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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889808030872/hx5075sup1.cif
Contains datablocks 90K, 120K, 150K, 180K, 210K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0021889808030872/hx507590Ksup2.hkl
Contains datablock 90K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0021889808030872/hx5075120Ksup3.hkl
Contains datablock 120K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0021889808030872/hx5075150Ksup4.hkl
Contains datablock 150K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0021889808030872/hx5075180Ksup5.hkl
Contains datablock 180K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0021889808030872/hx5075210Ksup6.hkl
Contains datablock 210K

txt

Text file https://doi.org/10.1107/S0021889808030872/hx5075sup7.txt
DASH xye file for chlorothiazide at 90 K

txt

Text file https://doi.org/10.1107/S0021889808030872/hx5075sup8.txt
DASH xye file for chlorothiazide at 120 K

txt

Text file https://doi.org/10.1107/S0021889808030872/hx5075sup9.txt
DASH xye file for chlorothiazide at 150 K

txt

Text file https://doi.org/10.1107/S0021889808030872/hx5075sup10.txt
DASH xye file for chlorothiazide at 180 K

txt

Text file https://doi.org/10.1107/S0021889808030872/hx5075sup11.txt
DASH xye file for chlorothiazide at 210 K

txt

Text file https://doi.org/10.1107/S0021889808030872/hx5075sup12.txt
SHELX res file for chlorothiazide at 90 K

txt

Text file https://doi.org/10.1107/S0021889808030872/hx5075sup13.txt
SHELX res file for chlorothiazide at 120 K

txt

Text file https://doi.org/10.1107/S0021889808030872/hx5075sup14.txt
SHELX res file for chlorothiazide at 150 K

txt

Text file https://doi.org/10.1107/S0021889808030872/hx5075sup15.txt
SHELX res file for chlorothiazide at 180 K

txt

Text file https://doi.org/10.1107/S0021889808030872/hx5075sup16.txt
SHELX res file for chlorothiazide at 210 K

CCDC references: 723184; 723185; 723186; 723187; 723188

Computing details top

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
(90K) top
Crystal data top
?β = 83.90 (3)°
Mr = ?γ = 80.53 (3)°
Triclinic, P1V = 260.25 Å3
a = 4.8481 (16) ÅZ = ?
b = 6.359 (2) Å? radiation, λ = ? Å
c = 8.900 (3) Å × × mm
α = 74.49 (3)°
Data collection top
h = ??l = ??
k = ??
Refinement top
Crystal data top
?β = 83.90 (3)°
Mr = ?γ = 80.53 (3)°
Triclinic, P1V = 260.25 Å3
a = 4.8481 (16) ÅZ = ?
b = 6.359 (2) Å? radiation, λ = ? Å
c = 8.900 (3) Å × × mm
α = 74.49 (3)°
Data collection top
Refinement top
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
CL10.3697720.9354260.68618
S11.32030.5954780.244913
S20.7055570.4306390.796024
C20.9278360.9029290.331621
C50.7842520.6188420.616897
O21.19750.460840.172209
N21.002541.048660.192304
H20.8999131.178810.164898
O40.8769940.2258150.79456
O30.4089120.4369020.818177
C11.225410.9995460.097153
H11.267771.11480.009009
O11.569710.4953380.322402
C41.000660.5513630.518144
H41.101950.4071170.548062
C70.7118640.9744840.430439
H70.6139981.120020.401104
C31.070820.6915690.376592
N11.38830.8129990.112322
C60.6410570.8341340.57017
N30.8023530.516780.933394
H1NA0.6939140.6324640.94969
H1NB0.9638040.5390180.922739
(120K) top
Crystal data top
?β = 83.93 (3)°
Mr = ?γ = 80.56 (3)°
Triclinic, P1V = 262.38 Å3
a = 4.8619 (17) ÅZ = ?
b = 6.377 (2) Å? radiation, λ = ? Å
c = 8.926 (3) Å × × mm
α = 74.40 (3)°
Data collection top
h = ??l = ??
k = ??
Refinement top
Crystal data top
?β = 83.93 (3)°
Mr = ?γ = 80.56 (3)°
Triclinic, P1V = 262.38 Å3
a = 4.8619 (17) ÅZ = ?
b = 6.377 (2) Å? radiation, λ = ? Å
c = 8.926 (3) Å × × mm
α = 74.40 (3)°
Data collection top
Refinement top
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
S10.4839990.0006870.018508
CL10.464230.3405780.459874
S20.1299710.1641350.56956
C20.0919640.3090760.105347
C50.0520660.0246530.389852
O30.0418330.3686260.568026
O40.4265910.1575080.592147
O20.3609720.1335730.053653
N20.1680720.4537510.034125
H2A0.0666480.5838860.062018
C40.1647630.0431910.290984
H4A0.2656570.1871140.320954
C10.3905260.4035330.128638
H1A0.4338380.5186310.216321
O10.7334950.1001570.095629
C30.2343730.0965680.150008
C70.1237570.3800290.204241
H7A0.2214520.5252050.17525
N30.0342860.0780190.706656
C60.1938160.2391350.343352
N10.5513750.2178060.114079
H1NB0.126410.0592540.700941
H1NA0.1411090.0345090.723199
(150K) top
Crystal data top
?β = 83.786 (14)°
Mr = ?γ = 80.459 (15)°
Triclinic, P1V = 264.01 Å3
a = 4.8707 (9) ÅZ = ?
b = 6.3951 (12) Å? radiation, λ = ? Å
c = 8.9448 (16) Å × × mm
α = 74.368 (16)°
Data collection top
h = ??l = ??
k = ??
Refinement top
Crystal data top
?β = 83.786 (14)°
Mr = ?γ = 80.459 (15)°
Triclinic, P1V = 264.01 Å3
a = 4.8707 (9) ÅZ = ?
b = 6.3951 (12) Å? radiation, λ = ? Å
c = 8.9448 (16) Å × × mm
α = 74.368 (16)°
Data collection top
Refinement top
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
CL10.3724410.9353260.686121
S11.318450.5952170.245036
S20.7055910.4310290.795886
C20.9278550.9026660.332384
C50.7844110.6193050.617006
O21.195330.4613650.173047
N21.004681.048060.1935
H20.9044851.178550.166766
O40.8775480.2260460.794328
O30.4089580.4376560.818207
C11.227340.9979540.09715
H11.270211.112290.009169
O11.568170.4947370.321805
C40.9997160.551820.517714
H41.100220.40810.547511
C70.7126360.9746730.431082
H70.6151691.119570.402162
C31.069640.6906370.376408
N11.385590.8128630.112375
C60.6437930.8341280.569899
N30.8020570.5173960.932325
H1NA0.690720.6338480.94607
H1NB0.9634730.5292430.92617
(180K) top
Crystal data top
?β = 83.751 (15)°
Mr = ?γ = 80.449 (16)°
Triclinic, P1V = 264.79 Å3
a = 4.8737 (9) ÅZ = ?
b = 6.4046 (13) Å? radiation, λ = ? Å
c = 8.9548 (16) Å × × mm
α = 74.324 (17)°
Data collection top
h = ??l = ??
k = ??
Refinement top
Crystal data top
?β = 83.751 (15)°
Mr = ?γ = 80.449 (16)°
Triclinic, P1V = 264.79 Å3
a = 4.8737 (9) ÅZ = ?
b = 6.4046 (13) Å? radiation, λ = ? Å
c = 8.9548 (16) Å × × mm
α = 74.324 (17)°
Data collection top
Refinement top
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
CL10.3740980.9353230.686239
S11.31750.5949640.245076
S20.705530.4312440.795755
C20.9286580.9022430.332499
C50.7841990.6193780.617053
O21.194810.4615730.173222
N21.005381.048530.19309
H20.9057791.179050.166196
O40.8768080.2271220.794378
O30.4102190.4380260.818531
C11.227110.9969530.097917
H11.271411.111070.01025
O11.566750.4947960.321494
C40.9988050.5519840.517105
H41.098170.4080060.546504
C70.7141480.9750430.430971
H70.6180391.120220.402241
C31.069930.6907290.375892
N11.384580.8111820.112616
C60.6441530.8342690.56959
N30.801920.5177260.932554
H1NA0.6941630.6370210.943993
H1NB0.9565670.5326620.92064
(210K) top
Crystal data top
?β = 83.693 (15)°
Mr = ?γ = 80.445 (16)°
Triclinic, P1V = 265.64 Å3
a = 4.8786 (9) ÅZ = ?
b = 6.4126 (13) Å? radiation, λ = ? Å
c = 8.9665 (16) Å × × mm
α = 74.266 (16)°
Data collection top
h = ??l = ??
k = ??
Refinement top
Crystal data top
?β = 83.693 (15)°
Mr = ?γ = 80.445 (16)°
Triclinic, P1V = 265.64 Å3
a = 4.8786 (9) ÅZ = ?
b = 6.4126 (13) Å? radiation, λ = ? Å
c = 8.9665 (16) Å × × mm
α = 74.266 (16)°
Data collection top
Refinement top
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
CL10.3755270.9353810.686169
S11.316650.5948610.245163
S20.7056260.4314480.795608
C20.9292490.9022320.332325
C50.7840790.618240.616993
O21.193680.461970.173647
N21.006441.047640.193981
H20.9084911.176770.167807
O40.8769370.2277230.794263
O30.4101940.4378850.818622
C11.227450.9970040.098226
H11.270451.110050.011458
O11.565580.4945770.321188
C40.996560.5511960.517412
H41.093730.4084720.546101
C70.7144510.9749850.431125
H70.6190131.118330.402692
C31.068670.6903520.376375
N11.384630.8121730.112628
C60.6450160.8335150.570562
N30.8021370.5172350.931508
H1NA0.6930380.6455890.94504
H1NB0.9566560.5308010.926158

Experimental details

(90K)(120K)(150K)(180K)
Crystal data
Chemical formula????
Mr????
Crystal system, space groupTriclinic, P1Triclinic, P1Triclinic, P1Triclinic, P1
Temperature (K)????
a, b, c (Å)4.8481 (16), 6.359 (2), 8.900 (3)4.8619 (17), 6.377 (2), 8.926 (3)4.8707 (9), 6.3951 (12), 8.9448 (16)4.8737 (9), 6.4046 (13), 8.9548 (16)
α, β, γ (°)74.49 (3), 83.90 (3), 80.53 (3)74.40 (3), 83.93 (3), 80.56 (3)74.368 (16), 83.786 (14), 80.459 (15)74.324 (17), 83.751 (15), 80.449 (16)
V3)260.25262.38264.01264.79
Z????
Radiation type?, λ = ? Å?, λ = ? Å?, λ = ? Å?, λ = ? Å
µ (mm1)????
Crystal size (mm) × × × × × × × ×
Data collection
Diffractometer????
Absorption correction????
No. of measured, independent and
observed (?) reflections
?, ?, ? ?, ?, ? ?, ?, ? ?, ?, ?
Rint????
Refinement
R[F2 > 2σ(F2)], wR(F2), S ?, ?, ? ?, ?, ? ?, ?, ? ?, ?, ?
No. of reflections????
No. of parameters????
No. of restraints????
Δρmax, Δρmin (e Å3)?, ??, ??, ??, ?


(210K)
Crystal data
Chemical formula?
Mr?
Crystal system, space groupTriclinic, P1
Temperature (K)?
a, b, c (Å)4.8786 (9), 6.4126 (13), 8.9665 (16)
α, β, γ (°)74.266 (16), 83.693 (15), 80.445 (16)
V3)265.64
Z?
Radiation type?, λ = ? Å
µ (mm1)?
Crystal size (mm) × ×
Data collection
Diffractometer?
Absorption correction?
No. of measured, independent and
observed (?) reflections
?, ?, ?
Rint?
Refinement
R[F2 > 2σ(F2)], wR(F2), S ?, ?, ?
No. of reflections?
No. of parameters?
No. of restraints?
Δρmax, Δρmin (e Å3)?, ?

 

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