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Acta Crystallographica Section E: Structure Reports Online logoLink to Acta Crystallographica Section E: Structure Reports Online
. 2007 Dec 12;64(Pt 1):m158. doi: 10.1107/S1600536807064239

(Triphenyl­phosphine-κP)[tris­(indazol-1-yl)borato-κ3 N,N′,N′′]silver(I)

Moayad Hossaini Sadr a, Shiva Alipouri Niaz a, Saina Gorbani a, Shan Gao b, Seik Weng Ng c,*
PMCID: PMC2915096  PMID: 21200508

Abstract

The phosphine-coordinated AgI atom in the title compound, [Ag(C21H17BN6)(C18H15P)], is also N,N′,N′′-chelated by the tris­(indazol­yl)borate anion. The resultant N3P coordination geometry is tetra­hedral.

Related literature

For related literature; see Janiak et al. (2000).graphic file with name e-64-0m158-scheme1.jpg

Experimental

Crystal data

  • [Ag(C21H17BN6)(C18H15P)]

  • M r = 734.36

  • Triclinic, Inline graphic

  • a = 10.2950 (6) Å

  • b = 12.6644 (6) Å

  • c = 13.9555 (7) Å

  • α = 87.003 (1)°

  • β = 77.966 (2)°

  • γ = 79.903 (1)°

  • V = 1751.7 (2) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 0.66 mm−1

  • T = 295 (2) K

  • 0.31 × 0.28 × 0.15 mm

Data collection

  • Rigaku R-AXIS RAPID IP diffractometer

  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995) T min = 0.551, T max = 0.908

  • 17380 measured reflections

  • 7925 independent reflections

  • 4255 reflections with I > 2σ(I)

  • R int = 0.038

Refinement

  • R[F 2 > 2σ(F 2)] = 0.044

  • wR(F 2) = 0.159

  • S = 1.08

  • 7925 reflections

  • 433 parameters

  • H-atom parameters constrained

  • Δρmax = 0.87 e Å−3

  • Δρmin = −0.95 e Å−3

Data collection: RAPID-AUTO (Rigaku Corporation, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536807064239/tk2225sup1.cif

e-64-0m158-sup1.cif (29KB, cif)

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807064239/tk2225Isup2.hkl

e-64-0m158-Isup2.hkl (387.7KB, hkl)

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

We thank the Research Office of Azarbaijan University of Tarbiat Moallem, the Heilongjiang Province Natural Science Foundation (No. B200501), the Scientific Fund for Remarkable Teachers of Heilongjiang Province (No. 1054 G036) and the University of Malaya for supporting this study.

supplementary crystallographic information

Comment

Hydrotris(indazolyl)borate, Tp4Bo, is suggested to be a suitable tripodal ligand for supramolecular assembly (Janiak et al., 2000). In the title silver derivative, Ag(C21H17N6B)(C18H15P), the Tp4Bo anion functions as a tridentate ligand (Fig. 1). The triphenylphosphine ligand completes the N3P coordination geometry for Ag. The Ag center is tetrahedrally coordinated, but the N–Ag–N angles are significantly less than 90°, i.e. range from 82.3 (1) to 83.8 (2)°.

Experimental

Under a dry nitrogen atmosphere, K[HB(Indazolyl)3] (0.2 g, 1 mmol) was added to a mixture of AgNO3 (0.17 g, 1 mmol) and PPh3 (0.26 g, 2 mmol) in methanol (40 ml). After being stirred for 3 h, the colorless solution was filtered. Crystals were obtained from the filtrate after a week.

Refinement

The H atoms were included in the refinement in the riding model approximation with = C–H 0.93, and with U(H) = 1.2Ueq(C).

Figures

Fig. 1.

Fig. 1.

The molecular structure of (I) showing atom numbering scheme, displacement ellipsoids at the 50% probability level and H atoms as spheres of arbitrary radii.

Crystal data

[Ag(C21H17BN6)(C18H15P)] Z = 2
Mr = 734.36 F(000) = 750
Triclinic, P1 Dx = 1.392 Mg m3
Hall symbol: -P 1 Mo Kα radiation, λ = 0.71073 Å
a = 10.2950 (6) Å Cell parameters from 10642 reflections
b = 12.6644 (6) Å θ = 3.0–27.5°
c = 13.9555 (7) Å µ = 0.66 mm1
α = 87.003 (1)° T = 295 K
β = 77.966 (2)° Block, colorless
γ = 79.903 (1)° 0.31 × 0.28 × 0.15 mm
V = 1751.7 (2) Å3

Data collection

Rigaku R-AXIS RAPID IP diffractometer 7925 independent reflections
Radiation source: fine-focus sealed tube 4255 reflections with I > 2σ(I)
graphite Rint = 0.038
ω scans θmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) h = −13→13
Tmin = 0.551, Tmax = 0.908 k = −16→14
17380 measured reflections l = −18→17

Refinement

Refinement on F2 Primary atom site location: structure-invariant direct methods
Least-squares matrix: full Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.044 Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.159 H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.0652P)2 + 1.2113P] where P = (Fo2 + 2Fc2)/3
7925 reflections (Δ/σ)max = 0.001
433 parameters Δρmax = 0.87 e Å3
0 restraints Δρmin = −0.95 e Å3

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

x y z Uiso*/Ueq
Ag1 0.46371 (4) 0.69276 (3) 0.81804 (3) 0.06680 (17)
P1 0.28241 (12) 0.80700 (9) 0.90871 (9) 0.0525 (3)
N1 0.5981 (4) 0.7791 (3) 0.6910 (3) 0.0682 (11)
N2 0.7025 (4) 0.7136 (3) 0.6353 (3) 0.0587 (9)
N3 0.4898 (4) 0.5627 (3) 0.7017 (3) 0.0660 (11)
N4 0.6162 (4) 0.5350 (3) 0.6461 (3) 0.0610 (10)
N5 0.6709 (4) 0.5973 (3) 0.8415 (3) 0.0637 (10)
N6 0.7627 (4) 0.5686 (3) 0.7583 (3) 0.0590 (9)
C1 0.6028 (6) 0.8787 (4) 0.6578 (4) 0.0772 (15)
H1 0.5422 0.9386 0.6837 0.093*
C2 0.7101 (6) 0.8818 (4) 0.5794 (4) 0.0704 (14)
C3 0.7642 (8) 0.9632 (6) 0.5185 (5) 0.105 (2)
H3 0.7241 1.0349 0.5260 0.126*
C4 0.8754 (10) 0.9333 (8) 0.4497 (6) 0.132 (3)
H4 0.9140 0.9858 0.4102 0.158*
C5 0.9350 (8) 0.8255 (8) 0.4357 (6) 0.125 (3)
H5 1.0101 0.8080 0.3856 0.150*
C6 0.8851 (6) 0.7453 (6) 0.4941 (4) 0.0890 (17)
H6 0.9253 0.6739 0.4849 0.107*
C7 0.7729 (5) 0.7747 (4) 0.5670 (4) 0.0638 (12)
C8 0.4152 (6) 0.4946 (4) 0.6823 (4) 0.0736 (14)
H8 0.3245 0.4971 0.7101 0.088*
C9 0.4908 (6) 0.4181 (4) 0.6143 (4) 0.0672 (13)
C10 0.4641 (8) 0.3292 (5) 0.5697 (5) 0.0900 (19)
H10 0.3785 0.3108 0.5828 0.108*
C11 0.5667 (10) 0.2717 (5) 0.5075 (5) 0.104 (2)
H11 0.5511 0.2126 0.4774 0.125*
C12 0.6947 (9) 0.2981 (5) 0.4871 (4) 0.100 (2)
H12 0.7627 0.2556 0.4442 0.120*
C13 0.7254 (7) 0.3861 (4) 0.5285 (4) 0.0816 (17)
H13 0.7589 0.4337 0.4760 0.098*
H13B 0.7977 0.3609 0.5632 0.098*
C14 0.6182 (6) 0.4457 (4) 0.5935 (3) 0.0615 (12)
C15 0.7202 (6) 0.5533 (4) 0.9166 (4) 0.0696 (13)
H15 0.6759 0.5614 0.9817 0.083*
C16 0.8488 (5) 0.4923 (4) 0.8855 (4) 0.0686 (13)
C17 0.9442 (6) 0.4265 (4) 0.9313 (5) 0.0844 (17)
H17 0.9291 0.4168 0.9990 0.101*
C18 1.0592 (7) 0.3777 (5) 0.8726 (7) 0.101 (2)
H18 1.1232 0.3333 0.9011 0.121*
C19 1.0845 (6) 0.3920 (5) 0.7716 (6) 0.096 (2)
H19 1.1655 0.3584 0.7344 0.115*
C20 0.9923 (5) 0.4547 (4) 0.7253 (5) 0.0768 (15)
H20 1.0093 0.4637 0.6575 0.092*
C21 0.8725 (5) 0.5043 (3) 0.7836 (4) 0.0619 (12)
C22 0.1187 (5) 0.7991 (3) 0.8834 (3) 0.0576 (11)
C23 0.1166 (6) 0.7634 (5) 0.7923 (4) 0.0804 (15)
H23 0.1973 0.7414 0.7486 0.096*
C24 −0.0051 (7) 0.7600 (6) 0.7647 (5) 0.099 (2)
H24 −0.0047 0.7364 0.7027 0.119*
C25 −0.1241 (7) 0.7907 (5) 0.8274 (5) 0.0873 (17)
H25 −0.2053 0.7902 0.8083 0.105*
C26 −0.1224 (5) 0.8227 (5) 0.9196 (5) 0.0811 (16)
H26 −0.2033 0.8413 0.9640 0.097*
C27 −0.0024 (5) 0.8276 (4) 0.9475 (4) 0.0654 (12)
H27 −0.0034 0.8504 1.0100 0.079*
C28 0.3049 (4) 0.9449 (3) 0.8736 (3) 0.0495 (10)
C29 0.2260 (6) 1.0098 (4) 0.8192 (4) 0.0774 (15)
H29 0.1512 0.9871 0.8048 0.093*
C30 0.2568 (7) 1.1094 (4) 0.7852 (5) 0.094 (2)
H30 0.2043 1.1516 0.7461 0.113*
C31 0.3624 (7) 1.1457 (4) 0.8083 (5) 0.0825 (16)
H31 0.3813 1.2130 0.7865 0.099*
C32 0.4409 (6) 1.0826 (4) 0.8639 (4) 0.0731 (14)
H32 0.5135 1.1071 0.8801 0.088*
C33 0.4127 (5) 0.9823 (4) 0.8963 (4) 0.0626 (12)
H33 0.4670 0.9396 0.9338 0.075*
C34 0.2676 (5) 0.8030 (4) 1.0407 (3) 0.0563 (11)
C35 0.3329 (5) 0.7129 (4) 1.0828 (4) 0.0667 (13)
H35 0.3793 0.6558 1.0435 0.080*
C36 0.3300 (7) 0.7069 (5) 1.1818 (5) 0.0879 (18)
H36 0.3739 0.6458 1.2090 0.105*
C37 0.2629 (7) 0.7904 (6) 1.2403 (4) 0.093 (2)
H37 0.2615 0.7861 1.3072 0.111*
C38 0.1973 (6) 0.8808 (6) 1.2007 (4) 0.0872 (17)
H38 0.1517 0.9376 1.2408 0.105*
C39 0.1992 (5) 0.8872 (4) 1.1014 (4) 0.0692 (13)
H39 0.1545 0.9484 1.0749 0.083*
B1 0.7306 (5) 0.5929 (4) 0.6564 (4) 0.0608 (14)
H1B 0.8105 0.5624 0.6084 0.073*

Atomic displacement parameters (Å2)

U11 U22 U33 U12 U13 U23
Ag1 0.0566 (2) 0.0586 (2) 0.0756 (3) −0.00108 (16) 0.00227 (18) −0.00611 (17)
P1 0.0478 (7) 0.0523 (6) 0.0537 (7) −0.0065 (5) −0.0036 (5) −0.0012 (5)
N1 0.068 (3) 0.059 (2) 0.066 (3) −0.0076 (19) 0.008 (2) −0.0010 (19)
N2 0.054 (2) 0.064 (2) 0.055 (2) −0.0135 (18) −0.0013 (18) −0.0005 (18)
N3 0.060 (3) 0.060 (2) 0.079 (3) −0.0117 (19) −0.013 (2) −0.010 (2)
N4 0.061 (3) 0.059 (2) 0.062 (2) −0.0072 (18) −0.013 (2) −0.0086 (19)
N5 0.056 (2) 0.066 (2) 0.064 (2) 0.0058 (18) −0.014 (2) −0.0028 (19)
N6 0.045 (2) 0.065 (2) 0.064 (2) −0.0014 (17) −0.0100 (19) −0.0067 (18)
C1 0.089 (4) 0.055 (3) 0.079 (4) −0.007 (3) −0.001 (3) −0.001 (3)
C2 0.075 (4) 0.076 (3) 0.059 (3) −0.024 (3) −0.003 (3) 0.004 (2)
C3 0.130 (6) 0.096 (5) 0.083 (4) −0.035 (4) 0.003 (4) 0.012 (4)
C4 0.143 (8) 0.134 (7) 0.112 (6) −0.054 (6) 0.008 (6) 0.034 (5)
C5 0.104 (6) 0.160 (8) 0.093 (5) −0.036 (5) 0.029 (4) 0.018 (5)
C6 0.075 (4) 0.107 (4) 0.075 (4) −0.016 (3) 0.007 (3) −0.003 (3)
C7 0.057 (3) 0.078 (3) 0.058 (3) −0.016 (2) −0.009 (2) −0.006 (2)
C8 0.065 (3) 0.069 (3) 0.091 (4) −0.014 (3) −0.025 (3) 0.003 (3)
C9 0.083 (4) 0.063 (3) 0.066 (3) −0.017 (3) −0.037 (3) 0.004 (2)
C10 0.125 (6) 0.076 (4) 0.085 (4) −0.027 (4) −0.052 (4) 0.002 (3)
C11 0.165 (8) 0.081 (4) 0.085 (5) −0.029 (5) −0.058 (5) −0.008 (4)
C12 0.153 (7) 0.083 (4) 0.060 (4) 0.002 (4) −0.027 (4) −0.021 (3)
C13 0.117 (5) 0.078 (3) 0.046 (3) 0.001 (3) −0.023 (3) −0.001 (3)
C14 0.080 (4) 0.057 (3) 0.050 (3) −0.004 (2) −0.026 (3) 0.000 (2)
C15 0.073 (4) 0.064 (3) 0.072 (3) −0.009 (3) −0.019 (3) −0.004 (2)
C16 0.069 (3) 0.051 (3) 0.092 (4) −0.014 (2) −0.027 (3) 0.003 (3)
C17 0.087 (4) 0.066 (3) 0.109 (5) −0.015 (3) −0.041 (4) 0.013 (3)
C18 0.074 (4) 0.077 (4) 0.153 (7) −0.003 (3) −0.039 (5) 0.017 (4)
C19 0.061 (4) 0.070 (4) 0.147 (7) 0.003 (3) −0.011 (4) 0.004 (4)
C20 0.058 (3) 0.067 (3) 0.102 (4) −0.004 (2) −0.011 (3) −0.005 (3)
C21 0.051 (3) 0.049 (2) 0.088 (4) −0.011 (2) −0.016 (3) −0.004 (2)
C22 0.070 (3) 0.051 (2) 0.052 (3) −0.016 (2) −0.008 (2) 0.000 (2)
C23 0.073 (4) 0.103 (4) 0.069 (4) −0.024 (3) −0.011 (3) −0.018 (3)
C24 0.100 (5) 0.127 (5) 0.085 (4) −0.036 (4) −0.035 (4) −0.024 (4)
C25 0.084 (4) 0.085 (4) 0.107 (5) −0.028 (3) −0.038 (4) −0.005 (4)
C26 0.045 (3) 0.088 (4) 0.110 (5) −0.019 (3) −0.006 (3) −0.006 (3)
C27 0.055 (3) 0.074 (3) 0.067 (3) −0.012 (2) −0.008 (2) −0.010 (2)
C28 0.044 (2) 0.057 (2) 0.046 (2) −0.0053 (18) −0.0074 (19) −0.0032 (18)
C29 0.079 (4) 0.065 (3) 0.098 (4) −0.014 (3) −0.041 (3) 0.009 (3)
C30 0.104 (5) 0.062 (3) 0.132 (6) −0.022 (3) −0.060 (4) 0.026 (3)
C31 0.098 (4) 0.058 (3) 0.095 (4) −0.022 (3) −0.025 (4) 0.019 (3)
C32 0.074 (4) 0.074 (3) 0.075 (3) −0.032 (3) −0.008 (3) 0.002 (3)
C33 0.057 (3) 0.073 (3) 0.059 (3) −0.018 (2) −0.012 (2) 0.005 (2)
C34 0.051 (3) 0.062 (3) 0.056 (3) −0.014 (2) −0.008 (2) 0.004 (2)
C35 0.070 (3) 0.060 (3) 0.075 (3) −0.019 (2) −0.021 (3) 0.014 (2)
C36 0.099 (5) 0.096 (4) 0.081 (4) −0.040 (4) −0.036 (4) 0.032 (4)
C37 0.096 (5) 0.136 (6) 0.057 (3) −0.055 (4) −0.019 (3) 0.022 (4)
C38 0.077 (4) 0.125 (5) 0.057 (3) −0.023 (4) 0.000 (3) −0.006 (3)
C39 0.064 (3) 0.081 (3) 0.060 (3) −0.011 (3) −0.009 (3) 0.003 (3)
B1 0.041 (3) 0.071 (3) 0.068 (4) −0.003 (2) −0.006 (3) −0.014 (3)

Geometric parameters (Å, °)

Ag1—N1 2.358 (4) C15—H15 0.9300
Ag1—N3 2.316 (4) C16—C21 1.397 (7)
Ag1—N5 2.337 (4) C16—C17 1.410 (7)
Ag1—P1 2.332 (1) C17—C18 1.359 (9)
P1—C22 1.814 (5) C17—H17 0.9300
P1—C34 1.814 (5) C18—C19 1.387 (10)
P1—C28 1.830 (4) C18—H18 0.9300
N1—C1 1.326 (6) C19—C20 1.373 (8)
N1—N2 1.361 (5) C19—H19 0.9300
N2—C7 1.365 (6) C20—C21 1.394 (7)
N2—B1 1.529 (7) C20—H20 0.9300
N3—C8 1.322 (6) C22—C27 1.377 (7)
N3—N4 1.366 (5) C22—C23 1.377 (7)
N4—C14 1.375 (6) C23—C24 1.393 (8)
N4—B1 1.526 (7) C23—H23 0.9300
N5—C15 1.316 (6) C24—C25 1.356 (9)
N5—N6 1.356 (5) C24—H24 0.9300
N6—C21 1.370 (6) C25—C26 1.373 (8)
N6—B1 1.531 (7) C25—H25 0.9300
C1—C2 1.388 (7) C26—C27 1.383 (7)
C1—H1 0.9300 C26—H26 0.9300
C2—C7 1.400 (7) C27—H27 0.9300
C2—C3 1.416 (8) C28—C29 1.368 (6)
C3—C4 1.343 (11) C28—C33 1.379 (6)
C3—H3 0.9300 C29—C30 1.390 (7)
C4—C5 1.401 (11) C29—H29 0.9300
C4—H4 0.9300 C30—C31 1.354 (8)
C5—C6 1.372 (9) C30—H30 0.9300
C5—H5 0.9300 C31—C32 1.365 (8)
C6—C7 1.382 (7) C31—H31 0.9300
C6—H6 0.9300 C32—C33 1.385 (7)
C8—C9 1.403 (7) C32—H32 0.9300
C8—H8 0.9300 C33—H33 0.9300
C9—C14 1.386 (7) C34—C39 1.391 (7)
C9—C10 1.408 (7) C34—C35 1.387 (6)
C10—C11 1.347 (10) C35—C36 1.374 (8)
C10—H10 0.9300 C35—H35 0.9300
C11—C12 1.385 (10) C36—C37 1.364 (9)
C11—H11 0.9300 C36—H36 0.9300
C12—C13 1.394 (8) C37—C38 1.376 (9)
C12—H12 0.9300 C37—H37 0.9300
C13—C14 1.404 (7) C38—C39 1.380 (7)
C13—H13 0.9700 C38—H38 0.9300
C13—H13B 0.9700 C39—H39 0.9300
C15—C16 1.405 (7) B1—H1B 0.9800
N1—Ag1—N3 83.8 (2) C21—C16—C15 103.7 (4)
N1—Ag1—N5 83.7 (2) C21—C16—C17 120.4 (5)
N1—Ag1—P1 114.3 (1) C15—C16—C17 135.8 (6)
N3—Ag1—N5 82.3 (1) C18—C17—C16 117.3 (6)
N3—Ag1—P1 135.6 (1) C18—C17—H17 121.3
N5—Ag1—P1 137.2 (1) C16—C17—H17 121.3
C22—P1—C34 108.0 (2) C17—C18—C19 122.3 (6)
C22—P1—C28 103.7 (2) C17—C18—H18 118.9
C34—P1—C28 104.0 (2) C19—C18—H18 118.9
C22—P1—Ag1 115.48 (15) C20—C19—C18 121.4 (6)
C34—P1—Ag1 116.65 (15) C20—C19—H19 119.3
C28—P1—Ag1 107.61 (14) C18—C19—H19 119.3
C1—N1—N2 107.6 (4) C19—C20—C21 117.5 (6)
C1—N1—Ag1 137.0 (3) C19—C20—H20 121.2
N2—N1—Ag1 115.3 (3) C21—C20—H20 121.2
N1—N2—C7 108.7 (4) N6—C21—C20 130.5 (5)
N1—N2—B1 121.5 (4) N6—C21—C16 108.5 (4)
C7—N2—B1 129.7 (4) C20—C21—C16 121.0 (5)
C8—N3—N4 107.6 (4) C27—C22—C23 118.2 (5)
C8—N3—Ag1 135.3 (4) C27—C22—P1 124.9 (4)
N4—N3—Ag1 116.4 (3) C23—C22—P1 116.9 (4)
N3—N4—C14 108.3 (4) C22—C23—C24 120.7 (6)
N3—N4—B1 121.1 (4) C22—C23—H23 119.6
C14—N4—B1 130.3 (4) C24—C23—H23 119.6
C15—N5—N6 108.3 (4) C25—C24—C23 120.8 (6)
C15—N5—Ag1 136.0 (4) C25—C24—H24 119.6
N6—N5—Ag1 115.3 (3) C23—C24—H24 119.6
N5—N6—C21 108.4 (4) C24—C25—C26 118.7 (6)
N5—N6—B1 122.2 (4) C24—C25—H25 120.7
C21—N6—B1 128.7 (4) C26—C25—H25 120.7
N1—C1—C2 111.2 (5) C27—C26—C25 121.2 (6)
N1—C1—H1 124.4 C27—C26—H26 119.4
C2—C1—H1 124.4 C25—C26—H26 119.4
C1—C2—C7 104.3 (4) C22—C27—C26 120.4 (5)
C1—C2—C3 135.7 (6) C22—C27—H27 119.8
C7—C2—C3 120.0 (6) C26—C27—H27 119.8
C4—C3—C2 117.7 (7) C29—C28—C33 118.3 (4)
C4—C3—H3 121.2 C29—C28—P1 122.9 (4)
C2—C3—H3 121.2 C33—C28—P1 118.6 (3)
C3—C4—C5 121.9 (7) C28—C29—C30 120.5 (5)
C3—C4—H4 119.0 C28—C29—H29 119.7
C5—C4—H4 119.0 C30—C29—H29 119.7
C6—C5—C4 121.5 (7) C31—C30—C29 120.7 (5)
C6—C5—H5 119.3 C31—C30—H30 119.7
C4—C5—H5 119.3 C29—C30—H30 119.7
C5—C6—C7 117.5 (6) C30—C31—C32 119.5 (5)
C5—C6—H6 121.3 C30—C31—H31 120.2
C7—C6—H6 121.3 C32—C31—H31 120.2
N2—C7—C6 130.4 (5) C31—C32—C33 120.1 (5)
N2—C7—C2 108.2 (4) C31—C32—H32 119.9
C6—C7—C2 121.4 (5) C33—C32—H32 119.9
N3—C8—C9 111.3 (5) C28—C33—C32 120.8 (5)
N3—C8—H8 124.4 C28—C33—H33 119.6
C9—C8—H8 124.4 C32—C33—H33 119.6
C14—C9—C8 104.1 (4) C39—C34—C35 118.1 (5)
C14—C9—C10 120.7 (6) C39—C34—P1 123.5 (4)
C8—C9—C10 135.2 (6) C35—C34—P1 118.3 (4)
C11—C10—C9 117.8 (7) C36—C35—C34 121.0 (5)
C11—C10—H10 121.1 C36—C35—H35 119.5
C9—C10—H10 121.1 C34—C35—H35 119.5
C10—C11—C12 121.8 (6) C37—C36—C35 120.1 (6)
C10—C11—H11 119.1 C37—C36—H36 119.9
C12—C11—H11 119.1 C35—C36—H36 119.9
C11—C12—C13 122.4 (6) C36—C37—C38 120.3 (6)
C11—C12—H12 118.8 C36—C37—H37 119.9
C13—C12—H12 118.8 C38—C37—H37 119.9
C12—C13—C14 115.6 (6) C39—C38—C37 119.9 (6)
C12—C13—H13 108.4 C39—C38—H38 120.0
C14—C13—H13 108.4 C37—C38—H38 120.0
C12—C13—H13B 108.4 C38—C39—C34 120.5 (5)
C14—C13—H13B 108.4 C38—C39—H39 119.7
H13—C13—H13B 107.4 C34—C39—H39 119.7
N4—C14—C9 108.8 (4) N4—B1—N2 113.6 (4)
N4—C14—C13 129.6 (5) N4—B1—N6 108.9 (4)
C9—C14—C13 121.7 (5) N2—B1—N6 111.7 (4)
N5—C15—C16 111.0 (5) N4—B1—H1B 107.4
N5—C15—H15 124.5 N2—B1—H1B 107.4
C16—C15—H15 124.5 N6—B1—H1B 107.4
N3—Ag1—P1—C22 −2.1 (2) C12—C13—C14—N4 179.4 (5)
N5—Ag1—P1—C22 −147.2 (2) C12—C13—C14—C9 −0.2 (7)
N1—Ag1—P1—C22 104.8 (2) N6—N5—C15—C16 −0.2 (6)
N3—Ag1—P1—C34 126.3 (2) Ag1—N5—C15—C16 171.9 (3)
N5—Ag1—P1—C34 −18.7 (2) N5—C15—C16—C21 0.2 (6)
N1—Ag1—P1—C34 −126.8 (2) N5—C15—C16—C17 −177.2 (6)
N3—Ag1—P1—C28 −117.4 (2) C21—C16—C17—C18 1.1 (8)
N5—Ag1—P1—C28 97.6 (2) C15—C16—C17—C18 178.1 (6)
N1—Ag1—P1—C28 −10.5 (2) C16—C17—C18—C19 0.7 (10)
N3—Ag1—N1—C1 141.2 (6) C17—C18—C19—C20 −1.5 (11)
P1—Ag1—N1—C1 3.5 (6) C18—C19—C20—C21 0.5 (9)
N5—Ag1—N1—C1 −136.0 (6) N5—N6—C21—C20 179.9 (5)
N3—Ag1—N1—N2 −40.6 (3) B1—N6—C21—C20 9.3 (8)
P1—Ag1—N1—N2 −178.3 (3) N5—N6—C21—C16 0.1 (5)
N5—Ag1—N1—N2 42.2 (3) B1—N6—C21—C16 −170.5 (5)
C1—N1—N2—C7 0.4 (6) C19—C20—C21—N6 −178.5 (5)
Ag1—N1—N2—C7 −178.4 (3) C19—C20—C21—C16 1.3 (8)
C1—N1—N2—B1 177.5 (5) C15—C16—C21—N6 −0.1 (5)
Ag1—N1—N2—B1 −1.2 (5) C17—C16—C21—N6 177.7 (4)
P1—Ag1—N3—C8 −29.4 (6) C15—C16—C21—C20 180.0 (5)
N5—Ag1—N3—C8 127.4 (5) C17—C16—C21—C20 −2.1 (7)
N1—Ag1—N3—C8 −148.1 (5) C34—P1—C22—C27 23.4 (5)
P1—Ag1—N3—N4 161.9 (2) C28—P1—C22—C27 −86.5 (4)
N5—Ag1—N3—N4 −41.2 (3) Ag1—P1—C22—C27 156.0 (4)
N1—Ag1—N3—N4 43.3 (3) C34—P1—C22—C23 −157.7 (4)
C8—N3—N4—C14 −1.6 (5) C28—P1—C22—C23 92.4 (4)
Ag1—N3—N4—C14 170.0 (3) Ag1—P1—C22—C23 −25.1 (4)
C8—N3—N4—B1 −175.6 (4) C27—C22—C23—C24 2.3 (8)
Ag1—N3—N4—B1 −3.9 (5) P1—C22—C23—C24 −176.7 (5)
N3—Ag1—N5—C15 −127.3 (5) C22—C23—C24—C25 −0.7 (10)
P1—Ag1—N5—C15 28.9 (6) C23—C24—C25—C26 −1.7 (10)
N1—Ag1—N5—C15 148.2 (5) C24—C25—C26—C27 2.5 (9)
N3—Ag1—N5—N6 44.4 (3) C23—C22—C27—C26 −1.5 (7)
P1—Ag1—N5—N6 −159.5 (2) P1—C22—C27—C26 177.4 (4)
N1—Ag1—N5—N6 −40.2 (3) C25—C26—C27—C22 −0.9 (8)
C15—N5—N6—C21 0.1 (5) C22—P1—C28—C29 −14.0 (5)
Ag1—N5—N6—C21 −173.8 (3) C34—P1—C28—C29 −126.8 (4)
C15—N5—N6—B1 171.4 (4) Ag1—P1—C28—C29 108.8 (4)
Ag1—N5—N6—B1 −2.5 (5) C22—P1—C28—C33 171.2 (4)
N2—N1—C1—C2 0.1 (7) C34—P1—C28—C33 58.4 (4)
Ag1—N1—C1—C2 178.4 (4) Ag1—P1—C28—C33 −65.9 (4)
N1—C1—C2—C7 −0.4 (7) C33—C28—C29—C30 2.1 (8)
N1—C1—C2—C3 −178.4 (7) P1—C28—C29—C30 −172.7 (5)
C1—C2—C3—C4 178.1 (8) C28—C29—C30—C31 −2.5 (10)
C7—C2—C3—C4 0.4 (10) C29—C30—C31—C32 1.4 (10)
C2—C3—C4—C5 1.8 (14) C30—C31—C32—C33 0.1 (9)
C3—C4—C5—C6 −2.3 (15) C29—C28—C33—C32 −0.7 (7)
C4—C5—C6—C7 0.5 (12) P1—C28—C33—C32 174.4 (4)
N1—N2—C7—C6 −179.3 (6) C31—C32—C33—C28 −0.4 (8)
B1—N2—C7—C6 3.8 (9) C22—P1—C34—C39 −71.4 (5)
N1—N2—C7—C2 −0.6 (6) C28—P1—C34—C39 38.3 (5)
B1—N2—C7—C2 −177.5 (5) Ag1—P1—C34—C39 156.6 (4)
C5—C6—C7—N2 −179.8 (6) C22—P1—C34—C35 111.5 (4)
C5—C6—C7—C2 1.7 (9) C28—P1—C34—C35 −138.7 (4)
C1—C2—C7—N2 0.6 (6) Ag1—P1—C34—C35 −20.5 (4)
C3—C2—C7—N2 179.0 (5) C39—C34—C35—C36 0.1 (8)
C1—C2—C7—C6 179.4 (5) P1—C34—C35—C36 177.3 (4)
C3—C2—C7—C6 −2.2 (9) C34—C35—C36—C37 −0.3 (9)
N4—N3—C8—C9 1.1 (6) C35—C36—C37—C38 0.2 (10)
Ag1—N3—C8—C9 −168.2 (3) C36—C37—C38—C39 0.1 (10)
N3—C8—C9—C14 −0.2 (6) C37—C38—C39—C34 −0.3 (9)
N3—C8—C9—C10 179.2 (6) C35—C34—C39—C38 0.2 (8)
C14—C9—C10—C11 0.8 (8) P1—C34—C39—C38 −176.9 (4)
C8—C9—C10—C11 −178.6 (6) N3—N4—B1—N2 −59.2 (6)
C9—C10—C11—C12 −0.1 (9) C14—N4—B1—N2 128.3 (5)
C10—C11—C12—C13 −0.7 (10) N3—N4—B1—N6 66.0 (5)
C11—C12—C13—C14 0.8 (9) C14—N4—B1—N6 −106.5 (5)
N3—N4—C14—C9 1.5 (5) N1—N2—B1—N4 62.3 (6)
B1—N4—C14—C9 174.7 (5) C7—N2—B1—N4 −121.2 (5)
N3—N4—C14—C13 −178.2 (5) N1—N2—B1—N6 −61.5 (6)
B1—N4—C14—C13 −5.0 (8) C7—N2—B1—N6 115.1 (5)
C8—C9—C14—N4 −0.8 (5) N5—N6—B1—N4 −61.8 (5)
C10—C9—C14—N4 179.7 (4) C21—N6—B1—N4 107.6 (5)
C8—C9—C14—C13 178.9 (4) N5—N6—B1—N2 64.5 (6)
C10—C9—C14—C13 −0.6 (7) C21—N6—B1—N2 −126.1 (5)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK2225).

References

  1. Barbour, L. J. (2001). J. Supramol. Chem.1, 189–191.
  2. Higashi, T. (1995). ABSCOR Rigaku Corporation, Tokyo, Japan.
  3. Janiak, C., Temizdemir, S. & Dechert, S. (2000). Inorg. Chem. Commun.3, 271–275.
  4. Rigaku Corporation (1998). RAPID-AUTO Rigaku Corporation, Tokyo, Japan.
  5. Rigaku/MSC (2002). CrystalStructure Rigaku/MSC Inc. The Woodlands, Texas, USA.
  6. Sheldrick, G. M. (1997). SHELXS97 and SHELXL97 University of Göttingen, Germany.
  7. Westrip, S. P. (2007). publCIF In preparation.

Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536807064239/tk2225sup1.cif

e-64-0m158-sup1.cif (29KB, cif)

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807064239/tk2225Isup2.hkl

e-64-0m158-Isup2.hkl (387.7KB, hkl)

Additional supplementary materials: crystallographic information; 3D view; checkCIF report


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