Abstract
C7H4IrNO4, triclinic, P
Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Data collection and handling.
Crystal: | Red needle |
Size: | 0.10 × 0.04 × 0.02 mm |
Wavelength: | Mo Kα radiation (0.71073 Å) |
μ: | 16.7 mm−1 |
Diffractometer, scan mode: | Bruker (Venture), θ/2θ scans |
θ max, completeness: | 28.4°, >99 % |
N(hkl)measured, N(hkl)unique, R int: | 13437, 2009, 0.042 |
Criterion for I obs, N(hkl)gt: | I obs > 2 σ(I obs), 1,978 |
N(param)refined: | 118 |
Programs: | SHELX 1 , Bruker 2 , Olex2 3 , Diamond 4 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).
Atom | x | y | z | U iso */U eq |
---|---|---|---|---|
Ir1 | 0.52333 (4) | 0.31437 (2) | 0.27591 (2) | 0.01459 (6) |
O1 | 0.7167 (12) | 0.1772 (4) | 0.0776 (3) | 0.0310 (8) |
O2 | 0.7426 (10) | 0.5685 (3) | 0.0830 (3) | 0.0249 (7) |
O4 | 0.3791 (9) | 0.3916 (3) | 0.4231 (3) | 0.0190 (6) |
O3 | 0.3683 (9) | 0.1513 (3) | 0.4225 (3) | 0.0188 (6) |
C3 | 0.2335 (11) | 0.3036 (4) | 0.5300 (4) | 0.0128 (7) |
N1 | 0.2294 (11) | 0.1782 (4) | 0.5296 (4) | 0.0181 (7) |
C7 | 0.0797 (13) | 0.0822 (4) | 0.6377 (4) | 0.0202 (8) |
H7 | 0.075533 | −0.005285 | 0.636924 | 0.024* |
C6 | −0.0632 (12) | 0.1147 (5) | 0.7464 (4) | 0.0207 (8) |
H6 | −0.165828 | 0.049568 | 0.821465 | 0.025* |
C5 | −0.0574 (12) | 0.2436 (5) | 0.7467 (4) | 0.0201 (8) |
H5 | −0.155687 | 0.265986 | 0.821916 | 0.024* |
C4 | 0.0891 (13) | 0.3374 (4) | 0.6389 (4) | 0.0186 (8) |
H4 | 0.092059 | 0.425238 | 0.638630 | 0.022* |
C1 | 0.6452 (13) | 0.2322 (4) | 0.1517 (4) | 0.0212 (9) |
C2 | 0.6604 (13) | 0.4695 (4) | 0.1557 (4) | 0.0192 (8) |
1 Source of materials
The complex was synthesized by modifying the method used before by reduction of hydrated IrCl3 in DMF, which was refluxed for approximately 20 min to give a yellow solution of di-μ-chloro-tetra-carbonyldiiridium(I), [IrCl(CO)2]2. 5 , 6 , 7
The addition of an equivalent of 2-oxopyridine (opoH) to the aforementioned yellow solution followed by addition of ice water to precipitate the dicarbonyliridium(I) complex, [Ir(opo)(CO)2]. The precipitate was filtered off and dried. Red needle crystals were obtained from DCM and benzene.
2 Experimental details
The aromatic H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms, with fixed C–H distances for aromatic C–H of 0.93 Å (C–H) [U iso(H) = 1.2U eq]. The graphics were obtained using the DIAMOND 4 program with 50 % probability ellipsoids.
3 Comment
Important stages in many catalytic processes, like the carbonylation of methanol, are represented by oxidative addition reactions to metal complexes. 5 Research has shown that in the catalytic cycles of some processes, the oxidative addition phase is the rate-determining step. Consequently, any alteration to this step may dictate the trajectory of the whole catalytic cycle. Owing to the importance of this reaction, a great deal of study has been done on oxidative addition processes to comprehend its kinetic behavior and reactions to both internal and external influences. 6 , 7 There has been much discussion regarding the synthesis of M(I) and M(III) complexes (M = Rh and Ir). Many studies involve the synthesis of the precursor complex [M(L,L′-BID)(CO)2], in which one of the carbonyl ligands may be replaced by tertiary phosphine ligands to form [M(L,L′-BID)(CO)(PX3)], where M represents Rh or Ir, L,L′-BID represents monocharged bidentate ligands with different donor atoms (L,L′) such as O,O′, O,N, O,S, and N,S, and PX3 represents various neutral monodentate tertiary phosphine ligands. 5 , 6 , 7 , 8 , 9 , 10 , 11 , 12 , 13 , 14 , 15 , 16 , 17 , 18 , 19 , 20 , 21 , 22
The 2-oxopyridine (opoH) ligand of the title complex was selected because of its small bite angle, forming a five-membered metallocycle ring when coordinated.
In the title structure, a slightly distorted square planar geometry is observed indicated by the small bite angle of 79.661(2)° for O3–Ir1–O4. The angles between the other atoms of the coordination sphere are affected as a consequence of the small bite angle and have values differing from the ideal 90°; 89.492(2)° for C1–Ir1–C2, 94.903(2)° for C2–Ir1–O4 and 95.942(2)° for C1–Ir1–O3. The Ir1–O3, Ir1–O4, Ir1–C1 and Ir1–C2 bond distances are 2.0372(1), 2.0302(1), 1.8371(1) and 1.8350(1) Å, respectively.
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Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.
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Research funding: The authors acknowledge funding under the Swiss–South Africa joint research program (SSAJRP) from the SANRF (A. Roodt: UID: 107802) as well as from the Competitive Program for Rated Researchers of the SANRF (A. Roodt: UID: 111698), from the South African Department of Science Innovation (DSI) and the Department of Science and Technology (DST) respectively, “Department of Science and Innovation, Republic of South Africa” and “Department of Science and Technology, Republic of South Africa”.
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Conflict of interest statement: The authors declare no conflicts of interest regarding this article.
References
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© 2024 the author(s), published by De Gruyter, Berlin/Boston
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Artikel in diesem Heft
- Frontmatter
- New Crystal Structures
- Crystal structure of the co-crystal 2,4,6-triamino-1,3,5-triazine-1,3-dioxide — acetic acid (1/2) C7H14N6O6
- Crystal structure of the dinuclear mercury(II) complex bis(μ2-bromido)-dibromido-bis{1-[(benzotriazol-1-yl)methyl]-1-H-1,3-(2-ethyl-5-methyl-imidazol)-κ1 N} dimercury(II), C26H30N10Hg2Br4
- Crystal structure of poly[hexaqua-pentakis(μ4-2,2′-bipyridine-4,4′-dicarboxylato-κ4 O:O′:O″:O‴)-(μ2-2,2′-bipyridine-4,4′-dicarboxylato-κ2 O:O)tetraytterbium(III)] hydrate, C36H26N6O16Yb2
- Hydrothermal synthesis and crystal structure of catena-poly[(1,10-phenanthroline-κ 2 N,N′)-bis(μ 2-nitroisophthalato-κ 3 O,O′:O″)nickel(II)], C20H13NiN3O7
- Crystal structure of 72,73,75,76-tetrafluoro-25,44-dimethyl-31,33,36,38-tetraoxo-31,32,33,36,37,38-hexahydro-3(2,7)-benzo[lmn][3,8]phenanthrolina-1,5(4,1)-dipyridin-1-iuma-2,4(1,2),7(1,4)-tribenzenacyclooctaphane-11,51-diium hexafluoridophosphate, [C46H28F4N4O4][PF6]2, a dicationic cyclophane
- Crystal structure of (E)-2-(4-(1H-imidazol-1-yl)benzylidene)-7-fluoro-3,4-dihydronaphthalen-1(2H)-one, C20H15FN2O
- The salt crystal structure of etoricoxib hydrochloride, C18H16Cl2N2O2S
- The structure of t-butyl 7-[2-(4-fluorophenyl)-3-phenyl-4-(phenylcarbamoyl)-5-(propan-2-yl)-1H-pyrrol-1-yl]-3,5-dihydroxyheptanoate, C37H43FN2O5
- The crystal structure of (μ4-oxo)-tri(μ4-2,2′-bipyridine-6,6′-bis(olato)-κ5 O,O′:N:N′:O″)tetrazinc(II) – methylformamide (1/1), C33H25N7O8Zn4
- The co-crystal structure of 4-chlorobenzophenone–salicylhydrazide(1/1), C20H17ClN2O3
- Crystal structure of 9-fluoro-4-(6-methoxypyridin-2-yl)-5,6-dihydrobenzo[h]quinazolin-2-amine, C18H15FN4O
- The crystal structure of the co-crystal composed of benzhydrazide and 5-aminoisophthalic acid, C8H7NO4⋅C7H8N2O
- The cocrystal structure of praziquantel-hesperetin (1/1), C35H38N2O8
- Crystal structure of new barium manganese fluorides dihydrates, Ba10Mn2F25·2H2O
- The crystal structure of bis[μ2-(3-(3-(pyridin-2-yl)-1H-pyrazol-1-yl)propanoate-κ2O:N)-bis(2,2′-bipyridine-κ2 N, N′)dicopper(II)]dinitrate, C42H36Cu2N12O10
- Crystal structure of (3,6-di(2-pyridyl)-4-phenylaminopyridazine-κ2N,N′)-bis(2-(p-toluene)pyridinyl-κ2C,N)-iridium(III) hexafluorophosphate –dichloromethane (1/1), C45H37Cl2F6IrN7P
- The crystal structure of 2-(2′-carboxybenzyl)benzoic acid, C15H12O5
- The crystal structure of dichlorido-[(E)-N′,N″-bis((2E,3E)-3-(hydroxyimino)butan-2-ylidene)-2-((E)-3-(hydroxyimino)butan-2-ylidene)hydrazine-1-carbohydrazonhydrazide-κ 4 N 4]cobalt(II), C13H22N9O3Cl2Co
- Crystal structure of (−)-flavesine H, C15H22N2O2
- Crystal structure of 3-methoxybenzyl 2-(6-methoxynaphthalen-2-yl)propanoate, C22H22O4
- Crystal structure of dicarbonyl(2-oxopyridin-1(2H)-olato-κ 2 O,O)iridium(I), C7H4IrNO4
- The crystal structure of 4-(3-(triphenylphosphonio)propyl)piperazin-1-ium dibromide trihydrate, C25H37Br2N2O3P
- The crystal structure of ethyl 5,6-dihydroxybenzofuran-3-carboxylate, C11H10O5
- Crystal structure of 14-(R)-(2′-cyano-phenoxy)-3,19-diacetyl andrographolide, C31H37NO7
- The twinned crystal structure of 10-(4-methyl benzoate)-2,8-diethyl-5,5-difluoro-1,3,7,9-tetramethyl-5H-di-pyrrolo[1,2-c:2′,1′-f] [1,3,2]diazaborinin-4-ium-5-uide, C25H29BF2N2O2
- The crystal structure of (9H-thioxanthen-9- ylidene)hydrazine monohydrate, C13H11N2SO0.5
- The crystal structure of pyridinium diaqua-{1,2-phenylenebis((carboxylatocarbonyl)amido-κ4 N,N′,O,O′)manganese(III), C15H14MnN3O8
- Crystal structure of the hydrogen storage active high entropy phase Tb0.82Sm0.18Ni0.83Co0.17Mg
- Crystal structure of diaqua-bis[5-methyl-1-(1H-pyrazol-3-yl)-1H-1,2,3-triazole-4-carboxylato-κ 2 N,O)]manganese(II), C14H16MnN10O6
- Crystal structures of diiodido-3-((pyridin-2-ylmethylene)amino)-2-(pyridin-3-yl)-2,3-dihydroquinazolin-4(1H)-one-cadmium(II)
- Synthesis and crystal structure of methyl 4-(2-ethoxy-2-oxoethoxy)-3,5-dimethoxybenzoate, C14H18O7
- Crystal structure of isoxazolo[4,5-b]pyridin-3-amine, C6H5N3O
- Crystal structure of 4-chloro-1-isobutyl-1H-imidazo, C14H14ClN3
- The crystal structure of 1,1,1,2,2,2-hexakis(2-methyl-2-phenylpropyl)distannane,C60H78Sn2
- The crystal structure of (2,7-dimethoxynaphthalene-1,8-diyl)bis((3-nitrophenyl)methanone), C26H18N2O8
- Crystal structure of diaqua-tetra((E)-(RS)-1-(2,4-dichlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pent-1-en-3-ol-κ 1 N)zinc(II) dinitrate dihydrate, C60H76Cl8N14O14Zn
- The crystal structure of diphenyl bis(2-((diphenoxyphosphoryl)amino)ethyl)phosphoramidate monohydrate C40H42N3O10P3
- Crystal structure of 4,4′-bis(dibromomethyl)-1,1′-biphenyl, C14H10Br4
- Crystal structure of CaPtZn
- Crystal structure of 3-chloro-5-(trifluoromethyl)pyridine-2-carboxylic acid, C7H3ClF3NO2
- The crystal structure of (3′-(2-bromophenyl)-2-phenyl-[2,2′-bioxiran]-3-yl)(phenyl)methanone, C92H68O12Br4
- Crystal structure of ethyl 4-(4-benzylpiperazin-1-yl)benzoate, C20H24N2O2
- The crystal structure of bis(selenocyanato-κ1 N)-bis(methanol)-bis((1E,2E)-1,2-bis (1-(pyridin-4-yl)ethylidene)-hydrazine)iron(II) methanol solvate, C34H44FeN10O4Se2
- Crystal structure of (E)-1-(5-bromo-2-hydroxyphenyl)-3-(5-(4-methoxyphenoxy)-3-methyl-1-phenyl-1H-pyrazol-4-yl)prop-2-en-1-one, C26H21BrN2O4
- The crystal structure of methyl 4-(4-(methylsulfonyl)phenyl)-2-methyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, C19H21NO5S
- Crystal structure of 1′,3′-dihydro-2,2′-spirobi[indene]-1,3-dione, C17H12O2
- Crystal structure of (E)-2,2′,3,3′-tetrahydro-[1,1′-biindenylidene]-4,4′-diol, C18H16O2
- Crystal structure of di-glycylglycinium squarate dihydrate, C12H22N4O12, at 105 K
- Crystal structure of {[(4-fluorophenyl)methyl]triphenylphosphonium}dibromocopper(I), [C25H21FP]+[CuBr2]−
- Crystal structure of poly[diaqua-bis(μ2-5-((pyridin-4-yl-methyl)amino)benzene-1,3-dicarboxylato-κ 2 N:O)cadmium(II)], C28H26CdN4O10
Artikel in diesem Heft
- Frontmatter
- New Crystal Structures
- Crystal structure of the co-crystal 2,4,6-triamino-1,3,5-triazine-1,3-dioxide — acetic acid (1/2) C7H14N6O6
- Crystal structure of the dinuclear mercury(II) complex bis(μ2-bromido)-dibromido-bis{1-[(benzotriazol-1-yl)methyl]-1-H-1,3-(2-ethyl-5-methyl-imidazol)-κ1 N} dimercury(II), C26H30N10Hg2Br4
- Crystal structure of poly[hexaqua-pentakis(μ4-2,2′-bipyridine-4,4′-dicarboxylato-κ4 O:O′:O″:O‴)-(μ2-2,2′-bipyridine-4,4′-dicarboxylato-κ2 O:O)tetraytterbium(III)] hydrate, C36H26N6O16Yb2
- Hydrothermal synthesis and crystal structure of catena-poly[(1,10-phenanthroline-κ 2 N,N′)-bis(μ 2-nitroisophthalato-κ 3 O,O′:O″)nickel(II)], C20H13NiN3O7
- Crystal structure of 72,73,75,76-tetrafluoro-25,44-dimethyl-31,33,36,38-tetraoxo-31,32,33,36,37,38-hexahydro-3(2,7)-benzo[lmn][3,8]phenanthrolina-1,5(4,1)-dipyridin-1-iuma-2,4(1,2),7(1,4)-tribenzenacyclooctaphane-11,51-diium hexafluoridophosphate, [C46H28F4N4O4][PF6]2, a dicationic cyclophane
- Crystal structure of (E)-2-(4-(1H-imidazol-1-yl)benzylidene)-7-fluoro-3,4-dihydronaphthalen-1(2H)-one, C20H15FN2O
- The salt crystal structure of etoricoxib hydrochloride, C18H16Cl2N2O2S
- The structure of t-butyl 7-[2-(4-fluorophenyl)-3-phenyl-4-(phenylcarbamoyl)-5-(propan-2-yl)-1H-pyrrol-1-yl]-3,5-dihydroxyheptanoate, C37H43FN2O5
- The crystal structure of (μ4-oxo)-tri(μ4-2,2′-bipyridine-6,6′-bis(olato)-κ5 O,O′:N:N′:O″)tetrazinc(II) – methylformamide (1/1), C33H25N7O8Zn4
- The co-crystal structure of 4-chlorobenzophenone–salicylhydrazide(1/1), C20H17ClN2O3
- Crystal structure of 9-fluoro-4-(6-methoxypyridin-2-yl)-5,6-dihydrobenzo[h]quinazolin-2-amine, C18H15FN4O
- The crystal structure of the co-crystal composed of benzhydrazide and 5-aminoisophthalic acid, C8H7NO4⋅C7H8N2O
- The cocrystal structure of praziquantel-hesperetin (1/1), C35H38N2O8
- Crystal structure of new barium manganese fluorides dihydrates, Ba10Mn2F25·2H2O
- The crystal structure of bis[μ2-(3-(3-(pyridin-2-yl)-1H-pyrazol-1-yl)propanoate-κ2O:N)-bis(2,2′-bipyridine-κ2 N, N′)dicopper(II)]dinitrate, C42H36Cu2N12O10
- Crystal structure of (3,6-di(2-pyridyl)-4-phenylaminopyridazine-κ2N,N′)-bis(2-(p-toluene)pyridinyl-κ2C,N)-iridium(III) hexafluorophosphate –dichloromethane (1/1), C45H37Cl2F6IrN7P
- The crystal structure of 2-(2′-carboxybenzyl)benzoic acid, C15H12O5
- The crystal structure of dichlorido-[(E)-N′,N″-bis((2E,3E)-3-(hydroxyimino)butan-2-ylidene)-2-((E)-3-(hydroxyimino)butan-2-ylidene)hydrazine-1-carbohydrazonhydrazide-κ 4 N 4]cobalt(II), C13H22N9O3Cl2Co
- Crystal structure of (−)-flavesine H, C15H22N2O2
- Crystal structure of 3-methoxybenzyl 2-(6-methoxynaphthalen-2-yl)propanoate, C22H22O4
- Crystal structure of dicarbonyl(2-oxopyridin-1(2H)-olato-κ 2 O,O)iridium(I), C7H4IrNO4
- The crystal structure of 4-(3-(triphenylphosphonio)propyl)piperazin-1-ium dibromide trihydrate, C25H37Br2N2O3P
- The crystal structure of ethyl 5,6-dihydroxybenzofuran-3-carboxylate, C11H10O5
- Crystal structure of 14-(R)-(2′-cyano-phenoxy)-3,19-diacetyl andrographolide, C31H37NO7
- The twinned crystal structure of 10-(4-methyl benzoate)-2,8-diethyl-5,5-difluoro-1,3,7,9-tetramethyl-5H-di-pyrrolo[1,2-c:2′,1′-f] [1,3,2]diazaborinin-4-ium-5-uide, C25H29BF2N2O2
- The crystal structure of (9H-thioxanthen-9- ylidene)hydrazine monohydrate, C13H11N2SO0.5
- The crystal structure of pyridinium diaqua-{1,2-phenylenebis((carboxylatocarbonyl)amido-κ4 N,N′,O,O′)manganese(III), C15H14MnN3O8
- Crystal structure of the hydrogen storage active high entropy phase Tb0.82Sm0.18Ni0.83Co0.17Mg
- Crystal structure of diaqua-bis[5-methyl-1-(1H-pyrazol-3-yl)-1H-1,2,3-triazole-4-carboxylato-κ 2 N,O)]manganese(II), C14H16MnN10O6
- Crystal structures of diiodido-3-((pyridin-2-ylmethylene)amino)-2-(pyridin-3-yl)-2,3-dihydroquinazolin-4(1H)-one-cadmium(II)
- Synthesis and crystal structure of methyl 4-(2-ethoxy-2-oxoethoxy)-3,5-dimethoxybenzoate, C14H18O7
- Crystal structure of isoxazolo[4,5-b]pyridin-3-amine, C6H5N3O
- Crystal structure of 4-chloro-1-isobutyl-1H-imidazo, C14H14ClN3
- The crystal structure of 1,1,1,2,2,2-hexakis(2-methyl-2-phenylpropyl)distannane,C60H78Sn2
- The crystal structure of (2,7-dimethoxynaphthalene-1,8-diyl)bis((3-nitrophenyl)methanone), C26H18N2O8
- Crystal structure of diaqua-tetra((E)-(RS)-1-(2,4-dichlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pent-1-en-3-ol-κ 1 N)zinc(II) dinitrate dihydrate, C60H76Cl8N14O14Zn
- The crystal structure of diphenyl bis(2-((diphenoxyphosphoryl)amino)ethyl)phosphoramidate monohydrate C40H42N3O10P3
- Crystal structure of 4,4′-bis(dibromomethyl)-1,1′-biphenyl, C14H10Br4
- Crystal structure of CaPtZn
- Crystal structure of 3-chloro-5-(trifluoromethyl)pyridine-2-carboxylic acid, C7H3ClF3NO2
- The crystal structure of (3′-(2-bromophenyl)-2-phenyl-[2,2′-bioxiran]-3-yl)(phenyl)methanone, C92H68O12Br4
- Crystal structure of ethyl 4-(4-benzylpiperazin-1-yl)benzoate, C20H24N2O2
- The crystal structure of bis(selenocyanato-κ1 N)-bis(methanol)-bis((1E,2E)-1,2-bis (1-(pyridin-4-yl)ethylidene)-hydrazine)iron(II) methanol solvate, C34H44FeN10O4Se2
- Crystal structure of (E)-1-(5-bromo-2-hydroxyphenyl)-3-(5-(4-methoxyphenoxy)-3-methyl-1-phenyl-1H-pyrazol-4-yl)prop-2-en-1-one, C26H21BrN2O4
- The crystal structure of methyl 4-(4-(methylsulfonyl)phenyl)-2-methyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, C19H21NO5S
- Crystal structure of 1′,3′-dihydro-2,2′-spirobi[indene]-1,3-dione, C17H12O2
- Crystal structure of (E)-2,2′,3,3′-tetrahydro-[1,1′-biindenylidene]-4,4′-diol, C18H16O2
- Crystal structure of di-glycylglycinium squarate dihydrate, C12H22N4O12, at 105 K
- Crystal structure of {[(4-fluorophenyl)methyl]triphenylphosphonium}dibromocopper(I), [C25H21FP]+[CuBr2]−
- Crystal structure of poly[diaqua-bis(μ2-5-((pyridin-4-yl-methyl)amino)benzene-1,3-dicarboxylato-κ 2 N:O)cadmium(II)], C28H26CdN4O10