RbPbPS₄

Rubidium lead phospho­rus tetra­sulfide, RbPbPS₄, possesses the CsSmGeS₄ structure type, crystallizing in space group P2₁2₁2₁ of the orthorhombic system. The structure consists of two-dimensional [PbPS₄] layers built from PbS₇ monocapped trigonal prisms and PS₄ tetrahedra. The layers are separated by Rb atoms.

Key indicators

• Single-crystal X-ray study
• T = 153 K
• Mean [sigma](S-P) = 0.002 Å
• R factor = 0.020
• wR factor = 0.049
• Data-to-parameter ratio = 27.8

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.96

Alert level C
STRVA01_ALERT_4_C           Flack test results are ambiguous.
           From the CIF: _refine_ls_abs_structure_Flack    0.550
           From the CIF: _refine_ls_abs_structure_Flack_su    0.007
PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero .......       0.55
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?

Alert level G
ABSTM02_ALERT_3_G  The ratio of expected to reported Tmax/Tmin(RR) is > 2.00
            Tmin and Tmax reported:      0.047     0.603
            Tmin and Tmax expected:      0.010     0.613
            RR =      4.708
            Please check that your absorption correction is appropriate.
REFLT03_ALERT_4_G 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.
           From the CIF: _diffrn_reflns_theta_max           28.82
           From the CIF: _reflns_number_total               1807
           Count of symmetry unique reflns         1153
           Completeness (_total/calc)            156.72%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured       654
           Fraction of Friedel pairs measured     0.567
           Are heavy atom types Z>Si present          yes

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   3 ALERT level C = Check and explain
   2 ALERT level G = General alerts; check

   1 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
   2 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 2003); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Sheldrick, 2003); program(s) used to refine structure: SHELXTL; molecular graphics: XP in SHELXTL; software used to prepare material for publication: SHELXTL.

Rubidium lead phosphorus tetrasulfide

Crystal data

RbPbPS4	F(000) = 792
Mr = 451.87	Dx = 4.053 Mg m^−3
Orthorhombic, P212121	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2ab	Cell parameters from 7200 reflections
a = 6.3987 (7) Å	θ = 2.4–28.8°
b = 6.6899 (7) Å	µ = 30.54 mm^−1
c = 17.2975 (19) Å	T = 153 K
V = 740.45 (14) Å^3	Plate, yellow
Z = 4	0.18 × 0.16 × 0.02 mm

Data collection

Bruker SMART 1000 CCD diffractometer	1807 independent reflections
Radiation source: fine-focus sealed tube	1759 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.032
ω scans	θmax = 28.8°, θmin = 2.4°
Absorption correction: numerical face indexed (SHELXTL; Sheldrick, 2003)	h = −8→8
Tmin = 0.047, Tmax = 0.603	k = −9→9
8784 measured reflections	l = −23→23

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.020	w = 1/[σ^2(Fo^2) + (0.02P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.049	(Δ/σ)max = 0.001
S = 1.39	Δρmax = 2.11 e Å^−3
1807 reflections	Δρmin = −1.57 e Å^−3
65 parameters	Absolute structure: Flack (1983): 704 Friedel pairs
0 restraints	Absolute structure parameter: 0.550 (7)

Special details

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. The structure was refined as an enantiomeric twin, the final twin ratio being 0.55:0.45.

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

	x	y	z	Uiso*/Ueq
Rb	0.02119 (9)	0.00342 (8)	0.04319 (3)	0.02110 (13)
Pb	0.28891 (3)	0.47494 (3)	0.230842 (12)	0.01418 (7)
P	0.2189 (2)	0.01031 (19)	0.34791 (8)	0.0100 (3)
S1	0.1533 (2)	0.0316 (2)	0.23134 (8)	0.0131 (3)
S2	0.3990 (2)	0.25142 (19)	0.37520 (10)	0.0142 (3)
S3	0.6101 (3)	0.25876 (19)	0.13163 (10)	0.0134 (3)
S4	0.0472 (2)	0.5039 (2)	0.08806 (8)	0.0135 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rb	0.0374 (3)	0.0118 (3)	0.0142 (3)	−0.0009 (2)	0.0062 (2)	−0.0007 (2)
Pb	0.01344 (10)	0.01498 (11)	0.01413 (11)	0.00007 (8)	−0.00011 (8)	0.00066 (9)
P	0.0121 (6)	0.0077 (6)	0.0103 (6)	−0.0002 (6)	0.0001 (5)	0.0003 (5)
S1	0.0152 (6)	0.0152 (6)	0.0089 (6)	−0.0015 (5)	0.0010 (5)	0.0003 (7)
S2	0.0181 (8)	0.0069 (6)	0.0178 (8)	−0.0015 (5)	−0.0035 (7)	0.0000 (5)
S3	0.0176 (7)	0.0070 (6)	0.0155 (8)	−0.0013 (5)	0.0000 (6)	0.0004 (5)
S4	0.0158 (6)	0.0130 (7)	0.0116 (6)	0.0004 (6)	0.0045 (5)	0.0004 (6)

Geometric parameters (Å, º)

Rb—S1	3.3680 (15)	Pb—Pb^viii	4.3504 (4)
Rb—S2^i	3.4075 (17)	Pb—Pb^ix	4.3504 (4)
Rb—S4^ii	3.4345 (16)	Pb—Rb^vii	4.3877 (7)
Rb—S4	3.4412 (16)	P—S4^iv	2.0320 (18)
Rb—S3^iii	3.4639 (17)	P—S2	2.038 (2)
Rb—S2^iv	3.4734 (17)	P—S3^ix	2.0381 (19)
Rb—S3^v	3.4898 (17)	P—S1	2.0644 (19)
Rb—P^i	3.7660 (15)	P—Pb^ix	3.4392 (14)
Rb—S4^iii	3.7887 (14)	P—Pb^iv	3.5315 (14)
Rb—Pb^iv	4.3877 (7)	P—Rb^x	3.7660 (15)
Rb—Rb^vi	4.8324 (9)	S1—Pb^iv	2.9290 (13)
Rb—Rb^iii	4.8324 (9)	S2—Pb^ix	3.2823 (16)
Pb—S4	2.9204 (14)	S2—Rb^x	3.4075 (17)
Pb—S1^vii	2.9290 (14)	S2—Rb^vii	3.4733 (17)
Pb—S2	2.9945 (16)	S3—P^viii	2.0381 (19)
Pb—S3	3.0430 (16)	S3—Pb^ix	3.1116 (16)
Pb—S1	3.0900 (14)	S3—Rb^vi	3.4640 (17)
Pb—S3^viii	3.1116 (16)	S3—Rb^xi	3.4898 (17)
Pb—S2^viii	3.2823 (16)	S4—P^vii	2.0320 (18)
Pb—P^viii	3.4392 (14)	S4—Rb^xii	3.4345 (16)
Pb—P^vii	3.5315 (14)	S4—Rb^vi	3.7888 (14)
S1—Rb—S2^i	144.54 (4)	S1^vii—Pb—P^vii	35.75 (4)
S1—Rb—S4^ii	79.86 (4)	S2—Pb—P^vii	124.86 (4)
S2^i—Rb—S4^ii	72.46 (3)	S3—Pb—P^vii	115.83 (4)
S1—Rb—S4	73.46 (3)	S1—Pb—P^vii	78.87 (3)
S2^i—Rb—S4	132.22 (4)	S3^viii—Pb—P^vii	116.43 (4)
S4^ii—Rb—S4	153.30 (5)	S2^viii—Pb—P^vii	107.85 (4)
S1—Rb—S3^iii	140.96 (4)	P^viii—Pb—P^vii	133.25 (4)
S2^i—Rb—S3^iii	57.37 (3)	S4—Pb—Pb^viii	113.99 (3)
S4^ii—Rb—S3^iii	129.51 (4)	S1^vii—Pb—Pb^viii	117.80 (3)
S4—Rb—S3^iii	75.05 (3)	S2—Pb—Pb^viii	96.36 (3)
S1—Rb—S2^iv	80.14 (4)	S3—Pb—Pb^viii	91.83 (3)
S2^i—Rb—S2^iv	102.70 (4)	S1—Pb—Pb^viii	155.77 (3)
S4^ii—Rb—S2^iv	58.23 (3)	S3^viii—Pb—Pb^viii	44.38 (3)
S4—Rb—S2^iv	114.71 (3)	S2^viii—Pb—Pb^viii	43.45 (3)
S3^iii—Rb—S2^iv	134.82 (4)	P^viii—Pb—Pb^viii	55.87 (2)
S1—Rb—S3^v	74.82 (4)	P^vii—Pb—Pb^viii	125.36 (2)
S2^i—Rb—S3^v	137.03 (4)	S4—Pb—Pb^ix	120.58 (3)
S4^ii—Rb—S3^v	114.44 (3)	S1^vii—Pb—Pb^ix	131.72 (3)
S4—Rb—S3^v	57.41 (3)	S2—Pb—Pb^ix	48.92 (3)
S3^iii—Rb—S3^v	106.36 (4)	S3—Pb—Pb^ix	45.66 (3)
S2^iv—Rb—S3^v	58.39 (3)	S1—Pb—Pb^ix	55.66 (3)
S1—Rb—P^i	139.22 (4)	S3^viii—Pb—Pb^ix	102.93 (3)
S2^i—Rb—P^i	32.52 (3)	S2^viii—Pb—Pb^ix	98.08 (3)
S4^ii—Rb—P^i	99.07 (3)	P^viii—Pb—Pb^ix	62.91 (2)
S4—Rb—P^i	101.81 (3)	P^vii—Pb—Pb^ix	132.98 (2)
S3^iii—Rb—P^i	32.40 (3)	Pb^viii—Pb—Pb^ix	100.508 (12)
S2^iv—Rb—P^i	133.99 (4)	S4—Pb—Rb^vii	120.73 (3)
S3^v—Rb—P^i	137.56 (4)	S1^vii—Pb—Rb^vii	50.10 (3)
S1—Rb—S4^iii	141.33 (3)	S2—Pb—Rb^vii	52.07 (3)
S2^i—Rb—S4^iii	66.58 (4)	S3—Pb—Rb^vii	145.94 (3)
S4^ii—Rb—S4^iii	99.30 (3)	S1—Pb—Rb^vii	84.96 (3)
S4—Rb—S4^iii	100.75 (3)	S3^viii—Pb—Rb^vii	52.15 (3)
S3^iii—Rb—S4^iii	67.31 (4)	S2^viii—Pb—Rb^vii	138.46 (3)
S2^iv—Rb—S4^iii	67.52 (4)	P^viii—Pb—Rb^vii	139.81 (2)
S3^v—Rb—S4^iii	70.47 (4)	P^vii—Pb—Rb^vii	85.67 (2)
P^i—Rb—S4^iii	79.38 (3)	Pb^viii—Pb—Rb^vii	96.413 (11)
S1—Rb—Pb^iv	41.85 (2)	Pb^ix—Pb—Rb^vii	100.282 (11)
S2^i—Rb—Pb^iv	143.68 (3)	S4^iv—P—S2	111.36 (9)
S4^ii—Rb—Pb^iv	77.19 (2)	S4^iv—P—S3^ix	109.75 (8)
S4—Rb—Pb^iv	82.14 (2)	S2—P—S3^ix	108.05 (8)
S3^iii—Rb—Pb^iv	150.68 (3)	S4^iv—P—S1	111.30 (8)
S2^iv—Rb—Pb^iv	42.84 (3)	S2—P—S1	106.65 (8)
S3^v—Rb—Pb^iv	44.75 (3)	S3^ix—P—S1	109.62 (8)
P^i—Rb—Pb^iv	176.05 (3)	S4^iv—P—Pb^ix	169.07 (7)
S4^iii—Rb—Pb^iv	99.86 (3)	S2—P—Pb^ix	68.19 (6)
S1—Rb—Rb^vi	95.41 (3)	S3^ix—P—Pb^ix	61.34 (6)
S2^i—Rb—Rb^vi	88.78 (3)	S1—P—Pb^ix	78.71 (5)
S4^ii—Rb—Rb^vi	134.59 (3)	S4^iv—P—Pb^iv	55.78 (5)
S4—Rb—Rb^vi	51.20 (3)	S2—P—Pb^iv	131.50 (7)
S3^iii—Rb—Rb^vi	46.20 (3)	S3^ix—P—Pb^iv	120.37 (7)
S2^iv—Rb—Rb^vi	165.82 (3)	S1—P—Pb^iv	56.00 (5)
S3^v—Rb—Rb^vi	107.48 (3)	Pb^ix—P—Pb^iv	133.25 (4)
P^i—Rb—Rb^vi	56.43 (2)	S4^iv—P—Rb^x	83.15 (6)
S4^iii—Rb—Rb^vi	110.71 (3)	S2—P—Rb^x	64.02 (6)
Pb^iv—Rb—Rb^vi	127.191 (19)	S3^ix—P—Rb^x	65.62 (6)
S1—Rb—Rb^iii	115.26 (3)	S1—P—Rb^x	165.34 (7)
S2^i—Rb—Rb^iii	100.20 (3)	Pb^ix—P—Rb^x	87.09 (3)
S4^ii—Rb—Rb^iii	140.01 (3)	Pb^iv—P—Rb^x	138.64 (4)
S4—Rb—Rb^iii	55.77 (3)	P—S1—Pb^iv	88.25 (6)
S3^iii—Rb—Rb^iii	61.66 (3)	P—S1—Pb	90.69 (6)
S2^iv—Rb—Rb^iii	86.82 (3)	Pb^iv—S1—Pb	113.34 (4)
S3^v—Rb—Rb^iii	45.76 (3)	P—S1—Rb	172.30 (7)
P^i—Rb—Rb^iii	91.82 (3)	Pb^iv—S1—Rb	88.05 (4)
S4^iii—Rb—Rb^iii	45.06 (2)	Pb—S1—Rb	96.98 (4)
Pb^iv—Rb—Rb^iii	90.325 (13)	P—S2—Pb	93.96 (7)
Rb^vi—Rb—Rb^iii	82.914 (19)	P—S2—Pb^ix	76.61 (6)
S4—Pb—S1^vii	70.65 (4)	Pb—S2—Pb^ix	87.63 (4)
S4—Pb—S2	149.64 (4)	P—S2—Rb^x	83.47 (6)
S1^vii—Pb—S2	96.07 (4)	Pb—S2—Rb^x	174.99 (6)
S4—Pb—S3	84.97 (4)	Pb^ix—S2—Rb^x	95.93 (4)
S1^vii—Pb—S3	147.13 (4)	P—S2—Rb^vii	92.33 (7)
S2—Pb—S3	94.25 (4)	Pb—S2—Rb^vii	85.09 (4)
S4—Pb—S1	85.27 (4)	Pb^ix—S2—Rb^vii	166.32 (5)
S1^vii—Pb—S1	81.51 (3)	Rb^x—S2—Rb^vii	90.70 (4)
S2—Pb—S1	65.45 (4)	P^viii—S3—Pb	82.66 (6)
S3—Pb—S1	74.64 (4)	P^viii—S3—Pb^ix	105.04 (7)
S4—Pb—S3^viii	135.72 (4)	Pb—S3—Pb^ix	89.95 (4)
S1^vii—Pb—S3^viii	87.19 (4)	P^viii—S3—Rb^vi	81.98 (6)
S2—Pb—S3^viii	67.56 (4)	Pb—S3—Rb^vi	99.39 (4)
S3—Pb—S3^viii	125.51 (2)	Pb^ix—S3—Rb^vi	169.05 (5)
S1—Pb—S3^viii	129.93 (4)	P^viii—S3—Rb^xi	94.34 (7)
S4—Pb—S2^viii	79.17 (4)	Pb—S3—Rb^xi	171.47 (6)
S1^vii—Pb—S2^viii	129.76 (4)	Pb^ix—S3—Rb^xi	83.10 (4)
S2—Pb—S2^viii	127.17 (2)	Rb^vi—S3—Rb^xi	88.04 (4)
S3—Pb—S2^viii	62.73 (3)	P^vii—S4—Pb	89.10 (6)
S1—Pb—S2^viii	135.50 (4)	P^vii—S4—Rb^xii	93.56 (6)
S3^viii—Pb—S2^viii	87.53 (4)	Pb—S4—Rb^xii	106.35 (4)
S4—Pb—P^viii	98.36 (3)	P^vii—S4—Rb	95.90 (6)
S1^vii—Pb—P^viii	164.61 (4)	Pb—S4—Rb	98.73 (4)
S2—Pb—P^viii	98.58 (4)	Rb^xii—S4—Rb	153.29 (5)
S3—Pb—P^viii	36.00 (4)	P^vii—S4—Rb^vi	176.19 (7)
S1—Pb—P^viii	108.92 (3)	Pb—S4—Rb^vi	94.70 (4)
S3^viii—Pb—P^viii	94.05 (4)	Rb^xii—S4—Rb^vi	85.18 (3)
S2^viii—Pb—P^viii	35.20 (3)	Rb—S4—Rb^vi	83.74 (3)
S4—Pb—P^vii	35.12 (3)

Symmetry codes: (i) −x+1/2, −y, z−1/2; (ii) x, y−1, z; (iii) x−1/2, −y+1/2, −z; (iv) −x, y−1/2, −z+1/2; (v) x−1, y, z; (vi) x+1/2, −y+1/2, −z; (vii) −x, y+1/2, −z+1/2; (viii) −x+1, y+1/2, −z+1/2; (ix) −x+1, y−1/2, −z+1/2; (x) −x+1/2, −y, z+1/2; (xi) x+1, y, z; (xii) x, y+1, z.