Di-μ-tricyanido-tetra­cyanidobis[hydro­tris­(pyrazoylborato)]tetra­methanol­diiron(III)iron(II) di­methanol disolvate

Zhang, K.; Sato, O.

doi:10.1107/S1600536814001019

metal-organic compounds

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ISSN: 2056-9890

Volume 70| Part 2| February 2014| Page m56

doi:10.1107/S1600536814001019

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Di-μ-tricyanido-tetracyanidobis[hydrotris(pyrazoylborato)]tetramethanoldiiron(III)iron(II) dimethanol disolvate

Kuirun Zhang ^a and Osamu Sato ^a ^*

^aInstitute for Materials Chemistry and Engineering, Kyushu University, 6-1, Kasuga-koen, Fukuoka 816-0811, Japan
^*Correspondence e-mail: sato@cm.kyushu-u.ac.jp

(Received 18 December 2013; accepted 15 January 2014; online 22 January 2014)

In the title complex, [Fe^IIFe^III₂(C₉H₁₀BN₆)₂(CN)₆(CH₃OH)₄]·2CH₃OH, two [Fe^III(Tp)(CN)₃]⁻ anions [Tp is hydrotris(pyrazoylborate)] are bridged by an [Fe^II(MeOH)₄]²⁺ cation, forming a centrosymmetric trinuclear unit. These units are connected via O—H⋯O and O—H⋯N hydrogen bonds involving the uncoordinated methanol solvent molecules, forming a three-dimensional network.

CCDC reference: 981575

Related literature

For the synthesis of bis{tricyano[hydrotris(pyrazoylborate)]ferrate(III)}, see Lescouëzec et al. (2002 ). For a related structure, see Kim et al. (2004 ).

Experimental

Crystal data

[Fe₃(C₉H₁₀BN₆)₂(CN)₆(CH₄O)₄]·2CH₄O
M_r = 942.00
Monoclinic, P 2₁ /c
a = 9.261 (4) Å
b = 16.405 (7) Å
c = 14.331 (6) Å
β = 94.671 (2)°
V = 2169.9 (16) Å³
Z = 2
Mo Kα radiation
μ = 1.05 mm⁻¹
T = 123 K
0.30 × 0.20 × 0.10 mm

Data collection

Rigaku Saturn70 diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2000 ) T_min = 0.743, T_max = 0.902
16575 measured reflections
4922 independent reflections
4557 reflections with I > 2σ(I)
R_int = 0.097

Refinement

R[F² > 2σ(F²)] = 0.064
wR(F²) = 0.167
S = 1.13
4922 reflections
269 parameters
H-atom parameters constrained
Δρ_max = 0.95 e Å⁻³
Δρ_min = −0.82 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1O⋯O3	0.93	1.75	2.645 (4)	161
O2—H2O⋯N7ⁱ	0.83	1.97	2.769 (4)	161
O3—H3O⋯N9ⁱⁱ	0.85	1.97	2.815 (4)	172
O1—H1O⋯O3	0.93	1.75	2.645 (4)	161
O2—H2O⋯N7ⁱ	0.83	1.97	2.769 (4)	161
C8—H8⋯N9ⁱⁱⁱ	0.95	2.62	3.523 (5)	158
O3—H3O⋯N9ⁱⁱ	0.85	1.97	2.815 (4)	172
Symmetry codes: (i) -x, -y+1, -z+1; (ii) $[-x+1, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (iii) -x+1, -y+1, -z+2.

Data collection: CrystalClear (Rigaku, 2008 ); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

CCDC reference: 981575

Crystal structure: contains datablock I. DOI: 10.1107/S1600536814001019/pk2510sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536814001019/pk2510Isup2.hkl

checkCIF report

Introduction top

A trinuclear cyanide bridged complex was synthesized by slow evaporation. In this compound, the central iron(II) ion is coordinated by two nitrogen atoms from cyanide bridging of [Fe^III(Tp)(CN)3]^- (Tp = hydrotris(pyrazoylborate) with trans geometry, and four oxygen atoms from coordinated methanol molecules. While, the Fe^III in the [Fe^III(Tp)(CN)3]^- part is coordinated by three nitrogen atoms from Tp^- and three carbon atoms from cyanide. The Fe1—N—C—Fe2 structure unit is almost linear with Fe1—C—N and Fe2—N—C angles of 176.1 (3)° and 168.2 (3)°, respectively. Two types of hydrogen bonds O1—H10···O3 and O3—H30···N9 are present between the uncoordinated methanol molecules and [Fe^III(Tp)(CN)₃]₂[Fe^II(MeOH)₄] units, linking the trinuclear units into a three-dimensional supra-molecule. The carbon atom of the uncoordinated methanol molecules is probably disordered. An isostructural compound [Fe^III(Tp)(CN)₃]₂[Mn^II(MeOH)₄] and two methanol molecules was reported previously (Kim et al., 2004).

Experimental top

Tetra-n-butylammonium bis-[tricyano-hydrotris(pyrazoylborate)-ferrate(III)] (0.589g,0.1mmol) and ferrous perchlorate hydrated (0.018g. 0.05 mmol) in 10 ml methanol were reacted for 30 min at room temperature. Slow evaporation of the filtrate gave red crystals.

Refinement top

Carbon-bound H-atoms of pyrazole were placed in calculated positions (C—H 0.95 Å) and were included in the refinement in the riding model approximation, with U_iso(H) set to 1.2U_eq(C). The carbon-bound H-atoms of methanol, O-bound H-atoms and B-bound H-atoms were located in a difference Fourier map, and were refined with a distance restraints of C—H, O—H and B—H 0.98±0.01 Å, 0.82±0.1 Å, 1.12 Å, respectively; with U_iso(H) set to 1.2U_eq(N).

Crystal data, data collection and structure refinement details are summarized in Table 1.

Related literature top

For the synthesis of bis[tricyano[hydrotris(pyrazoylborate)]ferrate(III)], see Lescouëzec et al. (2002). For a related structure, see Kim et al. (2004).

Structure description top

For the synthesis of bis[tricyano[hydrotris(pyrazoylborate)]ferrate(III)], see Lescouëzec et al. (2002). For a related structure, see Kim et al. (2004).

Refinement details top

Crystal data, data collection and structure refinement details are summarized in Table 1.

Computing details top

Data collection: CrystalClear (Rigaku, 2008); cell refinement: CrystalClear (Rigaku, 2008); data reduction: CrystalClear (Rigaku, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

	Fig. 1. The displacement ellipsoid plot (50% probability level) of the title compound. Unlabelled atoms are related to their labelled counterparts by the symmetry operation (–x + 1, -y + 1, -z + 1).
	Fig. 2. The packing diagram of the title compound viewed along the crystallographic a–axis. H atoms are omitted to enhance clarity.

Di-µ-tricyanido-tetracyanidobis[hydrotris(pyrazoylborato)]tetramethanoldiiron(III)iron(II) dimethanol disolvate top

Crystal data top

[Fe₃(C₉H₁₀BN₆)₂(CN)₆(CH₄O)₄]·2CH₄O	F(000) = 972
M_r = 942.00	D_x = 1.442 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybc	Cell parameters from 4554 reflections
a = 9.261 (4) Å	θ = 3.1–27.5°
b = 16.405 (7) Å	µ = 1.05 mm⁻¹
c = 14.331 (6) Å	T = 123 K
β = 94.671 (2)°	Block, red
V = 2169.9 (16) Å³	0.30 × 0.20 × 0.10 mm
Z = 2

Data collection top

Rigaku Saturn70 diffractometer	4922 independent reflections
Radiation source: fine-focus sealed tube	4557 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.097
Detector resolution: 7.314 pixels mm^-1	θ_max = 27.5°, θ_min = 3.1°
ω scans	h = −12→11
Absorption correction: multi-scan (SADABS; Bruker, 2000)	k = −21→21
T_min = 0.743, T_max = 0.902	l = −18→16
16575 measured reflections

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)] = 0.064	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.167	H-atom parameters constrained
S = 1.13	w = 1/[σ²(F_o²) + (0.0721P)² + 4.4189P] where P = (F_o² + 2F_c²)/3
4922 reflections	(Δ/σ)_max = 0.001
269 parameters	Δρ_max = 0.95 e Å⁻³
0 restraints	Δρ_min = −0.82 e Å⁻³

Crystal data top

[Fe₃(C₉H₁₀BN₆)₂(CN)₆(CH₄O)₄]·2CH₄O	V = 2169.9 (16) Å³
M_r = 942.00	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 9.261 (4) Å	µ = 1.05 mm⁻¹
b = 16.405 (7) Å	T = 123 K
c = 14.331 (6) Å	0.30 × 0.20 × 0.10 mm
β = 94.671 (2)°

Data collection top

Rigaku Saturn70 diffractometer	4922 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2000)	4557 reflections with I > 2σ(I)
T_min = 0.743, T_max = 0.902	R_int = 0.097
16575 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.064	0 restraints
wR(F²) = 0.167	H-atom parameters constrained
S = 1.13	Δρ_max = 0.95 e Å⁻³
4922 reflections	Δρ_min = −0.82 e Å⁻³
269 parameters

Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe1	0.16211 (4)	0.53724 (3)	0.76431 (3)	0.01108 (15)
Fe2	0.5000	0.5000	0.5000	0.01447 (18)
O1	0.6195 (3)	0.61004 (16)	0.52139 (18)	0.0259 (6)
H1O	0.5856	0.6453	0.5654	0.031*
O2	0.3481 (3)	0.57099 (18)	0.41549 (19)	0.0295 (6)
H2O	0.2586	0.5732	0.4119	0.035*
O3	0.5843 (4)	0.71803 (18)	0.6547 (2)	0.0424 (8)
H3O	0.6238	0.7647	0.6527	0.051*
N1	0.1053 (3)	0.64652 (16)	0.71911 (18)	0.0132 (5)
N2	0.0729 (3)	0.70462 (16)	0.78192 (18)	0.0139 (5)
N3	0.0040 (3)	0.54145 (16)	0.84969 (18)	0.0136 (5)
N4	−0.0165 (3)	0.61102 (16)	0.89905 (18)	0.0146 (5)
N5	0.2907 (3)	0.58953 (16)	0.86392 (18)	0.0133 (5)
N6	0.2409 (3)	0.65368 (16)	0.91250 (18)	0.0151 (5)
N7	−0.0531 (3)	0.45434 (18)	0.6197 (2)	0.0223 (6)
N8	0.3854 (3)	0.52601 (18)	0.6178 (2)	0.0192 (6)
N9	0.2724 (3)	0.36947 (17)	0.8348 (2)	0.0210 (6)
C1	0.0913 (4)	0.6807 (2)	0.6342 (2)	0.0180 (6)
H1	0.1081	0.6539	0.5774	0.022*
C2	0.0484 (4)	0.7615 (2)	0.6417 (2)	0.0218 (7)
H2	0.0302	0.7998	0.5924	0.026*
C3	0.0379 (4)	0.77434 (19)	0.7362 (2)	0.0191 (7)
H3	0.0107	0.8239	0.7642	0.023*
C4	−0.0966 (4)	0.4884 (2)	0.8710 (2)	0.0169 (6)
H4	−0.1068	0.4348	0.8462	0.020*
C5	−0.1852 (4)	0.5225 (2)	0.9348 (2)	0.0199 (7)
H5	−0.2653	0.4978	0.9612	0.024*
C6	−0.1310 (3)	0.5999 (2)	0.9513 (2)	0.0180 (6)
H6	−0.1676	0.6390	0.9922	0.022*
C7	0.4266 (3)	0.5739 (2)	0.9010 (2)	0.0179 (6)
H7	0.4877	0.5322	0.8805	0.021*
C8	0.4640 (4)	0.6281 (2)	0.9736 (2)	0.0225 (7)
H8	0.5528	0.6307	1.0116	0.027*
C9	0.3438 (4)	0.6775 (2)	0.9786 (2)	0.0197 (7)
H9	0.3353	0.7210	1.0216	0.024*
C10	0.2287 (3)	0.4314 (2)	0.8080 (2)	0.0150 (6)
C11	0.3056 (3)	0.53102 (18)	0.6750 (2)	0.0138 (6)
C12	0.0301 (3)	0.48514 (19)	0.6716 (2)	0.0149 (6)
C13	0.7555 (5)	0.6320 (3)	0.4880 (4)	0.0401 (11)
H13A	0.7890	0.6835	0.5168	0.048*
H13B	0.7438	0.6384	0.4198	0.048*
H13C	0.8267	0.5891	0.5043	0.048*
C14	0.3792 (5)	0.6167 (3)	0.3344 (3)	0.0386 (10)
H14A	0.3525	0.5845	0.2780	0.046*
H14B	0.4830	0.6293	0.3376	0.046*
H14C	0.3235	0.6676	0.3321	0.046*
C15	0.6291 (13)	0.6822 (4)	0.7417 (4)	0.123 (5)
H15A	0.7292	0.6981	0.7604	0.148*
H15B	0.6232	0.6227	0.7362	0.148*
H15C	0.5658	0.7007	0.7891	0.148*
B1	0.0838 (4)	0.6841 (2)	0.8869 (2)	0.0150 (7)
H10	0.0501	0.7378	0.9281	0.018*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.0115 (2)	0.0095 (2)	0.0126 (2)	0.00115 (15)	0.00292 (16)	0.00043 (15)
Fe2	0.0125 (3)	0.0171 (3)	0.0143 (3)	−0.0025 (2)	0.0040 (2)	−0.0033 (2)
O1	0.0240 (13)	0.0255 (13)	0.0297 (14)	−0.0087 (11)	0.0112 (10)	−0.0113 (11)
O2	0.0152 (12)	0.0420 (16)	0.0312 (14)	0.0014 (11)	0.0002 (10)	0.0111 (12)
O3	0.065 (2)	0.0274 (15)	0.0368 (16)	−0.0274 (15)	0.0179 (15)	−0.0142 (12)
N1	0.0154 (12)	0.0117 (12)	0.0127 (12)	0.0005 (10)	0.0030 (9)	0.0004 (9)
N2	0.0175 (12)	0.0117 (12)	0.0126 (12)	0.0018 (10)	0.0022 (9)	−0.0003 (10)
N3	0.0144 (13)	0.0112 (12)	0.0156 (13)	0.0019 (10)	0.0033 (10)	−0.0001 (9)
N4	0.0146 (12)	0.0141 (13)	0.0154 (12)	0.0045 (10)	0.0028 (10)	−0.0012 (10)
N5	0.0126 (12)	0.0145 (12)	0.0131 (12)	0.0008 (10)	0.0028 (9)	−0.0008 (10)
N6	0.0177 (13)	0.0135 (12)	0.0146 (12)	−0.0001 (10)	0.0043 (10)	−0.0017 (10)
N7	0.0203 (14)	0.0233 (15)	0.0231 (15)	−0.0024 (12)	0.0006 (12)	0.0013 (12)
N8	0.0192 (14)	0.0198 (14)	0.0194 (14)	−0.0016 (11)	0.0059 (11)	−0.0040 (11)
N9	0.0241 (15)	0.0135 (13)	0.0252 (15)	0.0025 (11)	0.0001 (11)	0.0003 (11)
C1	0.0218 (16)	0.0173 (15)	0.0151 (15)	0.0010 (13)	0.0018 (12)	0.0008 (12)
C2	0.0341 (19)	0.0143 (15)	0.0167 (15)	0.0032 (14)	−0.0004 (14)	0.0049 (12)
C3	0.0255 (17)	0.0099 (14)	0.0217 (16)	0.0019 (13)	0.0001 (13)	0.0013 (12)
C4	0.0156 (15)	0.0158 (15)	0.0195 (15)	−0.0003 (12)	0.0033 (12)	0.0024 (12)
C5	0.0157 (15)	0.0239 (17)	0.0210 (16)	0.0028 (13)	0.0068 (12)	0.0039 (13)
C6	0.0158 (15)	0.0235 (16)	0.0154 (14)	0.0034 (13)	0.0052 (11)	0.0015 (12)
C7	0.0132 (14)	0.0202 (16)	0.0202 (15)	0.0011 (12)	0.0010 (12)	0.0011 (13)
C8	0.0169 (15)	0.0267 (18)	0.0234 (17)	−0.0024 (14)	−0.0011 (13)	−0.0015 (14)
C9	0.0225 (16)	0.0202 (16)	0.0162 (15)	−0.0027 (13)	0.0009 (12)	−0.0025 (12)
C10	0.0140 (14)	0.0170 (15)	0.0140 (14)	0.0013 (12)	0.0012 (11)	−0.0017 (11)
C11	0.0148 (14)	0.0107 (14)	0.0160 (15)	0.0002 (11)	0.0019 (11)	0.0001 (11)
C12	0.0139 (14)	0.0136 (14)	0.0175 (15)	0.0023 (12)	0.0040 (11)	0.0008 (12)
C13	0.027 (2)	0.037 (2)	0.057 (3)	−0.0175 (18)	0.0123 (19)	−0.009 (2)
C14	0.027 (2)	0.049 (3)	0.041 (2)	0.0047 (19)	0.0040 (17)	0.018 (2)
C15	0.272 (13)	0.069 (4)	0.027 (3)	−0.107 (7)	0.007 (5)	0.001 (3)
B1	0.0174 (16)	0.0145 (16)	0.0134 (15)	0.0013 (13)	0.0030 (12)	−0.0008 (12)

Geometric parameters (Å, º) top

Fe1—C11	1.922 (3)	N6—B1	1.554 (4)
Fe1—C10	1.930 (3)	N7—C12	1.144 (5)
Fe1—C12	1.930 (3)	N8—C11	1.150 (4)
Fe1—N1	1.963 (3)	N9—C10	1.148 (4)
Fe1—N5	1.979 (3)	C1—C2	1.391 (5)
Fe1—N3	1.984 (3)	C1—H1	0.9500
Fe2—N8ⁱ	2.109 (3)	C2—C3	1.382 (5)
Fe2—N8	2.109 (3)	C2—H2	0.9500
Fe2—O1ⁱ	2.127 (3)	C3—H3	0.9500
Fe2—O1	2.127 (3)	C4—C5	1.395 (5)
Fe2—O2	2.127 (3)	C4—H4	0.9500
Fe2—O2ⁱ	2.127 (3)	C5—C6	1.379 (5)
O1—C13	1.429 (5)	C5—H5	0.9500
O1—H1O	0.9286	C6—H6	0.9500
O2—C14	1.432 (5)	C7—C8	1.390 (5)
O2—H2O	0.8267	C7—H7	0.9500
O3—C15	1.410 (8)	C8—C9	1.383 (5)
O3—H3O	0.8500	C8—H8	0.9500
N1—C1	1.336 (4)	C9—H9	0.9500
N1—N2	1.361 (4)	C13—H13A	0.9800
N2—C3	1.344 (4)	C13—H13B	0.9800
N2—B1	1.537 (4)	C13—H13C	0.9800
N3—C4	1.329 (4)	C14—H14A	0.9800
N3—N4	1.364 (4)	C14—H14B	0.9800
N4—C6	1.359 (4)	C14—H14C	0.9800
N4—B1	1.535 (5)	C15—H15A	0.9800
N5—C7	1.350 (4)	C15—H15B	0.9800
N5—N6	1.363 (4)	C15—H15C	0.9800
N6—C9	1.345 (4)	B1—H10	1.1191

C11—Fe1—C10	87.03 (13)	C11—N8—Fe2	168.2 (3)
C11—Fe1—C12	87.23 (14)	N1—C1—C2	109.7 (3)
C10—Fe1—C12	89.59 (13)	N1—C1—H1	125.1
C11—Fe1—N1	90.58 (12)	C2—C1—H1	125.1
C10—Fe1—N1	176.91 (12)	C3—C2—C1	105.3 (3)
C12—Fe1—N1	92.27 (12)	C3—C2—H2	127.4
C11—Fe1—N5	95.46 (12)	C1—C2—H2	127.4
C10—Fe1—N5	89.89 (12)	N2—C3—C2	108.3 (3)
C12—Fe1—N5	177.23 (12)	N2—C3—H3	125.8
N1—Fe1—N5	88.37 (11)	C2—C3—H3	125.8
C11—Fe1—N3	176.14 (12)	N3—C4—C5	110.4 (3)
C10—Fe1—N3	93.65 (12)	N3—C4—H4	124.8
C12—Fe1—N3	88.97 (13)	C5—C4—H4	124.8
N1—Fe1—N3	88.87 (11)	C6—C5—C4	104.9 (3)
N5—Fe1—N3	88.34 (11)	C6—C5—H5	127.6
N8ⁱ—Fe2—N8	179.999 (1)	C4—C5—H5	127.6
N8ⁱ—Fe2—O1ⁱ	90.17 (10)	N4—C6—C5	108.6 (3)
N8—Fe2—O1ⁱ	89.83 (10)	N4—C6—H6	125.7
N8ⁱ—Fe2—O1	89.83 (10)	C5—C6—H6	125.7
N8—Fe2—O1	90.17 (10)	N5—C7—C8	109.9 (3)
O1ⁱ—Fe2—O1	179.998 (1)	N5—C7—H7	125.0
N8ⁱ—Fe2—O2	90.45 (11)	C8—C7—H7	125.0
N8—Fe2—O2	89.55 (11)	C9—C8—C7	105.1 (3)
O1ⁱ—Fe2—O2	94.03 (11)	C9—C8—H8	127.4
O1—Fe2—O2	85.97 (11)	C7—C8—H8	127.4
N8ⁱ—Fe2—O2ⁱ	89.55 (11)	N6—C9—C8	108.7 (3)
N8—Fe2—O2ⁱ	90.45 (11)	N6—C9—H9	125.7
O1ⁱ—Fe2—O2ⁱ	85.97 (11)	C8—C9—H9	125.7
O1—Fe2—O2ⁱ	94.03 (11)	N9—C10—Fe1	177.9 (3)
O2—Fe2—O2ⁱ	180.000 (1)	N8—C11—Fe1	176.1 (3)
C13—O1—Fe2	128.9 (2)	N7—C12—Fe1	176.7 (3)
C13—O1—H1O	115.3	O1—C13—H13A	109.5
Fe2—O1—H1O	115.2	O1—C13—H13B	109.5
C14—O2—Fe2	125.5 (2)	H13A—C13—H13B	109.5
C14—O2—H2O	101.2	O1—C13—H13C	109.5
Fe2—O2—H2O	132.2	H13A—C13—H13C	109.5
C15—O3—H3O	108.1	H13B—C13—H13C	109.5
C1—N1—N2	107.3 (3)	O2—C14—H14A	109.5
C1—N1—Fe1	133.4 (2)	O2—C14—H14B	109.5
N2—N1—Fe1	119.27 (19)	H14A—C14—H14B	109.5
C3—N2—N1	109.3 (3)	O2—C14—H14C	109.5
C3—N2—B1	131.1 (3)	H14A—C14—H14C	109.5
N1—N2—B1	119.6 (2)	H14B—C14—H14C	109.5
C4—N3—N4	107.4 (3)	O3—C15—H15A	109.5
C4—N3—Fe1	133.3 (2)	O3—C15—H15B	109.5
N4—N3—Fe1	119.4 (2)	H15A—C15—H15B	109.5
C6—N4—N3	108.8 (3)	O3—C15—H15C	109.5
C6—N4—B1	132.3 (3)	H15A—C15—H15C	109.5
N3—N4—B1	118.9 (3)	H15B—C15—H15C	109.5
C7—N5—N6	106.8 (3)	N4—B1—N2	106.8 (3)
C7—N5—Fe1	133.6 (2)	N4—B1—N6	106.7 (3)
N6—N5—Fe1	119.6 (2)	N2—B1—N6	106.7 (2)
C9—N6—N5	109.5 (3)	N4—B1—H10	111.0
C9—N6—B1	132.0 (3)	N2—B1—H10	110.1
N5—N6—B1	118.5 (2)	N6—B1—H10	115.1

N8ⁱ—Fe2—O1—C13	−20.3 (4)	N8ⁱ—Fe2—N8—C11	164 (4)
N8—Fe2—O1—C13	159.7 (4)	O1ⁱ—Fe2—N8—C11	−20.8 (14)
O1ⁱ—Fe2—O1—C13	−88 (7)	O1—Fe2—N8—C11	159.2 (14)
O2—Fe2—O1—C13	−110.8 (4)	O2—Fe2—N8—C11	73.2 (14)
O2ⁱ—Fe2—O1—C13	69.2 (4)	O2ⁱ—Fe2—N8—C11	−106.8 (14)
N8ⁱ—Fe2—O2—C14	−31.2 (3)	N2—N1—C1—C2	−0.4 (4)
N8—Fe2—O2—C14	148.8 (3)	Fe1—N1—C1—C2	−179.5 (2)
O1ⁱ—Fe2—O2—C14	−121.4 (3)	N1—C1—C2—C3	0.3 (4)
O1—Fe2—O2—C14	58.5 (3)	N1—N2—C3—C2	−0.3 (4)
O2ⁱ—Fe2—O2—C14	12 (53)	B1—N2—C3—C2	178.1 (3)
C11—Fe1—N1—C1	38.3 (3)	C1—C2—C3—N2	0.0 (4)
C10—Fe1—N1—C1	78 (2)	N4—N3—C4—C5	0.0 (4)
C12—Fe1—N1—C1	−48.9 (3)	Fe1—N3—C4—C5	−178.8 (2)
N5—Fe1—N1—C1	133.8 (3)	N3—C4—C5—C6	−0.3 (4)
N3—Fe1—N1—C1	−137.9 (3)	N3—N4—C6—C5	−0.4 (4)
C11—Fe1—N1—N2	−140.6 (2)	B1—N4—C6—C5	178.7 (3)
C10—Fe1—N1—N2	−101 (2)	C4—C5—C6—N4	0.4 (4)
C12—Fe1—N1—N2	132.1 (2)	N6—N5—C7—C8	0.1 (4)
N5—Fe1—N1—N2	−45.2 (2)	Fe1—N5—C7—C8	−177.2 (2)
N3—Fe1—N1—N2	43.2 (2)	N5—C7—C8—C9	−0.1 (4)
C1—N1—N2—C3	0.4 (4)	N5—N6—C9—C8	0.0 (4)
Fe1—N1—N2—C3	179.6 (2)	B1—N6—C9—C8	177.9 (3)
C1—N1—N2—B1	−178.2 (3)	C7—C8—C9—N6	0.0 (4)
Fe1—N1—N2—B1	1.0 (4)	C11—Fe1—C10—N9	63 (8)
C11—Fe1—N3—C4	53.1 (19)	C12—Fe1—C10—N9	150 (8)
C10—Fe1—N3—C4	−47.0 (3)	N1—Fe1—C10—N9	23 (10)
C12—Fe1—N3—C4	42.5 (3)	N5—Fe1—C10—N9	−33 (8)
N1—Fe1—N3—C4	134.8 (3)	N3—Fe1—C10—N9	−121 (8)
N5—Fe1—N3—C4	−136.8 (3)	Fe2—N8—C11—Fe1	−25 (6)
C11—Fe1—N3—N4	−125.6 (17)	C10—Fe1—C11—N8	100 (4)
C10—Fe1—N3—N4	134.3 (2)	C12—Fe1—C11—N8	10 (4)
C12—Fe1—N3—N4	−136.2 (2)	N1—Fe1—C11—N8	−82 (4)
N1—Fe1—N3—N4	−43.9 (2)	N5—Fe1—C11—N8	−170 (4)
N5—Fe1—N3—N4	44.5 (2)	N3—Fe1—C11—N8	0 (6)
C4—N3—N4—C6	0.2 (3)	C11—Fe1—C12—N7	179 (100)
Fe1—N3—N4—C6	179.2 (2)	C10—Fe1—C12—N7	92 (5)
C4—N3—N4—B1	−179.1 (3)	N1—Fe1—C12—N7	−91 (5)
Fe1—N3—N4—B1	−0.1 (4)	N5—Fe1—C12—N7	12 (7)
C11—Fe1—N5—C7	−47.6 (3)	N3—Fe1—C12—N7	−2 (5)
C10—Fe1—N5—C7	39.4 (3)	C6—N4—B1—N2	−122.6 (3)
C12—Fe1—N5—C7	119 (2)	N3—N4—B1—N2	56.4 (3)
N1—Fe1—N5—C7	−138.0 (3)	C6—N4—B1—N6	123.6 (3)
N3—Fe1—N5—C7	133.0 (3)	N3—N4—B1—N6	−57.4 (3)
C11—Fe1—N5—N6	135.3 (2)	C3—N2—B1—N4	124.2 (4)
C10—Fe1—N5—N6	−137.6 (2)	N1—N2—B1—N4	−57.6 (3)
C12—Fe1—N5—N6	−58 (3)	C3—N2—B1—N6	−122.0 (4)
N1—Fe1—N5—N6	44.9 (2)	N1—N2—B1—N6	56.2 (3)
N3—Fe1—N5—N6	−44.0 (2)	C9—N6—B1—N4	−119.9 (4)
C7—N5—N6—C9	−0.1 (3)	N5—N6—B1—N4	57.8 (3)
Fe1—N5—N6—C9	177.7 (2)	C9—N6—B1—N2	126.1 (3)
C7—N5—N6—B1	−178.3 (3)	N5—N6—B1—N2	−56.1 (3)
Fe1—N5—N6—B1	−0.5 (3)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1O···O3	0.93	1.75	2.645 (4)	161
O2—H2O···N7ⁱⁱ	0.83	1.97	2.769 (4)	161
O3—H3O···N9ⁱⁱⁱ	0.85	1.97	2.815 (4)	172
O1—H1O···O3	0.93	1.75	2.645 (4)	161
O2—H2O···N7ⁱⁱ	0.83	1.97	2.769 (4)	161
C8—H8···N9^iv	0.95	2.62	3.523 (5)	158
O3—H3O···N9ⁱⁱⁱ	0.85	1.97	2.815 (4)	172

Symmetry codes: (ii) −x, −y+1, −z+1; (iii) −x+1, y+1/2, −z+3/2; (iv) −x+1, −y+1, −z+2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1O···O3	0.93	1.75	2.645 (4)	160.6
O2—H2O···N7ⁱ	0.83	1.97	2.769 (4)	161.4
O3—H3O···N9ⁱⁱ	0.85	1.97	2.815 (4)	172.1
O1—H1O···O3	0.93	1.75	2.645 (4)	160.6
O2—H2O···N7ⁱ	0.83	1.97	2.769 (4)	161.4
C8—H8···N9ⁱⁱⁱ	0.95	2.62	3.523 (5)	158.0
O3—H3O···N9ⁱⁱ	0.85	1.97	2.815 (4)	172.1

Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, y+1/2, −z+3/2; (iii) −x+1, −y+1, −z+2.

References

Bruker (2000). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Kim, J., Han, S., Cho, I. K., Choi, K. Y., Heu, M., Yoon, S. & Suh, B. J. (2004). Polyhedron, 23, 1333–1339. Web of Science CSD CrossRef CAS Google Scholar
Lescouëzec, R., Vaissermann, J., Lloret, F., Julve, M. & Verdaguer, M. (2002). Inorg. Chem. 41, 5943–5945. Web of Science PubMed Google Scholar
Rigaku (2008). CrystalClear. Rigaku Corporation, Tokyo, Japan. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar

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Volume 70| Part 2| February 2014| Page m56

doi:10.1107/S1600536814001019

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Di-μ-tricyanido-tetra­cyanidobis[hydro­tris­­(pyrazoylborato)]tetra­methanol­diiron(III)iron(II) di­methanol disolvate

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Experimental

Crystal data

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metal-organic compounds

Di-μ-tricyanido-tetracyanidobis[hydrotris(pyrazoylborato)]tetramethanoldiiron(III)iron(II) dimethanol disolvate