Tetra­methyl­ammonium di­chloro­tri­phenyl­plumbate

The title compound, an unexpected reaction product formulated [NMe₄]⁺[Cl₂Ph₃Pb]^- or (C₄H₁₂N)[PbCl₂(C₆H₅)₃], is isostructural with the corresponding tin compound as reported by Ng [Acta Cryst. (1995), C51, 1124-1125]. Both cation and anion occupy special positions on the twofold axes.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C) = 0.011 Å
• R factor = 0.031
• wR factor = 0.079
• Data-to-parameter ratio = 18.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



ABSTM_02  Alert C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
          Tmin and Tmax reported:      0.344     0.625
          Tmin and Tmax expected:      0.221     0.450
          RR =      1.119
          Please check that your absorption correction is appropriate.

PLAT_213  Alert C Atom  C10    has ADP max/min Ratio ...........       3.20

General Notes



ABSTM_02  When printed, the submitted absorption T values will be replaced
          by the scaled T values. Since the ratio of scaled T's is
          identical to the ratio of reported T values, the scaling does
          not imply a change to the absorption corrections used in the
          study.
          Ratio of Tmax expected/reported      0.720
          Tmax scaled      0.450 Tmin scaled      0.248

REFLT_03
         From the CIF: _diffrn_reflns_theta_max           27.50
         From the CIF: _reflns_number_total               2200
         Count of symmetry unique reflns         1336
         Completeness (_total/calc)            164.67%
         TEST3: Check Friedels for noncentro structure
         Estimate of Friedel pairs measured       864
         Fraction of Friedel pairs measured     0.647
         Are heavy atom types Z>Si present          yes
          Please check that the estimate of the number of Friedel pairs is
          correct. If it is not, please give the correct count in the
          _publ_section_exptl_refinement section of the submitted CIF.


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 2 Alert Level C = Please check

---

Computing details

Data collection: DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998); cell refinement: DENZO and COLLECT; data reduction: DENZO and COLLECT; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Tetramethylammonium dichlorotriphenylplumbate

Crystal data

(C4H12N)[PbCl2(C6H5)3]	F(000) = 564
Mr = 583.54	Dx = 1.777 Mg m^−3
Monoclinic, I2	Mo Kα radiation, λ = 0.71073 Å
a = 10.3759 (3) Å	Cell parameters from 3028 reflections
b = 9.7074 (3) Å	θ = 2.9–27.5°
c = 10.8400 (3) Å	µ = 7.98 mm^−1
β = 92.432 (1)°	T = 100 K
V = 1090.85 (6) Å^3	Block, red
Z = 2	0.20 × 0.20 × 0.10 mm

Data collection

Enraf Nonius KappaCCD area-detector diffractometer	2200 independent reflections
Radiation source: Enraf Nonius FR591 rotating-anode	2198 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.041
Detector resolution: 9.091 pixels mm^-1	θmax = 27.5°, θmin = 3.8°
φ and ω scans to fill the Ewald sphere	h = −13→13
Absorption correction: multi-scan (SORTAV; Blessing, 1995, 1997)	k = −11→12
Tmin = 0.344, Tmax = 0.625	l = −14→13
3885 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.031	H-atom parameters constrained
wR(F^2) = 0.079	w = 1/[σ^2(Fo^2) + (0.0524P)^2 + 2.6404P] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max < 0.001
2200 reflections	Δρmax = 3.21 e Å^−3
119 parameters	Δρmin = −4.68 e Å^−3
1 restraint	Absolute structure: (Flack, 1983). 884 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.022 (12)

Special details

Experimental. Lattice absences excluded from the. hkl file at the time of its creation.

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.

All non-H refined anisotropically except C4 which was refined isotropically to suppress persistent non-positive definite behaviour subsequent to the placement of H4. H in calculated positions and refined with a riding model.

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

	x	y	z	Uiso*/Ueq
Pb1	0.5000	0.4964	0.5000	0.00950 (11)
Cl1	0.25618 (13)	0.5062 (5)	0.39506 (13)	0.0136 (4)
C1	0.5000	0.2682 (10)	0.5000	0.0100 (18)
C2	0.5743 (7)	0.1958 (8)	0.5884 (6)	0.0129 (13)
H2	0.6264	0.2445	0.6480	0.015*
C3	0.5724 (7)	0.0536 (9)	0.5895 (7)	0.0153 (14)
H3	0.6207	0.0046	0.6517	0.018*
C4	0.5000	−0.0179 (16)	0.5000	0.017 (2)*
H4	0.5000	−0.1157	0.5000	0.020*
C5	0.5661 (7)	0.6038 (8)	0.3354 (6)	0.0123 (13)
C6	0.4918 (7)	0.7061 (7)	0.2786 (6)	0.0115 (13)
H6	0.4112	0.7311	0.3106	0.014*
C7	0.5365 (8)	0.7731 (8)	0.1727 (7)	0.0161 (15)
H7	0.4879	0.8460	0.1353	0.019*
C8	0.6510 (8)	0.7322 (9)	0.1240 (7)	0.0165 (15)
H8	0.6805	0.7761	0.0521	0.020*
C9	0.7239 (7)	0.6265 (9)	0.1798 (7)	0.0155 (15)
H9	0.8023	0.5984	0.1452	0.019*
C10	0.6826 (7)	0.5625 (8)	0.2855 (6)	0.0123 (13)
H10	0.7327	0.4913	0.3238	0.015*
N1	0.0000	0.8165 (10)	0.5000	0.0175 (18)
C11	0.0687 (10)	0.7292 (11)	0.5931 (8)	0.029 (2)
H11A	0.0064	0.6715	0.6347	0.043*
H11B	0.1145	0.7879	0.6541	0.043*
H11C	0.1308	0.6704	0.5524	0.043*
C12	0.0927 (11)	0.9040 (11)	0.4348 (9)	0.037 (2)
H12A	0.1536	0.8452	0.3925	0.055*
H12B	0.1401	0.9626	0.4948	0.055*
H12C	0.0457	0.9620	0.3742	0.055*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1	0.00869 (14)	0.01444 (16)	0.00520 (14)	0.000	−0.00173 (9)	0.000
Cl1	0.0087 (5)	0.0218 (11)	0.0100 (6)	0.0006 (13)	−0.0047 (4)	0.0023 (14)
C1	0.013 (4)	0.012 (5)	0.005 (4)	0.000	−0.001 (3)	0.000
C2	0.012 (3)	0.016 (4)	0.011 (3)	0.001 (3)	−0.001 (2)	−0.001 (3)
C3	0.012 (3)	0.024 (3)	0.009 (3)	0.003 (3)	−0.003 (3)	0.007 (3)
C5	0.013 (3)	0.018 (4)	0.006 (3)	−0.004 (3)	−0.002 (2)	−0.003 (2)
C6	0.016 (3)	0.008 (3)	0.010 (3)	0.001 (3)	0.000 (3)	0.001 (2)
C7	0.021 (4)	0.014 (4)	0.012 (4)	−0.002 (3)	−0.007 (3)	0.004 (3)
C8	0.017 (4)	0.026 (4)	0.006 (3)	−0.007 (3)	−0.002 (3)	0.003 (3)
C9	0.010 (3)	0.027 (4)	0.009 (3)	−0.004 (3)	−0.002 (3)	−0.005 (3)
C10	0.012 (3)	0.015 (3)	0.009 (3)	−0.003 (3)	−0.008 (3)	0.000 (3)
N1	0.020 (4)	0.018 (5)	0.013 (4)	0.000	−0.008 (3)	0.000
C11	0.036 (5)	0.038 (5)	0.011 (4)	0.021 (4)	−0.006 (4)	0.004 (4)
C12	0.045 (6)	0.033 (5)	0.031 (5)	−0.024 (5)	−0.009 (4)	0.004 (4)

Geometric parameters (Å, º)

Pb1—C5^i	2.201 (7)	C7—C8	1.378 (12)
Pb1—C5	2.201 (7)	C7—H7	0.9500
Pb1—C1	2.215 (10)	C8—C9	1.397 (12)
Pb1—Cl1^i	2.7312 (14)	C8—H8	0.9500
Pb1—Cl1	2.7312 (14)	C9—C10	1.388 (10)
C1—C2^i	1.394 (9)	C9—H9	0.9500
C1—C2	1.394 (9)	C10—H10	0.9500
C2—C3	1.381 (12)	N1—C11^ii	1.478 (10)
C2—H2	0.9500	N1—C11	1.478 (10)
C3—C4	1.387 (11)	N1—C12	1.485 (11)
C3—H3	0.9500	N1—C12^ii	1.485 (11)
C4—C3^i	1.387 (11)	C11—H11A	0.9800
C4—H4	0.9500	C11—H11B	0.9800
C5—C6	1.386 (10)	C11—H11C	0.9800
C5—C10	1.403 (10)	C12—H12A	0.9800
C6—C7	1.415 (10)	C12—H12B	0.9800
C6—H6	0.9500	C12—H12C	0.9800
C5^i—Pb1—C5	123.5 (4)	C8—C7—H7	120.1
C5^i—Pb1—C1	118.27 (19)	C6—C7—H7	120.1
C5—Pb1—C1	118.27 (19)	C7—C8—C9	120.4 (7)
C5^i—Pb1—Cl1^i	87.8 (2)	C7—C8—H8	119.8
C5—Pb1—Cl1^i	90.3 (2)	C9—C8—H8	119.8
C1—Pb1—Cl1^i	92.01 (10)	C10—C9—C8	120.4 (7)
C5^i—Pb1—Cl1	90.3 (2)	C10—C9—H9	119.8
C5—Pb1—Cl1	87.8 (2)	C8—C9—H9	119.8
C1—Pb1—Cl1	92.01 (10)	C9—C10—C5	119.5 (7)
Cl1^i—Pb1—Cl1	176.0 (2)	C9—C10—H10	120.3
C2^i—C1—C2	119.5 (9)	C5—C10—H10	120.3
C2^i—C1—Pb1	120.3 (5)	C11^ii—N1—C11	110.0 (10)
C2—C1—Pb1	120.3 (5)	C11^ii—N1—C12	107.9 (5)
C3—C2—C1	120.1 (7)	C11—N1—C12	110.5 (6)
C3—C2—H2	119.9	C11^ii—N1—C12^ii	110.5 (6)
C1—C2—H2	119.9	C11—N1—C12^ii	107.9 (5)
C2—C3—C4	120.1 (8)	C12—N1—C12^ii	110.2 (11)
C2—C3—H3	120.0	N1—C11—H11A	109.5
C4—C3—H3	120.0	N1—C11—H11B	109.5
C3—C4—C3^i	120.0 (13)	H11A—C11—H11B	109.5
C3—C4—H4	120.0	N1—C11—H11C	109.5
C3^i—C4—H4	120.0	H11A—C11—H11C	109.5
C6—C5—C10	120.4 (6)	H11B—C11—H11C	109.5
C6—C5—Pb1	120.9 (5)	N1—C12—H12A	109.5
C10—C5—Pb1	118.7 (5)	N1—C12—H12B	109.5
C5—C6—C7	119.6 (7)	H12A—C12—H12B	109.5
C5—C6—H6	120.2	N1—C12—H12C	109.5
C7—C6—H6	120.2	H12A—C12—H12C	109.5
C8—C7—C6	119.7 (7)	H12B—C12—H12C	109.5
C5^i—Pb1—C1—C2^i	119.5 (4)	Cl1^i—Pb1—C5—C6	−138.7 (6)
C5—Pb1—C1—C2^i	−60.5 (4)	Cl1—Pb1—C5—C6	37.7 (6)
Cl1^i—Pb1—C1—C2^i	−151.9 (3)	C5^i—Pb1—C5—C10	131.6 (6)
Cl1—Pb1—C1—C2^i	28.1 (3)	C1—Pb1—C5—C10	−48.4 (6)
C5^i—Pb1—C1—C2	−60.5 (4)	Cl1^i—Pb1—C5—C10	44.1 (5)
C5—Pb1—C1—C2	119.5 (4)	Cl1—Pb1—C5—C10	−139.4 (5)
Cl1^i—Pb1—C1—C2	28.1 (3)	C10—C5—C6—C7	−2.7 (11)
Cl1—Pb1—C1—C2	−151.9 (3)	Pb1—C5—C6—C7	−179.8 (5)
C2^i—C1—C2—C3	−1.1 (5)	C5—C6—C7—C8	2.6 (11)
Pb1—C1—C2—C3	178.9 (5)	C6—C7—C8—C9	−1.0 (12)
C1—C2—C3—C4	2.3 (9)	C7—C8—C9—C10	−0.6 (12)
C2—C3—C4—C3^i	−1.1 (5)	C8—C9—C10—C5	0.6 (11)
C5^i—Pb1—C5—C6	−51.2 (5)	C6—C5—C10—C9	1.1 (10)
C1—Pb1—C5—C6	128.8 (5)	Pb1—C5—C10—C9	178.2 (5)

Symmetry codes: (i) −x+1, y, −z+1; (ii) −x, y, −z+1.