catena-Poly[[[cis-diaqua­(1,10-phenanthroline-κ²N,N′)manganese(II)]-μ₂-3-sulfonatobenzoato-κ²O:O′] 0.32-hydrate]

In the title polymeric compound, [Mn(C₇H₄O₅S)(C₁₂H₈N₂)(H₂O)₂]·0.32H₂O, which was synthesized by a combination of hydro­thermal reaction and solution evaporation, each Mn^II ion approximates an octa­hedral geometry and each 3-sulfonatobenzoate ligand links two metal atoms in a μ₂ mode. Extensive hydrogen bonds between water mol­ecules and sulfonate groups give rise to a three-dimensional network in the crystal structure.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.006 Å
• Disorder in solvent or counterion
• R factor = 0.052
• wR factor = 0.125
• Data-to-parameter ratio = 11.9

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT245_ALERT_2_B U(iso) H1WA    Smaller than U(eq) O1W     by ...       0.07 AngSq
PLAT245_ALERT_2_B U(iso) H1WB    Smaller than U(eq) O1W     by ...       0.07 AngSq

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       2.62 Ratio
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      32.00 Perc.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          2

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

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 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
   0 ALERT type 5 Informative message, check

---

Computing details

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

catena-Poly[[[cis-diaqua(1,10-phenanthroline-κ²N,N')manganese(II)]-µ₂– 3-sulfonatobenzoato-κ²O:O'] 0.32-hydrate]

Crystal data

[Mn(C7H4O5S)(C12H8N2)(H2O)2]·0.32H2O	F(000) = 984
Mr = 477.10	Dx = 1.598 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 3170 reflections
a = 14.4739 (11) Å	θ = 2.3–26.2°
b = 7.6406 (6) Å	µ = 0.81 mm^−1
c = 18.9230 (15) Å	T = 295 K
β = 107.413 (1)°	Block, yellow
V = 1996.8 (3) Å^3	0.26 × 0.24 × 0.21 mm
Z = 4

Data collection

Bruker APEX area-detector diffractometer	3539 independent reflections
Radiation source: fine-focus sealed tube	3193 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.026
φ and ω scans	θmax = 25.1°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −16→17
Tmin = 0.816, Tmax = 0.848	k = −8→9
10076 measured reflections	l = −22→20

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)] = 0.052	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.125	H atoms treated by a mixture of independent and constrained refinement
S = 0.99	w = 1/[σ^2(Fo^2) + (0.064P)^2 + 2.9349P] where P = (Fo^2 + 2Fc^2)/3
3539 reflections	(Δ/σ)max < 0.001
298 parameters	Δρmax = 0.45 e Å^−3
9 restraints	Δρmin = −0.28 e Å^−3

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mn1	0.27970 (4)	0.08302 (7)	0.20370 (3)	0.03228 (18)
S1	0.35380 (6)	0.48243 (10)	0.15613 (4)	0.0295 (2)
O1	0.2619 (2)	0.6122 (4)	−0.13668 (14)	0.0645 (9)
O2	0.3097 (2)	0.3740 (4)	−0.18294 (13)	0.0588 (8)
O3	0.35674 (18)	0.3283 (3)	0.20179 (12)	0.0399 (6)
O4	0.26010 (17)	0.5636 (3)	0.13016 (13)	0.0431 (6)
O5	0.42978 (17)	0.6042 (3)	0.19477 (13)	0.0412 (6)
O6	0.2072 (2)	−0.1681 (3)	0.21593 (14)	0.0453 (6)
O7	0.41160 (18)	−0.0434 (3)	0.20236 (17)	0.0505 (7)
N1	0.1343 (2)	0.2153 (4)	0.17122 (16)	0.0405 (7)
N2	0.2223 (2)	0.0678 (4)	0.07831 (15)	0.0375 (7)
C1	0.0902 (3)	0.2821 (6)	0.2168 (3)	0.0612 (11)
H1	0.1216	0.2777	0.2674	0.073*
C2	−0.0007 (4)	0.3587 (7)	0.1928 (3)	0.0769 (15)
H2	−0.0291	0.4047	0.2268	0.092*
C3	−0.0476 (3)	0.3660 (6)	0.1195 (3)	0.0710 (14)
H3	−0.1088	0.4162	0.1028	0.085*
C4	−0.0038 (3)	0.2974 (5)	0.0685 (2)	0.0518 (10)
C5	−0.0492 (3)	0.2971 (6)	−0.0094 (3)	0.0667 (14)
H5	−0.1100	0.3477	−0.0286	0.080*
C6	−0.0054 (3)	0.2250 (6)	−0.0555 (3)	0.0663 (14)
H6	−0.0368	0.2261	−0.1062	0.080*
C7	0.0886 (3)	0.1460 (5)	−0.0288 (2)	0.0482 (10)
C8	0.1365 (4)	0.0652 (6)	−0.0733 (2)	0.0643 (13)
H8	0.1085	0.0642	−0.1244	0.077*
C9	0.2242 (3)	−0.0128 (6)	−0.0432 (2)	0.0627 (12)
H9	0.2559	−0.0681	−0.0731	0.075*
C10	0.2650 (3)	−0.0078 (6)	0.0331 (2)	0.0495 (10)
H10	0.3252	−0.0599	0.0536	0.059*
C11	0.0878 (2)	0.2217 (4)	0.09750 (19)	0.0376 (8)
C12	0.1353 (2)	0.1438 (4)	0.04822 (18)	0.0367 (8)
C13	0.3051 (3)	0.4708 (5)	−0.13034 (18)	0.0400 (8)
C14	0.3593 (2)	0.4061 (4)	−0.05334 (18)	0.0350 (8)
C15	0.3349 (2)	0.4678 (4)	0.00770 (17)	0.0319 (7)
H15	0.2851	0.5487	0.0016	0.038*
C16	0.3850 (2)	0.4080 (4)	0.07766 (17)	0.0293 (7)
C17	0.4613 (2)	0.2927 (4)	0.08794 (19)	0.0371 (8)
H17	0.4957	0.2555	0.1353	0.044*
C18	0.4862 (3)	0.2330 (5)	0.0270 (2)	0.0429 (9)
H18	0.5376	0.1554	0.0334	0.051*
C19	0.4346 (3)	0.2886 (5)	−0.04352 (19)	0.0404 (8)
H19	0.4508	0.2465	−0.0844	0.048*
O1W	0.3205 (17)	−0.016 (2)	−0.1705 (10)	0.147 (7)	0.32
H6A	0.221 (3)	−0.262 (3)	0.198 (2)	0.080*
H6B	0.220 (3)	−0.178 (5)	0.2626 (6)	0.080*
H7A	0.420 (3)	−0.1531 (15)	0.202 (2)	0.080*
H7B	0.460 (2)	0.006 (4)	0.232 (2)	0.080*
H1WA	0.333 (10)	0.093 (4)	−0.170 (8)	0.080*	0.32
H1WB	0.353 (10)	−0.070 (13)	−0.194 (8)	0.080*	0.32

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mn1	0.0361 (3)	0.0321 (3)	0.0258 (3)	0.0014 (2)	0.0048 (2)	−0.0005 (2)
S1	0.0341 (4)	0.0270 (4)	0.0254 (4)	0.0028 (3)	0.0059 (3)	−0.0009 (3)
O1	0.082 (2)	0.076 (2)	0.0344 (14)	0.0382 (18)	0.0155 (14)	0.0056 (14)
O2	0.096 (2)	0.0512 (17)	0.0262 (13)	0.0108 (16)	0.0142 (14)	−0.0020 (12)
O3	0.0561 (15)	0.0315 (13)	0.0323 (12)	−0.0042 (11)	0.0133 (11)	0.0016 (10)
O4	0.0392 (13)	0.0540 (16)	0.0341 (13)	0.0127 (12)	0.0082 (10)	−0.0031 (11)
O5	0.0462 (14)	0.0263 (12)	0.0438 (14)	−0.0012 (10)	0.0022 (11)	−0.0049 (10)
O6	0.0534 (15)	0.0403 (15)	0.0402 (14)	−0.0023 (13)	0.0113 (12)	−0.0056 (12)
O7	0.0379 (14)	0.0287 (13)	0.0714 (19)	0.0044 (11)	−0.0041 (13)	−0.0084 (13)
N1	0.0394 (16)	0.0404 (17)	0.0418 (17)	0.0034 (13)	0.0122 (13)	−0.0027 (13)
N2	0.0366 (15)	0.0407 (17)	0.0337 (15)	−0.0070 (13)	0.0082 (12)	−0.0033 (13)
C1	0.059 (3)	0.067 (3)	0.061 (3)	0.011 (2)	0.025 (2)	−0.007 (2)
C2	0.063 (3)	0.077 (3)	0.100 (4)	0.016 (3)	0.039 (3)	−0.010 (3)
C3	0.041 (2)	0.056 (3)	0.113 (4)	0.012 (2)	0.017 (3)	0.005 (3)
C4	0.037 (2)	0.034 (2)	0.076 (3)	−0.0039 (17)	0.005 (2)	0.0090 (19)
C5	0.043 (2)	0.051 (3)	0.085 (4)	−0.004 (2)	−0.012 (2)	0.025 (2)
C6	0.063 (3)	0.058 (3)	0.052 (3)	−0.022 (2)	−0.021 (2)	0.022 (2)
C7	0.052 (2)	0.047 (2)	0.0341 (19)	−0.0209 (19)	−0.0035 (17)	0.0127 (17)
C8	0.085 (3)	0.074 (3)	0.029 (2)	−0.035 (3)	0.009 (2)	−0.001 (2)
C9	0.076 (3)	0.074 (3)	0.047 (2)	−0.023 (3)	0.031 (2)	−0.020 (2)
C10	0.052 (2)	0.056 (2)	0.042 (2)	−0.0086 (19)	0.0168 (18)	−0.0117 (19)
C11	0.0336 (18)	0.0308 (18)	0.044 (2)	−0.0057 (15)	0.0045 (15)	0.0055 (15)
C12	0.0408 (19)	0.0311 (18)	0.0332 (17)	−0.0133 (15)	0.0037 (14)	0.0057 (14)
C13	0.042 (2)	0.050 (2)	0.0291 (18)	0.0003 (18)	0.0127 (15)	0.0020 (16)
C14	0.0353 (17)	0.0362 (19)	0.0342 (18)	−0.0026 (15)	0.0114 (14)	−0.0006 (14)
C15	0.0348 (17)	0.0295 (17)	0.0311 (17)	0.0017 (14)	0.0095 (14)	−0.0004 (13)
C16	0.0319 (16)	0.0262 (16)	0.0294 (16)	−0.0027 (13)	0.0087 (13)	−0.0025 (13)
C17	0.0371 (18)	0.0363 (19)	0.0351 (18)	0.0054 (15)	0.0067 (14)	0.0048 (15)
C18	0.042 (2)	0.037 (2)	0.051 (2)	0.0092 (16)	0.0173 (17)	−0.0002 (17)
C19	0.047 (2)	0.042 (2)	0.0357 (19)	−0.0013 (17)	0.0180 (16)	−0.0055 (15)
O1W	0.28 (2)	0.086 (10)	0.110 (12)	−0.014 (14)	0.109 (14)	0.000 (9)

Geometric parameters (Å, º)

Mn1—O2^i	2.083 (2)	C4—C11	1.399 (5)
Mn1—O7	2.146 (3)	C4—C5	1.423 (6)
Mn1—O3	2.187 (2)	C5—C6	1.340 (7)
Mn1—O6	2.232 (3)	C5—H5	0.9300
Mn1—N1	2.247 (3)	C6—C7	1.436 (6)
Mn1—N2	2.270 (3)	C6—H6	0.9300
S1—O4	1.438 (2)	C7—C8	1.386 (6)
S1—O3	1.454 (2)	C7—C12	1.412 (5)
S1—O5	1.459 (2)	C8—C9	1.363 (6)
S1—C16	1.770 (3)	C8—H8	0.9300
O1—C13	1.236 (5)	C9—C10	1.386 (6)
O2—C13	1.257 (4)	C9—H9	0.9300
O2—Mn1^ii	2.083 (2)	C10—H10	0.9300
O6—H6A	0.84 (3)	C11—C12	1.442 (5)
O6—H6B	0.850 (10)	C13—C14	1.516 (5)
O7—H7A	0.847 (10)	C14—C19	1.381 (5)
O7—H7B	0.84 (3)	C14—C15	1.388 (5)
N1—C1	1.320 (5)	C15—C16	1.383 (4)
N1—C11	1.356 (4)	C15—H15	0.9300
N2—C10	1.329 (5)	C16—C17	1.382 (4)
N2—C12	1.348 (4)	C17—C18	1.383 (5)
C1—C2	1.387 (6)	C17—H17	0.9300
C1—H1	0.9300	C18—C19	1.387 (5)
C2—C3	1.351 (7)	C18—H18	0.9300
C2—H2	0.9300	C19—H19	0.9300
C3—C4	1.406 (7)	O1W—H1WA	0.850 (10)
C3—H3	0.9300	O1W—H1WB	0.850 (10)
O2^i—Mn1—O7	99.86 (12)	C6—C5—C4	120.9 (4)
O2^i—Mn1—O3	86.10 (10)	C6—C5—H5	119.6
O7—Mn1—O3	85.74 (10)	C4—C5—H5	119.6
O2^i—Mn1—O6	89.31 (10)	C5—C6—C7	121.8 (4)
O7—Mn1—O6	93.55 (10)	C5—C6—H6	119.1
O3—Mn1—O6	175.16 (9)	C7—C6—H6	119.1
O2^i—Mn1—N1	95.75 (12)	C8—C7—C12	116.8 (4)
O7—Mn1—N1	164.20 (11)	C8—C7—C6	124.6 (4)
O3—Mn1—N1	92.89 (10)	C12—C7—C6	118.6 (4)
O6—Mn1—N1	89.09 (10)	C9—C8—C7	120.8 (4)
O2^i—Mn1—N2	169.26 (12)	C9—C8—H8	119.6
O7—Mn1—N2	90.77 (11)	C7—C8—H8	119.6
O3—Mn1—N2	93.18 (9)	C8—C9—C10	118.5 (4)
O6—Mn1—N2	91.61 (10)	C8—C9—H9	120.7
N1—Mn1—N2	73.57 (10)	C10—C9—H9	120.7
O4—S1—O3	114.17 (15)	N2—C10—C9	123.1 (4)
O4—S1—O5	112.87 (15)	N2—C10—H10	118.4
O3—S1—O5	109.57 (14)	C9—C10—H10	118.4
O4—S1—C16	107.64 (14)	N1—C11—C4	122.6 (3)
O3—S1—C16	105.62 (14)	N1—C11—C12	117.6 (3)
O5—S1—C16	106.40 (15)	C4—C11—C12	119.7 (3)
C13—O2—Mn1^ii	132.7 (3)	N2—C12—C7	122.7 (3)
S1—O3—Mn1	141.24 (15)	N2—C12—C11	118.1 (3)
Mn1—O6—H6A	121 (3)	C7—C12—C11	119.3 (3)
Mn1—O6—H6B	103 (3)	O1—C13—O2	125.6 (3)
H6A—O6—H6B	110 (4)	O1—C13—C14	118.7 (3)
Mn1—O7—H7A	125 (3)	O2—C13—C14	115.8 (3)
Mn1—O7—H7B	111 (3)	C19—C14—C15	119.7 (3)
H7A—O7—H7B	110.6 (17)	C19—C14—C13	120.1 (3)
C1—N1—C11	118.0 (3)	C15—C14—C13	120.1 (3)
C1—N1—Mn1	126.3 (3)	C16—C15—C14	119.6 (3)
C11—N1—Mn1	115.7 (2)	C16—C15—H15	120.2
C10—N2—C12	118.1 (3)	C14—C15—H15	120.2
C10—N2—Mn1	126.9 (3)	C17—C16—C15	120.9 (3)
C12—N2—Mn1	115.0 (2)	C17—C16—S1	118.7 (2)
N1—C1—C2	123.1 (4)	C15—C16—S1	120.3 (2)
N1—C1—H1	118.4	C16—C17—C18	119.3 (3)
C2—C1—H1	118.4	C16—C17—H17	120.3
C3—C2—C1	119.3 (4)	C18—C17—H17	120.3
C3—C2—H2	120.4	C17—C18—C19	120.1 (3)
C1—C2—H2	120.4	C17—C18—H18	119.9
C2—C3—C4	119.9 (4)	C19—C18—H18	119.9
C2—C3—H3	120.0	C14—C19—C18	120.3 (3)
C4—C3—H3	120.0	C14—C19—H19	119.9
C11—C4—C3	117.0 (4)	C18—C19—H19	119.9
C11—C4—C5	119.7 (4)	H1WA—O1W—H1WB	109.7 (19)
C3—C4—C5	123.3 (4)
O4—S1—O3—Mn1	48.7 (3)	C8—C9—C10—N2	0.7 (7)
O5—S1—O3—Mn1	176.4 (2)	C1—N1—C11—C4	0.6 (5)
C16—S1—O3—Mn1	−69.4 (3)	Mn1—N1—C11—C4	179.1 (3)
O2^i—Mn1—O3—S1	−142.8 (3)	C1—N1—C11—C12	−178.3 (3)
O7—Mn1—O3—S1	117.0 (2)	Mn1—N1—C11—C12	0.2 (4)
N1—Mn1—O3—S1	−47.3 (2)	C3—C4—C11—N1	−0.9 (5)
N2—Mn1—O3—S1	26.4 (2)	C5—C4—C11—N1	−179.0 (3)
O2^i—Mn1—N1—C1	−3.5 (4)	C3—C4—C11—C12	178.0 (4)
O7—Mn1—N1—C1	−174.4 (4)	C5—C4—C11—C12	−0.1 (5)
O3—Mn1—N1—C1	−89.9 (3)	C10—N2—C12—C7	−0.1 (5)
O6—Mn1—N1—C1	85.7 (3)	Mn1—N2—C12—C7	−179.7 (3)
N2—Mn1—N1—C1	177.7 (4)	C10—N2—C12—C11	178.3 (3)
O2^i—Mn1—N1—C11	178.2 (2)	Mn1—N2—C12—C11	−1.3 (4)
O7—Mn1—N1—C11	7.3 (5)	C8—C7—C12—N2	0.0 (5)
O3—Mn1—N1—C11	91.8 (2)	C6—C7—C12—N2	177.9 (3)
O6—Mn1—N1—C11	−92.6 (2)	C8—C7—C12—C11	−178.3 (3)
N2—Mn1—N1—C11	−0.6 (2)	C6—C7—C12—C11	−0.5 (5)
O2^i—Mn1—N2—C10	175.2 (5)	N1—C11—C12—N2	0.8 (5)
O7—Mn1—N2—C10	3.6 (3)	C4—C11—C12—N2	−178.2 (3)
O3—Mn1—N2—C10	89.4 (3)	N1—C11—C12—C7	179.2 (3)
O6—Mn1—N2—C10	−90.0 (3)	C4—C11—C12—C7	0.3 (5)
N1—Mn1—N2—C10	−178.6 (3)	Mn1^ii—O2—C13—O1	15.5 (6)
O2^i—Mn1—N2—C12	−5.2 (7)	Mn1^ii—O2—C13—C14	−163.5 (2)
O7—Mn1—N2—C12	−176.8 (2)	O1—C13—C14—C19	−156.6 (4)
O3—Mn1—N2—C12	−91.0 (2)	O2—C13—C14—C19	22.5 (5)
O6—Mn1—N2—C12	89.6 (2)	O1—C13—C14—C15	21.9 (5)
N1—Mn1—N2—C12	1.0 (2)	O2—C13—C14—C15	−159.0 (3)
C11—N1—C1—C2	−0.3 (7)	C19—C14—C15—C16	−1.3 (5)
Mn1—N1—C1—C2	−178.5 (4)	C13—C14—C15—C16	−179.9 (3)
N1—C1—C2—C3	0.2 (8)	C14—C15—C16—C17	2.4 (5)
C1—C2—C3—C4	−0.5 (8)	C14—C15—C16—S1	−179.1 (2)
C2—C3—C4—C11	0.8 (7)	O4—S1—C16—C17	−166.1 (3)
C2—C3—C4—C5	178.8 (4)	O3—S1—C16—C17	−43.8 (3)
C11—C4—C5—C6	0.1 (6)	O5—S1—C16—C17	72.6 (3)
C3—C4—C5—C6	−177.9 (4)	O4—S1—C16—C15	15.3 (3)
C4—C5—C6—C7	−0.3 (7)	O3—S1—C16—C15	137.6 (3)
C5—C6—C7—C8	178.2 (4)	O5—S1—C16—C15	−106.0 (3)
C5—C6—C7—C12	0.5 (6)	C15—C16—C17—C18	−1.7 (5)
C12—C7—C8—C9	0.4 (6)	S1—C16—C17—C18	179.7 (3)
C6—C7—C8—C9	−177.4 (4)	C16—C17—C18—C19	−0.1 (5)
C7—C8—C9—C10	−0.7 (7)	C15—C14—C19—C18	−0.4 (5)
C12—N2—C10—C9	−0.3 (6)	C13—C14—C19—C18	178.1 (3)
Mn1—N2—C10—C9	179.3 (3)	C17—C18—C19—C14	1.1 (5)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6B···O1^i	0.85 (1)	1.89 (2)	2.696 (4)	158 (4)
O6—H6A···O4^iii	0.84 (3)	2.04 (2)	2.857 (4)	162 (4)
O7—H7A···O5^iii	0.85 (1)	1.87 (1)	2.714 (3)	175 (4)
O7—H7B···O5^iv	0.84 (3)	1.93 (3)	2.767 (3)	175 (5)
O1W—H1WA···O2	0.85 (1)	2.18 (5)	2.990 (16)	160 (14)

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