B-IncStrDB

Experimental Evidence of the Coexistence of Proper Magnetic and Structural Incommensurability on the [CH₃NH₃][Ni(COOH)₃] Compound

Authors:

Canadillas-Delgado, Laura; Mazzuca, Lidia; Fabelo, Oscar; Rodriguez-Carvajal, Juan; Petricek, Vaclav

Journal:

Inorganic Chemistry 59 17896-17905 (2020)

DOI:

https://doi.org/10.1021/acs.inorgchem.0c01722

B-IncStrDB ID: 16402EKE8SJ Entry date: 2020-06-17 Last revision: 2024-05-08

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Chemical data

Structural Formula Sum: C4 H9 N1 Ni1 O6 [ Help ]

Formula weight: 225.8 Da [ Help ]

Crystallographic data and experimental details

Crystal system: orthorhombic [ Help ]

Superspace group name: Pnma(00γ)0s0 [ 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: 8.1801(4) Å [ Help ]

b: 11.5419(10) Å [ Help ]

c: 8.0976(5) Å [ Help ]

α: 90 ° [ Help ]

β: 90 ° [ Help ]

γ: 90 ° [ Help ]

Volume: 764.53(9) 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	0.1426

Z: 4 [ Help ]

Cell determination reflection Nb.: 1000 [ Help ]

θ(min) for cell determination: 5.46 ° [ Help ]

θ(max) for cell determination: 61.28 ° [ Help ]

Cell measurement temperature: 40 K [ Help ]

μ: 0.231 mm^-1 [ Help ]

Absorption correction type: numerical [ Help ]

Absorption correction remarks: absorption corretion done through d19face, d19abs and d19abscan programs from ILL [ Help ]

Minimum transmission factor: 0.8002 [ Help ]

Maximum transmission factor: 0.8596 [ Help ]

Refinement details

Total nb. of reflections: 3371 [ Help ]

Nb. of observed reflections: 1989 [ Help ]

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

Refinement based on: F [ Help ]

R(obs): 0.0628 [ Help ]

wR(obs): 0.0796 [ Help ]

R(all): 0.0906 [ Help ]

wR(all): 0.0819 [ Help ]

S(all): 3.53 [ Help ]

S(obs): 4.57 [ Help ]

Nb. of reflections: 3371 [ Help ]

Nb. of parameters: 200 [ Help ]

Weighting scheme: sigma [ Help ]

Weighting scheme remarks: w=1/(σ²(F)+0.0001F²) [ Help ]

Refinement of hydrogen atoms: refall [ Help ]

Δ/σ(max): 0.0059 [ Help ]

Δ/σ(mean): 0.0006 [ Help ]

Δρ(max): 1.16 e_Å^-3 [ Help ]

Δρ(min): -1.22 e_Å^-3 [ Help ]

Extinction method: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974) [ Help ]

Extinction coefficient: 81(4) [ 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
Ni1	Ni	0.5	0	0	Uani	0.021(3)	4	1	d	?	?	?
O1	O	0.59681(13)	-0.0697(10)	-0.21214(13)	Uani	0.0235(4)	8	1	d	?	?	?
O2	O	0.77506(13)	-0.05809(10)	-0.41769(14)	Uani	0.023(4)	8	1	d	?	?	?
O3	O	0.47538(14)	0.15419(10)	-0.1254(13)	Uani	0.0235(3)	8	1	d	?	?	?
N1	N	0.91396(13)	0.25	-0.03043(14)	Uani	0.0247(4)	4	1	d	?	?	?
C1	C	0.72229(12)	-0.02843(10)	-0.27714(12)	Uani	0.0232(3)	8	1	d	?	?	?
C3	C	1.08771(18)	0.25	0.02356(19)	Uani	0.0267(5)	4	1	d	?	?	?
C2	C	0.49097(16)	0.25	-0.05298(17)	Uani	0.0222(5)	4	1	d	?	?	?
H1	H	0.7922(3)	0.0361(2)	-0.2098(3)	Uani	0.0452(8)	8	1	d	?	?	?
H2	H	0.5184(5)	0.25	0.081(4)	Uani	0.0425(11)	4	1	d	?	?	?
H6	H	0.9114(4)	0.25	-0.157(4)	Uani	0.0431(11)	4	1	d	?	?	?
H4	H	1.0918(4)	0.25	0.1572(4)	Uani	0.0519(13)	4	1	d	?	?	?
H5	H	0.8524(3)	0.1779(2)	0.0133(3)	Uani	0.0362(7)	8	1	d	?	?	?
H3	H	1.1464(3)	0.3261(2)	-0.0216(3)	Uani	0.051(9)	8	1	d	?	?	?

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

Atom site label	Atom site symbol	U11	U22	U33	U12	U13	U23
Ni1	Ni	0.019(5)	0.0205(6)	0.0236(5)	-0.0007(3)	-0.0002(3)	-0.0009(4)
O1	O	0.0204(6)	0.0237(7)	0.0263(6)	-0.0036(5)	0.0023(4)	-0.0006(5)
O2	O	0.0218(6)	0.0227(7)	0.0245(6)	-0.0002(5)	0.0012(4)	-0.0009(5)
O3	O	0.0259(6)	0.0187(6)	0.0259(5)	-0.0001(5)	0.0001(4)	-0.0014(5)
N1	N	0.0222(6)	0.023(7)	0.029(7)	0	-0.0001(4)	0
C1	C	0.0206(6)	0.0228(7)	0.0263(6)	-0.0005(4)	0.0013(4)	0.0002(4)
C3	C	0.0196(8)	0.0279(10)	0.0325(9)	0	-0.0013(6)	0
C2	C	0.0217(7)	0.0189(9)	0.026(8)	0	-0.0009(5)	0
H1	H	0.0433(14)	0.0478(15)	0.0446(13)	-0.0176(11)	0.0095(10)	-0.0139(11)
H2	H	0.063(2)	0.0306(18)	0.0334(16)	0	-0.0104(13)	0
H6	H	0.0404(17)	0.055(2)	0.0342(19)	0	-0.0007(12)	0
H4	H	0.0471(19)	0.071(3)	0.0377(19)	0	-0.0022(13)	0
H5	H	0.0313(12)	0.0355(15)	0.0416(10)	-0.0032(10)	0.0019(8)	0.0022(10)
H3	H	0.035(13)	0.05(17)	0.0679(15)	-0.0097(12)	-0.0022(11)	0.0135(13)

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

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

Modulation code	Atom site label	Displacement axis	Wave vector code
Ni1x1	Ni1	x	1
Ni1y1	Ni1	y	1
Ni1z1	Ni1	z	1
O1x1	O1	x	1
O1y1	O1	y	1
O1z1	O1	z	1
O2x1	O2	x	1
O2y1	O2	y	1
O2z1	O2	z	1
O3x1	O3	x	1
O3y1	O3	y	1
O3z1	O3	z	1
O3x2	O3	x	2
O3y2	O3	y	2
O3z2	O3	z	2
N1x1	N1	x	1
N1y1	N1	y	1
N1z1	N1	z	1
C1x1	C1	x	1
C1y1	C1	y	1
C1z1	C1	z	1
C3x1	C3	x	1
C3y1	C3	y	1
C3z1	C3	z	1
C2x1	C2	x	1
C2y1	C2	y	1
C2z1	C2	z	1
H1x1	H1	x	1
H1y1	H1	y	1
H1z1	H1	z	1
H1x2	H1	x	2
H1y2	H1	y	2
H1z2	H1	z	2
H2x1	H2	x	1
H2y1	H2	y	1
H2z1	H2	z	1
H2x2	H2	x	2
H2y2	H2	y	2
H2z2	H2	z	2
H6x1	H6	x	1
H6y1	H6	y	1
H6z1	H6	z	1
H6x2	H6	x	2
H6y2	H6	y	2
H6z2	H6	z	2
H4x1	H4	x	1
H4y1	H4	y	1
H4z1	H4	z	1
H4x2	H4	x	2
H4y2	H4	y	2
H4z2	H4	z	2
H5x1	H5	x	1
H5y1	H5	y	1
H5z1	H5	z	1
H5x2	H5	x	2
H5y2	H5	y	2
H5z2	H5	z	2
H3x1	H3	x	1
H3y1	H3	y	1
H3z1	H3	z	1
H3x2	H3	x	2
H3y2	H3	y	2
H3z2	H3	z	2

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

Modulation code	Cosine coefficient	Sine coefficient
Ni1x1	0	-0.00272(14)
Ni1y1	0	0.02274(11)
Ni1z1	0	0.00034(15)
O1x1	-0.00219(19)	-0.00246(18)
O1y1	0.00385(13)	0.02225(14)
O1z1	-0.00042(18)	0.00077(18)
O2x1	0.00067(19)	-0.00224(18)
O2y1	0.00125(13)	0.02226(14)
O2z1	0.00283(17)	-0.00049(19)
O3x1	-0.0032(19)	-0.002(19)
O3y1	0.00244(13)	0.02275(13)
O3z1	-0.00031(18)	0.0003(18)
O3x2	0.0005(4)	-0.0004(4)
O3y2	-0.00012(17)	-0.00005(17)
O3z2	-0.0004(3)	0.0001(3)
N1x1	0	0
N1y1	0.00627(13)	0.02132(13)
N1z1	0	0
C1x1	0.00041(17)	-0.00239(16)
C1y1	0.00123(12)	0.0222(13)
C1z1	0.00166(16)	0.00021(17)
C3x1	0	0
C3y1	0.00109(18)	0.02126(18)
C3z1	0	0
C2x1	0	0
C2y1	0.00094(16)	0.02319(17)
C2z1	0	0
H1x1	0.0031(4)	-0.002(4)
H1y1	-0.0011(3)	0.0224(3)
H1z1	0.001(4)	-0.0003(4)
H1x2	0.0002(8)	0.0013(8)
H1y2	-0.0007(3)	-0.0003(4)
H1z2	0.002(7)	-0.0006(7)
H2x1	0	0
H2y1	-0.0034(4)	0.0216(4)
H2z1	0	0
H2x2	-0.0002(11)	-0.0006(12)
H2y2	0	0
H2z2	-0.0019(8)	0(9)
H6x1	0	0
H6y1	0.0149(4)	0.0192(4)
H6z1	0	0
H6x2	0.001(11)	0.0001(11)
H6y2	0	0
H6z2	0.0012(9)	0.0012(10)
H4x1	0	0
H4y1	-0.0085(4)	0.0209(5)
H4z1	0	0
H4x2	-0.0009(12)	-0.0015(12)
H4y2	0	0
H4z2	0.0001(10)	0.0033(11)
H5x1	-0.0004(3)	-0.0009(3)
H5y1	0.0041(3)	0.0217(3)
H5z1	-0.006(3)	0.0011(3)
H5x2	0.0011(7)	-0.0006(7)
H5y2	0.0003(3)	0.0001(3)
H5z2	0.0012(6)	0.001(7)
H3x1	0.0007(4)	0.0005(4)
H3y1	0.0046(3)	0.0203(3)
H3z1	0.0084(4)	-0.0008(4)
H3x2	0.0018(8)	-0.0008(8)
H3y2	0.0001(4)	0(4)
H3z2	0.0002(8)	-0.0009(8)

Experimental Evidence of the Coexistence of Proper Magnetic and Structural Incommensurability on the [CH3NH3][Ni(COOH)3] Compound