Literature DB >> 21200510

Bis[1,3-bis-(diphenyl-phosphinoylimino)isoindolinato-κO,N,O']calcium(II).

Zhiying Li, Donglin Shang, Jianping Guo.   

Abstract

In the title compound, [Ca(C(32)H(24)N(3)O(2)P(2))(2)], the 1,3-bis-(diphenyl-phosphinoylimino)isoindoline ligand adopts a tridentate coordination mode. The compound exhibits a distorted octa-hedral geometry. The Ca atom lies on a twofold rotation axis.

Entities:  

Year:  2007        PMID: 21200510      PMCID: PMC2915098          DOI: 10.1107/S1600536807065440

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For a related compound with similar octa­hedral geometry, see: Cole et al. (2006 ▶). For related literature, see: Shang (2007 ▶).

Experimental

Crystal data

[Ca(C32H24N3O2P2)2] M = 1129.04 Monoclinic, a = 26.351 (2) Å b = 12.4790 (11) Å c = 21.1997 (19) Å β = 126.1720 (10)° V = 5627.4 (9) Å3 Z = 4 Mo Kα radiation μ = 0.28 mm−1 T = 293 (2) K 0.20 × 0.15 × 0.10 mm

Data collection

Bruker SMART CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.837, T max = 0.973 11452 measured reflections 4959 independent reflections 4175 reflections with I > 2σ(I) R int = 0.019

Refinement

R[F 2 > 2σ(F 2)] = 0.050 wR(F 2) = 0.135 S = 1.04 4959 reflections 357 parameters H-atom parameters constrained Δρmax = 0.40 e Å−3 Δρmin = −0.25 e Å−3 Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: SHELXTL/PC (Sheldrick, 1999 ▶); software used to prepare material for publication: SHELXTL/PC. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807065440/ww2103sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536807065440/ww2103Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ca(C32H24N3O2P2)2]F000 = 2344
Mr = 1129.04Dx = 1.333 Mg m3
Monoclinic, C2/cMo Kα radiation λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 4426 reflections
a = 26.351 (2) Åθ = 2.4–25.9º
b = 12.4790 (11) ŵ = 0.28 mm1
c = 21.1997 (19) ÅT = 293 (2) K
β = 126.1720 (10)ºBlock, pink
V = 5627.4 (9) Å30.20 × 0.15 × 0.10 mm
Z = 4
Bruker SMART CCD diffractometer4959 independent reflections
Radiation source: fine-focus sealed tube4175 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.019
T = 293(2) Kθmax = 25.0º
ω scanθmin = 1.9º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)h = −31→17
Tmin = 0.837, Tmax = 0.973k = −14→14
11452 measured reflectionsl = −22→25
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.050H-atom parameters constrained
wR(F2) = 0.135  w = 1/[σ2(Fo2) + (0.075P)2 + 4.1489P] where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
4959 reflectionsΔρmax = 0.40 e Å3
357 parametersΔρmin = −0.25 e Å3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.
xyzUiso*/Ueq
Ca10.00000.39576 (5)0.25000.03918 (18)
P10.12637 (3)0.56655 (5)0.33048 (4)0.04665 (19)
P20.02345 (3)0.23193 (6)0.13903 (4)0.0498 (2)
O10.06204 (8)0.53300 (15)0.26479 (10)0.0621 (5)
O20.04545 (8)0.27801 (16)0.21607 (10)0.0620 (5)
N10.16798 (9)0.49240 (15)0.40938 (11)0.0447 (5)
N20.09048 (8)0.37004 (14)0.39391 (10)0.0401 (4)
N3−0.05179 (10)0.22572 (18)0.06938 (12)0.0553 (6)
C10.17484 (14)0.57710 (19)0.29706 (17)0.0566 (7)
C20.23898 (16)0.5685 (3)0.3464 (2)0.0778 (9)
H2B0.25920.55830.39960.093*
C30.2736 (2)0.5750 (4)0.3164 (4)0.1129 (15)
H3B0.31710.56840.35020.135*
C40.2464 (4)0.5902 (4)0.2414 (5)0.137 (2)
H4A0.27070.59470.22280.164*
C50.1831 (4)0.5992 (4)0.1915 (3)0.1284 (19)
H5A0.16410.61050.13860.154*
C60.1460 (2)0.5919 (3)0.2183 (2)0.0868 (10)
H6A0.10250.59700.18360.104*
C70.12490 (12)0.6964 (2)0.36669 (15)0.0547 (6)
C80.07017 (16)0.7308 (3)0.3552 (2)0.0752 (9)
H8A0.03400.68910.32690.090*
C90.0699 (2)0.8278 (4)0.3864 (3)0.1074 (14)
H9A0.03300.85130.37840.129*
C100.1221 (2)0.8895 (3)0.4283 (3)0.1118 (15)
H10A0.12110.95390.44960.134*
C110.1762 (2)0.8569 (3)0.4391 (2)0.0951 (12)
H11A0.21200.89960.46720.114*
C120.17765 (14)0.7608 (2)0.40839 (18)0.0681 (8)
H12A0.21460.73900.41580.082*
C130.14975 (10)0.41314 (16)0.43053 (13)0.0380 (5)
C140.19536 (10)0.35340 (17)0.50380 (12)0.0391 (5)
C150.25946 (11)0.36174 (19)0.55869 (14)0.0460 (5)
H15A0.28230.41530.55530.055*
C160.28879 (12)0.2881 (2)0.61895 (14)0.0513 (6)
H16A0.33210.29190.65660.062*
C170.25463 (13)0.2089 (2)0.62393 (14)0.0547 (6)
H17A0.27520.16030.66510.066*
C180.19053 (12)0.2007 (2)0.56887 (14)0.0508 (6)
H18A0.16750.14730.57210.061*
C190.16168 (11)0.27412 (18)0.50904 (13)0.0415 (5)
C200.09548 (11)0.28795 (18)0.44013 (13)0.0426 (5)
C210.05040 (12)0.0949 (2)0.15292 (17)0.0561 (7)
C220.05167 (16)0.0416 (2)0.0977 (2)0.0803 (9)
H22A0.03690.07560.05080.096*
C230.0743 (2)−0.0612 (3)0.1100 (3)0.1070 (15)
H23A0.0739−0.09610.07100.128*
C240.0965 (2)−0.1109 (4)0.1762 (4)0.136 (2)
H24A0.1124−0.18000.18420.163*
C250.0960 (2)−0.0614 (4)0.2325 (3)0.127 (2)
H25A0.1112−0.09700.27900.152*
C260.07300 (17)0.0426 (3)0.2215 (2)0.0937 (12)
H26A0.07300.07640.26060.112*
C270.05800 (14)0.2982 (2)0.09748 (17)0.0580 (7)
C280.12267 (17)0.2995 (3)0.1398 (2)0.0836 (10)
H28A0.14720.26870.18930.100*
C290.1514 (2)0.3465 (4)0.1089 (3)0.1113 (14)
H29A0.19490.34600.13740.134*
C300.1164 (3)0.3927 (4)0.0380 (3)0.1186 (17)
H30A0.13580.42420.01750.142*
C310.0531 (3)0.3935 (4)−0.0037 (3)0.1218 (16)
H31A0.02920.4266−0.05230.146*
C320.0238 (2)0.3460 (3)0.0250 (2)0.0955 (11)
H32A−0.01990.3459−0.00500.115*
U11U22U33U12U13U23
Ca10.0386 (4)0.0401 (3)0.0360 (3)0.0000.0204 (3)0.000
P10.0463 (4)0.0371 (3)0.0518 (4)−0.0034 (3)0.0263 (3)0.0065 (3)
P20.0419 (4)0.0577 (4)0.0489 (4)0.0108 (3)0.0264 (3)−0.0027 (3)
O10.0561 (11)0.0557 (11)0.0553 (10)−0.0095 (9)0.0223 (9)0.0121 (8)
O20.0436 (10)0.0838 (13)0.0508 (10)0.0106 (9)0.0235 (8)−0.0090 (9)
N10.0411 (10)0.0383 (10)0.0520 (11)−0.0033 (8)0.0259 (9)0.0042 (8)
N20.0379 (10)0.0403 (10)0.0422 (10)−0.0024 (8)0.0236 (9)0.0005 (8)
N30.0466 (12)0.0641 (13)0.0494 (12)0.0124 (10)0.0252 (10)−0.0099 (10)
C10.0760 (19)0.0373 (12)0.0700 (17)−0.0044 (12)0.0506 (15)0.0060 (12)
C20.078 (2)0.073 (2)0.107 (3)0.0026 (16)0.068 (2)0.0189 (18)
C30.115 (3)0.099 (3)0.179 (5)0.010 (2)0.117 (4)0.033 (3)
C40.209 (6)0.100 (3)0.214 (7)0.000 (4)0.188 (6)0.021 (4)
C50.230 (7)0.102 (3)0.125 (4)−0.022 (4)0.145 (5)0.002 (3)
C60.123 (3)0.073 (2)0.079 (2)−0.011 (2)0.068 (2)0.0041 (17)
C70.0567 (15)0.0437 (13)0.0543 (14)0.0071 (12)0.0276 (13)0.0102 (11)
C80.0617 (19)0.074 (2)0.083 (2)0.0110 (15)0.0385 (17)0.0006 (17)
C90.092 (3)0.108 (3)0.121 (3)0.033 (3)0.062 (3)−0.007 (3)
C100.123 (4)0.075 (2)0.100 (3)0.025 (3)0.045 (3)−0.020 (2)
C110.097 (3)0.0507 (18)0.093 (2)0.0058 (18)0.032 (2)−0.0062 (17)
C120.0599 (17)0.0423 (14)0.0785 (19)0.0003 (12)0.0277 (15)0.0001 (13)
C130.0405 (12)0.0342 (11)0.0434 (12)−0.0013 (9)0.0271 (10)−0.0025 (9)
C140.0411 (12)0.0358 (11)0.0413 (12)−0.0008 (9)0.0247 (10)−0.0031 (9)
C150.0409 (13)0.0422 (12)0.0499 (13)−0.0036 (10)0.0240 (11)−0.0022 (10)
C160.0417 (13)0.0513 (14)0.0450 (13)0.0003 (11)0.0168 (11)−0.0042 (11)
C170.0599 (16)0.0496 (14)0.0438 (13)0.0060 (12)0.0246 (13)0.0061 (11)
C180.0520 (15)0.0495 (13)0.0479 (13)−0.0043 (11)0.0277 (12)0.0077 (11)
C190.0439 (13)0.0428 (12)0.0404 (11)−0.0031 (10)0.0262 (10)−0.0004 (10)
C200.0435 (13)0.0458 (12)0.0399 (12)−0.0051 (10)0.0254 (10)0.0002 (10)
C210.0401 (14)0.0548 (15)0.0686 (17)0.0039 (11)0.0294 (13)0.0092 (13)
C220.094 (2)0.0589 (18)0.116 (3)0.0194 (17)0.078 (2)0.0013 (18)
C230.097 (3)0.062 (2)0.186 (5)0.015 (2)0.097 (3)−0.006 (3)
C240.082 (3)0.058 (2)0.201 (6)0.013 (2)0.046 (4)0.018 (3)
C250.122 (4)0.066 (3)0.110 (3)−0.002 (2)0.023 (3)0.035 (2)
C260.093 (3)0.075 (2)0.077 (2)−0.0154 (19)0.030 (2)0.0097 (18)
C270.0699 (18)0.0457 (14)0.0656 (16)0.0075 (12)0.0440 (15)−0.0001 (12)
C280.075 (2)0.091 (2)0.089 (2)−0.0115 (18)0.0504 (19)0.0041 (19)
C290.111 (3)0.110 (3)0.145 (4)−0.030 (3)0.093 (3)−0.004 (3)
C300.185 (5)0.087 (3)0.144 (4)−0.023 (3)0.130 (4)0.002 (3)
C310.161 (5)0.121 (4)0.110 (3)0.015 (3)0.095 (4)0.040 (3)
C320.103 (3)0.103 (3)0.083 (2)0.023 (2)0.056 (2)0.029 (2)
Ca1—O12.2581 (18)C10—H10A0.9300
Ca1—O1i2.2581 (18)C11—C121.376 (4)
Ca1—O22.2646 (18)C11—H11A0.9300
Ca1—O2i2.2646 (18)C12—H12A0.9300
Ca1—N2i2.5513 (18)C13—C141.486 (3)
Ca1—N22.5513 (18)C14—C191.377 (3)
Ca1—P23.4369 (8)C14—C151.377 (3)
Ca1—P2i3.4369 (8)C15—C161.381 (3)
Ca1—P13.4403 (7)C15—H15A0.9300
Ca1—P1i3.4403 (7)C16—C171.382 (4)
P1—O11.4837 (18)C16—H16A0.9300
P1—N11.6406 (19)C17—C181.378 (4)
P1—C11.794 (3)C17—H17A0.9300
P1—C71.803 (3)C18—C191.374 (3)
P2—O21.4888 (19)C18—H18A0.9300
P2—N31.631 (2)C19—C201.483 (3)
P2—C271.799 (3)C20—N3i1.302 (3)
P2—C211.808 (3)C21—C221.363 (4)
N1—C131.290 (3)C21—C261.367 (4)
N2—C201.369 (3)C22—C231.373 (5)
N2—C131.378 (3)C22—H22A0.9300
N3—C20i1.302 (3)C23—C241.313 (7)
C1—C21.369 (4)C23—H23A0.9300
C1—C61.379 (4)C24—C251.351 (8)
C2—C31.388 (5)C24—H24A0.9300
C2—H2B0.9300C25—C261.393 (6)
C3—C41.316 (8)C25—H25A0.9300
C3—H3B0.9300C26—H26A0.9300
C4—C51.354 (7)C27—C321.377 (4)
C4—H4A0.9300C27—C281.380 (4)
C5—C61.393 (6)C28—C291.390 (5)
C5—H5A0.9300C28—H28A0.9300
C6—H6A0.9300C29—C301.344 (7)
C7—C81.382 (4)C29—H29A0.9300
C7—C121.382 (4)C30—C311.350 (7)
C8—C91.381 (5)C30—H30A0.9300
C8—H8A0.9300C31—C321.366 (6)
C9—C101.353 (6)C31—H31A0.9300
C9—H9A0.9300C32—H32A0.9300
C10—C111.365 (6)
O1—Ca1—O1i81.34 (11)C4—C5—H5A119.5
O1—Ca1—O293.49 (8)C6—C5—H5A119.5
O1i—Ca1—O2157.41 (7)C1—C6—C5119.0 (4)
O1—Ca1—O2i157.41 (7)C1—C6—H6A120.5
O1i—Ca1—O2i93.49 (8)C5—C6—H6A120.5
O2—Ca1—O2i99.09 (11)C8—C7—C12118.9 (3)
O1—Ca1—N2i110.51 (6)C8—C7—P1119.1 (2)
O1i—Ca1—N2i80.81 (6)C12—C7—P1121.9 (2)
O2—Ca1—N2i80.48 (6)C9—C8—C7119.2 (3)
O2i—Ca1—N2i90.12 (6)C9—C8—H8A120.4
O1—Ca1—N280.81 (6)C7—C8—H8A120.4
O1i—Ca1—N2110.51 (6)C10—C9—C8121.5 (4)
O2—Ca1—N290.12 (6)C10—C9—H9A119.2
O2i—Ca1—N280.48 (6)C8—C9—H9A119.2
N2i—Ca1—N2165.55 (9)C9—C10—C11119.8 (4)
O1—Ca1—P297.95 (6)C9—C10—H10A120.1
O1i—Ca1—P2139.82 (5)C11—C10—H10A120.1
O2—Ca1—P218.93 (4)C10—C11—C12119.9 (4)
O2i—Ca1—P2100.02 (6)C10—C11—H11A120.0
N2i—Ca1—P261.66 (4)C12—C11—H11A120.0
N2—Ca1—P2108.97 (4)C11—C12—C7120.7 (3)
O1—Ca1—P2i139.82 (5)C11—C12—H12A119.6
O1i—Ca1—P2i97.95 (6)C7—C12—H12A119.6
O2—Ca1—P2i100.02 (6)N1—C13—N2129.4 (2)
O2i—Ca1—P2i18.93 (4)N1—C13—C14120.7 (2)
N2i—Ca1—P2i108.97 (5)N2—C13—C14109.96 (18)
N2—Ca1—P2i61.66 (4)C19—C14—C15120.9 (2)
P2—Ca1—P2i107.00 (3)C19—C14—C13106.42 (19)
O1—Ca1—P118.51 (4)C15—C14—C13132.6 (2)
O1i—Ca1—P190.49 (5)C14—C15—C16118.0 (2)
O2—Ca1—P191.20 (5)C14—C15—H15A121.0
O2i—Ca1—P1141.54 (5)C16—C15—H15A121.0
N2i—Ca1—P1128.23 (4)C15—C16—C17120.8 (2)
N2—Ca1—P162.42 (4)C15—C16—H16A119.6
P2—Ca1—P1101.274 (17)C17—C16—H16A119.6
P2i—Ca1—P1122.787 (15)C18—C17—C16121.1 (2)
O1—Ca1—P1i90.49 (5)C18—C17—H17A119.5
O1i—Ca1—P1i18.51 (4)C16—C17—H17A119.5
O2—Ca1—P1i141.54 (5)C19—C18—C17117.8 (2)
O2i—Ca1—P1i91.20 (5)C19—C18—H18A121.1
N2i—Ca1—P1i62.42 (4)C17—C18—H18A121.1
N2—Ca1—P1i128.23 (4)C18—C19—C14121.4 (2)
P2—Ca1—P1i122.787 (15)C18—C19—C20132.5 (2)
P2i—Ca1—P1i101.274 (17)C14—C19—C20106.04 (19)
P1—Ca1—P1i103.44 (3)N3i—C20—N2129.2 (2)
O1—P1—N1120.24 (10)N3i—C20—C19120.1 (2)
O1—P1—C1109.60 (13)N2—C20—C19110.65 (18)
N1—P1—C1103.94 (12)C22—C21—C26117.6 (3)
O1—P1—C7110.69 (12)C22—C21—P2121.9 (2)
N1—P1—C7104.01 (11)C26—C21—P2120.4 (3)
C1—P1—C7107.54 (12)C21—C22—C23121.3 (4)
N1—P1—Ca191.43 (7)C21—C22—H22A119.3
C1—P1—Ca1123.78 (9)C23—C22—H22A119.3
C7—P1—Ca1120.67 (9)C24—C23—C22120.9 (5)
O2—P2—N3119.32 (10)C24—C23—H23A119.5
O2—P2—C27112.18 (13)C22—C23—H23A119.5
N3—P2—C27105.94 (13)C23—C24—C25119.8 (4)
O2—P2—C21108.99 (13)C23—C24—H24A120.1
N3—P2—C21104.66 (12)C25—C24—H24A120.1
C27—P2—C21104.56 (12)C24—C25—C26120.5 (4)
N3—P2—Ca191.97 (7)C24—C25—H25A119.7
C27—P2—Ca1114.13 (9)C26—C25—H25A119.7
C21—P2—Ca1131.54 (10)C21—C26—C25119.7 (4)
P1—O1—Ca1132.60 (10)C21—C26—H26A120.1
P2—O2—Ca1131.50 (10)C25—C26—H26A120.1
C13—N1—P1128.67 (17)C32—C27—C28117.7 (3)
C20—N2—C13106.88 (18)C32—C27—P2124.0 (3)
C20—N2—Ca1125.26 (14)C28—C27—P2118.3 (2)
C13—N2—Ca1124.95 (14)C27—C28—C29120.3 (4)
C20i—N3—P2127.09 (18)C27—C28—H28A119.9
C2—C1—C6119.0 (3)C29—C28—H28A119.9
C2—C1—P1122.6 (2)C30—C29—C28120.3 (4)
C6—C1—P1118.4 (3)C30—C29—H29A119.9
C1—C2—C3119.6 (4)C28—C29—H29A119.9
C1—C2—H2B120.2C29—C30—C31120.1 (4)
C3—C2—H2B120.2C29—C30—H30A120.0
C4—C3—C2121.7 (5)C31—C30—H30A120.0
C4—C3—H3B119.1C30—C31—C32120.7 (4)
C2—C3—H3B119.1C30—C31—H31A119.7
C3—C4—C5119.8 (4)C32—C31—H31A119.7
C3—C4—H4A120.1C31—C32—C27121.0 (4)
C5—C4—H4A120.1C31—C32—H32A119.5
C4—C5—C6120.9 (5)C27—C32—H32A119.5
Ca1—O12.2581 (18)
Ca1—O22.2646 (18)
Ca1—N22.5513 (18)
O1—Ca1—O1i81.34 (11)
O1—Ca1—O293.49 (8)
O1—Ca1—O2i157.41 (7)
O2—Ca1—O2i99.09 (11)
O1—Ca1—N2i110.51 (6)
O2—Ca1—N2i80.48 (6)
O1—Ca1—N280.81 (6)
O2—Ca1—N290.12 (6)
N2i—Ca1—N2165.55 (9)

Symmetry code: (i) .

  1 in total

1.  Synthesis and structural characterisation of heavy alkaline earth N,N'-bis(aryl)formamidinate complexes.

Authors:  Marcus L Cole; Glen B Deacon; Craig M Forsyth; Kristina Konstas; Peter C Junk
Journal:  Dalton Trans       Date:  2006-04-27       Impact factor: 4.390

  1 in total

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