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
CCDC reference: 638525
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean (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
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]-
1,3,5,2
λ5,4
λ5,6
λ5-triazatriphosphorine
top
Crystal data top
C16H48Cl2N7P3Si4 | F(000) = 1312 |
Mr = 614.78 | Dx = 1.215 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71069 Å |
a = 17.470 (3) Å | Cell parameters from 1418 reflections |
b = 11.360 (2) Å | θ = 5.8–24.3° |
c = 17.270 (3) Å | µ = 0.50 mm−1 |
β = 101.21 (3)° | T = 120 K |
V = 3362.0 (10) Å3 | Prism, white |
Z = 4 | 0.25 × 0.20 × 0.20 mm |
Data collection top
Kuma KM-4 CCD diffractometer | 2569 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.030 |
Graphite monochromator | θmax = 25.0°, θmin = 6.2° |
Detector resolution: 0.06 mm pixels mm-1 | h = −20→20 |
ω scans | k = −12→9 |
13131 measured reflections | l = −19→20 |
2829 independent reflections | |
Refinement top
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.097 | H-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 parameters | Δρmax = 0.54 e Å−3 |
0 restraints | Δρmin = −0.34 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Cl1 | −0.09664 (3) | 0.50519 (6) | 0.37040 (3) | 0.03357 (19) | |
P1 | −0.07751 (3) | 0.47951 (5) | 0.25684 (3) | 0.01812 (17) | |
N1 | −0.07913 (10) | 0.34082 (17) | 0.24385 (10) | 0.0194 (4) | |
N2 | 0.0000 | 0.5507 (2) | 0.2500 | 0.0211 (6) | |
N3 | −0.15300 (10) | 0.54423 (17) | 0.20083 (11) | 0.0233 (4) | |
C1 | −0.22923 (13) | 0.4839 (2) | 0.19835 (16) | 0.0321 (6) | |
H1A | −0.2199 | 0.4021 | 0.2156 | 0.048* | |
H1B | −0.2595 | 0.4854 | 0.1443 | 0.048* | |
H1C | −0.2583 | 0.5245 | 0.2335 | 0.048* | |
Si1 | −0.14974 (4) | 0.69097 (6) | 0.16436 (4) | 0.0316 (2) | |
C2 | −0.08887 (17) | 0.6989 (3) | 0.08648 (19) | 0.0471 (8) | |
H2A | −0.0356 | 0.6729 | 0.1086 | 0.071* | |
H2B | −0.0876 | 0.7803 | 0.0678 | 0.071* | |
H2C | −0.1115 | 0.6478 | 0.0422 | 0.071* | |
C3 | −0.11419 (17) | 0.7940 (3) | 0.2480 (2) | 0.0510 (8) | |
H3A | −0.1479 | 0.7878 | 0.2871 | 0.077* | |
H3B | −0.1155 | 0.8749 | 0.2281 | 0.077* | |
H3C | −0.0606 | 0.7733 | 0.2728 | 0.077* | |
C4 | −0.25285 (16) | 0.7329 (3) | 0.11920 (19) | 0.0448 (7) | |
H4A | −0.2737 | 0.6775 | 0.0768 | 0.067* | |
H4B | −0.2536 | 0.8127 | 0.0975 | 0.067* | |
H4C | −0.2851 | 0.7304 | 0.1597 | 0.067* | |
P2 | 0.0000 | 0.26464 (7) | 0.2500 | 0.0171 (2) | |
N4 | −0.01910 (11) | 0.17768 (17) | 0.17102 (10) | 0.0225 (4) | |
C5 | 0.04337 (16) | 0.0932 (2) | 0.16205 (16) | 0.0373 (6) | |
H5A | 0.0646 | 0.1141 | 0.1154 | 0.056* | |
H5B | 0.0217 | 0.0135 | 0.1558 | 0.056* | |
H5C | 0.0851 | 0.0964 | 0.2090 | 0.056* | |
Si2 | −0.10238 (4) | 0.19488 (6) | 0.09482 (4) | 0.0265 (2) | |
C6 | −0.19341 (16) | 0.1542 (3) | 0.13018 (18) | 0.0458 (7) | |
H6A | −0.1945 | 0.0689 | 0.1384 | 0.069* | |
H6B | −0.2390 | 0.1776 | 0.0907 | 0.069* | |
H6C | −0.1944 | 0.1947 | 0.1801 | 0.069* | |
C7 | −0.0912 (2) | 0.0879 (3) | 0.01451 (17) | 0.0534 (9) | |
H7A | −0.0442 | 0.1073 | −0.0058 | 0.080* | |
H7B | −0.1369 | 0.0929 | −0.0284 | 0.080* | |
H7C | −0.0867 | 0.0077 | 0.0360 | 0.080* | |
C8 | −0.10831 (17) | 0.3446 (3) | 0.04987 (15) | 0.0377 (6) | |
H8A | −0.1276 | 0.4006 | 0.0848 | 0.057* | |
H8B | −0.1441 | 0.3430 | −0.0014 | 0.057* | |
H8C | −0.0564 | 0.3690 | 0.0426 | 0.057* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cl1 | 0.0323 (3) | 0.0419 (4) | 0.0289 (3) | −0.0002 (3) | 0.0118 (2) | −0.0091 (3) |
P1 | 0.0159 (3) | 0.0182 (3) | 0.0206 (3) | 0.0005 (2) | 0.0045 (2) | −0.0017 (2) |
N1 | 0.0169 (9) | 0.0199 (11) | 0.0214 (9) | −0.0021 (7) | 0.0038 (7) | 0.0000 (8) |
N2 | 0.0183 (13) | 0.0167 (14) | 0.0286 (14) | 0.000 | 0.0054 (10) | 0.000 |
N3 | 0.0162 (9) | 0.0212 (11) | 0.0319 (10) | 0.0010 (8) | 0.0030 (8) | 0.0002 (8) |
C1 | 0.0179 (11) | 0.0309 (15) | 0.0465 (15) | −0.0004 (10) | 0.0040 (10) | −0.0009 (11) |
Si1 | 0.0229 (4) | 0.0203 (4) | 0.0491 (4) | 0.0046 (3) | 0.0008 (3) | 0.0053 (3) |
C2 | 0.0394 (15) | 0.0419 (18) | 0.0597 (19) | 0.0041 (13) | 0.0093 (13) | 0.0270 (15) |
C3 | 0.0336 (15) | 0.0282 (16) | 0.085 (2) | 0.0058 (12) | −0.0042 (15) | −0.0144 (15) |
C4 | 0.0324 (14) | 0.0346 (17) | 0.0628 (19) | 0.0098 (12) | −0.0019 (13) | 0.0089 (14) |
P2 | 0.0201 (4) | 0.0153 (4) | 0.0155 (4) | 0.000 | 0.0027 (3) | 0.000 |
N4 | 0.0263 (10) | 0.0202 (11) | 0.0193 (9) | 0.0027 (8) | 0.0006 (8) | −0.0036 (7) |
C5 | 0.0399 (14) | 0.0351 (16) | 0.0335 (14) | 0.0114 (12) | −0.0015 (11) | −0.0138 (11) |
Si2 | 0.0300 (4) | 0.0260 (4) | 0.0201 (3) | −0.0005 (3) | −0.0032 (3) | −0.0037 (3) |
C6 | 0.0323 (14) | 0.0506 (19) | 0.0501 (17) | −0.0153 (13) | −0.0029 (12) | 0.0007 (14) |
C7 | 0.064 (2) | 0.053 (2) | 0.0338 (15) | 0.0070 (16) | −0.0121 (14) | −0.0216 (14) |
C8 | 0.0450 (15) | 0.0399 (16) | 0.0251 (13) | 0.0056 (13) | −0.0009 (11) | 0.0058 (11) |
Geometric parameters (Å, º) top
Cl1—P1 | 2.0730 (9) | C4—H4C | 0.9800 |
P1—N1 | 1.591 (2) | P2—N1i | 1.6168 (18) |
P1—N2 | 1.6010 (15) | P2—N4 | 1.6645 (18) |
P1—N3 | 1.6491 (19) | P2—N4i | 1.6645 (18) |
N1—P2 | 1.6168 (18) | N4—C5 | 1.484 (3) |
N2—P1i | 1.6010 (15) | N4—Si2 | 1.773 (2) |
N3—C1 | 1.491 (3) | C5—H5A | 0.9800 |
N3—Si1 | 1.787 (2) | C5—H5B | 0.9800 |
C1—H1A | 0.9800 | C5—H5C | 0.9800 |
C1—H1B | 0.9800 | Si2—C8 | 1.864 (3) |
C1—H1C | 0.9800 | Si2—C6 | 1.869 (3) |
Si1—C3 | 1.869 (3) | Si2—C7 | 1.883 (3) |
Si1—C2 | 1.872 (3) | C6—H6A | 0.9800 |
Si1—C4 | 1.880 (3) | C6—H6B | 0.9800 |
C2—H2A | 0.9800 | C6—H6C | 0.9800 |
C2—H2B | 0.9800 | C7—H7A | 0.9800 |
C2—H2C | 0.9800 | C7—H7B | 0.9800 |
C3—H3A | 0.9800 | C7—H7C | 0.9800 |
C3—H3B | 0.9800 | C8—H8A | 0.9800 |
C3—H3C | 0.9800 | C8—H8B | 0.9800 |
C4—H4A | 0.9800 | C8—H8C | 0.9800 |
C4—H4B | 0.9800 | | |
| | | |
N1—P1—N2 | 118.79 (11) | H4B—C4—H4C | 109.5 |
N1—P1—N3 | 111.62 (10) | N1—P2—N1i | 115.28 (14) |
N2—P1—N3 | 108.85 (10) | N1—P2—N4 | 103.37 (9) |
N1—P1—Cl1 | 105.73 (7) | N1i—P2—N4 | 113.84 (9) |
N2—P1—Cl1 | 107.04 (5) | N1—P2—N4i | 113.84 (9) |
N3—P1—Cl1 | 103.57 (8) | N1i—P2—N4i | 103.37 (9) |
P1—N1—P2 | 121.96 (11) | N4—P2—N4i | 107.19 (14) |
P1—N2—P1i | 119.36 (17) | C5—N4—P2 | 115.78 (15) |
C1—N3—P1 | 114.83 (16) | C5—N4—Si2 | 120.53 (15) |
C1—N3—Si1 | 120.55 (15) | P2—N4—Si2 | 123.22 (11) |
P1—N3—Si1 | 123.09 (11) | N4—C5—H5A | 109.5 |
N3—C1—H1A | 109.5 | N4—C5—H5B | 109.5 |
N3—C1—H1B | 109.5 | H5A—C5—H5B | 109.5 |
H1A—C1—H1B | 109.5 | N4—C5—H5C | 109.5 |
N3—C1—H1C | 109.5 | H5A—C5—H5C | 109.5 |
H1A—C1—H1C | 109.5 | H5B—C5—H5C | 109.5 |
H1B—C1—H1C | 109.5 | N4—Si2—C8 | 112.38 (11) |
N3—Si1—C3 | 109.89 (13) | N4—Si2—C6 | 110.97 (11) |
N3—Si1—C2 | 111.10 (12) | C8—Si2—C6 | 112.33 (14) |
C3—Si1—C2 | 112.04 (16) | N4—Si2—C7 | 106.74 (12) |
N3—Si1—C4 | 106.80 (12) | C8—Si2—C7 | 106.73 (15) |
C3—Si1—C4 | 108.03 (14) | C6—Si2—C7 | 107.31 (16) |
C2—Si1—C4 | 108.79 (14) | Si2—C6—H6A | 109.5 |
Si1—C2—H2A | 109.5 | Si2—C6—H6B | 109.5 |
Si1—C2—H2B | 109.5 | H6A—C6—H6B | 109.5 |
H2A—C2—H2B | 109.5 | Si2—C6—H6C | 109.5 |
Si1—C2—H2C | 109.5 | H6A—C6—H6C | 109.5 |
H2A—C2—H2C | 109.5 | H6B—C6—H6C | 109.5 |
H2B—C2—H2C | 109.5 | Si2—C7—H7A | 109.5 |
Si1—C3—H3A | 109.5 | Si2—C7—H7B | 109.5 |
Si1—C3—H3B | 109.5 | H7A—C7—H7B | 109.5 |
H3A—C3—H3B | 109.5 | Si2—C7—H7C | 109.5 |
Si1—C3—H3C | 109.5 | H7A—C7—H7C | 109.5 |
H3A—C3—H3C | 109.5 | H7B—C7—H7C | 109.5 |
H3B—C3—H3C | 109.5 | Si2—C8—H8A | 109.5 |
Si1—C4—H4A | 109.5 | Si2—C8—H8B | 109.5 |
Si1—C4—H4B | 109.5 | H8A—C8—H8B | 109.5 |
H4A—C4—H4B | 109.5 | Si2—C8—H8C | 109.5 |
Si1—C4—H4C | 109.5 | H8A—C8—H8C | 109.5 |
H4A—C4—H4C | 109.5 | H8B—C8—H8C | 109.5 |
Symmetry code: (i) −x, y, −z+1/2. |