Synthesis, crystal structure and topological analysis of a three-dimensional polymeric network based on zinc(II), potassium and 5-sulfo­benzene-1,3-di­carboxyl­ate (SIP)

Silva, F.H.; Franco, C.H.J.; Corrêa, C.C.; Diniz, R.

doi:10.1107/S2053229618010264

Synthesis, crystal structure and topological analysis of a three-dimensional polymeric network based on zinc(II), potassium and 5-sulfobenzene-1,3-dicarboxylate (SIP)

F. H. Silva, C. H. J. Franco, C. C. Corrêa and R. Diniz

Aromatic polycarboxylate linkers provide structural rigidity and strong interactions among the metal centre and the carboxylate O atoms. A new three-dimensional coordination polymer namely, catena-poly[potassium [tetraaqua(μ-5-sulfobenzene-1,3-dicarboxylato)zinc(II)]], {K[Zn(C₈H₃O₇S)(H₂O)₄]}_n or {K[Zn(SIP)(H₂O)₄]}_n, where SIP is 5-sulfobenzene-1,3-dicarboxylate or 5-sulfoisophthalate, was obtained and characterized by elemental analysis and IR vibrational spectroscopy, and the single-crystal structure was determined by X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P2₁/n with Z = 4. Topological analysis revealed that K—O interactions form a two-dimensional network, which is uninodal 4-connected and can be described with a point symbol (4⁴.6²), and this plane network is classified as sql/Shubnikov. The layers are connected by Zn²⁺ ions coordinated to the SIP linker, forming a three-dimensional network. This net is a trinodal (3,5,6)-connected system with point symbol (3.4⁴.5².6².7³.8³).(3.4⁴.5².6².7).(3.7²).

Keywords: synthesis; three-dimensional coordination polymer; topological analysis; 5-sulfobenzene-1,3-dicarboxylic acid; crystal structure.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618010264/ov3111sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S2053229618010264/ov3111Isup2.hkl Contains datablock I

CCDC reference: 1526885

Computing details top

Data collection: CrysAlis PRO (Rigaku OD, 2015); cell refinement: CrysAlis PRO (Rigaku OD, 2015); data reduction: CrysAlis PRO (Rigaku OD, 2015); program(s) used to solve structure: SHELXS2014 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: Mercury (Macrae et al., 2008) and ORTEP 3 For Windows (Farrugia, 2012); software used to prepare material for publication: WinGX (Farrugia, 2012), publCIF (Westrip, 2010) and TOPOSPRO (Blatov et al., 2016).

catena-Poly[potassium [tetraaqua(µ-5-sulfobenzene-1,3-dicarboxylato)zinc(II)]] top

Crystal data top

K[Zn(C₈H₃O₇S)(H₂O)₄]	F(000) = 848
M_r = 419.7	D_x = 2.079 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2yn	Cell parameters from 19501 reflections
a = 6.7891 (1) Å	θ = 3.7–29.0°
b = 16.7667 (2) Å	µ = 2.36 mm⁻¹
c = 11.7793 (1) Å	T = 293 K
β = 90.752 (1)°	Prismatic, colorless
V = 1340.73 (3) Å³	0.40 × 0.31 × 0.09 mm
Z = 4

Data collection top

Oxford Diffraction SuperNova Dual Source diffractometer with an AtlasS2 detector	3640 independent reflections
Radiation source: micro-focus sealed X-ray tube	3313 reflections with I > 2σ(I)
Mirror monochromator	R_int = 0.044
Detector resolution: 5.2923 pixels mm^-1	θ_max = 29.7°, θ_min = 3.2°
ω scans	h = −8→9
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2015)	k = −22→23
T_min = 0.735, T_max = 1	l = −16→16
41833 measured reflections

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.027	w = 1/[σ²(F_o²) + (0.0313P)² + 0.8858P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.065	(Δ/σ)_max < 0.001
S = 1.03	Δρ_max = 0.39 e Å⁻³
3640 reflections	Δρ_min = −0.53 e Å⁻³
210 parameters

Special details top

Experimental. #__ type_ start__ end____ width___ exp.time_ 1 omega -76.00 100.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 11.79 0.0000 0.0000 176

#__ type_ start__ end____ width___ exp.time_ 2 omega -20.00 53.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 11.79 -99.0000 60.0000 73

#__ type_ start__ end____ width___ exp.time_ 3 omega -20.00 29.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 -99.0000 90.0000 49

#__ type_ start__ end____ width___ exp.time_ 4 omega -85.00 16.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 -57.0000 159.0000 101

#__ type_ start__ end____ width___ exp.time_ 5 omega -40.00 61.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 57.0000 -60.0000 101

#__ type_ start__ end____ width___ exp.time_ 6 omega -62.00 36.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 11.79 -38.0000 -180.0000 98

#__ type_ start__ end____ width___ exp.time_ 7 omega -20.00 53.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 11.79 -99.0000 -180.0000 73

#__ type_ start__ end____ width___ exp.time_ 8 omega -20.00 29.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 -99.0000 -60.0000 49

#__ type_ start__ end____ width___ exp.time_ 9 omega -20.00 29.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 -99.0000 30.0000 49

#__ type_ start__ end____ width___ exp.time_ 10 omega -20.00 29.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 -99.0000 0.0000 49

#__ type_ start__ end____ width___ exp.time_ 11 omega -20.00 53.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 11.79 -99.0000 -120.0000 73

#__ type_ start__ end____ width___ exp.time_ 12 omega -20.00 53.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 11.79 -99.0000 120.0000 73

#__ type_ start__ end____ width___ exp.time_ 13 omega -45.00 64.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 77.0000 -120.0000 109

#__ type_ start__ end____ width___ exp.time_ 14 omega -88.00 -40.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 -77.0000 -30.0000 48

#__ type_ start__ end____ width___ exp.time_ 15 omega -20.00 29.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 -99.0000 -90.0000 49

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. Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement.

_reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences.

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

	x	y	z	U_iso*/U_eq
Zn	0.32214 (3)	0.24186 (2)	0.25221 (2)	0.02170 (7)
K	0.64311 (6)	0.06941 (3)	−0.36694 (4)	0.03651 (11)
S1	0.17932 (6)	−0.00347 (2)	−0.34264 (3)	0.01782 (9)
O1	−0.02690 (19)	−0.02261 (8)	−0.36164 (11)	0.0294 (3)
O2	0.23130 (18)	0.07663 (7)	−0.37944 (10)	0.0229 (2)
O3	0.3137 (2)	−0.06239 (8)	−0.38961 (11)	0.0331 (3)
O4	0.3177 (2)	0.14336 (7)	0.14800 (10)	0.0260 (3)
O5	0.3302 (2)	0.20402 (7)	−0.02076 (11)	0.0315 (3)
O6	0.20630 (19)	−0.15456 (7)	0.15212 (10)	0.0247 (3)
O7	0.1604 (2)	−0.21618 (8)	−0.01355 (11)	0.0354 (3)
O8	0.2021 (3)	0.17067 (10)	0.37636 (12)	0.0603 (6)
H8B	0.159977	0.131735	0.372871	0.090*
H8A	0.223746	0.185196	0.436560	0.090*
O9	0.6146 (2)	0.21894 (8)	0.31278 (11)	0.0299 (3)
H9B	0.648586	0.244628	0.361743	0.045*
H9A	0.628231	0.173398	0.331105	0.045*
O10	0.41855 (19)	0.31583 (7)	0.12098 (10)	0.0254 (3)
H10B	0.517963	0.338394	0.120587	0.038*
H10A	0.413573	0.287824	0.065490	0.038*
O11	0.02081 (19)	0.27368 (8)	0.19839 (12)	0.0306 (3)
H11A	−0.027408	0.248246	0.143978	0.046*
H11B	−0.033653	0.269686	0.248681	0.046*
C1	0.2708 (2)	0.06554 (9)	−0.01814 (13)	0.0173 (3)
C2	0.2506 (2)	−0.00558 (9)	0.04116 (13)	0.0183 (3)
H2	0.261025	−0.005655	0.119965	0.022*
C3	0.2149 (2)	−0.07678 (9)	−0.01654 (13)	0.0179 (3)
C4	0.1975 (2)	−0.07603 (9)	−0.13446 (13)	0.0190 (3)
H4	0.173554	−0.123245	−0.173700	0.023*
C5	0.2160 (2)	−0.00484 (9)	−0.19337 (13)	0.0171 (3)
C6	0.2538 (2)	0.06559 (9)	−0.13614 (13)	0.0187 (3)
H6	0.267832	0.112947	−0.176340	0.022*
C7	0.3089 (2)	0.14364 (9)	0.04129 (14)	0.0202 (3)
C8	0.1920 (2)	−0.15534 (10)	0.04498 (14)	0.0201 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn	0.03106 (12)	0.01702 (11)	0.01700 (11)	−0.00144 (7)	−0.00039 (8)	−0.00263 (7)
K	0.0276 (2)	0.0373 (2)	0.0447 (3)	−0.00300 (17)	0.00112 (18)	−0.00491 (18)
S1	0.0253 (2)	0.01469 (18)	0.01347 (17)	0.00044 (14)	−0.00119 (14)	0.00050 (13)
O1	0.0321 (7)	0.0289 (7)	0.0270 (6)	−0.0093 (5)	−0.0088 (5)	0.0037 (5)
O2	0.0285 (6)	0.0201 (6)	0.0201 (6)	−0.0016 (5)	−0.0003 (5)	0.0057 (4)
O3	0.0510 (9)	0.0283 (7)	0.0201 (6)	0.0166 (6)	0.0022 (6)	−0.0029 (5)
O4	0.0410 (7)	0.0199 (6)	0.0171 (6)	−0.0006 (5)	−0.0016 (5)	−0.0046 (4)
O5	0.0540 (9)	0.0165 (6)	0.0235 (6)	−0.0053 (6)	−0.0097 (6)	−0.0009 (5)
O6	0.0370 (7)	0.0200 (6)	0.0171 (6)	0.0005 (5)	−0.0016 (5)	0.0060 (4)
O7	0.0620 (10)	0.0181 (6)	0.0258 (7)	−0.0075 (6)	−0.0141 (6)	0.0043 (5)
O8	0.1187 (17)	0.0398 (9)	0.0226 (7)	−0.0450 (10)	0.0058 (8)	−0.0034 (6)
O9	0.0416 (8)	0.0229 (6)	0.0251 (6)	0.0070 (6)	−0.0074 (5)	−0.0057 (5)
O10	0.0327 (7)	0.0222 (6)	0.0213 (6)	−0.0063 (5)	0.0029 (5)	−0.0049 (5)
O11	0.0275 (7)	0.0318 (7)	0.0324 (7)	−0.0026 (5)	−0.0036 (5)	−0.0051 (5)
C1	0.0191 (7)	0.0157 (7)	0.0170 (7)	0.0000 (6)	−0.0013 (6)	−0.0020 (5)
C2	0.0202 (7)	0.0201 (7)	0.0146 (7)	0.0014 (6)	−0.0016 (5)	0.0005 (6)
C3	0.0194 (7)	0.0174 (7)	0.0170 (7)	0.0004 (6)	−0.0002 (6)	0.0028 (6)
C4	0.0239 (8)	0.0148 (7)	0.0182 (7)	−0.0016 (6)	−0.0008 (6)	−0.0004 (5)
C5	0.0209 (7)	0.0170 (7)	0.0133 (7)	0.0006 (6)	−0.0003 (5)	0.0002 (5)
C6	0.0240 (8)	0.0145 (7)	0.0176 (7)	−0.0005 (6)	0.0006 (6)	0.0014 (5)
C7	0.0218 (8)	0.0182 (7)	0.0204 (8)	0.0018 (6)	−0.0030 (6)	−0.0033 (6)
C8	0.0211 (8)	0.0186 (7)	0.0203 (7)	−0.0008 (6)	−0.0021 (6)	0.0040 (6)

Geometric parameters (Å, º) top

Zn—O4	2.0578 (12)	O6—C8	1.2646 (19)
Zn—O8	2.0637 (15)	O7—C8	1.248 (2)
Zn—O6ⁱ	2.0806 (11)	C1—C2	1.390 (2)
Zn—O10	2.0935 (12)	C1—C6	1.393 (2)
Zn—O9	2.1360 (13)	C1—C7	1.506 (2)
Zn—O11	2.1994 (13)	C2—C3	1.393 (2)
Zn—Kⁱⁱ	3.6627 (5)	C3—C4	1.392 (2)
K—O10ⁱⁱⁱ	2.6882 (13)	C3—C8	1.513 (2)
K—O1^iv	2.7202 (14)	C4—C5	1.387 (2)
K—O2	2.8004 (13)	C5—C6	1.382 (2)
K—O11ⁱⁱⁱ	2.8671 (14)	O8—H8A	0.7600
K—O3^v	2.8889 (13)	O8—H8B	0.7100
K—O6^vi	3.0689 (13)	O9—H9A	0.8000
K—O3	3.1527 (16)	O9—H9B	0.7500
K—S1	3.3931 (6)	O10—H10B	0.7700
K—K^v	4.3428 (9)	O10—H10A	0.8100
S1—O1	1.4509 (13)	O11—H11B	0.7100
S1—O2	1.4561 (12)	O11—H11A	0.8300
S1—O3	1.4589 (13)	C2—H2	0.9300
S1—C5	1.7726 (15)	C4—H4	0.9300
O4—C7	1.258 (2)	C6—H6	0.9300
O5—C7	1.258 (2)

O4—Zn—O8	87.46 (5)	S1—K—K^v	57.383 (12)
O4—Zn—O6ⁱ	172.87 (5)	Znⁱⁱⁱ—K—K^v	151.97 (2)
O8—Zn—O6ⁱ	93.37 (6)	O1—S1—O2	113.28 (7)
O4—Zn—O10	92.14 (5)	O1—S1—O3	113.51 (9)
O8—Zn—O10	174.95 (7)	O2—S1—O3	110.88 (8)
O6ⁱ—Zn—O10	86.42 (5)	O1—S1—C5	105.83 (7)
O4—Zn—O9	93.51 (5)	O2—S1—C5	106.02 (7)
O8—Zn—O9	91.90 (7)	O3—S1—C5	106.68 (7)
O6ⁱ—Zn—O9	93.54 (5)	O1—S1—K	164.01 (5)
O10—Zn—O9	93.15 (5)	O2—S1—K	54.12 (5)
O4—Zn—O11	90.94 (5)	O3—S1—K	68.04 (6)
O8—Zn—O11	88.29 (7)	C5—S1—K	88.28 (5)
O6ⁱ—Zn—O11	82.01 (5)	S1—O1—K^vii	132.13 (8)
O10—Zn—O11	86.68 (5)	S1—O2—K	100.96 (6)
O9—Zn—O11	175.55 (5)	S1—O3—K^v	118.43 (7)
O4—Zn—Kⁱⁱ	117.56 (4)	S1—O3—K	86.54 (6)
O8—Zn—Kⁱⁱ	129.73 (6)	K^v—O3—K	91.81 (4)
O6ⁱ—Zn—Kⁱⁱ	56.89 (3)	C7—O4—Zn	126.39 (11)
O10—Zn—Kⁱⁱ	46.42 (4)	C8—O6—Zn^viii	121.69 (11)
O9—Zn—Kⁱⁱ	125.86 (4)	C8—O6—K^vi	148.01 (10)
O11—Zn—Kⁱⁱ	51.49 (4)	Zn^viii—O6—K^vi	88.51 (4)
O10ⁱⁱⁱ—K—O1^iv	80.44 (4)	Zn—O10—Kⁱⁱ	99.23 (5)
O10ⁱⁱⁱ—K—O2	131.37 (4)	Zn—O11—Kⁱⁱ	91.63 (4)
O1^iv—K—O2	147.90 (4)	C2—C1—C6	119.64 (14)
O10ⁱⁱⁱ—K—O11ⁱⁱⁱ	63.99 (4)	C2—C1—C7	122.01 (14)
O1^iv—K—O11ⁱⁱⁱ	139.08 (4)	C6—C1—C7	118.35 (14)
O2—K—O11ⁱⁱⁱ	71.46 (4)	C1—C2—C3	120.51 (14)
O10ⁱⁱⁱ—K—O3^v	84.08 (4)	C4—C3—C2	119.39 (14)
O1^iv—K—O3^v	84.58 (4)	C4—C3—C8	118.55 (14)
O2—K—O3^v	93.65 (4)	C2—C3—C8	122.06 (14)
O11ⁱⁱⁱ—K—O3^v	109.71 (4)	C5—C4—C3	119.99 (14)
O10ⁱⁱⁱ—K—O6^vi	59.09 (3)	C6—C5—C4	120.57 (14)
O1^iv—K—O6^vi	88.83 (4)	C6—C5—S1	119.69 (12)
O2—K—O6^vi	110.17 (4)	C4—C5—S1	119.67 (12)
O11ⁱⁱⁱ—K—O6^vi	56.38 (4)	C5—C6—C1	119.90 (14)
O3^v—K—O6^vi	143.17 (4)	O4—C7—O5	125.41 (15)
O10ⁱⁱⁱ—K—O3	172.03 (4)	O4—C7—C1	117.84 (14)
O1^iv—K—O3	100.80 (4)	O5—C7—C1	116.75 (14)
O2—K—O3	47.11 (3)	O7—C8—O6	124.76 (15)
O11ⁱⁱⁱ—K—O3	117.28 (4)	O7—C8—C3	117.72 (14)
O3^v—K—O3	88.19 (4)	O6—C8—C3	117.52 (14)
O6^vi—K—O3	128.62 (4)	Zn—O8—H8A	114.00
O10ⁱⁱⁱ—K—S1	155.39 (3)	Zn—O8—H8B	131.00
O1^iv—K—S1	123.97 (3)	H8A—O8—H8B	115.00
O2—K—S1	24.92 (2)	Zn—O9—H9B	115.00
O11ⁱⁱⁱ—K—S1	92.03 (3)	H9A—O9—H9B	108.00
O3^v—K—S1	100.10 (3)	Zn—O9—H9A	111.00
O6^vi—K—S1	113.42 (3)	Zn—O10—H10A	104.00
O3—K—S1	25.42 (2)	Zn—O10—H10B	125.00
O10ⁱⁱⁱ—K—Znⁱⁱⁱ	34.34 (3)	K—O10—H10A	116.00
O1^iv—K—Znⁱⁱⁱ	102.25 (3)	K—O10—H10B	105.00
O2—K—Znⁱⁱⁱ	107.99 (3)	H10A—O10—H10B	108.00
O11ⁱⁱⁱ—K—Znⁱⁱⁱ	36.89 (3)	K—O11—H11B	118.00
O3^v—K—Znⁱⁱⁱ	112.22 (3)	H11A—O11—H11B	113.00
O6^vi—K—Znⁱⁱⁱ	34.60 (2)	K—O11—H11A	112.00
O3—K—Znⁱⁱⁱ	150.40 (3)	Zn—O11—H11A	117.00
S1—K—Znⁱⁱⁱ	125.621 (15)	Zn—O11—H11B	103.00
O10ⁱⁱⁱ—K—K^v	130.57 (3)	C1—C2—H2	120.00
O1^iv—K—K^v	94.20 (3)	C3—C2—H2	120.00
O2—K—K^v	63.14 (3)	C3—C4—H4	120.00
O11ⁱⁱⁱ—K—K^v	123.86 (3)	C5—C4—H4	120.00
O3^v—K—K^v	46.52 (3)	C1—C6—H6	120.00
O6^vi—K—K^v	170.24 (3)	C5—C6—H6	120.00
O3—K—K^v	41.67 (2)

Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) x−1/2, −y+1/2, z+1/2; (iii) x+1/2, −y+1/2, z−1/2; (iv) x+1, y, z; (v) −x+1, −y, −z−1; (vi) −x+1, −y, −z; (vii) x−1, y, z; (viii) −x+1/2, y−1/2, −z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8A···O7ⁱ	0.76	2.04	2.653 (2)	138
O8—H8B···O1^ix	0.71	2.05	2.759 (2)	177
O9—H9A···O3^vi	0.80	2.02	2.8166 (19)	174
O9—H9B···O5^x	0.75	2.03	2.7536 (18)	160
O10—H10A···O5	0.81	1.82	2.5757 (17)	156
O10—H10B···O2^x	0.77	2.03	2.7854 (17)	165
O11—H11A···O7^ix	0.83	1.85	2.667 (2)	166
C4—H4···O7	0.93	2.45	2.761 (2)	100
C6—H6···O2	0.93	2.48	2.8741 (19)	106
C6—H6···O5	0.93	2.42	2.7358 (19)	100

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

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Synthesis, crystal structure and topological analysis of a three-dimensional polymeric network based on zinc(II), potassium and 5-sulfo­benzene-1,3-di­carboxyl­ate (SIP)

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Synthesis, crystal structure and topological analysis of a three-dimensional polymeric network based on zinc(II), potassium and 5-sulfobenzene-1,3-dicarboxylate (SIP)