A differential thermal expansion approach to crystal structure determination from powder diffraction data

Differential thermal expansion over the range 90-210 K has been applied successfully to determine the crystal structure of chlorothiazide from synchrotron powder diffraction data using direct methods. Key to the success of the approach is the use of a multi-data-set Pawley refinement to extract a set of reflection intensities that is more `single-crystal-like' than those extracted from a single data set. The improvement in reflection intensity estimates is quantified by comparison with reference single-crystal intensities.

Computing details

Figures

(90K)

Crystal data

?	β = 83.90 (3)°
Mr = ?	γ = 80.53 (3)°
Triclinic, P1	V = 260.25 Å^3
a = 4.8481 (16) Å	Z = ?
b = 6.359 (2) Å	? radiation, λ = ? Å
c = 8.900 (3) Å	× × mm
α = 74.49 (3)°

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

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

	x	y	z	Biso*/Beq
CL1	0.369772	0.935426	0.68618
S1	1.3203	0.595478	0.244913
S2	0.705557	0.430639	0.796024
C2	0.927836	0.902929	0.331621
C5	0.784252	0.618842	0.616897
O2	1.1975	0.46084	0.172209
N2	1.00254	1.04866	0.192304
H2	0.899913	1.17881	0.164898
O4	0.876994	0.225815	0.79456
O3	0.408912	0.436902	0.818177
C1	1.22541	0.999546	0.097153
H1	1.26777	1.1148	0.009009
O1	1.56971	0.495338	0.322402
C4	1.00066	0.551363	0.518144
H4	1.10195	0.407117	0.548062
C7	0.711864	0.974484	0.430439
H7	0.613998	1.12002	0.401104
C3	1.07082	0.691569	0.376592
N1	1.3883	0.812999	0.112322
C6	0.641057	0.834134	0.57017
N3	0.802353	0.51678	0.933394
H1NA	0.693914	0.632464	0.94969
H1NB	0.963804	0.539018	0.922739

(120K)

Crystal data

?	β = 83.93 (3)°
Mr = ?	γ = 80.56 (3)°
Triclinic, P1	V = 262.38 Å^3
a = 4.8619 (17) Å	Z = ?
b = 6.377 (2) Å	? radiation, λ = ? Å
c = 8.926 (3) Å	× × mm
α = 74.40 (3)°

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

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

	x	y	z	Biso*/Beq
S1	0.483999	0.000687	0.018508
CL1	−0.46423	0.340578	0.459874
S2	−0.129971	−0.164135	0.56956
C2	0.091964	0.309076	0.105347
C5	−0.052066	0.024653	0.389852
O3	0.041833	−0.368626	0.568026
O4	−0.426591	−0.157508	0.592147
O2	0.360972	−0.133573	−0.053653
N2	0.168072	0.453751	−0.034125
H2A	0.066648	0.583886	−0.062018
C4	0.164763	−0.043191	0.290984
H4A	0.265657	−0.187114	0.320954
C1	0.390526	0.403533	−0.128638
H1A	0.433838	0.518631	−0.216321
O1	0.733495	−0.100157	0.095629
C3	0.234373	0.096568	0.150008
C7	−0.123757	0.380029	0.204241
H7A	−0.221452	0.525205	0.17525
N3	−0.034286	−0.078019	0.706656
C6	−0.193816	0.239135	0.343352
N1	0.551375	0.217806	−0.114079
H1NB	0.12641	−0.059254	0.700941
H1NA	−0.141109	0.034509	0.723199

(150K)

Crystal data

?	β = 83.786 (14)°
Mr = ?	γ = 80.459 (15)°
Triclinic, P1	V = 264.01 Å^3
a = 4.8707 (9) Å	Z = ?
b = 6.3951 (12) Å	? radiation, λ = ? Å
c = 8.9448 (16) Å	× × mm
α = 74.368 (16)°

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

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

	x	y	z	Biso*/Beq
CL1	0.372441	0.935326	0.686121
S1	1.31845	0.595217	0.245036
S2	0.705591	0.431029	0.795886
C2	0.927855	0.902666	0.332384
C5	0.784411	0.619305	0.617006
O2	1.19533	0.461365	0.173047
N2	1.00468	1.04806	0.1935
H2	0.904485	1.17855	0.166766
O4	0.877548	0.226046	0.794328
O3	0.408958	0.437656	0.818207
C1	1.22734	0.997954	0.09715
H1	1.27021	1.11229	0.009169
O1	1.56817	0.494737	0.321805
C4	0.999716	0.55182	0.517714
H4	1.10022	0.4081	0.547511
C7	0.712636	0.974673	0.431082
H7	0.615169	1.11957	0.402162
C3	1.06964	0.690637	0.376408
N1	1.38559	0.812863	0.112375
C6	0.643793	0.834128	0.569899
N3	0.802057	0.517396	0.932325
H1NA	0.69072	0.633848	0.94607
H1NB	0.963473	0.529243	0.92617

(180K)

Crystal data

?	β = 83.751 (15)°
Mr = ?	γ = 80.449 (16)°
Triclinic, P1	V = 264.79 Å^3
a = 4.8737 (9) Å	Z = ?
b = 6.4046 (13) Å	? radiation, λ = ? Å
c = 8.9548 (16) Å	× × mm
α = 74.324 (17)°

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

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

	x	y	z	Biso*/Beq
CL1	0.374098	0.935323	0.686239
S1	1.3175	0.594964	0.245076
S2	0.70553	0.431244	0.795755
C2	0.928658	0.902243	0.332499
C5	0.784199	0.619378	0.617053
O2	1.19481	0.461573	0.173222
N2	1.00538	1.04853	0.19309
H2	0.905779	1.17905	0.166196
O4	0.876808	0.227122	0.794378
O3	0.410219	0.438026	0.818531
C1	1.22711	0.996953	0.097917
H1	1.27141	1.11107	0.01025
O1	1.56675	0.494796	0.321494
C4	0.998805	0.551984	0.517105
H4	1.09817	0.408006	0.546504
C7	0.714148	0.975043	0.430971
H7	0.618039	1.12022	0.402241
C3	1.06993	0.690729	0.375892
N1	1.38458	0.811182	0.112616
C6	0.644153	0.834269	0.56959
N3	0.80192	0.517726	0.932554
H1NA	0.694163	0.637021	0.943993
H1NB	0.956567	0.532662	0.92064

(210K)

Crystal data

?	β = 83.693 (15)°
Mr = ?	γ = 80.445 (16)°
Triclinic, P1	V = 265.64 Å^3
a = 4.8786 (9) Å	Z = ?
b = 6.4126 (13) Å	? radiation, λ = ? Å
c = 8.9665 (16) Å	× × mm
α = 74.266 (16)°

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

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

	x	y	z	Biso*/Beq
CL1	0.375527	0.935381	0.686169
S1	1.31665	0.594861	0.245163
S2	0.705626	0.431448	0.795608
C2	0.929249	0.902232	0.332325
C5	0.784079	0.61824	0.616993
O2	1.19368	0.46197	0.173647
N2	1.00644	1.04764	0.193981
H2	0.908491	1.17677	0.167807
O4	0.876937	0.227723	0.794263
O3	0.410194	0.437885	0.818622
C1	1.22745	0.997004	0.098226
H1	1.27045	1.11005	0.011458
O1	1.56558	0.494577	0.321188
C4	0.99656	0.551196	0.517412
H4	1.09373	0.408472	0.546101
C7	0.714451	0.974985	0.431125
H7	0.619013	1.11833	0.402692
C3	1.06867	0.690352	0.376375
N1	1.38463	0.812173	0.112628
C6	0.645016	0.833515	0.570562
N3	0.802137	0.517235	0.931508
H1NA	0.693038	0.645589	0.94504
H1NB	0.956656	0.530801	0.926158