Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The title paramagnetic compound, chloro-2[kappa]Cl-[di-tert-butyl­phos­phinic ethylamide-1[kappa]O]­bis­[[mu]-di-tert-butyl­phos­phin­ic ethyl­amidato(1-)-1:2[kappa]4O:N]­lithium(I)­nickel(II), [NiLiCl(C10H23NOP)2(C10H24NOP)], revealed an incomplete bischelation of Ni2+ by L- {L = [tBu2P(O)NEt]-}, with the formation of a pseudo-tetrahedral NiON2Cl chromophore. The Ni atom is coordinated by Cl-, bidentate L- and mono­dentate LLi (via N).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100012075/qa0381sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100012075/qa0381Isup2.hkl
Contains datablock I

CCDC reference: 152649

Comment top

The paramagnetic (µeff=3.3 BM at 300 K) title compound, (I), revealed an incomplete bischelation of Ni2+ by L with formation of a pseudo-tetrahedral NiON2Cl chromophore. The Ni atom is coordinated by Cl, bidentate L and monodentate LLi (via N). The coordination is pseudo-tetrahedral with a dihedral angle of 68.8 (1)° between the planes defined by Ni/O2/N2 and Ni/Cl/N1. A trigonal–planar LiO3 coordination [angles at Li of 107.9 (3), 123.4 (3) and 128.7 (3)°] is formed by bonds between Li and the pendant ligand [1.801 (6) Å], L [1.842 (6) Å] and the protonated L [1.825 (6) Å]. Preliminary results have been reported elsewhere (Wunderlich, 1996).

Experimental top

The paramagnetic title compound, (I), was isolated from the products obtained in a metathesis reaction of LLi and (PPh3)2NiCl2 {L = [tBu2P(O)NEt]} (Brück, 1995; Brück et al., 1996).

Refinement top

All H atoms have been calculated and included in a riding mode except for H3 which has been refined using a restrained N—H distance [N3—H3 0.853 (14) Å].

Computing details top

Data collection: Siemens/Bruker P3 (Siemens, 1989); cell refinement: Siemens/Bruker P3; data reduction: SHELXTL-Plus (Sheldrick, 1990); program(s) used to solve structure: SHELXTL-Plus; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
[NiLiCl(C10H23NOP)2(C10H24NOP)]Dx = 1.123 Mg m3
Mr = 714.90Melting point: 411 K K
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 17.304 (4) ÅCell parameters from 40 reflections
b = 13.055 (3) Åθ = 10.0–12.6°
c = 19.444 (4) ŵ = 0.67 mm1
β = 105.80 (2)°T = 300 K
V = 4226.5 (16) Å3Square bipyramid, metallic dark brown
Z = 40.50 × 0.50 × 0.50 mm
F(000) = 1548
Data collection top
Siemens/Bruker P3
diffractometer
Rint = 0.034
Radiation source: fine-focus sealed tubeθmax = 25.1°, θmin = 1.9°
Graphite monochromatorh = 020
ω:2θ scansk = 015
7746 measured reflectionsl = 2322
7461 independent reflections3 standard reflections every 100 reflections
4206 reflections with I > 2σ(I) intensity decay: 19%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.133H atoms treated by a mixture of independent and constrained refinement
S = 0.93 w = 1/[σ2(Fo2) + (0.0736P)2]
where P = (Fo2 + 2Fc2)/3
7468 reflections(Δ/σ)max < 0.001
421 parametersΔρmax = 0.27 e Å3
14 restraintsΔρmin = 0.25 e Å3
Crystal data top
[NiLiCl(C10H23NOP)2(C10H24NOP)]V = 4226.5 (16) Å3
Mr = 714.90Z = 4
Monoclinic, P21/nMo Kα radiation
a = 17.304 (4) ŵ = 0.67 mm1
b = 13.055 (3) ÅT = 300 K
c = 19.444 (4) Å0.50 × 0.50 × 0.50 mm
β = 105.80 (2)°
Data collection top
Siemens/Bruker P3
diffractometer
Rint = 0.034
7746 measured reflections3 standard reflections every 100 reflections
7461 independent reflections intensity decay: 19%
4206 reflections with I > 2σ(I)
Refinement top
R[F2 > 2σ(F2)] = 0.04514 restraints
wR(F2) = 0.133H atoms treated by a mixture of independent and constrained refinement
S = 0.93Δρmax = 0.27 e Å3
7468 reflectionsΔρmin = 0.25 e Å3
421 parameters
Special details top

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. Several C atoms show enlarged displacement parameters of which the ethyl groups C3, C4, and C5, C6 could be described by split atom positions with refined s.o.f. of 0.64 (1), 0.36 (1) and 0.61 (1), 0.39 (1), resp. For reasonable distances and angles several DFIX had to be used for these groups. All H atoms have been calculated and included in a riding mode except atom H3 which has been refined free using a restrained distance.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni0.49195 (3)0.25328 (3)0.24165 (2)0.05097 (16)
Cl0.47929 (7)0.33689 (9)0.33989 (6)0.0859 (4)
P10.53799 (6)0.02397 (7)0.27524 (5)0.0490 (2)
P20.41961 (6)0.29768 (7)0.10564 (5)0.0549 (3)
P30.23061 (6)0.07070 (8)0.06790 (6)0.0614 (3)
O10.46586 (15)0.00754 (17)0.21335 (13)0.0648 (7)
O20.40315 (14)0.20346 (17)0.14574 (11)0.0540 (6)
O30.29921 (15)0.00185 (19)0.08421 (14)0.0703 (8)
N10.56650 (16)0.1428 (2)0.27996 (13)0.0478 (7)
N20.4876 (2)0.3541 (2)0.16545 (16)0.0698 (10)
N30.1617 (3)0.0331 (3)0.1024 (3)0.1026 (14)
H30.125 (2)0.072 (3)0.109 (2)0.102 (18)*
C10.6410 (2)0.1782 (3)0.3313 (2)0.0709 (12)
H1A0.67320.11930.35190.085*
H1B0.62760.21530.36970.085*
C20.6892 (3)0.2466 (4)0.2963 (3)0.1094 (18)
H2A0.73720.26810.33120.131*
H2B0.65780.30550.27660.131*
H2C0.70340.20960.25880.131*
C3A0.5415 (9)0.4385 (8)0.1567 (7)0.118 (5)0.642 (15)
H3A10.52020.47110.11060.142*0.642 (15)
H3A20.59430.41150.15880.142*0.642 (15)
C4A0.5477 (10)0.5163 (7)0.2161 (8)0.156 (7)0.642 (15)
H4A10.58520.56890.21260.187*0.642 (15)
H4A20.56580.48280.26160.187*0.642 (15)
H4A30.49590.54640.21160.187*0.642 (15)
C3B0.5012 (8)0.4663 (5)0.1723 (16)0.095 (7)0.358 (15)
H3B10.47050.49520.20260.114*0.358 (15)
H3B20.48340.49840.12570.114*0.358 (15)
C4B0.5901 (9)0.4866 (12)0.205 (2)0.152 (14)0.358 (15)
H4B10.60050.55860.20270.183*0.358 (15)
H4B20.62060.44960.17840.183*0.358 (15)
H4B30.60540.46430.25370.183*0.358 (15)
C5A0.1334 (8)0.0735 (5)0.1078 (6)0.189 (8)0.613 (13)
H5A10.07810.08050.07960.227*0.613 (13)
H5A20.16600.12140.08980.227*0.613 (13)
C6A0.1400 (16)0.0962 (12)0.1859 (7)0.274 (15)0.613 (13)
H6A10.12290.16530.19040.329*0.613 (13)
H6A20.19480.08830.21360.329*0.613 (13)
H6A30.10660.04960.20300.329*0.613 (13)
C5B0.1808 (7)0.0452 (10)0.1604 (7)0.111 (7)0.387 (13)
H5B10.22950.08160.15990.133*0.387 (13)
H5B20.18910.01230.20650.133*0.387 (13)
C6B0.1108 (12)0.1196 (14)0.1479 (10)0.137 (9)0.387 (13)
H6B10.12250.17140.18440.164*0.387 (13)
H6B20.06310.08330.14960.164*0.387 (13)
H6B30.10250.15120.10190.164*0.387 (13)
C110.6179 (3)0.0630 (3)0.2603 (2)0.0694 (11)
C120.6890 (3)0.0848 (5)0.3255 (3)0.128 (2)
H12A0.71350.02130.34490.153*
H12B0.72770.12640.31130.153*
H12C0.67030.12030.36110.153*
C130.5818 (3)0.1661 (3)0.2326 (3)0.1100 (18)
H13A0.56160.19900.26830.132*
H13B0.62230.20840.22170.132*
H13C0.53860.15610.19010.132*
C140.6485 (4)0.0143 (4)0.2018 (3)0.116 (2)
H14A0.67160.05140.21760.139*
H14B0.60470.00570.15960.139*
H14C0.68850.05770.19110.139*
C150.5083 (2)0.0121 (3)0.3569 (2)0.0655 (11)
C160.5697 (3)0.0130 (5)0.4256 (2)0.136 (3)
H16A0.61800.02500.42850.163*
H16B0.54920.00490.46520.163*
H16C0.58130.08500.42720.163*
C170.4319 (3)0.0477 (4)0.3522 (3)0.1091 (18)
H17A0.39260.03140.30820.131*
H17B0.44330.11980.35360.131*
H17C0.41130.02990.39180.131*
C180.4852 (3)0.1253 (4)0.3570 (3)0.1098 (18)
H18A0.44560.14130.31320.132*
H18B0.46360.13850.39670.132*
H18C0.53200.16690.36120.132*
C210.4559 (3)0.2532 (4)0.0306 (2)0.0837 (13)
C220.5304 (4)0.1899 (6)0.0643 (3)0.169 (3)
H22A0.51670.13570.09230.202*
H22B0.57060.23290.09450.202*
H22C0.55090.16100.02740.202*
C230.3957 (5)0.1824 (6)0.0198 (3)0.178 (3)
H23A0.38000.12880.00740.214*
H23B0.42020.15290.05390.214*
H23C0.34920.22100.04440.214*
C240.4795 (5)0.3367 (5)0.0125 (3)0.160 (3)
H24A0.43340.37800.03420.192*
H24B0.50010.30700.04910.192*
H24C0.52020.37870.01810.192*
C250.3254 (3)0.3713 (3)0.0774 (2)0.0798 (13)
C260.3295 (4)0.4661 (4)0.0329 (4)0.148 (3)
H26A0.34150.44600.01060.178*
H26B0.37070.51110.05950.178*
H26C0.27870.50090.02160.178*
C270.2570 (3)0.3019 (5)0.0350 (4)0.154 (3)
H27A0.26820.28070.00860.184*
H27B0.20730.33920.02400.184*
H27C0.25290.24280.06310.184*
C280.3064 (4)0.4026 (6)0.1448 (3)0.170 (3)
H28A0.30390.34290.17300.204*
H28B0.25550.43720.13340.204*
H28C0.34750.44780.17140.204*
C310.2633 (3)0.1953 (3)0.1091 (3)0.0873 (14)
C320.2002 (3)0.2797 (4)0.0874 (4)0.130 (2)
H32A0.15170.25850.09830.156*
H32B0.21990.34120.11330.156*
H32C0.18920.29240.03710.156*
C330.2831 (5)0.1772 (5)0.1896 (3)0.169 (3)
H33A0.23550.15570.20190.203*
H33B0.32340.12500.20300.203*
H33C0.30280.23960.21430.203*
C340.3399 (3)0.2290 (4)0.0919 (4)0.147 (3)
H34A0.37960.17600.10550.176*
H34B0.32890.24170.04150.176*
H34C0.35960.29050.11770.176*
C350.1871 (4)0.0745 (5)0.0304 (3)0.1093 (19)
C360.1745 (4)0.0353 (5)0.0540 (3)0.177 (4)
H36A0.13720.06690.03200.212*
H36B0.15340.03790.10510.212*
H36C0.22480.07100.04010.212*
C370.1054 (4)0.1287 (6)0.0499 (4)0.197 (4)
H37A0.11240.19900.03510.236*
H37B0.08230.12560.10070.236*
H37C0.07030.09540.02630.236*
C380.2461 (5)0.1216 (7)0.0659 (3)0.196 (4)
H38A0.25530.19190.05150.235*
H38B0.29600.08470.05200.235*
H38C0.22470.11810.11690.235*
Li0.3848 (4)0.0645 (5)0.1458 (3)0.0569 (16)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni0.0534 (3)0.0439 (3)0.0478 (3)0.0026 (2)0.0004 (2)0.0020 (2)
Cl0.0971 (9)0.0803 (8)0.0839 (8)0.0025 (7)0.0307 (7)0.0200 (6)
P10.0493 (6)0.0463 (5)0.0459 (5)0.0046 (5)0.0036 (4)0.0061 (4)
P20.0632 (7)0.0431 (5)0.0506 (5)0.0059 (5)0.0025 (5)0.0088 (4)
P30.0530 (6)0.0479 (6)0.0773 (7)0.0143 (5)0.0078 (5)0.0047 (5)
O10.0670 (17)0.0470 (14)0.0619 (16)0.0042 (13)0.0139 (13)0.0069 (12)
O20.0567 (15)0.0430 (13)0.0532 (14)0.0073 (12)0.0006 (12)0.0094 (11)
O30.0638 (17)0.0599 (16)0.0716 (17)0.0247 (13)0.0080 (14)0.0073 (13)
N10.0439 (17)0.0503 (17)0.0434 (15)0.0035 (13)0.0020 (13)0.0007 (12)
N20.077 (2)0.0510 (19)0.067 (2)0.0239 (17)0.0046 (17)0.0134 (15)
N30.106 (3)0.052 (2)0.168 (4)0.019 (2)0.068 (3)0.020 (3)
C10.055 (2)0.070 (3)0.074 (3)0.005 (2)0.005 (2)0.003 (2)
C20.072 (3)0.121 (4)0.124 (4)0.043 (3)0.007 (3)0.012 (3)
C3A0.128 (12)0.088 (7)0.114 (10)0.050 (8)0.008 (8)0.027 (7)
C4A0.239 (18)0.077 (8)0.120 (9)0.068 (11)0.004 (13)0.006 (8)
C3B0.136 (19)0.037 (8)0.096 (13)0.037 (10)0.004 (14)0.001 (8)
C4B0.106 (15)0.054 (11)0.25 (3)0.023 (11)0.038 (18)0.011 (14)
C5A0.109 (11)0.090 (10)0.38 (3)0.011 (8)0.091 (14)0.012 (12)
C6A0.47 (4)0.143 (16)0.144 (16)0.02 (2)0.020 (19)0.064 (12)
C5B0.091 (12)0.104 (14)0.149 (17)0.008 (10)0.050 (11)0.038 (12)
C6B0.132 (15)0.119 (15)0.149 (18)0.070 (11)0.020 (14)0.080 (14)
C110.079 (3)0.066 (3)0.063 (2)0.016 (2)0.020 (2)0.000 (2)
C120.093 (4)0.151 (6)0.124 (4)0.064 (4)0.004 (3)0.010 (4)
C130.126 (5)0.063 (3)0.142 (5)0.027 (3)0.039 (4)0.009 (3)
C140.155 (5)0.093 (4)0.131 (5)0.034 (4)0.092 (4)0.007 (3)
C150.063 (3)0.068 (3)0.066 (3)0.007 (2)0.020 (2)0.018 (2)
C160.128 (5)0.230 (8)0.050 (3)0.047 (5)0.026 (3)0.003 (4)
C170.114 (4)0.088 (4)0.154 (5)0.020 (3)0.085 (4)0.034 (3)
C180.139 (5)0.079 (3)0.121 (4)0.002 (3)0.051 (4)0.041 (3)
C210.103 (4)0.088 (3)0.064 (3)0.004 (3)0.029 (3)0.011 (3)
C220.176 (7)0.230 (8)0.127 (5)0.104 (7)0.086 (5)0.045 (5)
C230.262 (10)0.183 (7)0.107 (5)0.062 (7)0.079 (6)0.065 (5)
C240.218 (8)0.159 (6)0.142 (5)0.002 (6)0.115 (6)0.053 (5)
C250.082 (3)0.066 (3)0.076 (3)0.016 (2)0.003 (3)0.019 (2)
C260.179 (6)0.089 (4)0.163 (6)0.050 (4)0.025 (5)0.052 (4)
C270.094 (4)0.136 (5)0.186 (7)0.006 (4)0.040 (4)0.017 (5)
C280.144 (6)0.232 (9)0.134 (6)0.121 (6)0.039 (5)0.016 (6)
C310.080 (3)0.061 (3)0.125 (4)0.008 (3)0.035 (3)0.008 (3)
C320.121 (5)0.055 (3)0.234 (7)0.017 (3)0.081 (5)0.001 (4)
C330.246 (9)0.115 (5)0.124 (5)0.010 (5)0.011 (6)0.059 (4)
C340.093 (4)0.098 (4)0.254 (8)0.020 (4)0.055 (5)0.042 (5)
C350.103 (4)0.112 (4)0.087 (4)0.043 (4)0.018 (3)0.009 (3)
C360.188 (7)0.143 (6)0.132 (5)0.033 (6)0.072 (5)0.049 (5)
C370.143 (6)0.215 (8)0.179 (7)0.107 (6)0.048 (5)0.022 (6)
C380.251 (10)0.251 (10)0.098 (5)0.024 (8)0.068 (6)0.039 (6)
Li0.056 (4)0.052 (3)0.054 (3)0.012 (3)0.001 (3)0.008 (3)
Geometric parameters (Å, º) top
Ni—N11.943 (3)N3—C5B1.490 (5)
Ni—N21.967 (3)C1—C21.505 (6)
Ni—O22.168 (2)C3A—C4A1.520 (5)
Ni—Cl2.2620 (12)C3B—C4B1.520 (5)
P1—O11.495 (2)C5A—C6A1.520 (5)
P1—N11.623 (3)C5B—C6B1.520 (5)
P1—C151.858 (4)C11—C141.520 (6)
P1—C111.871 (4)C11—C131.521 (6)
P2—O21.524 (2)C11—C121.533 (6)
P2—N21.592 (3)C15—C161.500 (6)
P2—C211.832 (5)C15—C171.517 (6)
P2—C251.842 (4)C15—C181.530 (6)
P3—O31.484 (2)C21—C241.499 (6)
P3—N31.596 (4)C21—C221.522 (7)
P3—C311.833 (5)C21—C231.531 (7)
P3—C351.854 (5)C25—C281.493 (7)
O1—Li1.801 (6)C25—C261.524 (6)
O2—Li1.842 (6)C25—C271.539 (7)
O3—Li1.824 (6)C31—C341.518 (7)
N1—C11.473 (4)C31—C331.527 (7)
N2—C3A1.483 (5)C31—C321.527 (6)
N2—C3B1.484 (5)C35—C361.502 (8)
N3—H30.853 (14)C35—C381.512 (9)
N3—C5A1.488 (5)C35—C371.533 (7)
N1—Ni—N2132.09 (14)N1—C1—C2111.7 (3)
N1—Ni—O2110.37 (10)N2—C3A—C4A109.0 (5)
N2—Ni—O271.34 (10)N2—C3B—C4B109.1 (5)
N1—Ni—Cl103.96 (9)N3—C5A—C6A108.5 (5)
N2—Ni—Cl108.71 (11)N3—C5B—C6B108.4 (5)
O2—Ni—Cl131.46 (8)C14—C11—C13107.3 (4)
O1—P1—N1110.92 (13)C14—C11—C12109.4 (4)
O1—P1—C15106.67 (18)C13—C11—C12106.8 (4)
N1—P1—C15110.15 (17)C14—C11—P1106.6 (3)
O1—P1—C11106.18 (17)C13—C11—P1110.0 (3)
N1—P1—C11111.26 (18)C12—C11—P1116.4 (3)
C15—P1—C11111.51 (18)C16—C15—C17109.6 (4)
O2—P2—N2101.73 (14)C16—C15—C18109.4 (4)
O2—P2—C21107.68 (18)C17—C15—C18105.9 (4)
N2—P2—C21112.5 (2)C16—C15—P1114.3 (3)
O2—P2—C25107.43 (18)C17—C15—P1104.9 (3)
N2—P2—C25113.2 (2)C18—C15—P1112.2 (3)
C21—P2—C25113.3 (2)C24—C21—C22108.0 (5)
O3—P3—N3111.1 (2)C24—C21—C23108.9 (5)
O3—P3—C31109.85 (19)C22—C21—C23107.2 (5)
N3—P3—C31105.4 (2)C24—C21—P2114.8 (4)
O3—P3—C35108.3 (2)C22—C21—P2105.3 (3)
N3—P3—C35107.5 (3)C23—C21—P2112.3 (4)
C31—P3—C35114.6 (3)C28—C25—C26109.4 (5)
P1—O1—Li147.3 (2)C28—C25—C27108.1 (5)
P2—O2—Li148.4 (2)C26—C25—C27108.7 (4)
P2—O2—Ni90.60 (11)C28—C25—P2105.7 (3)
Li—O2—Ni112.2 (2)C26—C25—P2114.7 (4)
P3—O3—Li152.3 (3)C27—C25—P2110.0 (3)
C1—N1—P1122.3 (2)C34—C31—C33107.8 (5)
C1—N1—Ni113.2 (2)C34—C31—C32109.4 (4)
P1—N1—Ni121.88 (15)C33—C31—C32109.8 (5)
C3A—N2—C3B35.7 (7)C34—C31—P3110.1 (4)
C3A—N2—P2128.5 (6)C33—C31—P3105.5 (4)
C3B—N2—P2126.1 (8)C32—C31—P3114.1 (4)
C3A—N2—Ni133.4 (7)C36—C35—C38107.9 (6)
C3B—N2—Ni128.3 (12)C36—C35—C37108.5 (6)
P2—N2—Ni96.32 (13)C38—C35—C37113.0 (6)
H3—N3—C5A106 (3)C36—C35—P3105.9 (4)
H3—N3—C5B108 (3)C38—C35—P3110.3 (4)
C5A—N3—C5B46.7 (7)C37—C35—P3110.9 (5)
H3—N3—P3124 (3)O1—Li—O3128.7 (4)
C5A—N3—P3128.0 (6)O1—Li—O2107.9 (3)
C5B—N3—P3119.5 (6)O3—Li—O2123.4 (3)

Experimental details

Crystal data
Chemical formula[NiLiCl(C10H23NOP)2(C10H24NOP)]
Mr714.90
Crystal system, space groupMonoclinic, P21/n
Temperature (K)300
a, b, c (Å)17.304 (4), 13.055 (3), 19.444 (4)
β (°) 105.80 (2)
V3)4226.5 (16)
Z4
Radiation typeMo Kα
µ (mm1)0.67
Crystal size (mm)0.50 × 0.50 × 0.50
Data collection
DiffractometerSiemens/Bruker P3
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
7746, 7461, 4206
Rint0.034
(sin θ/λ)max1)0.596
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.045, 0.133, 0.93
No. of reflections7468
No. of parameters421
No. of restraints14
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.27, 0.25

Computer programs: Siemens/Bruker P3 (Siemens, 1989), Siemens/Bruker P3, SHELXTL-Plus (Sheldrick, 1990), SHELXTL-Plus, SHELXL97 (Sheldrick, 1997), SHELXL97.

 

Subscribe to Acta Crystallographica Section C: Structural Chemistry

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. C
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds