5640 (3) | 0.78394 (12) | −0.01459 (16) | 0.0280 (6) | |
N10 | 0.5507 (3) | 0.84883 (13) | −0.03861 (16) | 0.0287 (6) | |
N11 | 0.3031 (3) | 0.79667 (13) | 0.01915 (17) | 0.0285 (6) | |
N12 | 0.3129 (3) | 0.86088 (12) | −0.00811 (16) | 0.0295 (6) | |
C1 | 0.3652 (3) | 0.65859 (17) | −0.0750 (2) | 0.0352 (8) | |
H1 | 0.3498 | 0.6913 | −0.1176 | 0.042* | |
C2 | 0.3415 (4) | 0.59092 (18) | −0.0893 (3) | 0.0435 (9) | |
H2 | 0.3083 | 0.5699 | −0.1416 | 0.052* | |
C3 | 0.3779 (3) | 0.56202 (17) | −0.0089 (2) | 0.0377 (9) | |
H3 | 0.3731 | 0.5169 | 0.0028 | 0.045* | |
C4 | 0.2856 (4) | 0.74516 (16) | 0.2121 (2) | 0.0324 (8) | |
H4 | 0.2576 | 0.7894 | 0.2075 | 0.039* | |
C5 | 0.2442 (4) | 0.69918 (18) | 0.2683 (2) | 0.0379 (8) | |
H5 | 0.1842 | 0.7060 | 0.3075 | 0.046* | |
C6 | 0.3109 (4) | 0.64139 (17) | 0.2536 (2) | 0.0354 (8) | |
H6 | 0.3041 | 0.6013 | 0.2821 | 0.042* | |
C7 | 0.7684 (3) | 0.71971 (17) | 0.1483 (2) | 0.0340 (8) | |
H7 | 0.8041 | 0.7608 | 0.1363 | 0.041* | |
C8 | 0.8470 (4) | 0.66644 (17) | 0.1867 (2) | 0.0373 (8) | |
H8 | 0.9426 | 0.6648 | 0.2048 | 0.045* | |
C9 | 0.7522 (4) | 0.61691 (18) | 0.1917 (2) | 0.0361 (8) | |
H9 | 0.7733 | 0.5746 | 0.2140 | 0.043* | |
C10 | 0.5729 (3) | 0.83931 (17) | 0.2266 (2) | 0.0331 (8) | |
H10 | 0.5903 | 0.8060 | 0.2682 | 0.040* | |
C11 | 0.5951 (4) | 0.90663 (17) | 0.2427 (2) | 0.0363 (8) | |
H11 | 0.6293 | 0.9270 | 0.2954 | 0.044* | |
C12 | 0.5553 (3) | 0.93648 (16) | 0.1636 (2) | 0.0331 (8) | |
H12 | 0.5577 | 0.9819 | 0.1532 | 0.040* | |
C13 | 0.6509 (4) | 0.75532 (17) | −0.0613 (2) | 0.0332 (8) | |
H13 | 0.6783 | 0.7110 | −0.0575 | 0.040* | |
C14 | 0.6935 (4) | 0.80227 (18) | −0.1161 (2) | 0.0376 (8) | |
H14 | 0.7531 | 0.7958 | −0.1556 | 0.045* | |
C15 | 0.6283 (4) | 0.86070 (18) | −0.0994 (2) | 0.0363 (8) | |
H15 | 0.6370 | 0.9014 | −0.1260 | 0.044* | |
C16 | 0.1678 (3) | 0.78144 (18) | 0.0032 (2) | 0.0373 (8) | |
H16 | 0.1309 | 0.7406 | 0.0152 | 0.045* | |
C17 | 0.0901 (4) | 0.83514 (18) | −0.0338 (2) | 0.0430 (9) | |
H17 | −0.0056 | 0.8374 | −0.0513 | 0.052* | |
C18 | 0.1854 (4) | 0.88390 (18) | −0.0387 (2) | 0.0377 (9) | |
H18 | 0.1649 | 0.9266 | −0.0600 | 0.045* | |
N13 | 0.2469 (5) | 0.41109 (19) | 0.0313 (3) | 0.0677 (11) | |
C19 | 0.1298 (6) | 0.4087 (2) | 0.0165 (3) | 0.0549 (11) | |
C20 | −0.0203 (6) | 0.4049 (3) | −0.0029 (4) | 0.0834 (16) | |
H20A | −0.0486 | 0.3869 | −0.0599 | 0.100* | |
H20B | −0.0587 | 0.4487 | −0.0003 | 0.100* | |
H20C | −0.0529 | 0.3768 | 0.0388 | 0.100* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0263 (3) | 0.0171 (3) | 0.0285 (3) | 0.00063 (17) | 0.0027 (2) | 0.00160 (17) |
Fe2 | 0.0290 (3) | 0.0433 (3) | 0.0496 (4) | −0.0035 (2) | 0.0004 (2) | 0.0146 (3) |
Cl1 | 0.0334 (5) | 0.1025 (10) | 0.0561 (7) | 0.0017 (5) | 0.0070 (5) | 0.0166 (6) |
Cl2 | 0.0375 (6) | 0.1176 (11) | 0.0575 (7) | −0.0051 (6) | −0.0065 (5) | 0.0275 (7) |
Cl3 | 0.0565 (7) | 0.0412 (6) | 0.0819 (8) | −0.0037 (5) | 0.0173 (6) | 0.0220 (5) |
Cl4 | 0.0613 (7) | 0.0382 (6) | 0.0959 (9) | −0.0041 (5) | −0.0015 (6) | 0.0050 (6) |
B1 | 0.038 (2) | 0.023 (2) | 0.039 (2) | 0.0021 (17) | 0.0036 (18) | 0.0053 (17) |
B2 | 0.041 (2) | 0.0214 (19) | 0.029 (2) | 0.0005 (16) | 0.0028 (17) | 0.0049 (16) |
N1 | 0.0314 (15) | 0.0196 (14) | 0.0337 (16) | 0.0016 (11) | 0.0018 (12) | 0.0019 (12) |
N2 | 0.0313 (15) | 0.0186 (14) | 0.0439 (17) | 0.0017 (11) | 0.0044 (13) | −0.0020 (12) |
N3 | 0.0345 (16) | 0.0213 (14) | 0.0341 (16) | 0.0023 (12) | 0.0057 (12) | 0.0037 (12) |
N4 | 0.0328 (16) | 0.0210 (14) | 0.0388 (16) | −0.0004 (12) | 0.0040 (13) | 0.0052 (12) |
N5 | 0.0310 (15) | 0.0228 (14) | 0.0330 (16) | 0.0017 (11) | 0.0026 (12) | 0.0020 (12) |
N6 | 0.0360 (16) | 0.0214 (15) | 0.0346 (15) | 0.0056 (12) | 0.0040 (12) | 0.0048 (12) |
N7 | 0.0305 (15) | 0.0208 (14) | 0.0268 (14) | −0.0002 (11) | 0.0028 (11) | 0.0046 (11) |
N8 | 0.0340 (15) | 0.0188 (14) | 0.0293 (15) | −0.0023 (11) | 0.0026 (12) | 0.0012 (12) |
N9 | 0.0329 (15) | 0.0241 (15) | 0.0258 (14) | −0.0005 (12) | 0.0018 (12) | 0.0007 (11) |
N10 | 0.0354 (16) | 0.0228 (14) | 0.0272 (15) | −0.0043 (12) | 0.0034 (12) | 0.0037 (12) |
N11 | 0.0304 (15) | 0.0209 (14) | 0.0327 (15) | −0.0003 (11) | 0.0016 (12) | −0.0011 (11) |
N12 | 0.0373 (16) | 0.0197 (14) | 0.0294 (15) | 0.0047 (12) | 0.0001 (12) | 0.0012 (11) |
C1 | 0.0350 (19) | 0.0322 (19) | 0.036 (2) | 0.0056 (15) | −0.0014 (15) | −0.0027 (15) |
C2 | 0.041 (2) | 0.035 (2) | 0.050 (2) | 0.0015 (16) | −0.0042 (18) | −0.0152 (17) |
C3 | 0.0311 (19) | 0.0208 (17) | 0.059 (2) | −0.0003 (14) | 0.0030 (17) | −0.0104 (16) |
C4 | 0.0344 (19) | 0.0292 (19) | 0.034 (2) | 0.0000 (14) | 0.0076 (16) | −0.0014 (15) |
C5 | 0.036 (2) | 0.038 (2) | 0.042 (2) | −0.0024 (16) | 0.0123 (16) | 0.0053 (17) |
C6 | 0.036 (2) | 0.035 (2) | 0.036 (2) | −0.0085 (15) | 0.0086 (16) | 0.0079 (15) |
C7 | 0.0324 (19) | 0.035 (2) | 0.0348 (19) | −0.0011 (15) | 0.0065 (15) | −0.0031 (15) |
C8 | 0.0287 (19) | 0.042 (2) | 0.039 (2) | 0.0072 (16) | −0.0016 (15) | −0.0035 (16) |
C9 | 0.041 (2) | 0.035 (2) | 0.0311 (19) | 0.0167 (16) | 0.0026 (16) | 0.0001 (15) |
C10 | 0.0352 (19) | 0.0331 (19) | 0.0293 (18) | 0.0025 (15) | 0.0009 (15) | 0.0029 (15) |
C11 | 0.041 (2) | 0.035 (2) | 0.0318 (19) | −0.0028 (16) | 0.0032 (16) | −0.0073 (15) |
C12 | 0.039 (2) | 0.0212 (17) | 0.038 (2) | −0.0039 (14) | 0.0044 (16) | −0.0052 (14) |
C13 | 0.0325 (19) | 0.036 (2) | 0.0308 (19) | 0.0020 (15) | 0.0051 (15) | −0.0069 (15) |
C14 | 0.040 (2) | 0.044 (2) | 0.031 (2) | −0.0098 (17) | 0.0144 (16) | −0.0038 (16) |
C15 | 0.043 (2) | 0.040 (2) | 0.0252 (18) | −0.0108 (16) | 0.0029 (15) | 0.0015 (15) |
C16 | 0.0304 (19) | 0.034 (2) | 0.046 (2) | −0.0028 (15) | 0.0022 (16) | −0.0061 (16) |
C17 | 0.0286 (19) | 0.046 (2) | 0.050 (2) | 0.0100 (17) | −0.0027 (16) | −0.0088 (18) |
C18 | 0.041 (2) | 0.033 (2) | 0.036 (2) | 0.0149 (16) | −0.0029 (16) | −0.0032 (16) |
N13 | 0.068 (3) | 0.059 (3) | 0.076 (3) | −0.002 (2) | 0.013 (2) | 0.002 (2) |
C19 | 0.075 (4) | 0.035 (2) | 0.059 (3) | −0.001 (2) | 0.022 (3) | −0.0015 (19) |
C20 | 0.078 (4) | 0.072 (4) | 0.103 (4) | −0.006 (3) | 0.027 (3) | 0.014 (3) |
Geometric parameters (Å, º) top
Fe1—N7 | 1.943 (3) | C1—C2 | 1.393 (5) |
Fe1—N11 | 1.945 (3) | C1—H1 | 0.9300 |
Fe1—N3 | 1.946 (3) | C2—C3 | 1.376 (5) |
Fe1—N9 | 1.947 (3) | C2—H2 | 0.9300 |
Fe1—N5 | 1.947 (3) | C3—H3 | 0.9300 |
Fe1—N1 | 1.950 (3) | C4—C5 | 1.385 (5) |
Fe2—Cl2 | 2.1741 (14) | C4—H4 | 0.9300 |
Fe2—Cl3 | 2.1915 (12) | C5—C6 | 1.372 (5) |
Fe2—Cl1 | 2.1933 (14) | C5—H5 | 0.9300 |
Fe2—Cl4 | 2.1994 (14) | C6—H6 | 0.9300 |
B1—N4 | 1.534 (5) | C7—C8 | 1.392 (5) |
B1—N2 | 1.537 (5) | C7—H7 | 0.9300 |
B1—N6 | 1.540 (5) | C8—C9 | 1.373 (5) |
B1—H1B | 1.10 (3) | C8—H8 | 0.9300 |
B2—N12 | 1.531 (5) | C9—H9 | 0.9300 |
B2—N10 | 1.541 (5) | C10—C11 | 1.388 (4) |
B2—N8 | 1.542 (5) | C10—H10 | 0.9300 |
B2—H2B | 1.09 (3) | C11—C12 | 1.371 (5) |
N1—C1 | 1.333 (4) | C11—H11 | 0.9300 |
N1—N2 | 1.368 (4) | C12—H12 | 0.9300 |
N2—C3 | 1.337 (4) | C13—C14 | 1.389 (5) |
N3—C4 | 1.343 (4) | C13—H13 | 0.9300 |
N3—N4 | 1.363 (4) | C14—C15 | 1.384 (5) |
N4—C6 | 1.342 (4) | C14—H14 | 0.9300 |
N5—C7 | 1.335 (4) | C15—H15 | 0.9300 |
N5—N6 | 1.368 (4) | C16—C17 | 1.388 (5) |
N6—C9 | 1.339 (4) | C16—H16 | 0.9300 |
N7—C10 | 1.329 (4) | C17—C18 | 1.365 (5) |
N7—N8 | 1.368 (3) | C17—H17 | 0.9300 |
N8—C12 | 1.328 (4) | C18—H18 | 0.9300 |
N9—C13 | 1.343 (4) | N13—C19 | 1.130 (6) |
N9—N10 | 1.359 (3) | C19—C20 | 1.448 (7) |
N10—C15 | 1.339 (4) | C20—H20A | 0.9600 |
N11—C16 | 1.339 (4) | C20—H20B | 0.9600 |
N11—N12 | 1.369 (4) | C20—H20C | 0.9600 |
N12—C18 | 1.338 (4) | | |
| | | |
N7—Fe1—N11 | 88.70 (11) | N12—N11—Fe1 | 120.0 (2) |
N7—Fe1—N3 | 90.69 (11) | C18—N12—N11 | 109.1 (3) |
N11—Fe1—N3 | 91.52 (11) | C18—N12—B2 | 132.6 (3) |
N7—Fe1—N9 | 89.00 (11) | N11—N12—B2 | 118.2 (2) |
N11—Fe1—N9 | 88.13 (11) | N1—C1—C2 | 109.8 (3) |
N3—Fe1—N9 | 179.54 (11) | N1—C1—H1 | 125.1 |
N7—Fe1—N5 | 91.27 (11) | C2—C1—H1 | 125.1 |
N11—Fe1—N5 | 179.79 (12) | C3—C2—C1 | 104.9 (3) |
N3—Fe1—N5 | 88.70 (11) | C3—C2—H2 | 127.5 |
N9—Fe1—N5 | 91.66 (11) | C1—C2—H2 | 127.5 |
N7—Fe1—N1 | 179.33 (10) | N2—C3—C2 | 109.2 (3) |
N11—Fe1—N1 | 91.67 (11) | N2—C3—H3 | 125.4 |
N3—Fe1—N1 | 88.74 (11) | C2—C3—H3 | 125.4 |
N9—Fe1—N1 | 91.57 (11) | N3—C4—C5 | 109.9 (3) |
N5—Fe1—N1 | 88.36 (11) | N3—C4—H4 | 125.0 |
Cl2—Fe2—Cl3 | 110.02 (5) | C5—C4—H4 | 125.0 |
Cl2—Fe2—Cl1 | 109.67 (6) | C6—C5—C4 | 105.0 (3) |
Cl3—Fe2—Cl1 | 108.29 (5) | C6—C5—H5 | 127.5 |
Cl2—Fe2—Cl4 | 110.63 (6) | C4—C5—H5 | 127.5 |
Cl3—Fe2—Cl4 | 109.01 (6) | N4—C6—C5 | 109.2 (3) |
Cl1—Fe2—Cl4 | 109.17 (5) | N4—C6—H6 | 125.4 |
N4—B1—N2 | 106.5 (3) | C5—C6—H6 | 125.4 |
N4—B1—N6 | 106.9 (3) | N5—C7—C8 | 110.0 (3) |
N2—B1—N6 | 106.6 (3) | N5—C7—H7 | 125.0 |
N4—B1—H1B | 111.0 (17) | C8—C7—H7 | 125.0 |
N2—B1—H1B | 112.7 (18) | C9—C8—C7 | 104.9 (3) |
N6—B1—H1B | 112.8 (18) | C9—C8—H8 | 127.6 |
N12—B2—N10 | 106.8 (3) | C7—C8—H8 | 127.6 |
N12—B2—N8 | 106.6 (3) | N6—C9—C8 | 109.3 (3) |
N10—B2—N8 | 106.9 (3) | N6—C9—H9 | 125.4 |
N12—B2—H2B | 113.5 (16) | C8—C9—H9 | 125.4 |
N10—B2—H2B | 112.2 (16) | N7—C10—C11 | 110.2 (3) |
N8—B2—H2B | 110.5 (16) | N7—C10—H10 | 124.9 |
C1—N1—N2 | 107.3 (3) | C11—C10—H10 | 124.9 |
C1—N1—Fe1 | 132.9 (2) | C12—C11—C10 | 104.6 (3) |
N2—N1—Fe1 | 119.8 (2) | C12—C11—H11 | 127.7 |
C3—N2—N1 | 108.8 (3) | C10—C11—H11 | 127.7 |
C3—N2—B1 | 132.7 (3) | N8—C12—C11 | 109.5 (3) |
N1—N2—B1 | 118.5 (3) | N8—C12—H12 | 125.3 |
C4—N3—N4 | 107.0 (3) | C11—C12—H12 | 125.3 |
C4—N3—Fe1 | 132.6 (2) | N9—C13—C14 | 109.3 (3) |
N4—N3—Fe1 | 120.4 (2) | N9—C13—H13 | 125.3 |
C6—N4—N3 | 108.8 (3) | C14—C13—H13 | 125.3 |
C6—N4—B1 | 133.0 (3) | C15—C14—C13 | 105.3 (3) |
N3—N4—B1 | 118.2 (3) | C15—C14—H14 | 127.4 |
C7—N5—N6 | 107.0 (3) | C13—C14—H14 | 127.4 |
C7—N5—Fe1 | 133.0 (2) | N10—C15—C14 | 108.6 (3) |
N6—N5—Fe1 | 120.0 (2) | N10—C15—H15 | 125.7 |
C9—N6—N5 | 108.9 (3) | C14—C15—H15 | 125.7 |
C9—N6—B1 | 132.8 (3) | N11—C16—C17 | 110.5 (3) |
N5—N6—B1 | 118.3 (3) | N11—C16—H16 | 124.7 |
C10—N7—N8 | 106.8 (2) | C17—C16—H16 | 124.7 |
C10—N7—Fe1 | 132.9 (2) | C18—C17—C16 | 104.7 (3) |
N8—N7—Fe1 | 120.33 (19) | C18—C17—H17 | 127.6 |
C12—N8—N7 | 108.9 (3) | C16—C17—H17 | 127.6 |
C12—N8—B2 | 133.2 (3) | N12—C18—C17 | 109.5 (3) |
N7—N8—B2 | 117.8 (2) | N12—C18—H18 | 125.3 |
C13—N9—N10 | 107.5 (3) | C17—C18—H18 | 125.3 |
C13—N9—Fe1 | 132.2 (2) | N13—C19—C20 | 179.4 (6) |
N10—N9—Fe1 | 120.3 (2) | C19—C20—H20A | 109.5 |
C15—N10—N9 | 109.2 (3) | C19—C20—H20B | 109.5 |
C15—N10—B2 | 132.6 (3) | H20A—C20—H20B | 109.5 |
N9—N10—B2 | 118.2 (3) | C19—C20—H20C | 109.5 |
C16—N11—N12 | 106.2 (3) | H20A—C20—H20C | 109.5 |
C16—N11—Fe1 | 133.7 (2) | H20B—C20—H20C | 109.5 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C3—H3···N13 | 0.93 | 2.54 | 3.398 (6) | 154 |
C2—H2···Cl1i | 0.93 | 2.87 | 3.752 (4) | 160 |
C17—H17···Cl2ii | 0.93 | 3.15 | 3.599 (4) | 112 |
C6—H6···Cl3 | 0.93 | 2.99 | 3.546 (4) | 120 |
C9—H9···Cl3iii | 0.93 | 3.10 | 3.684 (4) | 122 |
C4—H4···Cl4ii | 0.93 | 3.08 | 3.642 (4) | 121 |
C20—H20C···Cl4 | 0.96 | 2.95 | 3.764 (6) | 143 |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x, y+1/2, −z+1/2; (iii) x+1, y, z. |