Table 1 Experimental crystallographic and refinement data of the five VMN polymorph crystal structures solved in this work[a].

From: Direct structure determination of vemurafenib polymorphism from compact spherulites using 3D electron diffraction

 

α-VMN

β-VMN

γ-VMN

δ-VMN

ε-VMN

Discovery, year[b]

SC, 201584

MC, 201633

MC, 201633

MC, 201633

MC, this work

Structure

SCXRD,

3D ED,

SCXRD,

3D ED,

SCXRD,

3D ED,

3D ED,

3D ED,

elucidation, year[c]

This work

This work

This work

This work

This work

This work

This work

This work

Sample type[d]

SC

CS

SC

CS

SC

CS

CS

CS

CCDC No.

1893045

2169341

1893062

2169342

1893054

2169343

2169349

2169344

Temperature (K)

298

293

298

293

250

293

293

293

Crystal system

Monoclinic

Monoclinic

Triclinic

Monoclinic

Monoclinic

Space group

P21/n (14)

P21/c (14)

P\(\bar{1}\) (2)

P21/c (14)

P21 (4)

Z’, Z

1, 4

2, 8

1, 2

1, 4

2, 4

a (Å)

19.1792(2)

9.9495(1)

7.6759(1)

14.0790(1)

4.885(1)

b (Å)

5.6702(1)

13.0705(1)

10.3177(1)

8.5200(1)

22.377(1)

c (Å)

20.1250(2)

35.8432(3)

14.9190(2)

21.5220(1)

20.428 (1)

α (°)

90

90

98.481(1)

90

90

β (°)

96.096(1)

94.439(1)

100.478(1)

109.931(1)

94.952(2)

γ (°)

90

90

105.475(1)

90

90

Volume (Å3)

2176.22

4647.24

1095.51

2427.00

2224.70

Density (g·cm−3)

1.495

1.400

1.485

1.341

1.463

Total reflections

12783

10182

47896

9875

20854

10606

565 (653)

4912

Unique reflections

4284

2361

9370

3840

4419

3284

288 (230)

2783

Resolution (Å)

0.79

0.90

0.79

1.00

0.79

0.80

1.4 (2.0)

1.05

Completeness (%)

99.8

75.4

99.8

79.1

99.9

72.6

34.4 (71.0)

73.9

Rint

0.0337

0.1788

0.0285

0.1305

0.0298

0.2033

0.1160 (0.1478)

0.186

I/sigma

26

4.68

42.4

3.78

50.8

3.31

3.66 (8.40)

5.30

CC1/2[e]

NA

98.2

NA

98.7

NA

96.9

98.0 (98.5)

97.8

No. of parameters

299

299

597

507

299

299

97

268

No. of restraints

0

12

3

226

0

48

97

303

R1 (all)

0.0475

0.2321

0.0683

0.2720

0.0428

0.2540

0.3339

0.2754

wR2

0.1247

0.4200

0.1829

0.4816

0.1100

0.4277

0.6269

0.4745

No. of datasets

1

3

1

2

1

6

1 (4)

3

RMSD15 (Å) [f]

0.091

0.117

0.17

0.208

0.113

0.164

0.418

0.271

  1. [a]The unit cell parameters of α-, β- and γ-VMN are taken from the SCXRD data, whilst those of δ- and ε-VMN were refined against the PXRD data. The values for δ-VMN are the data used for the structure refinement (1.4 Å), whilst the values in parentheses are the data used during simulated annealing for the structure solution (2 Å).
  2. [b]Year and method of discovery: SC, solution crystallization; MC, melt crystallization.
  3. [c]Method used for structure elucidation: SCXRD, single-crystal X-ray diffraction; 3D ED, 3D electron diffraction.
  4. [d]Sample type used for structure elucidation: SC, single crystal; CS, compact spherulite.
  5. [e]NA, not available.
  6. [f]RMSD15 values are calculated between the experimental structure and the density functional theory (DFT) energy minimized structures using Mercury software.
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