Poly[tris-(μ-benzene-1,4-dicarboxylato)bis-(dipyrido[3,2-a:2',3'-c]phenazine)trimanganese(II)].

In the title compound, [Mn(3)(C(8)H(4)O(4))(3)(C(14)H(8)N(4))(2)](n), one Mn atom is located on an inversion centre and is six-coordinated by four carboxyl-ate O atoms from different benzene-1,4-dicarboxyl-ate (1,4-bdc) ligands and two phenanthrene N atoms from a dipyrido[3,2-a:2',3'-c]phenazine ligand. The other Mn atom is also six-coordinate, binding to six carboxyl-ate O atoms from different 1,4-bdc ligands. The dicarboxyl-ate groups chelate and bridge the two Mn atoms and a symmetry-related Mn atom to form a trimanganese unit. Bridging of the trinuclear Mn(II) clusters leads to a two-dimensional structure.

Related literature

For related structures, see: Chen & Liu (2002 ▶).

Experimental

Crystal data

[Mn3(C8H4O4)3(C14H8N4)2]

M = 1121.64

Monoclinic,

a = 13.323 (3) Å

b = 10.949 (2) Å

c = 16.315 (3) Å

β = 90.04 (3)°

V = 2379.9 (8) Å3

Z = 2

Mo Kα radiation

μ = 0.86 mm−1

T = 293 (2) K

0.28 × 0.21 × 0.19 mm

Data collection

Rigaku R-AXIS RAPID diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.783, T max = 0.847

21939 measured reflections

5424 independent reflections

3840 reflections with I > 2σ(I)

R int = 0.073

Refinement

R[F 2 > 2σ(F 2)] = 0.047

wR(F 2) = 0.098

S = 1.05

5424 reflections

340 parameters

H-atom parameters constrained

Δρmax = 0.30 e Å−3

Δρmin = −0.39 e Å−3

Data collection: PROCESS-AUTO (Rigaku, 1998 ▶); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL-Plus (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808019752/dn2359sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808019752/dn2359Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Mn3(C8H4O4)3(C14H8N4)2]	F000 = 1134
Mr = 1121.64	Dx = 1.565 Mg m−3
Monoclinic, P21/c	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 14328 reflections
a = 13.323 (3) Å	θ = 3.0–27.5º
b = 10.949 (2) Å	µ = 0.86 mm−1
c = 16.315 (3) Å	T = 293 (2) K
β = 90.04 (3)º	Block, pale yellow
V = 2379.9 (8) Å3	0.28 × 0.21 × 0.19 mm
Z = 2

Rigaku R-AXIS RAPID diffractometer	5424 independent reflections
Radiation source: rotating anode	3840 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.073
Detector resolution: 10.0 pixels mm-1	θmax = 27.5º
T = 293(2) K	θmin = 3.1º
ω scans	h = −17→17
Absorption correction: multi-scan(ABSCOR; Higashi, 1995)	k = −14→13
Tmin = 0.783, Tmax = 0.847	l = −21→20
21939 measured reflections

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.047	H-atom parameters constrained
wR(F2) = 0.098	w = 1/[σ2(Fo2) + (0.0202P)2 + 2.6391P] where P = (Fo2 + 2Fc2)/3
S = 1.05	(Δ/σ)max = 0.001
5424 reflections	Δρmax = 0.30 e Å−3
340 parameters	Δρmin = −0.39 e Å−3
Primary atom site location: structure-invariant direct methods	Extinction correction: none

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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.

	x	y	z	Uiso*/Ueq
C1	0.0322 (2)	0.6320 (3)	0.4463 (2)	0.0404 (8)
H1	0.0486	0.5660	0.4130	0.048*
C2	−0.0586 (3)	0.6896 (3)	0.4341 (2)	0.0482 (9)
H2	−0.1025	0.6616	0.3939	0.058*
C3	−0.0840 (3)	0.7882 (3)	0.4815 (2)	0.0459 (9)
H3	−0.1446	0.8286	0.4733	0.055*
C4	−0.0176 (2)	0.8268 (3)	0.54190 (19)	0.0328 (7)
C5	0.0715 (2)	0.7628 (3)	0.55150 (18)	0.0287 (7)
C6	0.1417 (2)	0.7963 (3)	0.61634 (18)	0.0289 (7)
C7	0.2902 (3)	0.7568 (3)	0.6832 (2)	0.0433 (8)
H7	0.3489	0.7113	0.6878	0.052*
C8	0.2726 (3)	0.8488 (3)	0.7401 (2)	0.0494 (9)
H8	0.3187	0.8648	0.7815	0.059*
C9	0.1856 (3)	0.9157 (3)	0.7339 (2)	0.0465 (9)
H9	0.1719	0.9771	0.7717	0.056*
C10	0.1185 (2)	0.8913 (3)	0.67094 (19)	0.0338 (7)
C11	−0.0389 (2)	0.9296 (3)	0.5959 (2)	0.0361 (7)
C12	0.0252 (2)	0.9581 (3)	0.6599 (2)	0.0374 (8)
C13	−0.0781 (3)	1.1090 (4)	0.6994 (3)	0.0612 (11)
H13	−0.0953	1.1723	0.7348	0.073*
C14	−0.1422 (3)	1.0841 (3)	0.6341 (3)	0.0570 (11)
H14	−0.1990	1.1323	0.6267	0.068*
C15	0.4005 (2)	0.7660 (3)	0.49542 (19)	0.0324 (7)
C16	0.4529 (2)	0.8864 (2)	0.4964 (2)	0.0335 (7)
C17	0.5458 (3)	0.8984 (3)	0.5301 (3)	0.0619 (12)
H17	0.5784	0.8299	0.5508	0.074*
C18	0.5926 (3)	1.0109 (3)	0.5339 (3)	0.0664 (13)
H18	0.6559	1.0170	0.5575	0.080*
C19	0.3513 (2)	0.4088 (3)	0.63506 (18)	0.0311 (7)
C20	0.3366 (2)	0.3233 (3)	0.70612 (18)	0.0297 (7)
C21	0.4127 (2)	0.2443 (3)	0.7294 (2)	0.0442 (9)
H21	0.4735	0.2450	0.7015	0.053*
C22	0.3987 (2)	0.1647 (3)	0.7938 (2)	0.0388 (8)
H22	0.4505	0.1130	0.8099	0.047*
C23	0.3081 (2)	0.1615 (2)	0.83462 (17)	0.0259 (6)
C24	0.2313 (2)	0.2385 (3)	0.8108 (2)	0.0366 (8)
H24	0.1696	0.2349	0.8372	0.044*
C25	0.2460 (2)	0.3212 (3)	0.74757 (19)	0.0368 (8)
H25	0.1951	0.3751	0.7330	0.044*
C26	0.2900 (2)	0.0716 (2)	0.90190 (17)	0.0253 (6)
N1	0.09707 (18)	0.6666 (2)	0.50352 (15)	0.0314 (6)
N2	0.22697 (19)	0.7308 (2)	0.62252 (16)	0.0331 (6)
N3	−0.1245 (2)	0.9939 (3)	0.58228 (19)	0.0483 (8)
N4	0.0048 (2)	1.0488 (3)	0.7141 (2)	0.0531 (8)
O1	0.43683 (17)	0.4150 (2)	0.60481 (14)	0.0475 (6)
O2	0.27522 (16)	0.46763 (19)	0.61136 (13)	0.0367 (5)
O3	0.31820 (17)	0.75629 (19)	0.45763 (15)	0.0401 (6)
O4	0.43671 (16)	0.67877 (17)	0.53665 (13)	0.0333 (5)
O5	0.36377 (16)	0.01648 (19)	0.93248 (13)	0.0370 (5)
O6	0.20305 (16)	0.0478 (2)	0.92461 (13)	0.0395 (6)
Mn1	0.5000	0.5000	0.5000	0.02269 (14)
Mn2	0.25609 (3)	0.59443 (4)	0.51712 (3)	0.02279 (11)

	U11	U22	U33	U12	U13	U23
C1	0.0354 (19)	0.047 (2)	0.039 (2)	−0.0036 (15)	−0.0036 (15)	−0.0090 (15)
C2	0.036 (2)	0.064 (2)	0.045 (2)	−0.0035 (18)	−0.0131 (16)	−0.0072 (18)
C3	0.0327 (19)	0.057 (2)	0.048 (2)	0.0051 (17)	−0.0031 (16)	0.0013 (17)
C4	0.0269 (16)	0.0366 (17)	0.0350 (18)	0.0020 (14)	0.0016 (13)	0.0037 (13)
C5	0.0292 (16)	0.0252 (15)	0.0317 (17)	0.0002 (12)	0.0033 (13)	0.0015 (12)
C6	0.0302 (16)	0.0241 (15)	0.0323 (17)	0.0035 (12)	0.0018 (13)	0.0002 (12)
C7	0.039 (2)	0.050 (2)	0.041 (2)	0.0085 (16)	−0.0090 (15)	−0.0107 (16)
C8	0.047 (2)	0.056 (2)	0.045 (2)	0.0042 (18)	−0.0160 (17)	−0.0207 (17)
C9	0.051 (2)	0.044 (2)	0.045 (2)	0.0041 (17)	−0.0037 (16)	−0.0180 (16)
C10	0.0363 (18)	0.0304 (17)	0.0348 (18)	0.0003 (14)	0.0012 (13)	−0.0014 (13)
C11	0.0318 (17)	0.0314 (18)	0.045 (2)	0.0060 (14)	0.0048 (14)	0.0062 (14)
C12	0.0397 (19)	0.0298 (17)	0.043 (2)	0.0064 (14)	0.0072 (15)	−0.0030 (14)
C13	0.061 (3)	0.046 (2)	0.077 (3)	0.020 (2)	0.006 (2)	−0.014 (2)
C14	0.049 (2)	0.042 (2)	0.079 (3)	0.0222 (19)	0.009 (2)	0.003 (2)
C15	0.0368 (18)	0.0235 (16)	0.0368 (18)	−0.0017 (13)	0.0047 (14)	−0.0001 (13)
C16	0.0309 (17)	0.0184 (15)	0.051 (2)	−0.0031 (13)	−0.0035 (14)	0.0056 (13)
C17	0.051 (2)	0.0238 (18)	0.111 (4)	−0.0033 (17)	−0.034 (2)	0.021 (2)
C18	0.049 (2)	0.0296 (19)	0.121 (4)	−0.0141 (18)	−0.042 (2)	0.020 (2)
C19	0.0385 (18)	0.0289 (16)	0.0258 (16)	−0.0024 (14)	0.0006 (13)	0.0048 (12)
C20	0.0344 (17)	0.0291 (16)	0.0256 (16)	−0.0025 (13)	−0.0002 (12)	0.0079 (12)
C21	0.0293 (18)	0.056 (2)	0.047 (2)	0.0019 (16)	0.0076 (15)	0.0238 (17)
C22	0.0276 (17)	0.048 (2)	0.041 (2)	0.0079 (15)	0.0021 (14)	0.0201 (15)
C23	0.0305 (16)	0.0253 (15)	0.0220 (15)	−0.0025 (12)	−0.0021 (12)	0.0036 (11)
C24	0.0335 (18)	0.0392 (18)	0.0371 (19)	0.0059 (14)	0.0103 (14)	0.0148 (14)
C25	0.0405 (19)	0.0358 (18)	0.0342 (18)	0.0115 (15)	0.0058 (14)	0.0110 (14)
C26	0.0330 (16)	0.0207 (14)	0.0223 (15)	−0.0003 (12)	−0.0008 (12)	0.0001 (11)
N1	0.0318 (14)	0.0299 (14)	0.0324 (15)	−0.0004 (11)	−0.0022 (11)	−0.0025 (11)
N2	0.0339 (15)	0.0334 (14)	0.0320 (15)	0.0071 (11)	−0.0013 (11)	−0.0065 (11)
N3	0.0420 (17)	0.0420 (17)	0.061 (2)	0.0127 (14)	0.0055 (14)	0.0061 (15)
N4	0.054 (2)	0.0421 (17)	0.064 (2)	0.0163 (15)	0.0024 (16)	−0.0168 (15)
O1	0.0393 (13)	0.0572 (16)	0.0462 (15)	0.0007 (12)	0.0114 (11)	0.0291 (12)
O2	0.0418 (13)	0.0353 (12)	0.0329 (13)	0.0052 (10)	0.0036 (10)	0.0149 (9)
O3	0.0385 (13)	0.0260 (11)	0.0560 (15)	−0.0088 (10)	−0.0080 (11)	0.0055 (10)
O4	0.0479 (13)	0.0159 (10)	0.0361 (12)	−0.0008 (9)	0.0007 (10)	0.0003 (8)
O5	0.0363 (12)	0.0400 (13)	0.0349 (13)	0.0057 (10)	−0.0038 (10)	0.0153 (10)
O6	0.0340 (13)	0.0456 (13)	0.0391 (13)	−0.0035 (10)	0.0021 (10)	0.0213 (10)
Mn1	0.0237 (3)	0.0192 (3)	0.0252 (3)	−0.0012 (2)	0.0033 (2)	0.0028 (2)
Mn2	0.0281 (2)	0.0183 (2)	0.0220 (2)	0.00027 (18)	0.00073 (16)	−0.00085 (17)

C1—N1	1.328 (4)	C17—H17	0.9300
C1—C2	1.379 (5)	C18—C16i	1.369 (4)
C1—H1	0.9300	C18—H18	0.9300
C2—C3	1.370 (5)	C19—O1	1.244 (4)
C2—H2	0.9300	C19—O2	1.262 (4)
C3—C4	1.390 (4)	C19—C20	1.503 (4)
C3—H3	0.9300	C20—C25	1.384 (4)
C4—C5	1.387 (4)	C20—C21	1.386 (4)
C4—C11	1.457 (4)	C21—C22	1.378 (4)
C5—N1	1.356 (4)	C21—H21	0.9300
C5—C6	1.458 (4)	C22—C23	1.379 (4)
C6—N2	1.347 (4)	C22—H22	0.9300
C6—C10	1.404 (4)	C23—C24	1.382 (4)
C7—N2	1.331 (4)	C23—C26	1.494 (4)
C7—C8	1.390 (5)	C24—C25	1.386 (4)
C7—H7	0.9300	C24—H24	0.9300
C8—C9	1.374 (5)	C25—H25	0.9300
C8—H8	0.9300	C26—O6	1.245 (3)
C9—C10	1.388 (4)	C26—O5	1.256 (3)
C9—H9	0.9300	N1—Mn2	2.272 (3)
C10—C12	1.454 (4)	N2—Mn2	2.311 (2)
C11—N3	1.358 (4)	O1—Mn1	2.121 (2)
C11—C12	1.385 (5)	O2—Mn2	2.087 (2)
C12—N4	1.357 (4)	O3—Mn2	2.184 (2)
C13—N4	1.309 (5)	O4—Mn1	2.214 (2)
C13—C14	1.392 (6)	O5—Mn1ii	2.130 (2)
C13—H13	0.9300	O5—Mn2iii	2.333 (2)
C14—N3	1.322 (5)	O6—Mn2iii	2.281 (2)
C14—H14	0.9300	Mn1—O1iv	2.121 (2)
C15—O3	1.262 (4)	Mn1—O5v	2.130 (2)
C15—O4	1.264 (3)	Mn1—O5vi	2.130 (2)
C15—C16	1.492 (4)	Mn1—O4iv	2.214 (2)
C16—C17	1.361 (4)	Mn2—O6v	2.281 (2)
C16—C18i	1.369 (4)	Mn2—O5v	2.333 (2)
C17—C18	1.382 (5)
N1—C1—C2	122.8 (3)	C20—C21—H21	119.9
N1—C1—H1	118.6	C21—C22—C23	120.2 (3)
C2—C1—H1	118.6	C21—C22—H22	119.9
C3—C2—C1	119.8 (3)	C23—C22—H22	119.9
C3—C2—H2	120.1	C22—C23—C24	119.8 (3)
C1—C2—H2	120.1	C22—C23—C26	120.8 (3)
C2—C3—C4	118.8 (3)	C24—C23—C26	119.3 (3)
C2—C3—H3	120.6	C23—C24—C25	120.2 (3)
C4—C3—H3	120.6	C23—C24—H24	119.9
C5—C4—C3	118.1 (3)	C25—C24—H24	119.9
C5—C4—C11	119.2 (3)	C20—C25—C24	119.9 (3)
C3—C4—C11	122.6 (3)	C20—C25—H25	120.1
N1—C5—C4	122.9 (3)	C24—C25—H25	120.1
N1—C5—C6	116.9 (3)	O6—C26—O5	120.6 (3)
C4—C5—C6	120.2 (3)	O6—C26—C23	120.5 (3)
N2—C6—C10	122.2 (3)	O5—C26—C23	118.8 (3)
N2—C6—C5	117.5 (3)	C1—N1—C5	117.6 (3)
C10—C6—C5	120.3 (3)	C1—N1—Mn2	125.2 (2)
N2—C7—C8	123.0 (3)	C5—N1—Mn2	116.66 (19)
N2—C7—H7	118.5	C7—N2—C6	118.4 (3)
C8—C7—H7	118.5	C7—N2—Mn2	125.8 (2)
C9—C8—C7	118.7 (3)	C6—N2—Mn2	115.48 (19)
C9—C8—H8	120.6	C14—N3—C11	115.7 (3)
C7—C8—H8	120.6	C13—N4—C12	114.7 (3)
C8—C9—C10	119.6 (3)	C19—O1—Mn1	135.1 (2)
C8—C9—H9	120.2	C19—O2—Mn2	131.5 (2)
C10—C9—H9	120.2	C15—O3—Mn2	100.40 (19)
C9—C10—C6	118.1 (3)	C15—O4—Mn1	132.0 (2)
C9—C10—C12	123.0 (3)	C26—O5—Mn1ii	155.8 (2)
C6—C10—C12	118.9 (3)	C26—O5—Mn2iii	90.23 (17)
N3—C11—C12	121.5 (3)	Mn1ii—O5—Mn2iii	100.02 (8)
N3—C11—C4	117.7 (3)	C26—O6—Mn2iii	92.95 (17)
C12—C11—C4	120.7 (3)	O1iv—Mn1—O1	180.0
N4—C12—C11	122.2 (3)	O1iv—Mn1—O5v	87.63 (9)
N4—C12—C10	117.3 (3)	O1—Mn1—O5v	92.37 (9)
C11—C12—C10	120.4 (3)	O1iv—Mn1—O5vi	92.37 (9)
N4—C13—C14	124.0 (4)	O1—Mn1—O5vi	87.63 (9)
N4—C13—H13	118.0	O5v—Mn1—O5vi	180.00 (10)
C14—C13—H13	118.0	O1iv—Mn1—O4iv	91.07 (9)
N3—C14—C13	121.8 (3)	O1—Mn1—O4iv	88.93 (9)
N3—C14—H14	119.1	O5v—Mn1—O4iv	96.31 (8)
C13—C14—H14	119.1	O5vi—Mn1—O4iv	83.69 (8)
O3—C15—O4	121.8 (3)	O1iv—Mn1—O4	88.93 (9)
O3—C15—C16	119.1 (3)	O1—Mn1—O4	91.07 (9)
O4—C15—C16	119.0 (3)	O5v—Mn1—O4	83.69 (8)
C17—C16—C18i	117.9 (3)	O5vi—Mn1—O4	96.31 (8)
C17—C16—C15	121.0 (3)	O4iv—Mn1—O4	180.00 (10)
C18i—C16—C15	121.0 (3)	O2—Mn2—O3	145.20 (9)
C16—C17—C18	121.0 (3)	O2—Mn2—N1	114.63 (9)
C16—C17—H17	119.5	O3—Mn2—N1	91.60 (9)
C18—C17—H17	119.5	O2—Mn2—O6v	94.06 (9)
C16i—C18—C17	121.1 (3)	O3—Mn2—O6v	112.18 (9)
C16i—C18—H18	119.5	N1—Mn2—O6v	83.37 (9)
C17—C18—H18	119.5	O2—Mn2—N2	84.38 (9)
O1—C19—O2	125.9 (3)	O3—Mn2—N2	82.54 (9)
O1—C19—C20	117.4 (3)	N1—Mn2—N2	71.99 (9)
O2—C19—C20	116.7 (3)	O6v—Mn2—N2	151.86 (9)
C25—C20—C21	119.6 (3)	O2—Mn2—O5v	90.86 (9)
C25—C20—C19	120.1 (3)	O3—Mn2—O5v	85.76 (9)
C21—C20—C19	120.3 (3)	N1—Mn2—O5v	134.20 (8)
C22—C21—C20	120.3 (3)	O6v—Mn2—O5v	56.17 (7)
C22—C21—H21	119.9	N2—Mn2—O5v	151.71 (8)