Poly­[tetra-μ₂-azido-di-μ₂-4,4′-bi­pyridine-sodium(I)­iron(III)]

In the crystal structure of the title compound, [FeNa(N₃)₄(C₁₀H₈N₂)₂]_n, the Fe and Na atoms are coord­inated by four N atoms of azide anions and two N atoms of 4,4′-bi­pyridine ligands within distorted octahedra. The azide anions are located in general positions whereas the Fe and Na atoms, as well as the 4,4′-bi­pyridine ligands, are located on twofold axes. The iron and the sodium cations are connected via the 4,4′-bi­pyridine ligands into chains, which are linked by the azide anions into a three-dimensional coordination network.

Key indicators

• Single-crystal X-ray study
• T = 150 K
• Mean [sigma](C-C) = 0.002 Å
• R factor = 0.029
• wR factor = 0.075
• Data-to-parameter ratio = 15.3

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT220_ALERT_2_C Large Non-Solvent    N     Ueq(max)/Ueq(min) ...       2.57 Ratio
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.14 Ratio

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           28.09
           From the CIF: _reflns_number_total               2728
           Count of symmetry unique reflns         1577
           Completeness (_total/calc)            172.99%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      1151
           Fraction of Friedel pairs measured     0.730
           Are heavy atom types Z>Si present          yes

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   2 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: IPDS (Stoe & Cie, 1998); cell refinement: IPDS; data reduction: IPDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: CIFTAB in SHELXL97.

Poly[tetra-µ₂-azido-di-µ₂-4,4'-bipyridine-sodium(I)iron(III)]

Crystal data

[FeNa(N3)4(C10H8N2)2]	F(000) = 1140
Mr = 559.33	Dx = 1.612 Mg m^−3
Orthorhombic, C2221	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c 2	Cell parameters from 8000 reflections
a = 11.4626 (6) Å	θ = 16–26°
b = 12.0032 (9) Å	µ = 0.72 mm^−1
c = 16.7541 (9) Å	T = 150 K
V = 2305.2 (2) Å^3	Block, red
Z = 4	0.07 × 0.06 × 0.06 mm

Data collection

Stoe Imaging Plate Diffraction System diffractometer	2576 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.049
Graphite monochromator	θmax = 28.1°, θmin = 2.4°
φ scans	h = −14→14
13692 measured reflections	k = −15→15
2728 independent reflections	l = −22→22

Refinement

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.029	w = 1/[σ^2(Fo^2) + (0.043P)^2 + 1.8553P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.075	(Δ/σ)max < 0.001
S = 1.09	Δρmax = 0.36 e Å^−3
2728 reflections	Δρmin = −0.48 e Å^−3
178 parameters	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0026 (4)
Primary atom site location: structure-invariant direct methods	Absolute structure: Flack (1983)
Secondary atom site location: difference Fourier map	Absolute structure parameter: 0.007 (15)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.69232 (3)	0.5000	0.0000	0.00854 (10)
N3	0.69258 (16)	0.41557 (14)	0.10494 (9)	0.0145 (3)
N4	0.66661 (14)	0.32129 (15)	0.11761 (9)	0.0141 (3)
N5	0.64264 (19)	0.22990 (16)	0.13373 (12)	0.0243 (4)
N6	0.69594 (16)	0.64899 (13)	0.06089 (10)	0.0146 (3)
N7	0.76363 (15)	0.66735 (14)	0.11328 (10)	0.0141 (3)
N8	0.82889 (19)	0.68931 (17)	0.16284 (12)	0.0261 (4)
N1	0.50296 (17)	0.5000	0.0000	0.0101 (3)
C1	0.44278 (14)	0.40438 (14)	0.00200 (15)	0.0129 (3)
H1	0.4848	0.3362	0.0034	0.015*
C2	0.32194 (14)	0.40041 (13)	0.00209 (13)	0.0118 (3)
H2	0.2825	0.3308	0.0036	0.014*
C3	0.2587 (2)	0.5000	0.0000	0.0108 (4)
C4	0.1295 (2)	0.5000	0.0000	0.0110 (4)
C5	0.06571 (18)	0.41411 (17)	0.03565 (12)	0.0146 (4)
H5	0.1049	0.3536	0.0605	0.018*
C6	−0.05449 (18)	0.41773 (17)	0.03451 (12)	0.0139 (4)
H6	−0.0962	0.3589	0.0595	0.017*
N2	−0.11587 (17)	0.5000	0.0000	0.0107 (4)
N11	0.5000	−0.59649 (19)	0.2500	0.0159 (5)
C11	0.5829 (2)	−0.53759 (17)	0.28723 (13)	0.0162 (4)
H11	0.6424	−0.5774	0.3145	0.019*
C12	0.58738 (19)	−0.42202 (18)	0.28841 (12)	0.0161 (4)
H12	0.6492	−0.3847	0.3151	0.019*
C13	0.5000	−0.3612 (2)	0.2500	0.0134 (5)
C14	0.5000	−0.2379 (2)	0.2500	0.0133 (5)
C15	0.60332 (18)	−0.17730 (17)	0.25538 (13)	0.0167 (4)
H15	0.6761	−0.2148	0.2590	0.020*
C16	0.59897 (19)	−0.06132 (16)	0.25546 (13)	0.0173 (4)
H16	0.6703	−0.0214	0.2596	0.021*
N12	0.5000	−0.0033 (2)	0.2500	0.0170 (4)
Na1	0.5000	0.19824 (9)	0.2500	0.0139 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.00420 (16)	0.00952 (17)	0.01192 (16)	0.000	0.000	−0.00006 (15)
N3	0.0123 (8)	0.0180 (8)	0.0133 (7)	0.0003 (7)	−0.0003 (6)	0.0043 (6)
N4	0.0087 (8)	0.0208 (9)	0.0127 (7)	0.0017 (6)	0.0010 (6)	0.0016 (6)
N5	0.0309 (11)	0.0180 (9)	0.0241 (10)	−0.0016 (8)	0.0052 (8)	0.0035 (7)
N6	0.0131 (8)	0.0106 (7)	0.0200 (8)	0.0010 (6)	−0.0056 (7)	−0.0033 (6)
N7	0.0153 (9)	0.0097 (7)	0.0174 (8)	0.0005 (6)	0.0006 (6)	−0.0015 (6)
N8	0.0263 (11)	0.0247 (10)	0.0271 (10)	0.0034 (8)	−0.0133 (8)	−0.0082 (8)
N1	0.0030 (8)	0.0134 (9)	0.0138 (9)	0.000	0.000	−0.0017 (10)
C1	0.0086 (8)	0.0115 (8)	0.0186 (7)	0.0008 (6)	0.0007 (9)	0.0001 (8)
C2	0.0063 (7)	0.0115 (8)	0.0177 (7)	−0.0018 (5)	0.0018 (10)	0.0006 (8)
C3	0.0081 (11)	0.0118 (11)	0.0126 (10)	0.000	0.000	−0.0001 (13)
C4	0.0082 (11)	0.0121 (11)	0.0128 (10)	0.000	0.000	0.0007 (13)
C5	0.0066 (9)	0.0145 (9)	0.0226 (9)	0.0016 (7)	−0.0023 (7)	0.0039 (8)
C6	0.0092 (10)	0.0118 (9)	0.0208 (8)	0.0003 (7)	0.0012 (7)	0.0043 (8)
N2	0.0035 (8)	0.0124 (9)	0.0162 (9)	0.000	0.000	−0.0001 (11)
N11	0.0184 (13)	0.0114 (11)	0.0177 (11)	0.000	0.0070 (9)	0.000
C11	0.0163 (11)	0.0140 (9)	0.0183 (9)	0.0020 (7)	0.0011 (7)	0.0033 (7)
C12	0.0176 (11)	0.0127 (9)	0.0179 (9)	0.0007 (8)	−0.0020 (7)	−0.0008 (8)
C13	0.0162 (14)	0.0094 (12)	0.0145 (12)	0.000	−0.0005 (10)	0.000
C14	0.0149 (15)	0.0092 (12)	0.0157 (13)	0.000	−0.0008 (11)	0.000
C15	0.0126 (11)	0.0132 (9)	0.0242 (10)	0.0007 (7)	−0.0027 (8)	−0.0016 (8)
C16	0.0146 (11)	0.0121 (10)	0.0253 (10)	−0.0012 (7)	−0.0017 (8)	−0.0021 (8)
N12	0.0146 (10)	0.0126 (10)	0.0237 (10)	0.000	−0.0004 (8)	0.000
Na1	0.0155 (6)	0.0093 (5)	0.0169 (5)	0.000	−0.0021 (4)	0.000

Geometric parameters (Å, º)

Fe1—N3^i	2.0294 (15)	C6—H6	0.9500
Fe1—N3	2.0294 (15)	N2—C6^i	1.343 (2)
Fe1—N6	2.0593 (16)	N2—Fe1^iv	2.199 (2)
Fe1—N6^i	2.0593 (16)	N11—C11^v	1.339 (3)
Fe1—N1	2.171 (2)	N11—C11	1.339 (3)
Fe1—N2^ii	2.199 (2)	N11—Na1^vi	2.464 (3)
N3—N4	1.189 (2)	C11—C12	1.388 (3)
N4—N5	1.163 (3)	C11—H11	0.9500
N5—Na1	2.572 (2)	C12—C13	1.397 (3)
N6—N7	1.192 (2)	C12—H12	0.9500
N7—N8	1.148 (3)	C13—C12^v	1.397 (3)
N8—Na1^iii	2.4476 (19)	C13—C14	1.480 (4)
N1—C1^i	1.3395 (19)	C14—C15	1.392 (2)
N1—C1	1.3395 (19)	C14—C15^v	1.392 (2)
C1—C2	1.386 (2)	C15—C16	1.393 (3)
C1—H1	0.9500	C15—H15	0.9500
C2—C3	1.3985 (19)	C16—N12	1.334 (3)
C2—H2	0.9500	C16—H16	0.9500
C3—C2^i	1.3985 (19)	N12—C16^v	1.334 (3)
C3—C4	1.480 (3)	N12—Na1	2.419 (3)
C4—C5^i	1.398 (2)	Na1—N8^vii	2.4476 (19)
C4—C5	1.398 (2)	Na1—N8^viii	2.4476 (19)
C5—C6	1.379 (3)	Na1—N11^ix	2.464 (3)
C5—H5	0.9500	Na1—N5^v	2.572 (2)
C6—N2	1.343 (2)
N3^i—Fe1—N3	179.83 (11)	C6—N2—C6^i	116.8 (2)
N3^i—Fe1—N6	89.74 (7)	C6—N2—Fe1^iv	121.59 (11)
N3—Fe1—N6	90.25 (7)	C6^i—N2—Fe1^iv	121.59 (11)
N3^i—Fe1—N6^i	90.25 (7)	C11^v—N11—C11	116.2 (2)
N3—Fe1—N6^i	89.74 (7)	C11^v—N11—Na1^vi	121.88 (12)
N6—Fe1—N6^i	177.69 (10)	C11—N11—Na1^vi	121.88 (12)
N3^i—Fe1—N1	90.08 (5)	N11—C11—C12	124.1 (2)
N3—Fe1—N1	90.08 (5)	N11—C11—H11	118.0
N6—Fe1—N1	91.16 (5)	C12—C11—H11	118.0
N6^i—Fe1—N1	91.16 (5)	C11—C12—C13	119.3 (2)
N3^i—Fe1—N2^ii	89.92 (5)	C11—C12—H12	120.3
N3—Fe1—N2^ii	89.92 (5)	C13—C12—H12	120.3
N6—Fe1—N2^ii	88.84 (5)	C12^v—C13—C12	116.9 (3)
N6^i—Fe1—N2^ii	88.84 (5)	C12^v—C13—C14	121.53 (13)
N1—Fe1—N2^ii	180.0	C12—C13—C14	121.53 (13)
N4—N3—Fe1	129.01 (14)	C15—C14—C15^v	117.1 (2)
N5—N4—N3	176.8 (2)	C15—C14—C13	121.47 (12)
N4—N5—Na1	117.75 (15)	C15^v—C14—C13	121.47 (12)
N7—N6—Fe1	122.58 (14)	C14—C15—C16	119.43 (19)
N8—N7—N6	177.3 (2)	C14—C15—H15	120.3
N7—N8—Na1^iii	164.48 (18)	C16—C15—H15	120.3
C1^i—N1—C1	118.0 (2)	N12—C16—C15	123.5 (2)
C1^i—N1—Fe1	120.99 (10)	N12—C16—H16	118.2
C1—N1—Fe1	120.99 (10)	C15—C16—H16	118.2
N1—C1—C2	122.97 (16)	C16^v—N12—C16	117.1 (3)
N1—C1—H1	118.5	C16^v—N12—Na1	121.47 (14)
C2—C1—H1	118.5	C16—N12—Na1	121.47 (14)
C1—C2—C3	119.25 (16)	N12—Na1—N8^vii	87.49 (5)
C1—C2—H2	120.4	N12—Na1—N8^viii	87.49 (5)
C3—C2—H2	120.4	N8^vii—Na1—N8^viii	174.98 (11)
C2^i—C3—C2	117.6 (2)	N12—Na1—N11^ix	180.0
C2^i—C3—C4	121.22 (11)	N8^vii—Na1—N11^ix	92.51 (5)
C2—C3—C4	121.22 (11)	N8^viii—Na1—N11^ix	92.51 (5)
C5^i—C4—C5	116.9 (2)	N12—Na1—N5^v	98.50 (5)
C5^i—C4—C3	121.56 (11)	N8^vii—Na1—N5^v	87.07 (7)
C5—C4—C3	121.56 (11)	N8^viii—Na1—N5^v	93.67 (7)
C6—C5—C4	119.59 (19)	N11^ix—Na1—N5^v	81.50 (5)
C6—C5—H5	120.2	N12—Na1—N5	98.50 (5)
C4—C5—H5	120.2	N8^vii—Na1—N5	93.67 (7)
N2—C6—C5	123.54 (19)	N8^viii—Na1—N5	87.07 (7)
N2—C6—H6	118.2	N11^ix—Na1—N5	81.50 (5)
C5—C6—H6	118.2	N5^v—Na1—N5	163.00 (10)

Symmetry codes: (i) x, −y+1, −z; (ii) x+1, y, z; (iii) x+1/2, y+1/2, z; (iv) x−1, y, z; (v) −x+1, y, −z+1/2; (vi) x, y−1, z; (vii) x−1/2, y−1/2, z; (viii) −x+3/2, y−1/2, −z+1/2; (ix) x, y+1, z.