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The title tetra­substituted phosphazene, C16H48Cl2N7P3Si4, is formed by the reaction of P3N3Cl6 with hepta­methyl­disilazane, HpMDSA. The compound is the first trans non-geminal tetra­substituted derivative of this class of compounds to be structurally characterized. The molecule lies on a crystallographic twofold rotation axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806055292/sg2112sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806055292/sg2112Isup2.hkl
Contains datablock I

CCDC reference: 638525

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](N-C) = 0.003 Å
  • R factor = 0.038
  • wR factor = 0.097
  • Data-to-parameter ratio = 17.2

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT230_ALERT_2_B Hirshfeld Test Diff for Cl1 - P1 .. 9.04 su
Alert level C PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 3
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: KM-4 Software (Kuma Diffraction, date?); data reduction: KUMA KM-4 Software; program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

trans-2,6-Dichloro-2,4,4,6-tetrakis[methyl(trimethylsilyl)amino]- 1,3,5,2λ5,4λ5,6λ5-triazatriphosphorine top
Crystal data top
C16H48Cl2N7P3Si4F(000) = 1312
Mr = 614.78Dx = 1.215 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71069 Å
a = 17.470 (3) ÅCell parameters from 1418 reflections
b = 11.360 (2) Åθ = 5.8–24.3°
c = 17.270 (3) ŵ = 0.50 mm1
β = 101.21 (3)°T = 120 K
V = 3362.0 (10) Å3Prism, white
Z = 40.25 × 0.20 × 0.20 mm
Data collection top
Kuma KM-4 CCD
diffractometer
2569 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.030
Graphite monochromatorθmax = 25.0°, θmin = 6.2°
Detector resolution: 0.06 mm pixels mm-1h = 2020
ω scansk = 129
13131 measured reflectionsl = 1920
2829 independent reflections
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)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.097H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.049P)2 + 7.9146P]
where P = (Fo2 + 2Fc2)/3
2620 reflections(Δ/σ)max = 0.001
154 parametersΔρmax = 0.54 e Å3
0 restraintsΔρmin = 0.34 e Å3
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cl10.09664 (3)0.50519 (6)0.37040 (3)0.03357 (19)
P10.07751 (3)0.47951 (5)0.25684 (3)0.01812 (17)
N10.07913 (10)0.34082 (17)0.24385 (10)0.0194 (4)
N20.00000.5507 (2)0.25000.0211 (6)
N30.15300 (10)0.54423 (17)0.20083 (11)0.0233 (4)
C10.22923 (13)0.4839 (2)0.19835 (16)0.0321 (6)
H1A0.21990.40210.21560.048*
H1B0.25950.48540.14430.048*
H1C0.25830.52450.23350.048*
Si10.14974 (4)0.69097 (6)0.16436 (4)0.0316 (2)
C20.08887 (17)0.6989 (3)0.08648 (19)0.0471 (8)
H2A0.03560.67290.10860.071*
H2B0.08760.78030.06780.071*
H2C0.11150.64780.04220.071*
C30.11419 (17)0.7940 (3)0.2480 (2)0.0510 (8)
H3A0.14790.78780.28710.077*
H3B0.11550.87490.22810.077*
H3C0.06060.77330.27280.077*
C40.25285 (16)0.7329 (3)0.11920 (19)0.0448 (7)
H4A0.27370.67750.07680.067*
H4B0.25360.81270.09750.067*
H4C0.28510.73040.15970.067*
P20.00000.26464 (7)0.25000.0171 (2)
N40.01910 (11)0.17768 (17)0.17102 (10)0.0225 (4)
C50.04337 (16)0.0932 (2)0.16205 (16)0.0373 (6)
H5A0.06460.11410.11540.056*
H5B0.02170.01350.15580.056*
H5C0.08510.09640.20900.056*
Si20.10238 (4)0.19488 (6)0.09482 (4)0.0265 (2)
C60.19341 (16)0.1542 (3)0.13018 (18)0.0458 (7)
H6A0.19450.06890.13840.069*
H6B0.23900.17760.09070.069*
H6C0.19440.19470.18010.069*
C70.0912 (2)0.0879 (3)0.01451 (17)0.0534 (9)
H7A0.04420.10730.00580.080*
H7B0.13690.09290.02840.080*
H7C0.08670.00770.03600.080*
C80.10831 (17)0.3446 (3)0.04987 (15)0.0377 (6)
H8A0.12760.40060.08480.057*
H8B0.14410.34300.00140.057*
H8C0.05640.36900.04260.057*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cl10.0323 (3)0.0419 (4)0.0289 (3)0.0002 (3)0.0118 (2)0.0091 (3)
P10.0159 (3)0.0182 (3)0.0206 (3)0.0005 (2)0.0045 (2)0.0017 (2)
N10.0169 (9)0.0199 (11)0.0214 (9)0.0021 (7)0.0038 (7)0.0000 (8)
N20.0183 (13)0.0167 (14)0.0286 (14)0.0000.0054 (10)0.000
N30.0162 (9)0.0212 (11)0.0319 (10)0.0010 (8)0.0030 (8)0.0002 (8)
C10.0179 (11)0.0309 (15)0.0465 (15)0.0004 (10)0.0040 (10)0.0009 (11)
Si10.0229 (4)0.0203 (4)0.0491 (4)0.0046 (3)0.0008 (3)0.0053 (3)
C20.0394 (15)0.0419 (18)0.0597 (19)0.0041 (13)0.0093 (13)0.0270 (15)
C30.0336 (15)0.0282 (16)0.085 (2)0.0058 (12)0.0042 (15)0.0144 (15)
C40.0324 (14)0.0346 (17)0.0628 (19)0.0098 (12)0.0019 (13)0.0089 (14)
P20.0201 (4)0.0153 (4)0.0155 (4)0.0000.0027 (3)0.000
N40.0263 (10)0.0202 (11)0.0193 (9)0.0027 (8)0.0006 (8)0.0036 (7)
C50.0399 (14)0.0351 (16)0.0335 (14)0.0114 (12)0.0015 (11)0.0138 (11)
Si20.0300 (4)0.0260 (4)0.0201 (3)0.0005 (3)0.0032 (3)0.0037 (3)
C60.0323 (14)0.0506 (19)0.0501 (17)0.0153 (13)0.0029 (12)0.0007 (14)
C70.064 (2)0.053 (2)0.0338 (15)0.0070 (16)0.0121 (14)0.0216 (14)
C80.0450 (15)0.0399 (16)0.0251 (13)0.0056 (13)0.0009 (11)0.0058 (11)
Geometric parameters (Å, º) top
Cl1—P12.0730 (9)C4—H4C0.9800
P1—N11.591 (2)P2—N1i1.6168 (18)
P1—N21.6010 (15)P2—N41.6645 (18)
P1—N31.6491 (19)P2—N4i1.6645 (18)
N1—P21.6168 (18)N4—C51.484 (3)
N2—P1i1.6010 (15)N4—Si21.773 (2)
N3—C11.491 (3)C5—H5A0.9800
N3—Si11.787 (2)C5—H5B0.9800
C1—H1A0.9800C5—H5C0.9800
C1—H1B0.9800Si2—C81.864 (3)
C1—H1C0.9800Si2—C61.869 (3)
Si1—C31.869 (3)Si2—C71.883 (3)
Si1—C21.872 (3)C6—H6A0.9800
Si1—C41.880 (3)C6—H6B0.9800
C2—H2A0.9800C6—H6C0.9800
C2—H2B0.9800C7—H7A0.9800
C2—H2C0.9800C7—H7B0.9800
C3—H3A0.9800C7—H7C0.9800
C3—H3B0.9800C8—H8A0.9800
C3—H3C0.9800C8—H8B0.9800
C4—H4A0.9800C8—H8C0.9800
C4—H4B0.9800
N1—P1—N2118.79 (11)H4B—C4—H4C109.5
N1—P1—N3111.62 (10)N1—P2—N1i115.28 (14)
N2—P1—N3108.85 (10)N1—P2—N4103.37 (9)
N1—P1—Cl1105.73 (7)N1i—P2—N4113.84 (9)
N2—P1—Cl1107.04 (5)N1—P2—N4i113.84 (9)
N3—P1—Cl1103.57 (8)N1i—P2—N4i103.37 (9)
P1—N1—P2121.96 (11)N4—P2—N4i107.19 (14)
P1—N2—P1i119.36 (17)C5—N4—P2115.78 (15)
C1—N3—P1114.83 (16)C5—N4—Si2120.53 (15)
C1—N3—Si1120.55 (15)P2—N4—Si2123.22 (11)
P1—N3—Si1123.09 (11)N4—C5—H5A109.5
N3—C1—H1A109.5N4—C5—H5B109.5
N3—C1—H1B109.5H5A—C5—H5B109.5
H1A—C1—H1B109.5N4—C5—H5C109.5
N3—C1—H1C109.5H5A—C5—H5C109.5
H1A—C1—H1C109.5H5B—C5—H5C109.5
H1B—C1—H1C109.5N4—Si2—C8112.38 (11)
N3—Si1—C3109.89 (13)N4—Si2—C6110.97 (11)
N3—Si1—C2111.10 (12)C8—Si2—C6112.33 (14)
C3—Si1—C2112.04 (16)N4—Si2—C7106.74 (12)
N3—Si1—C4106.80 (12)C8—Si2—C7106.73 (15)
C3—Si1—C4108.03 (14)C6—Si2—C7107.31 (16)
C2—Si1—C4108.79 (14)Si2—C6—H6A109.5
Si1—C2—H2A109.5Si2—C6—H6B109.5
Si1—C2—H2B109.5H6A—C6—H6B109.5
H2A—C2—H2B109.5Si2—C6—H6C109.5
Si1—C2—H2C109.5H6A—C6—H6C109.5
H2A—C2—H2C109.5H6B—C6—H6C109.5
H2B—C2—H2C109.5Si2—C7—H7A109.5
Si1—C3—H3A109.5Si2—C7—H7B109.5
Si1—C3—H3B109.5H7A—C7—H7B109.5
H3A—C3—H3B109.5Si2—C7—H7C109.5
Si1—C3—H3C109.5H7A—C7—H7C109.5
H3A—C3—H3C109.5H7B—C7—H7C109.5
H3B—C3—H3C109.5Si2—C8—H8A109.5
Si1—C4—H4A109.5Si2—C8—H8B109.5
Si1—C4—H4B109.5H8A—C8—H8B109.5
H4A—C4—H4B109.5Si2—C8—H8C109.5
Si1—C4—H4C109.5H8A—C8—H8C109.5
H4A—C4—H4C109.5H8B—C8—H8C109.5
Symmetry code: (i) x, y, z+1/2.
 

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