Rerefinement of poly­[[tetra-μ-oxo-dioxobis(1,10-phenanthroline-κ²N,N)­dimolybdenum(VI)­iron(II)]-di-μ-oxo] in the centrosymmetric space group P2₁/m

Polymeric [Fe₂{MoO₄}₂(C₁₂H₈N₂)₂]_n adopts a chain structure that propagates linearly along the b axis of the monoclinic unit cell. The (C₁₂H₈N₂)Fe moiety lies on a mirror plane, as does the MoO₄ moiety; two MoO₄ anions link two (C₁₂H₈N₂)Fe entities to form an eight-membered Fe—O—Mo—O—Fe—O—Mo—O— ring; the Fe atom is five-coordinate in a trigonal bipyramidal environment; the phenanthroline ligand spans the axial–equatorial sites.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.024
• wR factor = 0.065
• Data-to-parameter ratio = 12.4

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.97
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       2.00 Ratio
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....         O1
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....        Mo1
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          8
            O3  -MO1 -O2  -FE1     0.00  0.00   1.555   1.555   1.555   3.767
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          9
            O1  -MO1 -O2  -FE1   119.60  0.10   1.555   1.555   1.555   3.767
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         10
            O1  -MO1 -O2  -FE1  -119.60  0.10   4.575   1.555   1.555   3.767
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         21
            O2  -FE1 -N2  -C12   180.00  0.00   3.767   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         25
            O2  -FE1 -N2  -C9      0.00  0.00   3.767   1.555   1.555   1.555

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

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

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Computing details

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: atomic coordinates taken from the Zn analog (Hagrman & Zubieta, 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: OPTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Dimolybdato(VI)bis[(1,10-phenanthroline)iron(II)]

Crystal data

[Fe2Mo2O8(C12H8N2)2]	F(000) = 388
Mr = 791.99	Dx = 2.159 Mg m^−3
Monoclinic, P21/m	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yb	Cell parameters from 2636 reflections
a = 8.873 (1) Å	θ = 2.3–27.6°
b = 6.567 (1) Å	µ = 2.23 mm^−1
c = 10.629 (2) Å	T = 293 K
β = 100.437 (2)°	Prism, black
V = 609.1 (2) Å^3	0.13 × 0.11 × 0.11 mm
Z = 1

Data collection

Bruker APEX area-detector diffractometer	1469 independent reflections
Radiation source: fine-focus sealed tube	1360 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.025
φ and ω scans	θmax = 27.5°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2002)	h = −11→11
Tmin = 0.697, Tmax = 0.791	k = −8→8
4906 measured reflections	l = −13→13

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.065	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0414P)^2 + 0.0379P] where P = (Fo^2 + 2Fc^2)/3
1469 reflections	(Δ/σ)max = 0.001
118 parameters	Δρmax = 0.39 e Å^−3
0 restraints	Δρmin = −0.33 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Mo1	0.99329 (3)	0.7500	0.83276 (3)	0.0188 (1)
Fe1	0.80930 (5)	0.2500	0.81847 (5)	0.0206 (1)
O1	0.8794 (2)	0.5295 (3)	0.7894 (2)	0.0381 (5)
O2	1.0671 (3)	0.7500	0.9968 (2)	0.0388 (7)
O3	1.1433 (4)	0.7500	0.7522 (3)	0.0577 (9)
N1	0.5842 (3)	0.2500	0.8650 (3)	0.0252 (6)
N2	0.6595 (3)	0.2500	0.6304 (3)	0.0225 (6)
C1	0.5498 (4)	0.2500	0.9819 (3)	0.031 (1)
C2	0.3985 (4)	0.2500	1.0016 (4)	0.038 (1)
C3	0.2805 (4)	0.2500	0.8997 (4)	0.038 (1)
C4	0.3128 (4)	0.2500	0.7733 (4)	0.030 (1)
C5	0.4679 (4)	0.2500	0.7622 (3)	0.025 (1)
C6	0.1979 (4)	0.2500	0.6619 (4)	0.040 (1)
C7	0.2347 (4)	0.2500	0.5446 (4)	0.034 (1)
C8	0.3922 (4)	0.2500	0.5289 (3)	0.025 (1)
C9	0.5077 (3)	0.2500	0.6361 (3)	0.022 (1)
C10	0.4368 (4)	0.2500	0.4078 (3)	0.029 (1)
C11	0.5889 (4)	0.2500	0.4024 (4)	0.030 (1)
C12	0.6965 (4)	0.2500	0.5146 (3)	0.027 (1)
H1	0.6289	0.2500	1.0525	0.037*
H2	0.3782	0.2500	1.0844	0.045*
H3	0.1796	0.2500	0.9126	0.045*
H6	0.0953	0.2500	0.6699	0.048*
H7	0.1572	0.2500	0.4727	0.041*
H10	0.3635	0.2500	0.3332	0.034*
H11	0.6205	0.2500	0.3236	0.036*
H12	0.7998	0.2500	0.5086	0.032*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.0197 (2)	0.0169 (2)	0.0186 (2)	0.000	0.0005 (1)	0.000
Fe1	0.0187 (2)	0.0181 (2)	0.0227 (3)	0.000	−0.0024 (2)	0.000
O1	0.048 (1)	0.024 (1)	0.036 (1)	−0.013 (1)	−0.010 (1)	0.0042 (8)
O2	0.047 (2)	0.036 (2)	0.027 (1)	0.000	−0.012 (1)	0.000
O3	0.043 (2)	0.078 (2)	0.061 (2)	0.000	0.032 (2)	0.000
N1	0.026 (1)	0.025 (1)	0.023 (2)	0.000	0.001 (1)	0.000
N2	0.021 (1)	0.020 (1)	0.025 (2)	0.000	−0.001 (1)	0.000
C1	0.031 (2)	0.035 (2)	0.024 (2)	0.000	0.001 (2)	0.000
C2	0.041 (2)	0.045 (2)	0.031 (2)	0.000	0.015 (2)	0.000
C3	0.032 (2)	0.046 (2)	0.038 (2)	0.000	0.016 (2)	0.000
C4	0.024 (2)	0.033 (2)	0.033 (2)	0.000	0.003 (2)	0.000
C5	0.023 (2)	0.022 (2)	0.027 (2)	0.000	0.001 (1)	0.000
C6	0.017 (2)	0.053 (2)	0.047 (3)	0.000	0.002 (2)	0.000
C7	0.020 (2)	0.046 (2)	0.031 (2)	0.000	−0.005 (1)	0.000
C8	0.023 (2)	0.024 (2)	0.027 (2)	0.000	0.000 (1)	0.000
C9	0.022 (2)	0.016 (1)	0.027 (2)	0.000	0.002 (1)	0.000
C10	0.029 (2)	0.031 (2)	0.022 (2)	0.000	−0.004 (1)	0.000
C11	0.037 (2)	0.029 (2)	0.024 (2)	0.000	0.005 (2)	0.000
C12	0.022 (2)	0.027 (2)	0.032 (2)	0.000	0.004 (1)	0.000

Geometric parameters (Å, º)

Mo1—O1	1.778 (2)	C4—C6	1.416 (5)
Mo1—O1^i	1.778 (2)	C5—C9	1.447 (5)
Mo1—O2	1.748 (2)	C6—C7	1.345 (5)
Mo1—O3	1.708 (3)	C7—C8	1.437 (5)
Fe1—O1	1.980 (2)	C8—C9	1.388 (5)
Fe1—O1^ii	1.980 (2)	C8—C10	1.414 (5)
Fe1—O2^iii	2.068 (3)	C10—C11	1.361 (5)
Fe1—N1	2.143 (3)	C11—C12	1.386 (5)
Fe1—N2	2.190 (3)	C1—H1	0.93
N1—C1	1.332 (4)	C2—H2	0.93
N1—C5	1.361 (4)	C3—H3	0.93
N2—C12	1.331 (4)	C6—H6	0.93
N2—C9	1.359 (4)	C7—H7	0.93
C1—C2	1.395 (5)	C10—H10	0.93
C2—C3	1.364 (5)	C11—H11	0.93
C3—C4	1.423 (5)	C12—H12	0.93
C4—C5	1.403 (5)
O1—Mo1—O1^i	109.1 (1)	N1—C5—C4	123.1 (3)
O1—Mo1—O2	110.6 (1)	N1—C5—C9	117.8 (3)
O1—Mo1—O3	109.2 (1)	C4—C5—C9	119.1 (3)
O1^i—Mo1—O2	110.6 (1)	C7—C6—C4	121.1 (3)
O1^i—Mo1—O3	109.2 (1)	C6—C7—C8	120.8 (3)
O2—Mo1—O3	108.4 (2)	C9—C8—C10	117.4 (3)
O1—Fe1—O1^ii	135.9 (1)	C9—C8—C7	119.6 (3)
O1—Fe1—O2^iii	91.2 (1)	C10—C8—C7	123.0 (3)
O1—Fe1—N1	111.6 (1)	N2—C9—C8	123.7 (3)
O1—Fe1—N2	90.8 (1)	N2—C9—C5	116.8 (3)
O1^ii—Fe1—O2^iii	91.2 (1)	C8—C9—C5	119.5 (3)
O1^ii—Fe1—N1	111.6 (1)	C11—C10—C8	118.8 (3)
O1^ii—Fe1—N2	90.8 (1)	C10—C11—C12	119.8 (4)
O2^iii—Fe1—N1	97.9 (1)	N2—C12—C11	123.3 (3)
O2^iii—Fe1—N2	174.8 (1)	N1—C1—H1	119.0
N1—Fe1—N2	76.9 (1)	C2—C1—H1	119.0
Mo1—O1—Fe1	153.4 (1)	C3—C2—H2	119.9
Mo1—O2—Fe1^iii	170.2 (2)	C1—C2—H2	119.9
C1—N1—C5	118.7 (3)	C2—C3—H3	120.2
C1—N1—Fe1	126.6 (2)	C4—C3—H3	120.2
C5—N1—Fe1	114.7 (2)	C7—C6—H6	119.4
C12—N2—C9	117.0 (3)	C4—C6—H6	119.4
C12—N2—Fe1	129.3 (2)	C6—C7—H7	119.6
C9—N2—Fe1	113.7 (2)	C8—C7—H7	119.6
N1—C1—C2	122.0 (4)	C11—C10—H10	120.6
C3—C2—C1	120.1 (4)	C8—C10—H10	120.6
C2—C3—C4	119.6 (3)	C10—C11—H11	120.1
C5—C4—C6	119.9 (3)	C12—C11—H11	120.1
C5—C4—C3	116.6 (3)	N2—C12—H12	118.3
C6—C4—C3	123.5 (3)	C11—C12—H12	118.3
O3—Mo1—O1—Fe1	100.9 (3)	C1—N1—C5—C4	0.0
O2—Mo1—O1—Fe1	−18.2 (3)	Fe1—N1—C5—C4	180.0
O1^i—Mo1—O1—Fe1	−139.9 (2)	C1—N1—C5—C9	180.0
O1^ii—Fe1—O1—Mo1	−85.0 (3)	Fe1—N1—C5—C9	0.0
O2^iii—Fe1—O1—Mo1	7.9 (3)	C6—C4—C5—N1	180.0
N1—Fe1—O1—Mo1	106.8 (3)	C3—C4—C5—N1	0.0
N2—Fe1—O1—Mo1	−176.9 (3)	C6—C4—C5—C9	0.0
O3—Mo1—O2—Fe1^iii	0.0	C3—C4—C5—C9	180.0
O1—Mo1—O2—Fe1^iii	119.6 (1)	C5—C4—C6—C7	0.0
O1^i—Mo1—O2—Fe1^iii	−119.6 (1)	C3—C4—C6—C7	180.0
O1^ii—Fe1—N1—C1	94.4 (1)	C4—C6—C7—C8	0.0
O1—Fe1—N1—C1	−94.4 (1)	C6—C7—C8—C9	0.0
O2^iii—Fe1—N1—C1	0.0	C6—C7—C8—C10	180.0
N2—Fe1—N1—C1	180.0	C12—N2—C9—C8	0.0
O1^ii—Fe1—N1—C5	−85.6 (1)	Fe1—N2—C9—C8	180.0
O1—Fe1—N1—C5	85.6 (1)	C12—N2—C9—C5	180.0
O2^iii—Fe1—N1—C5	180.0	Fe1—N2—C9—C5	0.0
N2—Fe1—N1—C5	0.0	C10—C8—C9—N2	0.0
O1^ii—Fe1—N2—C12	−68.0 (1)	C7—C8—C9—N2	180.0
O1—Fe1—N2—C12	68.0 (1)	C10—C8—C9—C5	180.0
O2^iii—Fe1—N2—C12	180.0	C7—C8—C9—C5	0.0
N1—Fe1—N2—C12	180.0	N1—C5—C9—N2	0.0
O1^ii—Fe1—N2—C9	112.0 (1)	C4—C5—C9—N2	180.0
O1—Fe1—N2—C9	−112.0 (1)	N1—C5—C9—C8	180.0
O2^iii—Fe1—N2—C9	0.0	C4—C5—C9—C8	0.0
N1—Fe1—N2—C9	0.0	C9—C8—C10—C11	0.0
C5—N1—C1—C2	0.0	C7—C8—C10—C11	180.0
Fe1—N1—C1—C2	180.0	C8—C10—C11—C12	0.0
N1—C1—C2—C3	0.0	C9—N2—C12—C11	0.0
C1—C2—C3—C4	0.0	Fe1—N2—C12—C11	180.0
C2—C3—C4—C5	0.0	C10—C11—C12—N2	0.0
C2—C3—C4—C6	180.0

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