Literature DB >> 21200600

Bis[μ-methyl-enebis(diphenyl-phosphine)]bis-[(5-nitro-1,10-phenanthroline)silver(I)] bis-(hexa-fluoridoanti-monate).

Gangqiang Yin1.   

Abstract

In the title compound, [Ag(2)(C(12)H(7)N(3)O(2))(2)(C(25)H(22)P(2))(2)](SbF(6))(2), the two Ag(I) atoms are bridged by the two methyl-enebis(diphenyl-phosphine) ligands and an eight-membered centrosymmetric metallacyclic ring is formed. The metal atom exhibits a distorted tetra-hedral coordination geometry, coordinated by two P atoms of the bridging ligands and two N atoms of the chelating 5-nitro-1,10-phenanthroline ligand. The latter ligand shows minor disorder, adopting two orientations with site occupancy factors of 0.84 and 0.16.

Entities:  

Year:  2007        PMID： 21200600      PMCID： PMC2915175          DOI： 10.1107/S1600536807067013

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


Related literature

For related literature, see: Ho & Bau (1983 ▶); Smith & Cagle (1947 ▶).

Experimental

Crystal data

[Ag2(C12H7N3O2)2(C25H22P2)2](SbF6)2 M = 1906.38 Monoclinic, a = 12.8034 (7) Å b = 23.3993 (10) Å c = 13.5580 (11) Å β = 117.936 (2)° V = 3588.5 (4) Å3 Z = 2 Mo Kα radiation μ = 1.46 mm−1 T = 293 (2) K 0.35 × 0.35 × 0.28 mm

Data collection

Rigaku Mercury 70 CCD diffractometer Absorption correction: multi-scan (CrystalClear; Rigaku, 2000 ▶) T min = 0.816, T max = 1.000 (expected range = 0.543–0.665) 22441 measured reflections 6301 independent reflections 5851 reflections with I > 2σ(I) R int = 0.026

Refinement

R[F 2 > 2σ(F 2)] = 0.030 wR(F 2) = 0.060 S = 1.11 6301 reflections 623 parameters 486 restraints H-atom parameters constrained Δρmax = 0.66 e Å−3 Δρmin = −0.70 e Å−3 Data collection: CrystalClear (Rigaku, 2000 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: SHELXTL (Bruker, 1999 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807067013/gk2121sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536807067013/gk2121Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ag2(C12H7N3O2)2(C25H22P2)2](SbF6)2F000 = 1880
Mr = 1906.38Dx = 1.764 Mg m−3
Monoclinic, P21/nMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 7865 reflections
a = 12.8034 (7) Åθ = 3.0–25.0º
b = 23.3993 (10) ŵ = 1.46 mm−1
c = 13.5580 (11) ÅT = 293 (2) K
β = 117.936 (2)ºPrism, yellow
V = 3588.5 (4) Å30.35 × 0.35 × 0.28 mm
Z = 2
Rigaku Mercury 70 CCD diffractometer6301 independent reflections
Radiation source: fine-focus sealed tube5851 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.026
Detector resolution: 14.6306 pixels mm-1θmax = 25.0º
T = 293(2) Kθmin = 3.0º
ω scansh = −15→15
Absorption correction: multi-scan(CrystalClear; Rigaku, 2000)k = −27→26
Tmin = 0.816, Tmax = 1.000l = −16→15
22441 measured reflections
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.030H-atom parameters constrained
wR(F2) = 0.060  w = 1/[σ2(Fo2) + (0.0186P)2 + 5.1P] where P = (Fo2 + 2Fc2)/3
S = 1.11(Δ/σ)max = 0.002
6301 reflectionsΔρmax = 0.66 e Å−3
623 parametersΔρmin = −0.70 e Å−3
486 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
Experimental. 2007–03-05 # Formatted by publCIF
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*/UeqOcc. (<1)
Ag0.023652 (17)−0.075515 (9)1.091671 (17)0.01867 (6)
P1−0.17901 (6)−0.06326 (3)0.94206 (6)0.01775 (16)
P20.19380 (6)−0.02588 (3)1.22857 (6)0.01697 (15)
C21−0.2634 (2)−0.00996 (12)0.9721 (2)0.0216 (6)
C22−0.3864 (3)−0.00586 (13)0.9110 (3)0.0247 (7)
H22A−0.4286−0.03250.85550.030*
C23−0.4457 (3)0.03785 (14)0.9330 (3)0.0326 (8)
H23A−0.52740.04090.89130.039*
C24−0.3838 (3)0.07685 (15)1.0167 (3)0.0401 (9)
H24A−0.42410.10591.03150.048*
C25−0.2625 (3)0.07299 (15)1.0786 (3)0.0385 (8)
H25A−0.22110.09921.13510.046*
C26−0.2027 (3)0.02995 (13)1.0562 (3)0.0280 (7)
H26A−0.12090.02761.09770.034*
C31−0.2520 (2)−0.13177 (12)0.9320 (2)0.0205 (6)
C32−0.2280 (2)−0.17707 (13)0.8787 (2)0.0253 (7)
H32A−0.1866−0.17030.83890.030*
C33−0.2651 (3)−0.23201 (13)0.8845 (3)0.0313 (8)
H33A−0.2483−0.26200.84910.038*
C34−0.3271 (3)−0.24197 (14)0.9432 (3)0.0357 (8)
H34A−0.3513−0.27890.94800.043*
C35−0.3532 (3)−0.19762 (15)0.9945 (3)0.0351 (8)
H35A−0.3960−0.20461.03290.042*
C36−0.3163 (2)−0.14242 (14)0.9894 (3)0.0274 (7)
H36A−0.3343−0.11261.02420.033*
C410.1816 (2)−0.02647 (12)1.3574 (2)0.0200 (6)
C420.2094 (3)−0.07752 (14)1.4183 (3)0.0275 (7)
H42A0.2376−0.10851.39480.033*
C430.1952 (3)−0.08225 (15)1.5130 (3)0.0330 (8)
H43A0.2131−0.11651.55250.040*
C440.1546 (3)−0.03626 (16)1.5490 (3)0.0353 (8)
H44A0.1466−0.03931.61350.042*
C450.1261 (3)0.01406 (15)1.4896 (3)0.0352 (8)
H45A0.09830.04491.51380.042*
C460.1388 (3)0.01893 (13)1.3932 (3)0.0261 (7)
H46A0.11850.05291.35280.031*
C510.3399 (2)−0.05683 (13)1.2753 (2)0.0206 (6)
C520.3518 (3)−0.10922 (13)1.2338 (3)0.0283 (7)
H52A0.2852−0.12811.18080.034*
C530.4631 (3)−0.13370 (15)1.2712 (3)0.0389 (9)
H53A0.4709−0.16881.24300.047*
C540.5617 (3)−0.10585 (16)1.3500 (3)0.0371 (8)
H54A0.6360−0.12231.37510.044*
C550.5510 (3)−0.05397 (16)1.3916 (3)0.0349 (8)
H55A0.6182−0.03521.44390.042*
C560.4403 (2)−0.02935 (14)1.3558 (3)0.0262 (7)
H56A0.43320.00541.38560.031*
C61−0.2118 (2)−0.04967 (12)0.7965 (2)0.0206 (6)
H61A−0.1595−0.07260.77910.025*
H61B−0.2924−0.06130.74690.025*
C10.0907 (6)−0.1990 (2)1.0194 (7)0.0286 (12)0.842 (4)
H1A0.1206−0.17480.98430.034*0.842 (4)
C20.0947 (6)−0.2583 (2)1.0054 (5)0.0438 (16)0.842 (4)
H2A0.1270−0.27290.96190.053*0.842 (4)
C30.0510 (5)−0.2940 (2)1.0557 (5)0.0445 (16)0.842 (4)
H3A0.0541−0.33321.04710.053*0.842 (4)
C40.0010 (5)−0.2723 (2)1.1206 (4)0.0338 (12)0.842 (4)
C5−0.0497 (5)−0.3045 (2)1.1798 (5)0.0424 (17)0.842 (4)
C6−0.1018 (4)−0.2802 (2)1.2341 (4)0.0427 (13)0.842 (4)
H6A−0.1364−0.30331.26660.051*0.842 (4)
C7−0.1057 (5)−0.2198 (2)1.2435 (4)0.0323 (12)0.842 (4)
C8−0.1592 (4)−0.1931 (2)1.3008 (4)0.0411 (12)0.842 (4)
H8A−0.1969−0.21461.33240.049*0.842 (4)
C9−0.1552 (5)−0.1351 (2)1.3094 (4)0.0417 (12)0.842 (4)
H9A−0.1903−0.11651.34680.050*0.842 (4)
C10−0.0977 (5)−0.1041 (2)1.2612 (5)0.0326 (13)0.842 (4)
H10A−0.0943−0.06461.26900.039*0.842 (4)
C11−0.0517 (5)−0.18563 (19)1.1947 (5)0.0235 (10)0.842 (4)
C120.0005 (7)−0.2113 (2)1.1323 (5)0.0251 (11)0.842 (4)
N10.0456 (9)−0.1765 (2)1.0812 (9)0.0238 (10)0.842 (4)
N2−0.0478 (8)−0.12770 (18)1.2050 (7)0.0233 (10)0.842 (4)
N3−0.0420 (4)−0.36777 (18)1.1863 (4)0.0676 (16)0.842 (4)
O1−0.0046 (4)−0.39241 (17)1.1320 (6)0.121 (3)0.842 (4)
O2−0.0729 (8)−0.3919 (2)1.2455 (8)0.095 (3)0.842 (4)
C1'0.110 (4)−0.1903 (13)1.011 (4)0.023 (3)0.158 (4)
H1'A0.1420−0.16280.98420.027*0.158 (4)
C2'0.116 (3)−0.2481 (13)0.987 (3)0.027 (4)0.158 (4)
H2'A0.1480−0.25850.94050.032*0.158 (4)
C3'0.075 (3)−0.2885 (12)1.031 (3)0.028 (4)0.158 (4)
H3'A0.0816−0.32691.01730.034*0.158 (4)
C4'0.023 (3)−0.2733 (11)1.098 (3)0.024 (3)0.158 (4)
C5'−0.026 (2)−0.3121 (10)1.149 (2)0.026 (4)0.158 (4)
H5'A−0.0234−0.35111.13720.031*0.158 (4)
C6'−0.074 (3)−0.2941 (10)1.210 (3)0.032 (4)0.158 (4)
C7'−0.086 (3)−0.2346 (9)1.228 (3)0.026 (3)0.158 (4)
C8'−0.129 (2)−0.2136 (10)1.299 (2)0.031 (4)0.158 (4)
H8'A−0.1587−0.23901.33180.037*0.158 (4)
C9'−0.127 (3)−0.1569 (10)1.320 (2)0.031 (3)0.158 (4)
H9'A−0.1576−0.14331.36560.038*0.158 (4)
C10'−0.079 (3)−0.1187 (11)1.271 (3)0.031 (3)0.158 (4)
H10B−0.0756−0.07981.28620.037*0.158 (4)
C11'−0.034 (3)−0.1943 (10)1.185 (3)0.025 (3)0.158 (4)
C12'0.012 (4)−0.2131 (11)1.114 (3)0.022 (3)0.158 (4)
N1'0.059 (6)−0.1739 (13)1.072 (5)0.020 (3)0.158 (4)
N2'−0.038 (5)−0.1379 (11)1.204 (4)0.023 (3)0.158 (4)
N3'−0.1201 (15)−0.3401 (8)1.2576 (16)0.040 (3)0.158 (4)
O2'−0.1967 (14)−0.3283 (7)1.2810 (14)0.049 (3)0.158 (4)
O1'−0.091 (4)−0.3889 (11)1.259 (4)0.033 (3)0.158 (4)
Sb0.035784 (19)0.195912 (9)1.342401 (19)0.03131 (7)
F1−0.0552 (2)0.15895 (13)1.3963 (3)0.0868 (9)
F2−0.09810 (19)0.23510 (10)1.2379 (2)0.0632 (7)
F30.12724 (18)0.23192 (9)1.28696 (18)0.0447 (5)
F40.0682 (2)0.25534 (10)1.4442 (2)0.0624 (7)
F50.0064 (2)0.13675 (9)1.23847 (18)0.0559 (6)
F60.16940 (18)0.15634 (9)1.44683 (17)0.0461 (5)
U11U22U33U12U13U23
Ag0.01518 (11)0.01797 (12)0.02097 (11)−0.00183 (8)0.00690 (9)−0.00001 (9)
P10.0148 (3)0.0175 (4)0.0195 (4)−0.0012 (3)0.0069 (3)0.0020 (3)
P20.0140 (3)0.0155 (4)0.0193 (4)−0.0006 (3)0.0060 (3)0.0015 (3)
C210.0220 (14)0.0207 (16)0.0236 (15)0.0009 (12)0.0119 (13)0.0042 (12)
C220.0219 (15)0.0260 (17)0.0288 (16)−0.0009 (13)0.0141 (13)0.0049 (13)
C230.0249 (16)0.037 (2)0.041 (2)0.0085 (15)0.0203 (15)0.0085 (16)
C240.044 (2)0.034 (2)0.054 (2)0.0089 (17)0.0326 (19)−0.0018 (18)
C250.0392 (19)0.035 (2)0.045 (2)−0.0055 (16)0.0229 (17)−0.0149 (17)
C260.0250 (15)0.0286 (17)0.0316 (17)−0.0025 (14)0.0142 (14)−0.0036 (14)
C310.0122 (13)0.0225 (16)0.0190 (14)−0.0032 (12)0.0007 (11)0.0047 (12)
C320.0190 (14)0.0256 (17)0.0229 (16)−0.0019 (13)0.0027 (13)0.0019 (13)
C330.0229 (16)0.0212 (17)0.0294 (17)−0.0023 (13)−0.0048 (14)0.0023 (14)
C340.0225 (16)0.0249 (18)0.0349 (19)−0.0070 (14)−0.0071 (15)0.0109 (15)
C350.0212 (16)0.043 (2)0.0323 (18)−0.0082 (15)0.0050 (14)0.0169 (16)
C360.0175 (14)0.0321 (18)0.0274 (16)−0.0026 (13)0.0062 (13)0.0065 (14)
C410.0125 (13)0.0241 (16)0.0199 (14)−0.0032 (12)0.0047 (12)0.0002 (12)
C420.0230 (15)0.0291 (18)0.0303 (17)0.0016 (13)0.0125 (14)0.0067 (14)
C430.0233 (16)0.043 (2)0.0299 (17)−0.0013 (15)0.0099 (14)0.0136 (16)
C440.0332 (18)0.052 (2)0.0255 (17)−0.0073 (17)0.0174 (15)0.0033 (16)
C450.0382 (19)0.038 (2)0.0373 (19)−0.0051 (16)0.0239 (16)−0.0075 (16)
C460.0263 (16)0.0243 (17)0.0310 (17)−0.0030 (13)0.0161 (14)0.0007 (13)
C510.0165 (13)0.0235 (16)0.0209 (15)0.0007 (12)0.0080 (12)0.0062 (12)
C520.0208 (15)0.0215 (17)0.0403 (19)−0.0008 (13)0.0124 (14)−0.0002 (14)
C530.0352 (19)0.0238 (18)0.061 (2)0.0089 (15)0.0247 (18)0.0045 (17)
C540.0205 (16)0.043 (2)0.047 (2)0.0121 (15)0.0152 (16)0.0166 (17)
C550.0158 (15)0.048 (2)0.0332 (18)−0.0019 (15)0.0055 (14)0.0064 (16)
C560.0196 (15)0.0296 (18)0.0288 (16)−0.0015 (13)0.0108 (13)−0.0024 (14)
C610.0222 (14)0.0162 (15)0.0237 (15)−0.0003 (12)0.0111 (13)0.0000 (12)
C10.026 (3)0.029 (3)0.026 (2)0.005 (2)0.0082 (18)−0.001 (2)
C20.047 (3)0.035 (3)0.039 (3)0.012 (3)0.011 (2)−0.007 (3)
C30.047 (3)0.021 (2)0.038 (3)0.011 (2)−0.002 (2)−0.006 (2)
C40.028 (3)0.0185 (19)0.028 (3)0.0031 (17)−0.0086 (17)0.0019 (18)
C50.035 (3)0.017 (2)0.037 (4)−0.007 (2)−0.015 (2)0.014 (2)
C60.033 (2)0.039 (3)0.032 (2)−0.013 (2)−0.0048 (18)0.017 (2)
C70.026 (2)0.040 (3)0.018 (2)−0.014 (2)0.0001 (17)0.007 (2)
C80.034 (3)0.064 (4)0.024 (2)−0.023 (2)0.0132 (19)0.002 (2)
C90.037 (3)0.060 (3)0.033 (2)−0.018 (2)0.020 (2)−0.011 (2)
C100.030 (3)0.042 (3)0.029 (2)−0.012 (2)0.017 (2)−0.011 (2)
C110.016 (2)0.028 (2)0.0144 (18)−0.0046 (17)−0.0025 (14)0.0035 (17)
C120.020 (2)0.0213 (18)0.020 (3)−0.0026 (16)−0.0031 (16)0.0098 (17)
N10.019 (3)0.0228 (18)0.022 (3)0.0015 (16)0.0032 (14)−0.0027 (16)
N20.022 (2)0.025 (2)0.0200 (16)−0.008 (2)0.0071 (15)−0.002 (2)
N30.038 (2)0.026 (2)0.081 (3)−0.008 (2)−0.020 (2)0.018 (2)
O10.086 (3)0.023 (2)0.269 (8)0.004 (2)0.097 (4)0.008 (3)
O20.114 (7)0.034 (3)0.066 (5)−0.031 (3)−0.016 (3)0.030 (3)
C1'0.024 (5)0.024 (5)0.023 (5)0.004 (5)0.014 (4)−0.001 (4)
C2'0.029 (6)0.025 (6)0.029 (5)0.001 (5)0.016 (5)0.001 (5)
C3'0.033 (6)0.023 (5)0.030 (6)0.007 (5)0.016 (5)−0.004 (5)
C4'0.023 (5)0.020 (4)0.023 (5)0.001 (4)0.007 (4)0.003 (4)
C5'0.024 (5)0.019 (5)0.025 (6)−0.004 (5)0.003 (5)0.007 (5)
C6'0.028 (5)0.028 (5)0.029 (5)−0.007 (5)0.004 (5)0.010 (5)
C7'0.021 (4)0.032 (5)0.019 (4)−0.006 (4)0.004 (4)0.003 (4)
C8'0.025 (5)0.039 (6)0.023 (5)−0.011 (5)0.007 (5)0.000 (5)
C9'0.028 (5)0.046 (5)0.025 (4)−0.012 (5)0.016 (4)−0.005 (5)
C10'0.028 (5)0.037 (5)0.026 (4)−0.012 (5)0.012 (4)−0.003 (5)
C11'0.021 (4)0.022 (4)0.019 (4)−0.010 (4)−0.001 (4)0.005 (4)
C12'0.019 (4)0.022 (4)0.019 (5)0.002 (4)0.004 (4)−0.001 (4)
N1'0.020 (5)0.022 (4)0.019 (5)−0.005 (4)0.009 (4)0.006 (4)
N2'0.022 (5)0.033 (5)0.017 (4)−0.008 (5)0.010 (4)−0.002 (5)
N3'0.040 (5)0.039 (5)0.043 (5)−0.007 (5)0.021 (4)0.018 (5)
O2'0.045 (6)0.043 (6)0.053 (6)−0.007 (5)0.019 (5)0.020 (5)
O1'0.039 (5)0.038 (6)0.036 (6)−0.006 (5)0.030 (5)0.015 (5)
Sb0.03320 (12)0.02695 (13)0.03999 (14)0.00654 (9)0.02232 (11)0.00912 (10)
F10.0786 (18)0.091 (2)0.119 (2)−0.0047 (16)0.0694 (19)0.0431 (19)
F20.0377 (12)0.0606 (16)0.0893 (18)0.0241 (11)0.0282 (13)0.0301 (14)
F30.0464 (12)0.0476 (13)0.0557 (13)0.0058 (10)0.0370 (11)0.0089 (10)
F40.0965 (19)0.0479 (14)0.0622 (15)0.0149 (13)0.0533 (15)−0.0061 (12)
F50.0565 (14)0.0377 (12)0.0437 (13)0.0067 (11)−0.0013 (11)−0.0024 (10)
F60.0489 (12)0.0339 (11)0.0392 (12)0.0060 (10)0.0070 (10)0.0053 (9)
Ag—N12.392 (6)C1—N11.329 (5)
Ag—P22.3982 (7)C1—C21.404 (6)
Ag—N1'2.38 (3)C1—H1A0.9300
Ag—N2'2.49 (3)C2—C31.353 (7)
Ag—P12.4491 (7)C2—H2A0.9300
Ag—N22.451 (5)C3—C41.403 (7)
P1—C211.817 (3)C3—H3A0.9300
P1—C311.828 (3)C4—C121.437 (5)
P1—C611.843 (3)C4—C51.457 (8)
P2—C511.821 (3)C5—C61.330 (7)
P2—C411.825 (3)C5—N31.483 (6)
P2—C61i1.835 (3)C6—C71.424 (7)
C21—C261.395 (4)C6—H6A0.9300
C21—C221.398 (4)C7—C81.400 (7)
C22—C231.387 (4)C7—C111.408 (5)
C22—H22A0.9300C8—C91.359 (7)
C23—C241.381 (5)C8—H8A0.9300
C23—H23A0.9300C9—C101.395 (6)
C24—C251.380 (5)C9—H9A0.9300
C24—H24A0.9300C10—N21.322 (5)
C25—C261.383 (4)C10—H10A0.9300
C25—H25A0.9300C11—N21.361 (5)
C26—H26A0.9300C11—C121.432 (6)
C31—C361.395 (4)C12—N11.361 (5)
C31—C321.396 (4)N3—O21.191 (8)
C32—C331.385 (4)N3—O11.198 (7)
C32—H32A0.9300C1'—N1'1.325 (17)
C33—C341.382 (5)C1'—C2'1.405 (17)
C33—H33A0.9300C1'—H1'A0.9300
C34—C351.376 (5)C2'—C3'1.350 (18)
C34—H34A0.9300C2'—H2'A0.9300
C35—C361.388 (4)C3'—C4'1.397 (17)
C35—H35A0.9300C3'—H3'A0.9300
C36—H36A0.9300C4'—C12'1.440 (16)
C41—C461.383 (4)C4'—C5'1.447 (17)
C41—C421.400 (4)C5'—C6'1.322 (19)
C42—C431.384 (4)C5'—H5'A0.9300
C42—H42A0.9300C6'—C7'1.435 (18)
C43—C441.379 (5)C6'—N3'1.50 (3)
C43—H43A0.9300C7'—C8'1.387 (17)
C44—C451.376 (5)C7'—C11'1.429 (16)
C44—H44A0.9300C8'—C9'1.357 (18)
C45—C461.396 (4)C8'—H8'A0.9300
C45—H45A0.9300C9'—C10'1.417 (17)
C46—H46A0.9300C9'—H9'A0.9300
C51—C521.386 (4)C10'—N2'1.324 (17)
C51—C561.394 (4)C10'—H10B0.9300
C52—C531.392 (4)C11'—N2'1.349 (16)
C52—H52A0.9300C11'—C12'1.420 (16)
C53—C541.376 (5)C12'—N1'1.354 (16)
C53—H53A0.9300N3'—O2'1.197 (16)
C54—C551.372 (5)N3'—O1'1.197 (19)
C54—H54A0.9300Sb—F11.853 (2)
C55—C561.390 (4)Sb—F31.8630 (19)
C55—H55A0.9300Sb—F41.864 (2)
C56—H56A0.9300Sb—F21.874 (2)
C61—P2i1.835 (3)Sb—F61.8759 (19)
C61—H61A0.9700Sb—F51.883 (2)
C61—H61B0.9700
N1—Ag—P2115.8 (3)N1—C1—C2122.1 (5)
N1—Ag—N1'6.2 (7)N1—C1—H1A119.0
P2—Ag—N1'113.8 (17)C2—C1—H1A119.0
N1—Ag—N2'62.3 (6)C3—C2—C1119.4 (5)
P2—Ag—N2'104.1 (13)C3—C2—H2A120.3
N1'—Ag—N2'68.3 (7)C1—C2—H2A120.3
N1—Ag—P1100.1 (3)C2—C3—C4120.7 (4)
P2—Ag—P1144.11 (3)C2—C3—H3A119.6
N1'—Ag—P1101.7 (17)C4—C3—H3A119.6
N2'—Ag—P193.4 (14)C3—C4—C12117.1 (4)
N1—Ag—N268.51 (15)C3—C4—C5127.6 (4)
P2—Ag—N2103.1 (2)C12—C4—C5115.2 (5)
N1'—Ag—N274.5 (6)C6—C5—C4123.5 (4)
N2'—Ag—N26.3 (7)C6—C5—N3115.5 (6)
P1—Ag—N290.9 (2)C4—C5—N3121.0 (6)
C21—P1—C31106.38 (13)C5—C6—C7121.5 (5)
C21—P1—C61105.11 (13)C5—C6—H6A119.2
C31—P1—C61102.66 (13)C7—C6—H6A119.2
C21—P1—Ag113.91 (10)C8—C7—C11118.9 (4)
C31—P1—Ag105.39 (9)C8—C7—C6122.7 (4)
C61—P1—Ag121.90 (9)C11—C7—C6118.4 (5)
C51—P2—C41101.49 (13)C9—C8—C7118.9 (4)
C51—P2—C61i104.48 (13)C9—C8—H8A120.5
C41—P2—C61i104.99 (13)C7—C8—H8A120.5
C51—P2—Ag119.29 (10)C8—C9—C10119.0 (5)
C41—P2—Ag106.43 (9)C8—C9—H9A120.5
C61i—P2—Ag118.08 (10)C10—C9—H9A120.5
C26—C21—C22118.7 (3)N2—C10—C9123.8 (5)
C26—C21—P1118.7 (2)N2—C10—H10A118.1
C22—C21—P1122.5 (2)C9—C10—H10A118.1
C23—C22—C21120.1 (3)N2—C11—C7121.3 (4)
C23—C22—H22A119.9N2—C11—C12118.2 (4)
C21—C22—H22A119.9C7—C11—C12120.5 (4)
C24—C23—C22120.2 (3)N1—C12—C4120.8 (5)
C24—C23—H23A119.9N1—C12—C11118.5 (4)
C22—C23—H23A119.9C4—C12—C11120.7 (4)
C25—C24—C23120.4 (3)C1—N1—C12119.8 (4)
C25—C24—H24A119.8C1—N1—Ag121.8 (4)
C23—C24—H24A119.8C12—N1—Ag118.1 (3)
C24—C25—C26119.7 (3)C10—N2—C11118.0 (4)
C24—C25—H25A120.1C10—N2—Ag125.2 (3)
C26—C25—H25A120.1C11—N2—Ag116.0 (3)
C25—C26—C21120.9 (3)O2—N3—O1122.8 (6)
C25—C26—H26A119.5O2—N3—C5118.7 (7)
C21—C26—H26A119.5O1—N3—C5118.6 (6)
C36—C31—C32118.9 (3)N1'—C1'—C2'122 (2)
C36—C31—P1122.0 (2)N1'—C1'—H1'A119.1
C32—C31—P1118.4 (2)C2'—C1'—H1'A119.1
C33—C32—C31120.7 (3)C3'—C2'—C1'119 (2)
C33—C32—H32A119.6C3'—C2'—H2'A120.3
C31—C32—H32A119.6C1'—C2'—H2'A120.3
C34—C33—C32119.6 (3)C2'—C3'—C4'120.9 (19)
C34—C33—H33A120.2C2'—C3'—H3'A119.6
C32—C33—H33A120.2C4'—C3'—H3'A119.6
C35—C34—C33120.4 (3)C3'—C4'—C12'117.0 (16)
C35—C34—H34A119.8C3'—C4'—C5'126.3 (18)
C33—C34—H34A119.8C12'—C4'—C5'116.6 (16)
C34—C35—C36120.5 (3)C6'—C5'—C4'123 (2)
C34—C35—H35A119.8C6'—C5'—H5'A118.7
C36—C35—H35A119.8C4'—C5'—H5'A118.7
C35—C36—C31119.9 (3)C5'—C6'—C7'122 (2)
C35—C36—H36A120.1C5'—C6'—N3'115.7 (19)
C31—C36—H36A120.1C7'—C6'—N3'121.9 (18)
C46—C41—C42118.8 (3)C8'—C7'—C6'124.6 (17)
C46—C41—P2123.7 (2)C8'—C7'—C11'117.2 (16)
C42—C41—P2117.3 (2)C6'—C7'—C11'117.6 (17)
C43—C42—C41120.5 (3)C9'—C8'—C7'121.4 (18)
C43—C42—H42A119.7C9'—C8'—H8'A119.3
C41—C42—H42A119.7C7'—C8'—H8'A119.3
C44—C43—C42120.0 (3)C8'—C9'—C10'118.9 (18)
C44—C43—H43A120.0C8'—C9'—H9'A120.5
C42—C43—H43A120.0C10'—C9'—H9'A120.5
C45—C44—C43120.1 (3)N2'—C10'—C9'121 (2)
C45—C44—H44A119.9N2'—C10'—H10B119.7
C43—C44—H44A119.9C9'—C10'—H10B119.7
C44—C45—C46120.2 (3)N2'—C11'—C7'120.3 (17)
C44—C45—H45A119.9N2'—C11'—C12'119.5 (16)
C46—C45—H45A119.9C7'—C11'—C12'120.0 (17)
C41—C46—C45120.3 (3)N1'—C12'—C4'120.5 (17)
C41—C46—H46A119.8N1'—C12'—C11'118.7 (17)
C45—C46—H46A119.8C4'—C12'—C11'120.3 (17)
C52—C51—C56119.3 (3)C1'—N1'—C12'120 (2)
C52—C51—P2120.1 (2)C1'—N1'—Ag121.4 (17)
C56—C51—P2120.6 (2)C12'—N1'—Ag117.8 (15)
C51—C52—C53120.3 (3)C10'—N2'—C11'121.4 (19)
C51—C52—H52A119.9C10'—N2'—Ag124.1 (16)
C53—C52—H52A119.9C11'—N2'—Ag114.3 (14)
C54—C53—C52119.8 (3)O2'—N3'—O1'120.1 (19)
C54—C53—H53A120.1O2'—N3'—C6'118.5 (18)
C52—C53—H53A120.1O1'—N3'—C6'121 (2)
C55—C54—C53120.4 (3)F1—Sb—F3179.02 (13)
C55—C54—H54A119.8F1—Sb—F491.09 (13)
C53—C54—H54A119.8F3—Sb—F489.86 (10)
C54—C55—C56120.3 (3)F1—Sb—F290.32 (12)
C54—C55—H55A119.8F3—Sb—F289.92 (10)
C56—C55—H55A119.8F4—Sb—F290.14 (12)
C55—C56—C51119.8 (3)F1—Sb—F689.50 (11)
C55—C56—H56A120.1F3—Sb—F690.25 (9)
C51—C56—H56A120.1F4—Sb—F690.09 (10)
P2i—C61—P1112.26 (15)F2—Sb—F6179.72 (11)
P2i—C61—H61A109.2F1—Sb—F590.56 (14)
P1—C61—H61A109.2F3—Sb—F588.49 (10)
P2i—C61—H61B109.2F4—Sb—F5178.33 (11)
P1—C61—H61B109.2F2—Sb—F590.13 (11)
H61A—C61—H61B107.9F6—Sb—F589.65 (9)
N1—Ag—P1—C21143.06 (17)C61i—P2—C51—C5646.3 (3)
P2—Ag—P1—C21−39.37 (11)Ag—P2—C51—C56−179.1 (2)
N1'—Ag—P1—C21149.1 (6)C56—C51—C52—C53−0.9 (5)
N2'—Ag—P1—C2180.6 (6)P2—C51—C52—C53−178.5 (3)
N2—Ag—P1—C2174.73 (15)C51—C52—C53—C540.3 (5)
N1—Ag—P1—C3126.83 (17)C52—C53—C54—C55−0.3 (5)
P2—Ag—P1—C31−155.60 (10)C53—C54—C55—C561.0 (5)
N1'—Ag—P1—C3132.9 (6)C54—C55—C56—C51−1.6 (5)
N2'—Ag—P1—C31−35.7 (6)C52—C51—C56—C551.6 (4)
N2—Ag—P1—C31−41.50 (15)P2—C51—C56—C55179.2 (2)
N1—Ag—P1—C61−89.21 (17)C21—P1—C61—P2i49.57 (18)
P2—Ag—P1—C6188.35 (12)C31—P1—C61—P2i160.67 (15)
N1'—Ag—P1—C61−83.2 (6)Ag—P1—C61—P2i−81.92 (16)
N2'—Ag—P1—C61−151.7 (6)C2—C1—N1—Ag−174.5 (6)
N2—Ag—P1—C61−157.54 (15)C4—C12—N1—Ag174.2 (5)
N1—Ag—P2—C5124.36 (19)C11—C12—N1—Ag−3.4 (11)
N1'—Ag—P2—C5117.9 (7)P2—Ag—N1—C1−85.9 (8)
N2'—Ag—P2—C5190.1 (8)N1'—Ag—N1—C1−14 (18)
P1—Ag—P2—C51−152.97 (11)N2'—Ag—N1—C1−178.9 (18)
N2—Ag—P2—C5196.58 (17)P1—Ag—N1—C192.5 (8)
N1—Ag—P2—C41−89.44 (18)N2—Ag—N1—C1179.5 (9)
N1'—Ag—P2—C41−95.8 (7)P2—Ag—N1—C12100.1 (7)
N2'—Ag—P2—C41−23.7 (8)N1'—Ag—N1—C12172 (19)
P1—Ag—P2—C4193.23 (11)N2'—Ag—N1—C127.1 (17)
N2—Ag—P2—C41−17.21 (16)P1—Ag—N1—C12−81.5 (8)
N1—Ag—P2—C61i152.98 (18)N2—Ag—N1—C125.5 (7)
N1'—Ag—P2—C61i146.6 (7)C9—C10—N2—C11−0.7 (11)
N2'—Ag—P2—C61i−141.2 (8)C9—C10—N2—Ag168.8 (5)
P1—Ag—P2—C61i−24.35 (12)C7—C11—N2—C10−0.9 (11)
N2—Ag—P2—C61i−134.79 (17)C12—C11—N2—C10178.9 (7)
C31—P1—C21—C26133.8 (2)C7—C11—N2—Ag−171.3 (5)
C61—P1—C21—C26−117.8 (2)C12—C11—N2—Ag8.5 (9)
Ag—P1—C21—C2618.2 (3)N1—Ag—N2—C10−176.9 (8)
C31—P1—C21—C22−49.0 (3)P2—Ag—N2—C1070.2 (7)
C61—P1—C21—C2259.4 (3)N1'—Ag—N2—C10−178.3 (19)
Ag—P1—C21—C22−164.7 (2)N2'—Ag—N2—C10170 (15)
C26—C21—C22—C231.1 (4)P1—Ag—N2—C10−76.4 (7)
P1—C21—C22—C23−176.0 (2)N1—Ag—N2—C11−7.2 (6)
C21—C22—C23—C24−1.2 (5)P2—Ag—N2—C11−120.1 (6)
C22—C23—C24—C250.5 (5)N1'—Ag—N2—C11−8.7 (18)
C23—C24—C25—C260.3 (6)N2'—Ag—N2—C11−20 (14)
C24—C25—C26—C21−0.4 (5)P1—Ag—N2—C1193.2 (6)
C22—C21—C26—C25−0.3 (5)C6—C5—N3—O2−6.1 (8)
P1—C21—C26—C25176.9 (3)C4—C5—N3—O2171.9 (7)
C21—P1—C31—C36−27.8 (3)C6—C5—N3—O1174.2 (5)
C61—P1—C31—C36−138.0 (2)C4—C5—N3—O1−7.8 (7)
Ag—P1—C31—C3693.5 (2)N1—Ag—N1'—C1'169 (23)
C21—P1—C31—C32161.8 (2)P2—Ag—N1'—C1'−81 (5)
C61—P1—C31—C3251.7 (2)N2'—Ag—N1'—C1'−177 (5)
Ag—P1—C31—C32−76.9 (2)P1—Ag—N1'—C1'94 (5)
C36—C31—C32—C33−1.3 (4)N2—Ag—N1'—C1'−179 (5)
P1—C31—C32—C33169.4 (2)N1—Ag—N1'—C12'−3(15)
C31—C32—C33—C340.3 (4)P2—Ag—N1'—C12'107 (4)
C32—C33—C34—C350.8 (4)N2'—Ag—N1'—C12'10 (4)
C33—C34—C35—C36−0.9 (5)P1—Ag—N1'—C12'−79 (5)
C34—C35—C36—C31−0.1 (4)N2—Ag—N1'—C12'9(4)
C32—C31—C36—C351.2 (4)C9'—C10'—N2'—C11'−4(7)
P1—C31—C36—C35−169.2 (2)C9'—C10'—N2'—Ag171 (3)
C51—P2—C41—C46135.8 (2)C7'—C11'—N2'—C10'6(7)
C61i—P2—C41—C4627.2 (3)C12'—C11'—N2'—C10'−179 (5)
Ag—P2—C41—C46−98.7 (2)C7'—C11'—N2'—Ag−169 (3)
C51—P2—C41—C42−48.9 (2)C12'—C11'—N2'—Ag6(6)
C61i—P2—C41—C42−157.5 (2)N1—Ag—N2'—C10'178 (5)
Ag—P2—C41—C4276.5 (2)P2—Ag—N2'—C10'66 (4)
C46—C41—C42—C43−0.5 (4)N1'—Ag—N2'—C10'177 (5)
P2—C41—C42—C43−176.0 (2)P1—Ag—N2'—C10'−82 (4)
C41—C42—C43—C44−0.7 (5)N2—Ag—N2'—C10'−15 (11)
C42—C43—C44—C451.2 (5)N1—Ag—N2'—C11'−7(3)
C43—C44—C45—C46−0.4 (5)P2—Ag—N2'—C11'−119 (4)
C42—C41—C46—C451.3 (4)N1'—Ag—N2'—C11'−8(4)
P2—C41—C46—C45176.5 (2)P1—Ag—N2'—C11'93 (4)
C44—C45—C46—C41−0.8 (5)N2—Ag—N2'—C11'160 (17)
C41—P2—C51—C52114.9 (3)C5'—C6'—N3'—O2'−156 (3)
C61i—P2—C51—C52−136.2 (2)C7'—C6'—N3'—O2'23 (4)
Ag—P2—C51—C52−1.6 (3)C5'—C6'—N3'—O1'16 (5)
C41—P2—C51—C56−62.7 (3)C7'—C6'—N3'—O1'−166 (4)
D—H···AD—HH···AD···AD—H···A
C35—H35A···F4ii0.932.543.409 (4)155
C46—H46A···F50.932.503.398 (4)163
Ag—N12.392 (6)
Ag—P22.3982 (7)
Ag—P12.4491 (7)
Ag—N22.451 (5)
N1—Ag—P2115.8 (3)
N1—Ag—P1100.1 (3)
P2—Ag—P1144.11 (3)
N1—Ag—N268.51 (15)
P2—Ag—N2103.1 (2)
P1—Ag—N290.9 (2)
  1 in total

1.  The improved synthesis of 5-nitro-1,10-phenanthroline.

Authors:  G F SMITH; F W CAGLE
Journal:  J Org Chem       Date:  1947-11       Impact factor: 4.354
  1 in total

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