B-IncStrDB

Could incommensurability in sulfosalts be more common than thought? The case of meneghinite, CuPb₁₃Sb₇S₂₄

Authors:

Bindi, Luca; Petricek, Vaclav; Biagioni, Cristian; Plasil, Jakub; Moelo, Yves

Journal:

Acta Crystallographica, Section B 73 369-376 (2017)

DOI:

https://doi.org/10.1107/S2052520617002657

B-IncStrDB ID: 13202EGzpbI Entry date: 2017-06-06 Last revision: 2022-01-02

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I

Chemical data

Structural Formula Sum: Cu0.966 Pb13.196 S24 Sb6.804 [ Help ]

Formula weight: 4393.3 Da [ Help ]

Crystallographic data and experimental details

Crystal system: orthorhombic [ Help ]

Superspace group name: Pnma(0β0)00s [ Help ]

Symmetry operations of the superspace group: (Show/hide table) [ Help ]

Operation code	Operation in algebraic form
1	x1,x2,x3,x4
2	-x1+1/2,-x2,x3+1/2,-x4+1/2
3	-x1,x2+1/2,-x3,x4+1/2
4	x1+1/2,-x2+1/2,-x3+1/2,-x4
5	-x1,-x2,-x3,-x4
6	x1+1/2,x2,-x3+1/2,x4+1/2
7	x1,-x2+1/2,x3,-x4+1/2
8	-x1+1/2,x2+1/2,x3+1/2,x4

a: 24.0549(3) Å [ Help ]

b: 4.1291(6) Å [ Help ]

c: 11.3361(16) Å [ Help ]

α: 90(5) ° [ Help ]

β: 90(6) ° [ Help ]

γ: 90(5) ° [ Help ]

Volume: 1126(2) Å³ [ Help ]

Modulation dimension: 1 [ Help ]

Measured independent wave vectors: (Show/hide table) [ Help ]

Wave vector id	q_x	q_y	q_z
1	0	0.5433	0

Z: 1 [ Help ]

Cell measurement temperature: 297.4 K [ Help ]

μ: 54.685 mm^-1 [ Help ]

Refinement details

Total nb. of reflections: 6604 [ Help ]

Nb. of observed reflections: 4696 [ Help ]

Intense reflections threshold: I>3σ(I) [ Help ]

Refinement based on: Fsqd [ Help ]

R(obs): 0.0479 [ Help ]

wR(obs): 0.1076 [ Help ]

R(all): 0.0682 [ Help ]

wR(all): 0.1145 [ Help ]

S(all): 1.97 [ Help ]

S(obs): 2.21 [ Help ]

Nb. of reflections: 6604 [ Help ]

Nb. of parameters: 216 [ Help ]

Number of constraints: 78 [ Help ]

Weighting scheme: sigma [ Help ]

Weighting scheme remarks: w=1/(σ²(I)+0.0004I²) [ Help ]

Δ/σ(max): 0.8073 [ Help ]

Δ/σ(mean): 0.0432 [ Help ]

Extinction method: none [ Help ]

Structural Information

Average Structure: (Show/hide table) [ Help ]

Atom site label	Atom symbol	x	y	z	ADP type	Uiso/equiv	Symmetry multiplicity	Occupancy	Coords from (d)iffraction or (c)alculated	Coords restraints or constraints	Disordered cluster	Disordered group
Cu1	Cu	0.247(2)	0.25	-0.209(5)	Uani	0.0388(11)	4	0.239(4)	d	?	?	?
Pb1	Pb	0.125229(14)	0.25	0.15769(3)	Uani	0.02675(11)	4	1	d	?	?	?
Pb2	Pb	0.064759(19)	0.75	0.46575(4)	Uani	0.02537(16)	4	0.48(17)	d	?	?	?
Sb2	Sb	0.064759(19)	0.75	0.46575(4)	Uani	0.02537(16)	4	0.5199(17)	d	?	?	?
Pb3	Pb	0.025121(19)	0.25	-0.15251(4)	Uani	0.02636(16)	4	0.5246(18)	d	?	?	?
Sb3	Sb	0.025121(19)	0.25	-0.15251(4)	Uani	0.02636(16)	4	0.4754(18)	d	?	?	?
Pb4	Pb	0.215255(15)	0.25	0.48311(4)	Uani	0.03405(13)	4	1	d	?	?	?
Pb5	Pb	0.15041(2)	0.75	-0.21855(5)	Uani	0.02817(16)	4	0.2841	d	?	?	?
Sb5	Sb	0.15041(2)	0.75	-0.21855(5)	Uani	0.02817(16)	4	0.7159	d	?	?	?
S1	S	0.15229(8)	0.75	0.33925(19)	Uani	0.0214(6)	4	1	d	?	?	?
S2	S	-0.06368(9)	0.25	-0.02736(18)	Uani	0.0214(6)	4	1	d	?	?	?
S3	S	0.23688(9)	0.75	-0.3373(2)	Uani	0.0244(6)	4	1	d	?	?	?
S4	S	-0.02045(9)	0.75	-0.28375(19)	Uani	0.024(6)	4	1	d	?	?	?
S5	S	0.10735(9)	0.25	0.5944(2)	Uani	0.0263(6)	4	1	d	?	?	?
S6	S	0.18416(9)	0.25	-0.0896(2)	Uani	0.0353(7)	4	1	d	?	?	?

ADP components: (Show/hide table) [ Help ]

Atom site label	Atom site symbol	U11	U22	U33	U13
Cu1	Cu	0.0318(17)	0.0351(18)	0.05(2)	-0.0051(14)
Pb1	Pb	0.02884(19)	0.02372(18)	0.0277(2)	0.00114(13)
Pb2	Pb	0.0275(3)	0.0243(3)	0.0244(3)	0.00051(18)
Sb2	Sb	0.0275(3)	0.0243(3)	0.0244(3)	0.00051(18)
Pb3	Pb	0.0291(3)	0.0243(3)	0.0257(3)	0.00392(18)
Sb3	Sb	0.0291(3)	0.0243(3)	0.0257(3)	0.00392(18)
Pb4	Pb	0.02498(19)	0.0333(2)	0.0439(3)	0.00206(15)
Pb5	Pb	0.0236(3)	0.0335(3)	0.0275(3)	-0.0003(2)
Sb5	Sb	0.0236(3)	0.0335(3)	0.0275(3)	-0.0003(2)
S1	S	0.0222(10)	0.023(10)	0.0189(10)	0(8)
S2	S	0.024(10)	0.0214(10)	0.0188(10)	0.0008(8)
S3	S	0.0255(10)	0.0248(10)	0.0229(11)	0.0033(8)
S4	S	0.0252(10)	0.026(10)	0.0207(11)	-0.0007(8)
S5	S	0.0273(10)	0.0279(11)	0.0237(11)	0.0002(8)
S6	S	0.0259(11)	0.0552(15)	0.0247(12)	-0.0001(9)

Fourier Wave Vectors (explicit: q_x,q_y,q_z or coefficients: q_1,q_2,...): (Show/hide table) [ Help ]

Wave vector code	q_1
1	1
2	2

Table: (Show/hide table) [ Help ]

_jana_atom_site_occ_Fourier_absolute_site_label	_jana_atom_site_occ_Fourier_absolute
Cu1	0.239(4)
Pb2	0.4801(17)
Sb2	0.5199(17)
Pb3	0.5246(18)
Sb3	0.4754(18)
Pb5	0.2841
Sb5	0.7159

Definition of the occupation Fourier series: (Show/hide table) [ Help ]

Modulation code	Atom site label	Wave vector code
Cu1o1	Cu1	1
Cu1o2	Cu1	2
Pb2o1	Pb2	1
Pb2o2	Pb2	2
Sb2o1	Sb2	1
Sb2o2	Sb2	2
Pb3o1	Pb3	1
Pb3o2	Pb3	2
Sb3o1	Sb3	1
Sb3o2	Sb3	2
Pb5o1	Pb5	1
Pb5o2	Pb5	2
Sb5o1	Sb5	1
Sb5o2	Sb5	2

Occupation Fourier coefficients: (Show/hide table) [ Help ]

Modulation code	Cosine coefficient	Sine coefficient
Cu1o1	0	0.379(5)
Cu1o2	-0.174(4)	0
Pb2o1	0	0.548(4)
Pb2o2	0(5)	0
Sb2o1	0	-0.548(4)
Sb2o2	0(5)	0
Pb3o1	0	0.544(4)
Pb3o2	0.056(5)	0
Sb3o1	0	-0.544(4)
Sb3o2	-0.056(5)	0
Pb5o1	0	-0.394(4)
Pb5o2	-0.126(5)	0
Sb5o1	0	0.394(4)
Sb5o2	0.126(5)	0

Definition of the displacive (translational) Fourier series: (Show/hide table) [ Help ]

Modulation code	Atom site label	Displacement axis	Wave vector code
Cu1x1	Cu1	x	1
Cu1y1	Cu1	y	1
Cu1z1	Cu1	z	1
Cu1x2	Cu1	x	2
Cu1y2	Cu1	y	2
Cu1z2	Cu1	z	2
Pb1x1	Pb1	x	1
Pb1y1	Pb1	y	1
Pb1z1	Pb1	z	1
Pb1x2	Pb1	x	2
Pb1y2	Pb1	y	2
Pb1z2	Pb1	z	2
Pb2x1	Pb2	x	1
Pb2y1	Pb2	y	1
Pb2z1	Pb2	z	1
Pb2x2	Pb2	x	2
Pb2y2	Pb2	y	2
Pb2z2	Pb2	z	2
Sb2x1	Sb2	x	1
Sb2y1	Sb2	y	1
Sb2z1	Sb2	z	1
Sb2x2	Sb2	x	2
Sb2y2	Sb2	y	2
Sb2z2	Sb2	z	2
Pb3x1	Pb3	x	1
Pb3y1	Pb3	y	1
Pb3z1	Pb3	z	1
Pb3x2	Pb3	x	2
Pb3y2	Pb3	y	2
Pb3z2	Pb3	z	2
Sb3x1	Sb3	x	1
Sb3y1	Sb3	y	1
Sb3z1	Sb3	z	1
Sb3x2	Sb3	x	2
Sb3y2	Sb3	y	2
Sb3z2	Sb3	z	2
Pb4x1	Pb4	x	1
Pb4y1	Pb4	y	1
Pb4z1	Pb4	z	1
Pb4x2	Pb4	x	2
Pb4y2	Pb4	y	2
Pb4z2	Pb4	z	2
Pb5x1	Pb5	x	1
Pb5y1	Pb5	y	1
Pb5z1	Pb5	z	1
Pb5x2	Pb5	x	2
Pb5y2	Pb5	y	2
Pb5z2	Pb5	z	2
Sb5x1	Sb5	x	1
Sb5y1	Sb5	y	1
Sb5z1	Sb5	z	1
Sb5x2	Sb5	x	2
Sb5y2	Sb5	y	2
Sb5z2	Sb5	z	2
S1x1	S1	x	1
S1y1	S1	y	1
S1z1	S1	z	1
S1x2	S1	x	2
S1y2	S1	y	2
S1z2	S1	z	2
S2x1	S2	x	1
S2y1	S2	y	1
S2z1	S2	z	1
S2x2	S2	x	2
S2y2	S2	y	2
S2z2	S2	z	2
S3x1	S3	x	1
S3y1	S3	y	1
S3z1	S3	z	1
S3x2	S3	x	2
S3y2	S3	y	2
S3z2	S3	z	2
S4x1	S4	x	1
S4y1	S4	y	1
S4z1	S4	z	1
S4x2	S4	x	2
S4y2	S4	y	2
S4z2	S4	z	2
S5x1	S5	x	1
S5y1	S5	y	1
S5z1	S5	z	1
S5x2	S5	x	2
S5y2	S5	y	2
S5z2	S5	z	2
S6x1	S6	x	1
S6y1	S6	y	1
S6z1	S6	z	1
S6x2	S6	x	2
S6y2	S6	y	2
S6z2	S6	z	2

Displacive (translational) Fourier coefficients: (Show/hide table) [ Help ]

Modulation code	Cosine coefficient	Sine coefficient
Cu1x1	0	0.01(3)
Cu1y1	-0.014(17)	0
Cu1z1	0	-0.05(8)
Cu1x2	0.0043(13)	0
Cu1y2	0	0.011(13)
Cu1z2	-0.02(3)	0
Pb1x1	0	-0.000915(17)
Pb1y1	0.0039(9)	0
Pb1z1	0	-0.00257(4)
Pb1x2	-0.00048(2)	0
Pb1y2	0	-0.00178(11)
Pb1z2	0.00309(4)	0
Pb2x1	0	-0.00573(2)
Pb2y1	0.01408(13)	0
Pb2z1	0	-0.00509(5)
Pb2x2	-0.00155(3)	0
Pb2y2	0	0.00265(16)
Pb2z2	-0.0043(6)	0
Sb2x1	0	-0.00573(2)
Sb2y1	0.01408(13)	0
Sb2z1	0	-0.00509(5)
Sb2x2	-0.00155(3)	0
Sb2y2	0	0.00265(16)
Sb2z2	-0.0043(6)	0
Pb3x1	0	0.00647(2)
Pb3y1	-0.00187(12)	0
Pb3z1	0	0.0095(5)
Pb3x2	0.00047(3)	0
Pb3y2	0	-0.00186(15)
Pb3z2	0.00515(6)	0
Sb3x1	0	0.00647(2)
Sb3y1	-0.00187(12)	0
Sb3z1	0	0.0095(5)
Sb3x2	0.00047(3)	0
Sb3y2	0	-0.00186(15)
Sb3z2	0.00515(6)	0
Pb4x1	0	0.001366(17)
Pb4y1	-0.00326(10)	0
Pb4z1	0	0.00588(5)
Pb4x2	0.00061(2)	0
Pb4y2	0	-0.00386(13)
Pb4z2	0.01081(5)	0
Pb5x1	0	0.0017(2)
Pb5y1	-0.02717(16)	0
Pb5z1	0	0.0021(6)
Pb5x2	0.00005(3)	0
Pb5y2	0	0.00641(18)
Pb5z2	-0.00484(6)	0
Sb5x1	0	0.0017(2)
Sb5y1	-0.02717(16)	0
Sb5z1	0	0.0021(6)
Sb5x2	0.00005(3)	0
Sb5y2	0	0.00641(18)
Sb5z2	-0.00484(6)	0
S1x1	0	0.00301(10)
S1y1	-0.0075(6)	0
S1z1	0	0.0011(2)
S1x2	-0.00003(12)	0
S1y2	0	-0.0004(7)
S1z2	-0.0015(3)	0
S2x1	0	-0.00279(10)
S2y1	-0.0104(6)	0
S2z1	0	0(2)
S2x2	-0.00122(12)	0
S2y2	0	-0.0012(7)
S2z2	0.0021(3)	0
S3x1	0	-0.00467(11)
S3y1	0.0025(6)	0
S3z1	0	-0.0047(2)
S3x2	-0.00047(12)	0
S3y2	0	-0.0004(7)
S3z2	-0.0019(3)	0
S4x1	0	0.00085(10)
S4y1	-0.0513(6)	0
S4z1	0	0.0027(2)
S4x2	0.00103(13)	0
S4y2	0	-0.0016(7)
S4z2	-0.0011(3)	0
S5x1	0	-0.00317(11)
S5y1	-0.0575(7)	0
S5z1	0	-0.0019(3)
S5x2	-0.00106(13)	0
S5y2	0	0.002(7)
S5z2	0.002(3)	0
S6x1	0	0.00084(12)
S6y1	0.069(9)	0
S6z1	0	0.0049(3)
S6x2	-0.0006(14)	0
S6y2	0	0.0197(9)
S6z2	0.0039(3)	0

Definition of the ADP Fourier series: (Show/hide table) [ Help ]

Modulation code	Atom site label	Tensor element	Wave vector code
Pb1U111	Pb1	U11	1
Pb1U221	Pb1	U22	1
Pb1U331	Pb1	U33	1
Pb1U121	Pb1	U12	1
Pb1U131	Pb1	U13	1
Pb1U231	Pb1	U23	1
Pb1U112	Pb1	U11	2
Pb1U222	Pb1	U22	2
Pb1U332	Pb1	U33	2
Pb1U122	Pb1	U12	2
Pb1U132	Pb1	U13	2
Pb1U232	Pb1	U23	2
Pb2U111	Pb2	U11	1
Pb2U221	Pb2	U22	1
Pb2U331	Pb2	U33	1
Pb2U121	Pb2	U12	1
Pb2U131	Pb2	U13	1
Pb2U231	Pb2	U23	1
Pb2U112	Pb2	U11	2
Pb2U222	Pb2	U22	2
Pb2U332	Pb2	U33	2
Pb2U122	Pb2	U12	2
Pb2U132	Pb2	U13	2
Pb2U232	Pb2	U23	2
Sb2U111	Sb2	U11	1
Sb2U221	Sb2	U22	1
Sb2U331	Sb2	U33	1
Sb2U121	Sb2	U12	1
Sb2U131	Sb2	U13	1
Sb2U231	Sb2	U23	1
Sb2U112	Sb2	U11	2
Sb2U222	Sb2	U22	2
Sb2U332	Sb2	U33	2
Sb2U122	Sb2	U12	2
Sb2U132	Sb2	U13	2
Sb2U232	Sb2	U23	2
Pb3U111	Pb3	U11	1
Pb3U221	Pb3	U22	1
Pb3U331	Pb3	U33	1
Pb3U121	Pb3	U12	1
Pb3U131	Pb3	U13	1
Pb3U231	Pb3	U23	1
Pb3U112	Pb3	U11	2
Pb3U222	Pb3	U22	2
Pb3U332	Pb3	U33	2
Pb3U122	Pb3	U12	2
Pb3U132	Pb3	U13	2
Pb3U232	Pb3	U23	2
Sb3U111	Sb3	U11	1
Sb3U221	Sb3	U22	1
Sb3U331	Sb3	U33	1
Sb3U121	Sb3	U12	1
Sb3U131	Sb3	U13	1
Sb3U231	Sb3	U23	1
Sb3U112	Sb3	U11	2
Sb3U222	Sb3	U22	2
Sb3U332	Sb3	U33	2
Sb3U122	Sb3	U12	2
Sb3U132	Sb3	U13	2
Sb3U232	Sb3	U23	2
Pb4U111	Pb4	U11	1
Pb4U221	Pb4	U22	1
Pb4U331	Pb4	U33	1
Pb4U121	Pb4	U12	1
Pb4U131	Pb4	U13	1
Pb4U231	Pb4	U23	1
Pb4U112	Pb4	U11	2
Pb4U222	Pb4	U22	2
Pb4U332	Pb4	U33	2
Pb4U122	Pb4	U12	2
Pb4U132	Pb4	U13	2
Pb4U232	Pb4	U23	2
Pb5U111	Pb5	U11	1
Pb5U221	Pb5	U22	1
Pb5U331	Pb5	U33	1
Pb5U121	Pb5	U12	1
Pb5U131	Pb5	U13	1
Pb5U231	Pb5	U23	1
Pb5U112	Pb5	U11	2
Pb5U222	Pb5	U22	2
Pb5U332	Pb5	U33	2
Pb5U122	Pb5	U12	2
Pb5U132	Pb5	U13	2
Pb5U232	Pb5	U23	2
Sb5U111	Sb5	U11	1
Sb5U221	Sb5	U22	1
Sb5U331	Sb5	U33	1
Sb5U121	Sb5	U12	1
Sb5U131	Sb5	U13	1
Sb5U231	Sb5	U23	1
Sb5U112	Sb5	U11	2
Sb5U222	Sb5	U22	2
Sb5U332	Sb5	U33	2
Sb5U122	Sb5	U12	2
Sb5U132	Sb5	U13	2
Sb5U232	Sb5	U23	2

ADP Fourier coefficients: (Show/hide table) [ Help ]

Modulation code	Cosine coefficient	Sine coefficient
Pb1U111	0	0.0012(2)
Pb1U221	0	0.00131(20)
Pb1U331	0	0.0005(3)
Pb1U121	0.00111(16)	0
Pb1U131	0	-0.00119(18)
Pb1U231	0.00068(17)	0
Pb1U112	-0.0028(3)	0
Pb1U222	-0.0013(3)	0
Pb1U332	0.0003(3)	0
Pb1U122	0	-0.0002(2)
Pb1U132	-0.0004(2)	0
Pb1U232	0	-0.0005(2)
Pb2U111	0	0.0011(3)
Pb2U221	0	0.0016(3)
Pb2U331	0	0.0012(4)
Pb2U121	-0.0028(2)	0
Pb2U131	0	0.0012(2)
Pb2U231	-0.0014(2)	0
Pb2U112	0.0083(4)	0
Pb2U222	0.0023(4)	0
Pb2U332	0.0042(4)	0
Pb2U122	0	0.0006(3)
Pb2U132	0.0036(3)	0
Pb2U232	0	0.0015(3)
Sb2U111	0	0.0011(3)
Sb2U221	0	0.0016(3)
Sb2U331	0	0.0012(4)
Sb2U121	-0.0028(2)	0
Sb2U131	0	0.0012(2)
Sb2U231	-0.0014(2)	0
Sb2U112	0.0083(4)	0
Sb2U222	0.0023(4)	0
Sb2U332	0.0042(4)	0
Sb2U122	0	0.0006(3)
Sb2U132	0.0036(3)	0
Sb2U232	0	0.0015(3)
Pb3U111	0	0.0029(3)
Pb3U221	0	0.0023(3)
Pb3U331	0	0.0031(4)
Pb3U121	0.0003(2)	0
Pb3U131	0	-0.0002(2)
Pb3U231	-0.0013(2)	0
Pb3U112	0.0076(4)	0
Pb3U222	-0.0002(4)	0
Pb3U332	0.0065(4)	0
Pb3U122	0	0.0005(3)
Pb3U132	0.0061(3)	0
Pb3U232	0	-0.0004(3)
Sb3U111	0	0.0029(3)
Sb3U221	0	0.0023(3)
Sb3U331	0	0.0031(4)
Sb3U121	0.0003(2)	0
Sb3U131	0	-0.0002(2)
Sb3U231	-0.0013(2)	0
Sb3U112	0.0076(4)	0
Sb3U222	-0.0002(4)	0
Sb3U332	0.0065(4)	0
Sb3U122	0	0.0005(3)
Sb3U132	0.0061(3)	0
Sb3U232	0	-0.0004(3)
Pb4U111	0	0(2)
Pb4U221	0	-0.0031(2)
Pb4U331	0	-0.0128(3)
Pb4U121	-0.00145(17)	0
Pb4U131	0	0.0007(2)
Pb4U231	-0.0064(2)	0
Pb4U112	-0.0004(3)	0
Pb4U222	-0.0025(3)	0
Pb4U332	-0.0039(3)	0
Pb4U122	0	-0.0004(3)
Pb4U132	0.0024(2)	0
Pb4U232	0	0.0013(2)
Pb5U111	0	-0.0035(3)
Pb5U221	0	-0.0006(4)
Pb5U331	0	-0.0011(4)
Pb5U121	0.0024(3)	0
Pb5U131	0	-0.0001(2)
Pb5U231	0.0092(3)	0
Pb5U112	0.0007(5)	0
Pb5U222	0.0092(5)	0
Pb5U332	0.0059(5)	0
Pb5U122	0	0.0006(3)
Pb5U132	0.0008(3)	0
Pb5U232	0	0.0007(3)
Sb5U111	0	-0.0035(3)
Sb5U221	0	-0.0006(4)
Sb5U331	0	-0.0011(4)
Sb5U121	0.0024(3)	0
Sb5U131	0	-0.0001(2)
Sb5U231	0.0092(3)	0
Sb5U112	0.0007(5)	0
Sb5U222	0.0092(5)	0
Sb5U332	0.0059(5)	0
Sb5U122	0	0.0006(3)
Sb5U132	0.0008(3)	0
Sb5U232	0	0.0007(3)

Could incommensurability in sulfosalts be more common than thought? The case of meneghinite, CuPb13Sb7S24