μ-Terephthalato-κ²O¹:O⁴-bis­[bis­(propane-1,3-diamine-κ²N,N′)iron(II)] bis­(perchlorate)

The dinuclear title complex, [Fe₂(C₈H₄O₄)(C₃H₁₀N₂)₄](ClO₄)₂, is centrosymmetric about the central aromatic ring. The Fe centre is five-coordinated square pyramidal, being coordinated by four N atoms from two propane-1,3-diamine ligands and an O atom from a monodenate carboxyl­ate residue.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.009 Å
• R factor = 0.061
• wR factor = 0.184
• Data-to-parameter ratio = 18.9

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical .          ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Fe1    -   N2      ..       6.30 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Fe1    -   N3      ..       6.57 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Fe1    -   N4      ..       7.83 su
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O1
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         N3
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Fe1
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        Cl1
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          9
PLAT420_ALERT_2_C D-H Without Acceptor       N3     -   H3A    ...          ?

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
  13 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
   7 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
   1 ALERT type 4 Improvement, methodology, query or suggestion

---

Computing details

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

µ-Terephthalato-κ²O¹:O⁴-bis[bis(propane-1,3-diamine- κ²N,N')ferrate(II)] bis(perchlorate)

Crystal data

[Fe2(C8H4O4)(C3H10N2)4](ClO4)2	F(000) = 804
Mr = 771.23	Dx = 1.554 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 3781 reflections
a = 10.165 (2) Å	θ = 1.0–27.5°
b = 10.143 (2) Å	µ = 1.11 mm^−1
c = 16.012 (3) Å	T = 293 K
β = 93.05 (3)°	Block, black
V = 1648.6 (6) Å^3	0.34 × 0.28 × 0.22 mm
Z = 2

Data collection

Bruker SMART CCD area-detector diffractometer	3781 independent reflections
Radiation source: fine-focus sealed tube	2463 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.025
ω scans	θmax = 27.5°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = 0→13
Tmin = 0.696, Tmax = 0.784	k = 0→13
3980 measured reflections	l = −20→20

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.061	H-atom parameters constrained
wR(F^2) = 0.184	w = 1/[σ^2(Fo^2) + (0.0957P)^2 + 1.6922P] where P = (Fo^2 + 2Fc^2)/3
S = 1.03	(Δ/σ)max < 0.001
3781 reflections	Δρmax = 0.65 e Å^−3
200 parameters	Δρmin = −0.58 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.024 (3)

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	0.97061 (6)	0.38976 (6)	0.22144 (3)	0.0371 (2)
Cl1	0.31946 (16)	0.33021 (16)	0.34012 (10)	0.0732 (5)
O1	0.7985 (4)	0.4119 (4)	0.1265 (2)	0.0646 (10)
O2	0.6930 (4)	0.5629 (5)	0.1964 (2)	0.0767 (13)
O3	0.4389 (9)	0.2921 (10)	0.3726 (6)	0.224 (5)
O4	0.2631 (6)	0.2163 (6)	0.3034 (5)	0.140 (2)
O5	0.3307 (9)	0.4245 (8)	0.2824 (4)	0.176 (4)
O6	0.2561 (13)	0.3824 (9)	0.4063 (7)	0.235 (6)
N1	0.8450 (5)	0.3517 (5)	0.3129 (3)	0.0666 (13)
H1A	0.7652	0.3825	0.2953	0.080*
H1B	0.8378	0.2636	0.3171	0.080*
N2	0.9761 (6)	0.5788 (5)	0.2619 (4)	0.0775 (15)
H2A	1.0424	0.6189	0.2368	0.093*
H2B	0.9010	0.6175	0.2423	0.093*
N3	1.1092 (5)	0.4307 (5)	0.1369 (3)	0.0688 (13)
H3A	1.1084	0.5181	0.1274	0.083*
H3B	1.1889	0.4103	0.1605	0.083*
N4	0.9960 (4)	0.1958 (4)	0.1975 (3)	0.0573 (11)
H4A	1.0753	0.1713	0.2200	0.069*
H4B	0.9346	0.1501	0.2238	0.069*
C1	0.8748 (8)	0.4040 (8)	0.3980 (4)	0.094 (2)
H1C	0.9581	0.3682	0.4199	0.112*
H1D	0.8069	0.3757	0.4344	0.112*
C2	0.8823 (8)	0.5560 (9)	0.3985 (4)	0.094 (2)
H2C	0.7999	0.5909	0.3745	0.113*
H2D	0.8921	0.5861	0.4560	0.113*
C3	0.9920 (8)	0.6102 (7)	0.3516 (5)	0.091 (2)
H3C	0.9952	0.7052	0.3587	0.109*
H3D	1.0747	0.5741	0.3743	0.109*
C4	1.0942 (7)	0.3618 (6)	0.0546 (4)	0.0703 (17)
H4C	1.0098	0.3851	0.0274	0.084*
H4D	1.1628	0.3914	0.0191	0.084*
C5	1.1021 (6)	0.2162 (6)	0.0637 (4)	0.0682 (15)
H5A	1.1838	0.1939	0.0946	0.082*
H5B	1.1048	0.1769	0.0086	0.082*
C6	0.9884 (6)	0.1568 (6)	0.1081 (4)	0.0629 (14)
H6A	0.9057	0.1870	0.0817	0.075*
H6B	0.9912	0.0615	0.1037	0.075*
C7	0.7034 (5)	0.4881 (5)	0.1348 (3)	0.0497 (11)
C8	0.5971 (4)	0.4933 (5)	0.0654 (3)	0.0468 (11)
C9	0.6119 (5)	0.4246 (5)	−0.0077 (3)	0.0542 (13)
H9	0.6866	0.3733	−0.0136	0.065*
C10	0.4848 (5)	0.5687 (6)	0.0733 (3)	0.0595 (14)
H10	0.4734	0.6151	0.1225	0.071*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.0386 (3)	0.0433 (4)	0.0293 (3)	−0.0024 (3)	0.0000 (2)	0.0014 (3)
Cl1	0.0830 (10)	0.0606 (9)	0.0746 (10)	0.0035 (8)	−0.0091 (8)	0.0046 (8)
O1	0.058 (2)	0.075 (3)	0.059 (2)	0.0239 (19)	−0.0151 (17)	−0.0160 (19)
O2	0.074 (2)	0.102 (3)	0.051 (2)	0.033 (2)	−0.0177 (18)	−0.030 (2)
O3	0.208 (9)	0.217 (9)	0.228 (9)	0.117 (7)	−0.150 (8)	−0.093 (7)
O4	0.132 (5)	0.097 (4)	0.186 (6)	−0.030 (4)	−0.044 (5)	−0.024 (4)
O5	0.237 (9)	0.161 (6)	0.123 (5)	−0.104 (6)	−0.048 (6)	0.069 (5)
O6	0.317 (15)	0.174 (9)	0.230 (11)	0.063 (8)	0.167 (12)	−0.019 (7)
N1	0.064 (3)	0.090 (4)	0.046 (2)	−0.005 (3)	0.008 (2)	0.001 (2)
N2	0.086 (4)	0.070 (3)	0.078 (3)	−0.008 (3)	0.012 (3)	−0.012 (3)
N3	0.072 (3)	0.075 (3)	0.061 (3)	−0.017 (3)	0.010 (2)	0.002 (2)
N4	0.063 (3)	0.061 (3)	0.048 (2)	−0.001 (2)	0.0014 (19)	0.011 (2)
C1	0.103 (5)	0.136 (7)	0.043 (3)	0.000 (5)	0.009 (3)	0.001 (4)
C2	0.093 (5)	0.126 (7)	0.062 (4)	0.023 (5)	−0.004 (4)	−0.034 (4)
C3	0.092 (5)	0.086 (5)	0.092 (5)	0.003 (4)	−0.020 (4)	−0.040 (4)
C4	0.080 (4)	0.086 (5)	0.046 (3)	−0.009 (3)	0.013 (3)	0.007 (3)
C5	0.062 (3)	0.083 (4)	0.060 (3)	0.006 (3)	0.008 (3)	−0.004 (3)
C6	0.071 (3)	0.054 (3)	0.064 (3)	0.008 (3)	0.001 (3)	−0.003 (3)
C7	0.049 (2)	0.060 (3)	0.039 (2)	0.011 (2)	−0.0039 (19)	−0.008 (2)
C8	0.045 (2)	0.052 (3)	0.043 (2)	0.004 (2)	−0.0035 (19)	−0.005 (2)
C9	0.046 (2)	0.068 (3)	0.047 (3)	0.017 (2)	−0.005 (2)	−0.012 (2)
C10	0.055 (3)	0.075 (4)	0.047 (3)	0.013 (3)	−0.004 (2)	−0.017 (3)

Geometric parameters (Å, º)

Fe1—O1	2.267 (4)	C1—C2	1.544 (11)
Fe1—N1	2.030 (4)	C1—H1C	0.9700
Fe1—N2	2.024 (5)	C1—H1D	0.9700
Fe1—N3	2.047 (5)	C2—C3	1.482 (11)
Fe1—N4	2.024 (5)	C2—H2C	0.9700
Cl1—O5	1.339 (6)	C2—H2D	0.9700
Cl1—O3	1.352 (7)	C3—H3C	0.9700
Cl1—O6	1.375 (8)	C3—H3D	0.9700
Cl1—O4	1.405 (6)	C4—C5	1.486 (8)
O1—C7	1.250 (5)	C4—H4C	0.9700
O2—C7	1.253 (6)	C4—H4D	0.9700
N1—C1	1.479 (8)	C5—C6	1.514 (8)
N1—H1A	0.9000	C5—H5A	0.9700
N1—H1B	0.9000	C5—H5B	0.9700
N2—C3	1.472 (9)	C6—H6A	0.9700
N2—H2A	0.9000	C6—H6B	0.9700
N2—H2B	0.9000	C7—C8	1.509 (6)
N3—C4	1.493 (7)	C8—C9	1.377 (6)
N3—H3A	0.9000	C8—C10	1.385 (7)
N3—H3B	0.9000	C9—C10^i	1.401 (7)
N4—C6	1.483 (7)	C9—H9	0.9300
N4—H4A	0.9000	C10—C9^i	1.401 (7)
N4—H4B	0.9000	C10—H10	0.9300
O1—Fe1—N1	90.57 (18)	C2—C1—H1D	109.3
O1—Fe1—N2	97.4 (2)	H1C—C1—H1D	107.9
O1—Fe1—N3	94.04 (18)	C3—C2—C1	114.0 (6)
O1—Fe1—N4	94.06 (15)	C3—C2—H2C	108.7
N1—Fe1—N2	87.5 (2)	C1—C2—H2C	108.7
N1—Fe1—N3	175.23 (19)	C3—C2—H2D	108.7
N1—Fe1—N4	92.5 (2)	C1—C2—H2D	108.7
N2—Fe1—N3	90.7 (2)	H2C—C2—H2D	107.6
N2—Fe1—N4	168.6 (2)	N2—C3—C2	111.5 (6)
N3—Fe1—N4	88.4 (2)	N2—C3—H3C	109.3
O5—Cl1—O3	111.2 (7)	C2—C3—H3C	109.3
O5—Cl1—O6	108.5 (6)	N2—C3—H3D	109.3
O3—Cl1—O6	105.2 (7)	C2—C3—H3D	109.3
O5—Cl1—O4	110.3 (5)	H3C—C3—H3D	108.0
O3—Cl1—O4	105.3 (5)	C5—C4—N3	112.1 (5)
O6—Cl1—O4	116.3 (6)	C5—C4—H4C	109.2
C7—O1—Fe1	124.3 (3)	N3—C4—H4C	109.2
Fe1—N1—C1	119.4 (4)	C5—C4—H4D	109.2
C1—N1—H1A	107.5	N3—C4—H4D	109.2
Fe1—N1—H1A	107.5	H4C—C4—H4D	107.9
C1—N1—H1B	107.5	C4—C5—C6	113.8 (5)
Fe1—N1—H1B	107.5	C4—C5—H5A	108.8
H1A—N1—H1B	107.0	C6—C5—H5A	108.8
Fe1—N2—C3	121.2 (5)	C4—C5—H5B	108.8
C3—N2—H2A	107.0	C6—C5—H5B	108.8
Fe1—N2—H2A	107.0	H5A—C5—H5B	107.7
C3—N2—H2B	107.0	N4—C6—C5	110.2 (5)
Fe1—N2—H2B	107.0	N4—C6—H6A	109.6
H2A—N2—H2B	106.8	C5—C6—H6A	109.6
Fe1—N3—C4	116.6 (4)	N4—C6—H6B	109.6
C4—N3—H3A	108.2	C5—C6—H6B	109.6
Fe1—N3—H3A	108.2	H6A—C6—H6B	108.1
C4—N3—H3B	108.2	O1—C7—O2	123.8 (4)
Fe1—N3—H3B	108.2	O1—C7—C8	118.1 (4)
H3A—N3—H3B	107.3	O2—C7—C8	118.1 (4)
Fe1—N4—C6	116.2 (3)	C9—C8—C10	119.0 (4)
C6—N4—H4A	108.2	C9—C8—C7	120.1 (4)
Fe1—N4—H4A	108.2	C10—C8—C7	120.9 (4)
C6—N4—H4B	108.2	C8—C9—C10^i	120.6 (4)
Fe1—N4—H4B	108.2	C8—C9—H9	119.7
H4A—N4—H4B	107.4	C10^i—C9—H9	119.7
N1—C1—C2	111.7 (6)	C8—C10—C9^i	120.5 (5)
N1—C1—H1C	109.3	C8—C10—H10	119.8
C2—C1—H1C	109.3	C9^i—C10—H10	119.8
N1—C1—H1D	109.3

Symmetry code: (i) −x+1, −y+1, −z.