Estrada-Soto S, Sánchez-Recillas A, Navarrete-Vázquez G
… +1 more, Tlahuext H
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484772
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The asymmetric unit of the title compound, C13H14O3, contains two independent mol-ecules, A and B, that are inter-connected through an offset π-π inter-action [inter-centroid separation = 3.6087 (4) Å]. The fused benzene...The asymmetric unit of the title compound, C13H14O3, contains two independent mol-ecules, A and B, that are inter-connected through an offset π-π inter-action [inter-centroid separation = 3.6087 (4) Å]. The fused benzene and pyran-2-one rings in each mol-ecule are essentially coplanar, having dihedral angles of 1.22 (12) and 1.57 (12)° for mol-ecules A and B, respectively. Similarly, the coumarin ring system and the 7-prop-oxy substituent are close to being coplanar [C-C-O-C torsion angles = 2.9 (2) and 1.4 (2)° for mol-ecules A and B, respectively]. In the crystal, the mol-ecules are connected by C-H⋯O hydrogen bonds, forming supra-molecular tapes along [100] that are linked into a three-dimensional network by C-H⋯π inter-actions, as well as by the aforementioned π-π inter-actions.
Shibahara M, Watanabe M, Matsumoto T
… +2 more, Goto K, Shinmyozu T
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484771
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The title compound, C40H46N2 {systematic name: 12,30-di-aza-hepta-cyclo[21.13.1.1(5,19).1(6,18).1(10,14).1(24,36).1(28,32)]do-tetra-conta-1(37),5(40),6(41),10(42),11,13,18,23,28,30,32(39),36(38)-dodeca-ene}, has syn-anti...The title compound, C40H46N2 {systematic name: 12,30-di-aza-hepta-cyclo[21.13.1.1(5,19).1(6,18).1(10,14).1(24,36).1(28,32)]do-tetra-conta-1(37),5(40),6(41),10(42),11,13,18,23,28,30,32(39),36(38)-dodeca-ene}, has syn-anti-syn geometry wherein the two outer [3.3]meta-cyclo-phane (MCP) moieties have a syn geometry, and contain the facing benzene and pyridine rings at dihedral angles of 26.26 (10) and 26.46 (10)°, respectively. The rings of the central [3.3]MCP unit are not parallel, but orientated at a slight angle of 2.66 (9)°. Three bridging methyl-ene groups are disordered over two sets of sites in a 0.60:0.40 ratio. In the crystal, the mol-ecules are linked by C-H⋯N inter-actions and inter-molecular C-H⋯π short contacts, generating a three-dimensional network.
Bortel G, Kováts E, Oszlányi G
… +1 more, Pekker S
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484770
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The structure of the title compound, 5,6-[(1R,10S)-2,9-dioxatri-cyclo-[8.6.0(3,8).0(11,16)]hexa-decane-1,10-di-yl]-(C60-Ih)[5,6]fullerene methane-dithione 0.1-solvate, C74H10O2·0.1CS2, has tetra-gonal (P42/n) symmetry at...The structure of the title compound, 5,6-[(1R,10S)-2,9-dioxatri-cyclo-[8.6.0(3,8).0(11,16)]hexa-decane-1,10-di-yl]-(C60-Ih)[5,6]fullerene methane-dithione 0.1-solvate, C74H10O2·0.1CS2, has tetra-gonal (P42/n) symmetry at 100 K. It has a unique eight-membered ring, with two incorporated O atoms in place of the original central ring of the anthracene. The distortion of the mol-ecular geometry around the cyclo-adduct bonds corresponds to that seen in related fullerene derivatives. Close packing of the adduct forms cavities partially filled with disordered carbon di-sulfide solvent mol-ecule. The 41% occupancy of the cavities yields an overall 1:0.103 adduct-solvent ratio. Reaction steps are described as light-assisted singlet-oxygen generation, peroxide, epoxide and dioxocin derivative formation and the final step of thermally activated cyclo-addition.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484769
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In the title compound, C25H23Cl2N3, the cyclo-octene ring adopts a twist chair-chair conformation. The dihedral angles between the central pyridine ring (r.m.s. deviation = 0.013 Å) and the pendant chloro-benzene and ben...In the title compound, C25H23Cl2N3, the cyclo-octene ring adopts a twist chair-chair conformation. The dihedral angles between the central pyridine ring (r.m.s. deviation = 0.013 Å) and the pendant chloro-benzene and benzyl rings are 78.07 (11) and 87.47 (12)°, respectively. No directional inter-actions could be identified in the crystal and the packing is governed by van der Waals inter-actions.
Govindaraj J, Rajkumar K, Ganeshraja AS
… +2 more, Anbalagan K, SubbiahPandi A
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484768
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In the title compound, [Cu(ClO4)(C3H10N2)2(H2O)]ClO4, the Cu(II) atom has a distorted octa-hedral coordination sphere and is coordinated by the N atoms of two propane-1,3-di-amine ligands in the equatorial plane. The axi...In the title compound, [Cu(ClO4)(C3H10N2)2(H2O)]ClO4, the Cu(II) atom has a distorted octa-hedral coordination sphere and is coordinated by the N atoms of two propane-1,3-di-amine ligands in the equatorial plane. The axial positions are occupied by a water O atom and an O atom of a disordered perchlorate anion [occupancy ratio 0.631 (9):0.369 (9)]. In the crystal, the various components are linked via O-H⋯O, N-H⋯O and C-H⋯O hydrogen bonds, forming sheets lying parallel to (001).
Mangwala Kimpende P, Thi Da T, Nguyen Huu D
… +1 more, Van Meervelt L
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484767
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In the title compound, [Pt(C11H13O2)Cl(C5H11N)]·C2H5OH, the Pt(II) cation is penta-coordinated in a distorted square-planar geometry. In the crystal, inversion dimers showing C-H⋯Cl and C-H⋯π inter-actions are further st...In the title compound, [Pt(C11H13O2)Cl(C5H11N)]·C2H5OH, the Pt(II) cation is penta-coordinated in a distorted square-planar geometry. In the crystal, inversion dimers showing C-H⋯Cl and C-H⋯π inter-actions are further stacked in columns along the a axis via C-H⋯π inter-actions. The ethanol solvate mol-ecule inter-acts with neighbouring meth-oxy groups of methyl-eugenol through O-H⋯O hydrogen bonds.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484766
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The structures of the 1:1 anhydrous salts of nicotine (NIC) with 3,5-di-nitro-salicylic acid (DNSA) and 5-sulfosalicylic acid (5-SSA), namely (1R,2S)-1-methyl-2-(pyridin-3-yl)-1H-pyrrolidin-1-ium 2-carb-oxy-4,6-di-nitro-...The structures of the 1:1 anhydrous salts of nicotine (NIC) with 3,5-di-nitro-salicylic acid (DNSA) and 5-sulfosalicylic acid (5-SSA), namely (1R,2S)-1-methyl-2-(pyridin-3-yl)-1H-pyrrolidin-1-ium 2-carb-oxy-4,6-di-nitro-phenolate, C10H15N2 (+)·C7H3N2O7 (-), (I), and (1R,2S)-1-methyl-2-(pyridin-3-yl)-1H-pyrrolidin-1-ium 3-carb-oxy-4-hy-droxy-benzene-sulfonate, C10H15N2 (+)·C7H5O6S(-), (II), are reported. The asymmetric units of both (I) and (II) comprise two independent nicotinium cations (C and D) and either two DNSA or two 5-SSA anions (A and B), respectively. One of the DNSA anions shows a 25% rotational disorder in the benzene ring system. In the crystal of (I), inter-unit pyrrolidinium N-H⋯Npyridine hydrogen bonds generate zigzag NIC cation chains which extend along a, while the DNSA anions are not involved in any formal inter-species hydrogen bonding but instead form π-π-associated stacks which are parallel to the NIC cation chains along a [ring-centroid separation = 3.857 (2) Å]. Weak C-H⋯O inter-actions between chain substructures give an overall three-dimensional structure. In the crystal of (II), A and B anions form independent zigzag chains with C and D cations, respectively, through carb-oxy-lic acid O-H⋯Npyridine hydrogen bonds. These chains, which extend along b, are pseudocentrosymmetrically related and give π-π inter-actions between the benzene rings of anions A and B and the pyridine rings of the NIC cations C and D, respectively [ring centroid separations = 3.6422 (19) and 3.7117 (19) Å]. Also present are weak C-H⋯O hydrogen-bonding inter-actions between the chains, giving an overall three-dimensional structure.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484765
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The title mol-ecule, [Ir(C14H14FN2O)2(C5H7O2)], is located on a twofold rotation axis, which passes through the Ir(III) atom and the central C atom of the pentane-2,4-dionate anion. The Ir(III) atom adopts a distorted oc...The title mol-ecule, [Ir(C14H14FN2O)2(C5H7O2)], is located on a twofold rotation axis, which passes through the Ir(III) atom and the central C atom of the pentane-2,4-dionate anion. The Ir(III) atom adopts a distorted octa-hedral coordination geometry, being C,N-chelated by two 2-tert-but-oxy-6-fluoro-3-(pyridin-2-yl)pyridin-4-yl ligands and O,O'-chelated by the pentane-2,4-dionato ligand. The bipyridinate ligands, which are perpendicular to each other [dihedral angle between the two least-squares planes = 89.95 (5)°], are arranged in a cis-C,C' and trans-N,N' fashion relative to the central metal cation. Intra-molecular C-H⋯O and C-H⋯N hydrogen bonds and inter-molecular C-H⋯F hydrogen bonds as well as π-π inter-actions between neighbouring pyridine rings [centroid-centroid distance 3.680 (1) Å] contribute to the stabilization of the mol-ecular and crystal structure, respectively.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484764
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We report here the crystal structure of a ten-coordinate lanthanum(III) metal coordinated by five bidentate ethyl-enedi-amine ligands, [La(C2H8N2)5]Cl3·C2H8N2·CH2Cl2. One free ethyl-enedi-amine mol-ecule and three Cl(-)...We report here the crystal structure of a ten-coordinate lanthanum(III) metal coordinated by five bidentate ethyl-enedi-amine ligands, [La(C2H8N2)5]Cl3·C2H8N2·CH2Cl2. One free ethyl-enedi-amine mol-ecule and three Cl(-) anions are also located in the asymmetric unit. The overall structure is held together by an extensive hydrogen-bonding network between the Cl(-) anions and the NH groups on the metal-bound ethyl-enedi-amine ligands. The free ethyl-enedi-amine mol-ecule is held in an ordered position by additional hydrogen bonds involving both the chlorides and -NH groups on the metal-bound ligands. One highly disordered mol-ecule of di-chloro-methane is located on an inversion center; however, all attempts to model this disorder were unsuccessful. The electron density in this space was removed using the BYPASS procedure [van der Sluis & Spek (1990 ▶). Acta Cryst. A46, 194-201].
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484763
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In the mol-ecular structure of the dinuclear title compound [η(5)-(C5(CH3)5)(CO)Fe{(μ-BCl)(μ-CO)}PtCl(P(C6H11)3)]·C6H6, the two metal atoms, iron(II) and platinum(II), are bridged by one carbonyl (μ-CO) and one chlorido-...In the mol-ecular structure of the dinuclear title compound [η(5)-(C5(CH3)5)(CO)Fe{(μ-BCl)(μ-CO)}PtCl(P(C6H11)3)]·C6H6, the two metal atoms, iron(II) and platinum(II), are bridged by one carbonyl (μ-CO) and one chlorido-borylene ligand (μ-BCl). The Pt(II) atom is additionally bound to a chloride ligand situated trans to the bridging borylene, and a tri-cyclo-hexyl-phosphane ligand (PCy3) trans to the carbonyl ligand, forming a distorted square-planar structural motif at the Pt(II) atom. The Fe(II) atom is bound to a penta-methyl-cyclo-penta-dienyl ligand [η(5)-C5(CH3)5] and one carbonyl ligand (CO), forming a piano-stool structure. Additionally, one benzene solvent mol-ecule is incorporated into the crystal structure, positioned staggered relative to the penta-methyl-cyclo-penta-dienyl ligand at the Fe(II) atom, with a centroid-centroid separation of 3.630 (2) Å.
Sooksimuang T, Kamtonwong S, Parnchan W
… +2 more, Kangkaew L, Sahasithiwat S
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484762
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The title compound, C26H20O5, crystallizes with two independent molecules (A and B) in the asymmetric unit, which differ primarily in the location of the -OCH3 groups. In the crystal, the mol-ecules form a layered struct...The title compound, C26H20O5, crystallizes with two independent molecules (A and B) in the asymmetric unit, which differ primarily in the location of the -OCH3 groups. In the crystal, the mol-ecules form a layered structure parallel to (10-1) by C-H⋯O hydrogen-bonded networks. Adjacent layers are also linked by further C-H⋯O hydrogen bonds, forming a three-dimensional structure.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484761
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In the title compound, C14H11N3OS, the ace-naphthyl-ene ring system and hydrazinecarbo-thio-amide unit (=N-NH-C=S-NH-) are essentially coplanar [with maximum deviations from their mean planes of -0.009 (2) and 0.033 (2) ...In the title compound, C14H11N3OS, the ace-naphthyl-ene ring system and hydrazinecarbo-thio-amide unit (=N-NH-C=S-NH-) are essentially coplanar [with maximum deviations from their mean planes of -0.009 (2) and 0.033 (2) Å, respectively], and make a dihedral angle of 1.59 (9)°. The mol-ecular conformation is stabilized by two weak intra-molecular hydrogen bonds (N-H⋯O and N-H⋯N), which generate S(6) and S(5) ring motifs. In the crystal, mol-ecules are linked by N-H⋯S hydrogen bonds, forming chains along [010]. The chains are linked via pairs of C-H⋯O hydrogen bonds, enclosing R (2) 2(10) ring motifs, and C-H⋯π inter-actions, forming a three-dimensional framework. The absolute structure of the title compound was determined by resonant scattering.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484760
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The title compounds, C17H20O2 (1) and C17H18O2 (2), are allyl-ated caged compounds. In (1), the carbon atoms bearing the allyl groups are far apart [2.9417 (17) Å], hence the expected ring-closing metathesis (RCM) protoc...The title compounds, C17H20O2 (1) and C17H18O2 (2), are allyl-ated caged compounds. In (1), the carbon atoms bearing the allyl groups are far apart [2.9417 (17) Å], hence the expected ring-closing metathesis (RCM) protocol failed to give a ring-closing product. When these carbon atoms are connected by a C-C bond as in (2), the distance between them is much smaller [1.611 (3) Å] and consequently the RCM process was successful. The caged carbon skeleton of (1) can be described as a fusion of four five-membered rings and one six-membered ring. All four five-membered rings exhibit envelope conformations. The structure of compound (2) consists of four five-membered rings, of which two are cyclo-penta-none rings bonded at the 2, 4 and 5 positions and linked at the 3-carbons by a methyl-ene bridge. It also consists of one four-membered and two six-membered rings. All four five-membered rings adopt envelope conformations. In the crystal of (1), mol-ecules are linked via C-H⋯O hydrogen bonds, forming sheets lying parallel to (010). In the crystal of (2), mol-ecules are linked via C-H⋯O hydrogen bonds forming chains along [100].
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484759
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The title compound, K(+)·C5H11O8S(-) [systematic name: potassium (1R,2R,3R,4R)-1,2,3,4,5-penta-hydroxy-pentane-1-sulfonate], formed by reaction of d-ribose with potassium hydrogen sulfite in water, crystallizes as colour...The title compound, K(+)·C5H11O8S(-) [systematic name: potassium (1R,2R,3R,4R)-1,2,3,4,5-penta-hydroxy-pentane-1-sulfonate], formed by reaction of d-ribose with potassium hydrogen sulfite in water, crystallizes as colourless plates. The anion has an open-chain structure in which the S atom and the C atoms of the sugar chain, excepting that of the hy-droxy-methyl group, form an essentially all-trans chain; the C atom of the hy-droxy-methyl group lies in a gauche relationship with the three contiguous C atoms. Through complex cation coordination (through seven oxygen atoms of six different anions) and inter-molecular O-H⋯O hydrogen bonding, a three-dimensional bonding network exists in the crystal structure.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484758
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In the title salt, (C2H8N)2[Ni(H2O)6)](SO4)2·2H2O, the Ni(II) cation is located on a centre of inversion and exhibits a slightly distorted octa-hedral arrangement of water mol-ecules. The Ni-O bond lengths in the complex...In the title salt, (C2H8N)2[Ni(H2O)6)](SO4)2·2H2O, the Ni(II) cation is located on a centre of inversion and exhibits a slightly distorted octa-hedral arrangement of water mol-ecules. The Ni-O bond lengths in the complex [Ni(H2O)6](2+) cation show a distribution as in the related Tutton salt (NH4)2[Ni(H2O)6](SO4)2, but are longer in average [2.056 (13) versus 2.037 (12) Å]. The noncoordinating water mol-ecules and di-methyl-ammonium cations connect the sulfate and [Ni(H2O)6](2+) octa-hedra via O-H⋯O and N-H⋯O hydrogen bonds from weak up to medium strength into a three-dimensional framework whereby the complex metal cations and sulfate anions are arranged in sheets parallel (001).
Ambekar SP, Mahesh Kumar K, Shirahatti AK
… +2 more, Kotresh O, Anil Kumar GN
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484757
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In the title compound, C20H19NO4S2, the morpholine ring adopts the expected chair conformation. The central phenyl ring makes dihedral angles of 67.97 (4) and 7.74 (3)°, respectively, with the benzoate phenyl ring and th...In the title compound, C20H19NO4S2, the morpholine ring adopts the expected chair conformation. The central phenyl ring makes dihedral angles of 67.97 (4) and 7.74 (3)°, respectively, with the benzoate phenyl ring and the morpholine mean plane. In the crystal, mol-ecules are linked by C-H⋯O hydrogen bonds, forming zigzag chains along the b-axis direction. C-H⋯π inter-actions link centrosymmetrically related mol-ecules, reinforcing the three-dimensional structure.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484756
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The asymmetric unit of the title compound, NH4 (+)·C11H14N6O7P(-)·0.5H2O, contains one 3'-azido-3'-de-oxy-thymidine-5'amino-carbonyl-phospho-nate (ACP-AZT) anion, half of an NH4 (+) cation lying on a twofold rotation axi...The asymmetric unit of the title compound, NH4 (+)·C11H14N6O7P(-)·0.5H2O, contains one 3'-azido-3'-de-oxy-thymidine-5'amino-carbonyl-phospho-nate (ACP-AZT) anion, half of an NH4 (+) cation lying on a twofold rotation axis and in another position, occupied with equal probabilities of 0.5, an NH4 (+) cation and a water mol-ecule. The amide group of the ACP-AZT anion is disordered (occupancy ratio 0.5:0.5), with one part forming an N-H⋯O (involving C=O⋯H4N(+)) hydrogen bond and the other an O-H⋯N (involving C-NH2⋯OH2) hydrogen bond with the components of the split NH4 (+)/H2O position. The pseudorotation parameters of ACP-AZT set it apart from previously studied AZT and thymidine. In the crystal, the various components are linked by N-H⋯O, O-H⋯O, N-H⋯N, C-H⋯O and C-H⋯N hydrogen bonds, forming a three-dimensional framework.
Penthala NR, Madadi NR, Bommagani S
… +2 more, Parkin S, Crooks PA
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484755
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The title compound, C19H17N3O3S (I), was prepared by a [3 + 2]cyclo-addition azide condensation reaction using sodium azide and l-proline as a Lewis base catalyst. N-Methyl-ation of compound (I) using CH3I gave compound...The title compound, C19H17N3O3S (I), was prepared by a [3 + 2]cyclo-addition azide condensation reaction using sodium azide and l-proline as a Lewis base catalyst. N-Methyl-ation of compound (I) using CH3I gave compound (II), C20H19N3O3S. The benzo-thio-phene ring systems in (I) and (II) are almost planar, with r.m.s deviations from the mean plane = 0.0205 (14) in (I) and 0.016 (2) Å in (II). In (I) and (II), the triazole rings make dihedral angles of 32.68 (5) and 10.43 (8)°, respectively, with the mean planes of the benzo-thio-phene ring systems. The trimeth-oxy phenyl rings make dihedral angles with the benzo-thio-phene rings of 38.48 (4) in (I) and 60.43 (5)° in (II). In the crystal of (I), the mol-ecules are linked into chains by N-H⋯O hydrogen bonds with R (2) 1(5) ring motifs. After the N-methyl-ation of structure (I), no hydrogen-bonding inter-actions were observed for structure (II). The crystal structure of (II) has a minor component of disorder that corresponds to a 180° flip of the benzo-thio-phene ring system [occupancy ratio 0.9363 (14):0.0637 (14)].
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484754
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In the asymmetric unit of the title compound, {[Ag(C11H11N3)]CF3SO3} n , there are two Ag(I) atoms, two N-(pyridine-2-ylmeth-yl)pyridine-3-amine ligands (A and B) and two CF3SO3 (-) anions. Both Ag(I) atoms are bridged b...In the asymmetric unit of the title compound, {[Ag(C11H11N3)]CF3SO3} n , there are two Ag(I) atoms, two N-(pyridine-2-ylmeth-yl)pyridine-3-amine ligands (A and B) and two CF3SO3 (-) anions. Both Ag(I) atoms are bridged by two pyridine N atoms from two symmetry-related A or B ligands, forming right- or left-handed helical chains, respectively. The Ag(I) atom of the right-handed helical chain adopts a slightly distorted linear coordination geometry [N-Ag-N = 170.69 (14)°], while that of the left-handed helical chain adopts a bent geometry [N-Ag-N = 149.42 (14)°]. Both helical chains have the same pitch length [10.8437 (5) Å], propagate along the b-axial direction and are alternately arranged via Ag⋯Ag [3.0814 (5) Å] and π-π stacking inter-actions [centroid-centroid distances = 3.514 (3) and 3.487 (3) Å], resulting in the formation of a two-dimensional supra-molecular network extending parallel to the ab plane. Weak Ag⋯O [2.861 (4), 2.617 (3), and 2.624 (4) Å] and Ag⋯F [3.017 (3) Å] inter-actions as well as N-H⋯O and C-H⋯O, C-H⋯N and C-H⋯F hydrogen-bonding inter-actions occur between the helical chains and the anions.