Poly[diaqua­tris[(E)-4,4′-(ethene-1,2-diyl)dibenzoato]trimanganese(II)]

Wang, H.-Y.; Gao, S.; Zhao, J.-G.; Ng, S.W.

doi:10.1107/S1600536806044126

Poly[diaquatris[(E)-4,4'-(ethene-1,2-diyl)dibenzoato]trimanganese(II)]

H.-Y. Wang, S. Gao, J.-G. Zhao and S. W. Ng

One of the two independent Mn atoms of the polymeric title compound, [Mn₃(C₁₆H₁₀O₄)₃(H₂O)₂]_n, lies on a special position of 3 site symmetry and the other on a special position of $\overline{3}$ site symmetry. One end of the 4,4'-(ethene-1,2-diyl)dibenzoate dianion bridges the two independent Mn atoms. The water-coordinated Mn atom on the threefold axis is linked to the O atoms of three dianions in a tetrahedral environment. The Mn atom is linked to the O atoms of six different dianions in an octahedral geometry.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806044126/hg2119sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806044126/hg2119Isup2.hkl Contains datablock I

CCDC reference: 627788

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
Mean (O-C) = 0.006 Å
Disorder in main residue
R factor = 0.069
wR factor = 0.251
Data-to-parameter ratio = 20.6

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT242_ALERT_2_A Check Low       Ueq as Compared to Neighbors for        Mn1

Author Response: ... The U(Mn) is normal but that of the coordinated water is large. This water molecule is not hydrogen bonded to acceptor sites.

PLAT601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .     216.00 A   3

Author Response: ... The structure is porous.


Alert level B
PLAT301_ALERT_3_B Main Residue  Disorder .........................      39.00 Perc.

Alert level C
ABSTM02_ALERT_3_C  The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
            Tmin and Tmax reported:      0.661     0.892
            Tmin(prime) and Tmax expected:      0.788     0.890
            RR(prime) =      0.837
            Please check that your absorption correction is appropriate.
RFACR01_ALERT_3_C  The value of the weighted R factor is > 0.25
            Weighted R factor given   0.251
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 ............       3.00 Ratio
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large .............       0.83
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       2.71 Ratio
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         O2
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          4
            O2  -MN2 -O2  -C1     12.00  0.00  10.555   1.555   1.555   1.555

Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C48 H34 Mn3 O14
            Atom count from the _atom_site data:  C48 H33.96 Mn3 O14
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G ALERT: check formula stoichiometry or atom site occupancies.
           From the CIF: _cell_formula_units_Z    3
           From the CIF: _chemical_formula_sum  C48 H34 Mn3 O14
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C        144.00    144.00    0.00
           H        102.00    101.88    0.12
           Mn         9.00      9.00    0.00
           O         42.00     42.00    0.00
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K

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

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

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: SHELXL97.

Poly[diaquatris[(E)-4,4'-(ethene-1,2-diyl)dibenzoato]trimanganese(II)] top

Crystal data top

[Mn₃(C₁₆H₁₀O₄)₃(H₂O)₂]	D_x = 1.280 Mg m⁻³
M_r = 999.57	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3	Cell parameters from 10113 reflections
Hall symbol: -R 3	θ = 3.1–27.5°
a = 16.3366 (8) Å	µ = 0.78 mm⁻¹
c = 16.8286 (7) Å	T = 293 K
V = 3889.6 (2) Å³	Block, yellow
Z = 3	0.30 × 0.22 × 0.15 mm
F(000) = 1527

Data collection top

Rigaku R-AXIS RAPID IP diffractometer	1980 independent reflections
Radiation source: fine-focus sealed tube	1663 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.021
ω scans	θ_max = 27.5°, θ_min = 3.1°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −21→21
T_min = 0.661, T_max = 0.892	k = −21→21
12671 measured reflections	l = −20→21

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)] = 0.069	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.251	H-atom parameters constrained
S = 1.12	w = 1/[σ²(F_o²) + (0.1598P)² + 8.6886P] where P = (F_o² + 2F_c²)/3
1980 reflections	(Δ/σ)_max = 0.001
96 parameters	Δρ_max = 0.94 e Å⁻³
94 restraints	Δρ_min = −0.58 e Å⁻³

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Mn1	0.0000	0.0000	0.20525 (6)	0.0515 (4)
Mn2	0.0000	0.0000	0.0000	0.0352 (4)
O1	−0.0113 (3)	0.1201 (2)	0.1910 (2)	0.0728 (9)
O2	0.0565 (2)	0.1213 (2)	0.0776 (2)	0.0644 (8)
O1w	0.0000	0.0000	0.3285 (5)	0.175 (6)
H1W	−0.0027	0.0459	0.3448	0.209*	0.33
H2W	0.0486	0.0027	0.3448	0.209*	0.33
C1	0.0197 (3)	0.1546 (3)	0.1232 (3)	0.0562 (10)
C2	0.0151 (10)	0.2381 (7)	0.0948 (8)	0.0619 (12)	0.50
C3	−0.0557 (10)	0.2524 (8)	0.1254 (7)	0.067 (3)	0.50
H3	−0.1010	0.2079	0.1593	0.081*	0.50
C4	−0.0589 (8)	0.3333 (8)	0.1052 (7)	0.093 (2)	0.50
H4	−0.1063	0.3429	0.1256	0.112*	0.50
C5	0.0088 (7)	0.3998 (6)	0.0544 (6)	0.089 (2)	0.50
C6	0.0796 (6)	0.3854 (6)	0.0238 (6)	0.082 (3)	0.50
H6	0.1249	0.4299	−0.0102	0.098*	0.50
C7	0.0828 (7)	0.3046 (7)	0.0440 (7)	0.075 (3)	0.50
H7	0.1302	0.2950	0.0235	0.090*	0.50
C8	0.0007 (10)	0.4825 (8)	0.0363 (10)	0.093 (4)	0.50
H8	−0.0345	0.4954	0.0723	0.111*	0.50
C9	−0.0115 (10)	0.7608 (7)	−0.1007 (7)	0.0619 (12)	0.50
C10	0.0439 (11)	0.7353 (9)	−0.1452 (6)	0.067 (3)	0.50
H10	0.0710	0.7665	−0.1926	0.081*	0.50
C11	0.0588 (9)	0.6631 (8)	−0.1190 (7)	0.093 (2)	0.50
H11	0.0959	0.6460	−0.1488	0.112*	0.50
C12	0.0183 (6)	0.6164 (6)	−0.0482 (6)	0.089 (2)	0.50
C13	−0.0372 (6)	0.6420 (6)	−0.0037 (5)	0.082 (3)	0.50
H13	−0.0643	0.6108	0.0436	0.098*	0.50
C14	−0.0521 (8)	0.7141 (7)	−0.0300 (7)	0.075 (3)	0.50
H14	−0.0891	0.7312	−0.0002	0.090*	0.50
C15	0.0362 (10)	0.5416 (8)	−0.0237 (11)	0.093 (4)	0.50
H15	0.0792	0.5344	−0.0550	0.111*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mn1	0.0517 (5)	0.0517 (5)	0.0511 (6)	0.0258 (2)	0.000	0.000
Mn2	0.0344 (5)	0.0344 (5)	0.0367 (6)	0.0172 (2)	0.000	0.000
O1	0.104 (3)	0.0564 (17)	0.0649 (19)	0.0447 (18)	−0.0082 (17)	−0.0063 (14)
O2	0.0582 (16)	0.0481 (15)	0.090 (2)	0.0286 (13)	−0.0134 (15)	−0.0254 (14)
O1w	0.233 (9)	0.233 (9)	0.058 (5)	0.116 (5)	0.000	0.000
C1	0.061 (2)	0.0435 (18)	0.067 (2)	0.0278 (17)	−0.0161 (18)	−0.0164 (17)
C2	0.081 (3)	0.053 (2)	0.062 (3)	0.042 (2)	0.003 (2)	−0.0041 (18)
C3	0.082 (4)	0.062 (4)	0.067 (6)	0.043 (3)	0.006 (4)	−0.008 (4)
C4	0.114 (4)	0.088 (4)	0.108 (5)	0.073 (3)	0.023 (4)	0.006 (3)
C5	0.108 (6)	0.085 (4)	0.100 (4)	0.067 (4)	0.007 (4)	0.008 (3)
C6	0.101 (6)	0.071 (5)	0.076 (5)	0.044 (4)	0.008 (4)	0.011 (4)
C7	0.089 (6)	0.076 (4)	0.075 (4)	0.053 (5)	0.015 (4)	0.003 (3)
C8	0.100 (9)	0.085 (6)	0.111 (6)	0.059 (6)	0.019 (6)	0.010 (5)
C9	0.081 (3)	0.053 (2)	0.062 (3)	0.042 (2)	0.003 (2)	−0.0041 (18)
C10	0.082 (4)	0.062 (4)	0.067 (6)	0.043 (3)	0.006 (4)	−0.008 (4)
C11	0.114 (4)	0.088 (4)	0.108 (5)	0.073 (3)	0.023 (4)	0.006 (3)
C12	0.108 (6)	0.085 (4)	0.100 (4)	0.067 (4)	0.007 (4)	0.008 (3)
C13	0.101 (6)	0.071 (5)	0.076 (5)	0.044 (4)	0.008 (4)	0.011 (4)
C14	0.089 (6)	0.076 (4)	0.075 (4)	0.053 (5)	0.015 (4)	0.003 (3)
C15	0.100 (9)	0.085 (6)	0.111 (6)	0.059 (6)	0.019 (6)	0.010 (5)

Geometric parameters (Å, º) top

Mn1—O1	2.075 (3)	C4—H4	0.9300
Mn1—O1ⁱ	2.075 (3)	C5—C6	1.3900
Mn1—O1ⁱⁱ	2.075 (3)	C5—C8	1.453 (6)
Mn1—O1w	2.074 (9)	C6—C7	1.3900
Mn2—O2	2.158 (3)	C6—H6	0.9300
Mn2—O2ⁱ	2.158 (3)	C7—H7	0.9300
Mn2—O2ⁱⁱ	2.158 (3)	C8—C15	1.315 (8)
Mn2—O2ⁱⁱⁱ	2.158 (3)	C8—H8	0.9300
Mn2—O2^iv	2.158 (3)	C9—C10	1.3900
Mn2—O2^v	2.158 (3)	C9—C14	1.3900
O1—C1	1.261 (6)	C9—C1^vi	1.502 (8)
O2—C1	1.254 (5)	C10—C11	1.3900
O1w—H1W	0.8200	C10—H10	0.9300
O1w—H2W	0.8200	C11—C12	1.3900
C1—C2	1.482 (9)	C11—H11	0.9300
C1—C9^vi	1.502 (8)	C12—C13	1.3900
C2—C3	1.3900	C12—C15	1.453 (6)
C2—C7	1.3900	C13—C14	1.3900
C3—C4	1.3900	C13—H13	0.9300
C3—H3	0.9300	C14—H14	0.9300
C4—C5	1.3900	C15—H15	0.9300

O1w—Mn1—O1ⁱ	96.64 (10)	C3—C4—C5	120.0
O1w—Mn1—O1	96.64 (10)	C3—C4—H4	120.0
O1ⁱ—Mn1—O1	118.68 (4)	C5—C4—H4	120.0
O1w—Mn1—O1ⁱⁱ	96.64 (10)	C6—C5—C4	120.0
O1ⁱ—Mn1—O1ⁱⁱ	118.68 (4)	C6—C5—C8	123.3 (5)
O1—Mn1—O1ⁱⁱ	118.68 (4)	C4—C5—C8	116.7 (5)
O2—Mn2—O2ⁱⁱⁱ	180.00 (17)	C5—C6—C7	120.0
O2—Mn2—O2^v	92.85 (14)	C5—C6—H6	120.0
O2ⁱⁱⁱ—Mn2—O2^v	87.15 (14)	C7—C6—H6	120.0
O2—Mn2—O2ⁱ	87.15 (14)	C6—C7—C2	120.0
O2ⁱⁱⁱ—Mn2—O2ⁱ	92.85 (14)	C6—C7—H7	120.0
O2^v—Mn2—O2ⁱ	92.85 (14)	C2—C7—H7	120.0
O2—Mn2—O2^iv	92.85 (14)	C15—C8—C5	129.1 (7)
O2ⁱⁱⁱ—Mn2—O2^iv	87.15 (14)	C15—C8—H8	115.4
O2^v—Mn2—O2^iv	87.15 (14)	C5—C8—H8	115.4
O2ⁱ—Mn2—O2^iv	180.0	C10—C9—C14	120.0
O2—Mn2—O2ⁱⁱ	87.15 (14)	C10—C9—C1^vi	120.8 (9)
O2ⁱⁱⁱ—Mn2—O2ⁱⁱ	92.85 (14)	C14—C9—C1^vi	118.9 (9)
O2^v—Mn2—O2ⁱⁱ	180.00 (17)	C11—C10—C9	120.0
O2ⁱ—Mn2—O2ⁱⁱ	87.15 (14)	C11—C10—H10	120.0
O2^iv—Mn2—O2ⁱⁱ	92.85 (14)	C9—C10—H10	120.0
C1—O1—Mn1	108.7 (3)	C10—C11—C12	120.0
C1—O2—Mn2	133.7 (3)	C10—C11—H11	120.0
Mn1—O1w—H1W	109.5	C12—C11—H11	120.0
Mn1—O1w—H2W	109.5	C13—C12—C11	120.0
H1W—O1w—H2W	109.5	C13—C12—C15	122.4 (5)
O2—C1—O1	122.2 (4)	C11—C12—C15	117.6 (5)
O2—C1—C2	117.2 (6)	C14—C13—C12	120.0
O1—C1—C2	120.6 (6)	C14—C13—H13	120.0
O2—C1—C9^vi	121.8 (7)	C12—C13—H13	120.0
O1—C1—C9^vi	116.0 (6)	C13—C14—C9	120.0
C3—C2—C7	120.0	C13—C14—H14	120.0
C3—C2—C1	117.7 (9)	C9—C14—H14	120.0
C7—C2—C1	122.1 (9)	C8—C15—C12	129.5 (8)
C2—C3—C4	120.0	C8—C15—H15	115.3
C2—C3—H3	120.0	C12—C15—H15	115.3
C4—C3—H3	120.0

O1w—Mn1—O1—C1	157.2 (3)	C3—C4—C5—C6	0.0
O1ⁱ—Mn1—O1—C1	−101.5 (3)	C3—C4—C5—C8	−179.9 (3)
O1ⁱⁱ—Mn1—O1—C1	55.9 (4)	C4—C5—C6—C7	0.0
O2ⁱⁱⁱ—Mn2—O2—C1	−123 (38)	C8—C5—C6—C7	179.8 (3)
O2^v—Mn2—O2—C1	66.0 (4)	C5—C6—C7—C2	0.0
O2ⁱ—Mn2—O2—C1	−26.7 (5)	C3—C2—C7—C6	0.0
O2^iv—Mn2—O2—C1	153.3 (5)	C1—C2—C7—C6	−175.0 (9)
O2ⁱⁱ—Mn2—O2—C1	−114.0 (4)	C6—C5—C8—C15	20.6 (12)
Mn2—O2—C1—O1	78.4 (6)	C4—C5—C8—C15	−159.6 (11)
Mn2—O2—C1—C2	−102.4 (7)	C14—C9—C10—C11	0.0
Mn2—O2—C1—C9^vi	−102.6 (7)	C1^vi—C9—C10—C11	173.2 (9)
Mn1—O1—C1—O2	−4.5 (5)	C9—C10—C11—C12	0.0
Mn1—O1—C1—C2	176.4 (6)	C10—C11—C12—C13	0.0
Mn1—O1—C1—C9^vi	176.5 (6)	C10—C11—C12—C15	−180.0 (3)
O2—C1—C2—C3	154.0 (5)	C11—C12—C13—C14	0.0
O1—C1—C2—C3	−26.9 (8)	C15—C12—C13—C14	180.0 (3)
C9^vi—C1—C2—C3	−28 (12)	C12—C13—C14—C9	0.0
O2—C1—C2—C7	−30.9 (9)	C10—C9—C14—C13	0.0
O1—C1—C2—C7	148.3 (6)	C1^vi—C9—C14—C13	−173.3 (9)
C9^vi—C1—C2—C7	147 (12)	C5—C8—C15—C12	170.6 (8)
C7—C2—C3—C4	0.0	C13—C12—C15—C8	6.1 (12)
C1—C2—C3—C4	175.2 (9)	C11—C12—C15—C8	−174.0 (11)
C2—C3—C4—C5	0.0

Symmetry codes: (i) −y, x−y, z; (ii) −x+y, −x, z; (iii) −x, −y, −z; (iv) y, −x+y, −z; (v) x−y, x, −z; (vi) −x, −y+1, −z.

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Poly[diaqua­tris[(E)-4,4'-(ethene-1,2-diyl)dibenzoato]trimanganese(II)]

Supporting information

Key indicators

checkCIF/PLATON results

Poly[diaquatris[(E)-4,4'-(ethene-1,2-diyl)dibenzoato]trimanganese(II)]