B-IncStrDB

Catching new modulated high-pressure phases of δ-chlorpropamide: when the experimental setup matters

Authors:

Bogdanov, Nikita E.; Rashchenko, Sergey V.; Zakharov, Boris A.; Seryotkin, Yurii V.; Boldyrev, Elena V.

Journal:

IUCrJ 13 146-158 (2026)

DOI:

https://doi.org/10.1107/S2052252525011601

B-IncStrDB ID: V9VuwNzvTbh Entry date: 2026-01-15 Last revision: 2026-03-03

I

Chemical data

Structural Formula Sum: C10 H0 Cl1 N2 O3 S1 [ Help ]

Formula weight: 263.6 Da [ Help ]

Absolute configuration: . [ Help ]

Crystallographic data and experimental details

Crystal system: orthorhombic [ Help ]

Superspace group name: Pbca(0β0)s00 [ 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
3	-x1,x2+1/2,-x3+1/2,x4+1/2
4	x1+1/2,-x2+1/2,-x3,-x4+1/2
5	-x1,-x2,-x3,-x4
6	x1+1/2,x2,-x3+1/2,x4
7	x1,-x2+1/2,x3+1/2,-x4+1/2
8	-x1+1/2,x2+1/2,x3,x4+1/2

a: 9.234(2) Å [ Help ]

b: 9.187(2) Å [ Help ]

c: 24.895(5) Å [ Help ]

α: 90 ° [ Help ]

β: 90 ° [ Help ]

γ: 90 ° [ Help ]

Volume: 2111.9(8) Å³ [ Help ]

Modulation dimension: 1 [ Help ]

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

Wave vector id	q_x	q_y	q_z
1	0.000000	0.278200	0.000000

Z: 8 [ Help ]

Cell determination reflection Nb.: 710 [ Help ]

θ(min) for cell determination: 2.24 ° [ Help ]

θ(max) for cell determination: 28.22 ° [ Help ]

Cell measurement temperature: 293 K [ Help ]

μ: 0.549 mm^-1 [ Help ]

Absorption correction type: multi-scan [ Help ]

Absorption correction remarks: CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. [ Help ]

Minimum transmission factor: 0.828 [ Help ]

Maximum transmission factor: 1 [ Help ]

Refinement details

Total nb. of reflections: 3268 [ Help ]

Nb. of observed reflections: 1881 [ Help ]

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

Refinement based on: Fsqd [ Help ]

R(obs): 0.2999 [ Help ]

wR(obs): 0.5529 [ Help ]

R(all): 0.3498 [ Help ]

wR(all): 0.5818 [ Help ]

S(all): 9.2782 [ Help ]

S(obs): 11.6266 [ Help ]

Nb. of reflections: 3268 [ Help ]

Nb. of parameters: 13 [ Help ]

Number of restraints: 67 [ Help ]

Number of constraints: 570 [ Help ]

Weighting scheme: sigma [ Help ]

Weighting scheme remarks: calc w=1/[σ²(Fo²)+(0.02P)²+0.0000P] where P=(Fo²+2Fc²)/3 [ Help ]

Refinement of hydrogen atoms: constr [ Help ]

Δ/σ(max): 0.0455 [ Help ]

Δ/σ(mean): 0.0455 [ Help ]

Δρ(max): 2.11 e_Å^-3 [ Help ]

Δρ(min): -1.31 e_Å^-3 [ 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
S1	S	0.644274	0.569039	0.573519	Uani	0.0648	8	1	d	.	.	.
Cl1a	Cl	0.602805	1.007038	0.766212	Uani	0.1149	8	0.5584	d	.	.	.
Cl1b	Cl	0.716063	1.00977	0.758694	Uani	0.1004	8	0.4416	d	.	.	.
O1	O	0.53371	0.463289	0.583758	Uani	0.049	8	1	d	.	.	.
O3	O	0.794426	0.7745	0.499172	Uani	0.0667	8	1	d	.	.	.
O2	O	0.789851	0.521837	0.561701	Uani	0.0784	8	1	d	.	.	.
N2	N	0.578494	0.851415	0.463697	Uani	0.0378	8	1	d	.	.	.
N1	N	0.584428	0.662669	0.520291	Uani	0.0488	8	1	d	.	.	.
C3a	C	0.753694	0.767438	0.64364	Uiso	0.0392	8	0.5584	d	.	.	.
C3b	C	0.799643	0.721748	0.647226	Uiso	0.0664	8	0.4416	d	.	.	.
C4a	C	0.635378	0.691925	0.627299	Uiso	0.0443	8	0.5584	d	.	.	.
C4b	C	0.665199	0.686688	0.625926	Uiso	0.0326	8	0.4416	d	.	.	.
C8	C	0.635984	0.969934	0.428328	Uiso	0.0472	8	1	d	.	.	.
C2a	C	0.745411	0.859962	0.687133	Uiso	0.055	8	0.5584	d	.	.	.
C2b	C	0.81724	0.819153	0.690414	Uiso	0.0751	8	0.4416	d	.	.	.
C5a	C	0.509455	0.708497	0.662384	Uiso	0.0738	8	0.5584	d	.	.	.
C5b	C	0.549983	0.743551	0.651327	Uiso	0.0694	8	0.4416	d	.	.	.
C1a	C	0.619521	0.883174	0.71521	Uiso	0.0574	8	0.5584	d	.	.	.
C1b	C	0.700229	0.878433	0.709971	Uiso	0.0617	8	0.4416	d	.	.	.
C6a	C	0.50031	0.809207	0.698812	Uiso	0.0752	8	0.5584	d	.	.	.
C6b	C	0.562615	0.847446	0.687264	Uiso	0.0814	8	0.4416	d	.	.	.
C7	C	0.657516	0.768245	0.495148	Uani	0.0349	8	1	d	.	.	.
C9a	C	1.081318	0.533966	0.633312	Uiso	0.075	8	0.4495	d	.	.	.
C9b	C	0.232214	0.595934	0.612337	Uiso	0.0622	8	0.5505	d	.	.	.
C10a	C	1.113729	0.689242	0.659806	Uiso	0.0613	8	0.4495	d	.	.	.
C10b	C	0.666666	0.794542	0.346524	Uiso	0.0701	8	0.5505	d	.	.	.

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

Atom site label	Atom site symbol	U11	U22	U33	U12	U13	U23
S1	S	0.025921	0.033207	0.135182	-0.007455	0.002629	-0.003211
Cl1a	Cl	0.107192	0.049069	0.188371	-0.011685	-0.000791	-0.020244
Cl1b	Cl	0.109123	0.052809	0.139281	0.008872	-0.007445	-0.010635
O1	O	0.040235	0.034302	0.072604	-0.009857	0.013256	-0.004347
O3	O	0.024293	0.030905	0.144946	0.000665	-0.005627	-0.001466
O2	O	0.021507	0.041326	0.172467	0.004521	0.00769	-0.005948
N2	N	0.041859	0.032795	0.038741	-0.004067	-0.005564	-0.012898
N1	N	0.027544	0.036859	0.082088	-0.00359	0.005489	-0.007725
C7	C	0.028951	0.036798	0.039038	-0.003855	0.012237	-0.00681

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

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

Atom site label	Center (x0)	Width
Cl1a	0.0279	0.5584
Cl1b	0.5287	0.4416
C3a	-0.0388	0.5584
C3b	0.4485	0.4416
C4a	-0.0598	0.5584
C4b	0.4388	0.4416
C2a	-0.013	0.5584
C2b	0.4756	0.4416
C5a	-0.0552	0.5584
C5b	0.4546	0.4416
C1a	-0.0066	0.5584
C1b	0.4921	0.4416
C6a	-0.0271	0.5584
C6b	0.4835	0.4416
C9a	0.2525	0.4495
C9b	0.7697	0.5505
C10a	0.2957	0.4495
C10b	0.825	0.5505

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

Modulation code	Atom site label	Displacement axis	Wave vector code
S1x1	S1	x	1
S1y1	S1	y	1
S1z1	S1	z	1
S1x2	S1	x	2
S1y2	S1	y	2
S1z2	S1	z	2
O1x1	O1	x	1
O1y1	O1	y	1
O1z1	O1	z	1
O1x2	O1	x	2
O1y2	O1	y	2
O1z2	O1	z	2
O3x1	O3	x	1
O3y1	O3	y	1
O3z1	O3	z	1
O3x2	O3	x	2
O3y2	O3	y	2
O3z2	O3	z	2
O2x1	O2	x	1
O2y1	O2	y	1
O2z1	O2	z	1
O2x2	O2	x	2
O2y2	O2	y	2
O2z2	O2	z	2
N2x1	N2	x	1
N2y1	N2	y	1
N2z1	N2	z	1
N2x2	N2	x	2
N2y2	N2	y	2
N2z2	N2	z	2
N1x1	N1	x	1
N1y1	N1	y	1
N1z1	N1	z	1
N1x2	N1	x	2
N1y2	N1	y	2
N1z2	N1	z	2
C8x1	C8	x	1
C8y1	C8	y	1
C8z1	C8	z	1
C8x2	C8	x	2
C8y2	C8	y	2
C8z2	C8	z	2
C7x1	C7	x	1
C7y1	C7	y	1
C7z1	C7	z	1
C7x2	C7	x	2
C7y2	C7	y	2
C7z2	C7	z	2

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

Modulation code	Cosine coefficient	Sine coefficient
S1x1	0.0032	-0.0185
S1y1	0.0021	0.0142
S1z1	-0.0034	-0.0032
S1x2	-0.0022	0.004
S1y2	0.0002	0.0004
S1z2	0.0004	0.0004
O1x1	-0.0005	-0.0191
O1y1	0.0057	0.0123
O1z1	-0.0023	-0.0065
O1x2	0.001	0.0047
O1y2	-0.0019	-0.0012
O1z2	0.0002	0.0001
O3x1	-0.0006	-0.0099
O3y1	0.0011	-0.0003
O3z1	-0.0017	-0.0073
O3x2	-0.0068	-0.0008
O3y2	0.0009	0.001
O3z2	0.0021	0.0011
O2x1	-0.0005	-0.0164
O2y1	0.0008	0.0147
O2z1	-0.0039	-0.0006
O2x2	-0.0022	0.0055
O2y2	-0.0003	0.0004
O2z2	-0.0002	0.0001
N2x1	-0.0034	-0.0094
N2y1	-0.0011	0.0123
N2z1	0.0032	-0.0051
N2x2	-0.0048	-0.0055
N2y2	0.0014	-0.0003
N2z2	-0.0004	0.0007
N1x1	0.0011	-0.0131
N1y1	-0.0007	0.0099
N1z1	-0.0011	-0.007
N1x2	-0.0064	0.0007
N1y2	-0.001	-0.001
N1z2	0.0009	0.0026
C8x1	-0.0021	-0.0069
C8y1	-0.0032	0.0112
C8z1	0.0039	-0.0037
C8x2	-0.0039	-0.0057
C8y2	0.0041	-0.0008
C8z2	0.0004	-0.0001
C7x1	0.0001	-0.0096
C7y1	0.0011	0.0088
C7z1	-0.0021	-0.0065
C7x2	-0.0057	-0.0008
C7y2	-0.0009	0.0008
C7z2	0.0006	0.0003

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

Atom site label	Displacement axis	Polynomial order	Polynomial coeff.
Cl1a	x	1	0.0335
Cl1a	y	1	0.0038
Cl1a	z	1	0.0017
Cl1a	x	2	0.0251
Cl1a	y	2	0.0022
Cl1a	z	2	0.0002
Cl1b	x	1	-0.017
Cl1b	y	1	0.0024
Cl1b	z	1	0.002
Cl1b	x	2	-0.0138
Cl1b	y	2	-0.0026
Cl1b	z	2	0.0003
C3a	x	1	0.0154
C3a	y	1	0.0177
C3a	z	1	-0.005
C3a	x	2	0.0183
C3a	y	2	-0.0024
C3a	z	2	0.0006
C3b	x	1	-0.0242
C3b	y	1	-0.0183
C3b	z	1	0.0085
C3b	x	2	-0.0156
C3b	y	2	-0.0022
C3b	z	2	0.0003
C4a	x	1	0.0263
C4a	y	1	-0.0234
C4a	z	1	0.01
C4a	x	2	0.0255
C4a	y	2	0.0011
C4a	z	2	0.001
C4b	x	1	-0.0205
C4b	y	1	0.0165
C4b	z	1	-0.0025
C4b	x	2	-0.0102
C4b	y	2	-0.0028
C4b	z	2	0.0004
C2a	x	1	0.0198
C2a	y	1	0.0252
C2a	z	1	-0.0071
C2a	x	2	0.0187
C2a	y	2	-0.0017
C2a	z	2	0.0003
C2b	x	1	-0.0249
C2b	y	1	-0.0257
C2b	z	1	0.0109
C2b	x	2	-0.0176
C2b	y	2	-0.002
C2b	z	2	0.0003
C5a	x	1	0.047
C5a	y	1	-0.0539
C5a	z	1	0.0225
C5a	x	2	0.0326
C5a	y	2	0.0054
C5a	z	2	0.0009
C5b	x	1	-0.0208
C5b	y	1	0.0487
C5b	z	1	-0.0128
C5b	x	2	-0.0053
C5b	y	2	-0.0032
C5b	z	2	0.0003
C1a	x	1	0.035
C1a	y	1	-0.0071
C1a	z	1	0.0054
C1a	x	2	0.0261
C1a	y	2	0.0021
C1a	z	2	0.0004
C1b	x	1	-0.0224
C1b	y	1	0.0057
C1b	z	1	0.0009
C1b	x	2	-0.0129
C1b	y	2	-0.0025
C1b	z	2	0.0003
C6a	x	1	0.0451
C6a	y	1	-0.05
C6a	z	1	0.0209
C6a	x	2	0.0338
C6a	y	2	0.0055
C6a	z	2	0.0009
C6b	x	1	-0.0162
C6b	y	1	0.0419
C6b	z	1	-0.0105
C6b	x	2	-0.0073
C6b	y	2	-0.0035
C6b	z	2	0.0004
C9a	x	1	-0.0118
C9a	y	1	0.0113
C9a	z	1	-0.0026
C9a	x	2	0.0062
C9a	y	2	-0.0015
C9a	z	2	-0.0077
C9b	x	1	0.0108
C9b	y	1	-0.0036
C9b	z	1	-0.0002
C9b	x	2	-0.0237
C9b	y	2	-0.0148
C9b	z	2	-0.0004
C10a	x	1	-0.0197
C10a	y	1	0.0078
C10a	z	1	-0.0012
C10a	x	2	0.0231
C10a	y	2	0.007
C10a	z	2	-0.0042
C10b	x	1	-0.0147
C10b	y	1	-0.0078
C10b	z	1	0.0043
C10b	x	2	-0.0195
C10b	y	2	0.0095
C10b	z	2	-0.0034