Supplementary Information
Idealized powder diffraction patterns for cellulose polymorphs
Alfred D. French
Southern Regional Research Center, U.S. Department of Agriculture, 1100 Robert E. Lee Blvd.,
New Orleans, Louisiana, USA 70124 and Editor-in-Chief, Cellulose
Version of Tuesday, February 09, 2016, 7:07 PM
#Modified Crystal Information File for I cellulose (copy the contents for I into a text editor
like Notepad and save the file as a simple text file, e.g., cellulose_Ialpha.cif) for input to the
Mercury program. Alternatively, copy everything below into the text editor, save it as e.g.,
all_cellulose.cif, and Mercury will let you select the structure of your choice.
data_Ialpha
_audit_creation_method AD French axis conversion from Nishiyama Y, Sugiyama
J, Chanzy H, Langan P (2003) Crystal structure and hydrogen bonding system in
cellulose Ia, from synchrotron X-ray and neutron fiber diffraction. J Am Chem
Soc 125:14300–14306. DOI: 10.1021/ja037055w
_chemical_name_common
'cellulose I alpha'
_symmetry_cell_setting
_symmetry_space_group_name_H-M
'P1'
?
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
_cell_length_a
_cell_length_b
_cell_length_c
6.717(6)
5.962(7)
10.4000(5)
_cell_angle_alpha
_cell_angle_beta
_cell_angle_gamma
_cell_volume
_cell_formula_units_Z
118.08(5)
114.80(5)
80.37(5)
333.3(5)
1
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
H31 H -0.188(16) 0.235(13) -0.117(8) 0.008(9) Uiso 1 1 d D . .
H21A H -0.296(9) 0.40(2) 0.326(3) 0.008(9) Uiso 0.56(6) 1 d PD A 1
H21B H -0.430(14) 0.34(4) 0.115(14) 0.008(9) Uiso 0.44(6) 1 d PD A 2
H22A H 0.333(14) -0.23(3) 0.839(8) 0.008(9) Uiso 0.56(6) 1 d PD A 1
H22B H 0.451(8) -0.23(4) 0.71(2) 0.008(9) Uiso 0.44(6) 1 d PD A 2
H61A H 0.43(2) -0.559(12) -0.039(8) 0.008(9) Uiso 0.56(6) 1 d PD A 1
H61B H 0.25(2) -0.35(3) -0.129(6) 0.008(9) Uiso 0.44(6) 1 d PD A 2
H62A H -0.508(18) 0.51(2) 0.481(17) 0.008(9) Uiso 0.56(6) 1 d PD A 1
H62B H -0.245(13) 0.39(3) 0.45(2) 0.008(9) Uiso 0.44(6) 1 d PD A 2
H32 H 0.302(14) -0.148(9) 0.422(8) 0.008(9) Uiso 1 1 d D . .
O51 O 0.1516 -0.0442 0.2391 0.005(6) Uiso 1 1 d G . .
C11 C -0.0545 0.031 0.2536 0.005(6) Uiso 1 1 d G . .
H11 H -0.1585 -0.114 0.1973 0.006 Uiso 1 1 d G . .
O11 O -0.009 0.1569 0.4163 0.005(6) Uiso 1 1 d G . .
C21 C -0.1431 0.2337 0.193 0.005(6) Uiso 1 1 d GD A .
H21 H -0.0383 0.3792 0.255 0.006 Uiso 1 1 d G . .
C31 C -0.1743 0.1136 0.0215 0.005(6) Uiso 1 1 d GD . .
H31 H -0.2902 -0.0201 -0.0404 0.006 Uiso 1 1 d G . .
C41 C 0.0346 -0.003 -0.0003 0.005(6) Uiso 1 1 d G . .
H41 H 0.141 0.1359 0.0464 0.006 Uiso 1 1 d G . .
C51 C 0.1377 -0.1754 0.0794 0.005(6) Uiso 1 1 d G . .
H51 H 0.0485 -0.3333 0.022 0.006 Uiso 1 1 d G . .
C61 C 0.3736 -0.2361 0.0919 0.005(6) Uiso 1 1 d GD A .
H61A H 0.454 -0.0814 0.1302 0.006 Uiso 1 1 d G . .
H61B H 0.4464 -0.3072 0.1664 0.006 Uiso 1 1 d G . .
O21 O -0.3461 0.3131 0.2112 0.005(6) Uiso 1 1 d GD . .
O31 O -0.2431 0.3067 -0.0314 0.005(6) Uiso 1 1 d GD . .
O61 O 0.3714 -0.413 -0.0595 0.005(6) Uiso 1 1 d GD . .
O52 O -0.1584 0.0461 0.6796 0.005(6) Uiso 1 1 d G . .
C12 C 0.0478 -0.0255 0.7664 0.005(6) Uiso 1 1 d G . .
H12 H 0.1471 0.1231 0.8462 0.006 Uiso 1 1 d G . .
O12 O 0.0031 -0.1524 0.8366 0.005(6) Uiso 1 1 d G . .
C22 C 0.147 -0.2178 0.6499 0.005(6) Uiso 1 1 d GD A .
H22 H 0.0483 -0.368 0.5732 0.006 Uiso 1 1 d G . .
C32 C 0.1799 -0.0864 0.5661 0.005(6) Uiso 1 1 d GD . .
H32 H 0.2833 0.0593 0.6442 0.006 Uiso 1 1 d G . .
C42 C -0.0375 0.0079 0.4832 0.005(6) Uiso 1 1 d G . .
H42 H -0.1353 -0.1395 0.3980 0.006 Uiso 1 1 d G . .
C52 C -0.148 0.1747 0.5957 0.005(6) Uiso 1 1 d G . .
H52 H -0.0623 0.335 0.6716 0.006 Uiso 1 1 d G . .
C62 C -0.3823 0.2313 0.5122 0.005(6) Uiso 1 1 d GD A .
H62A H -0.46 0.0751 0.4236 0.006 Uiso 1 1 d G . .
H62B H -0.4562 0.2993 0.5849 0.006 Uiso 1 1 d G . .
O22 O 0.3522 -0.2877 0.7397 0.005(6) Uiso 1 1 d GD . .
O32 O 0.2697 -0.2607 0.455 0.005(6) Uiso 1 1 d GD . .
O62 O -0.3869 0.4092 0.4567 0.005(6) Uiso 1 1 dG D . .
#==END
#Simplified Crystal information file for Cellulose I
data_Ibeta
_audit_creation_method Adapted from Nishiyama Y, Langan P, Chanzy H (2002)
Crystal structure and hydrogen-bonding system in cellulose Ib from
synchrotron X-ray and neutron fiber diffraction. J Am Chem Soc
124(31):9074–9082. DOI:10.1021/ja0257319
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
_cell_length_a
_cell_length_b
_cell_length_c
_cell_angle_alpha
_cell_angle_beta
_cell_angle_gamma
_cell_volume
_cell_formula_units_Z
_cell_measurement_temperature
7.784(8)
8.201(8)
10.380(10)
90.00
90.00
96.55(5)
658.3(11)
2
293(2)
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.0138 -0.0415 0.0433 0.025(4) Uiso 1 1 d D . .
H11 H 0.1382 -0.0188 0.0598 0.030 Uiso 1 1 calc R . .
C21 C -0.0260 -0.1843 -0.0516 0.025(4) Uiso 1 1 d D . .
H21 H -0.1508 -0.2177 -0.0546 0.030 Uiso 1 1 calc R . .
C31 C 0.0403 -0.1369 -0.1848 0.025(4) Uiso 1 1 d D . .
H31 H 0.1667 -0.1323 -0.1840 0.030 Uiso 1 1 calc R . .
C41 C -0.0071 0.0304 -0.2250 0.025(4) Uiso 1 1 d D . .
H41 H -0.1316 0.0176 -0.2425 0.030 Uiso 1 1 calc R . .
C51 C 0.0258 0.1594 -0.1232 0.025(4) Uiso 1 1 d D . .
H51 H 0.1507 0.1821 -0.1090 0.030 Uiso 1 1 calc R . .
C61 C -0.0467 0.3187 -0.1529 0.025(4) Uiso 1 1 d D . .
H61A H -0.1672 0.2959 -0.1778 0.030 Uiso 1 1 calc R . .
H61B H -0.0407 0.3872 -0.0765 0.030 Uiso 1 1 calc R . .
O21 O 0.0609 -0.3144 -0.0003 0.025(4) Uiso 1 1 d D . .
H21A H 0.0366 -0.3194 0.0920 0.038 Uiso 1.0(2) 1 d PD . .
H21B H -0.0001 -0.3537 0.0771 0.038 Uiso 0.0(2) 1 d PD . .
O31 O -0.0268 -0.2607 -0.2759 0.025(4) Uiso 1 1 d D . .
H31 H 0.0475 -0.2400 -0.3517 0.038 Uiso 1 1 d D . .
O11 O 0.0786 0.0865 -0.3424 0.025(4) Uiso 1 1 d D . .
O51 O -0.0556 0.0991 -0.0053 0.025(4) Uiso 1 1 d D . .
O61 O 0.0480 0.4030 -0.2540 0.025(4) Uiso 1 1 d D . .
H61A H -0.0144 0.4924 -0.2850 0.038 Uiso 0.85(18) 1 d PD . .
H61B H 0.0292 0.3391 -0.3329 0.038 Uiso 0.15(18) 1 d PD . .
C12 C 0.5329 0.4548 0.3043 0.025(4) Uiso 1 1 d D . .
H12 H 0.6577 0.4616 0.3200 0.030 Uiso 1 1 calc R . .
C22 C 0.4745 0.3178 0.2094 0.025(4) Uiso 1 1 d D . .
H22 H 0.3480 0.3058 0.2052 0.030 Uiso 1 1 calc R . .
C32 C 0.5449 0.3626 0.0765 0.025(4) Uiso 1 1 d D . .
H32 H 0.6716 0.3753 0.0793 0.030 Uiso 1 1 calc R . .
C42 C 0.4823 0.5263 0.0375 0.025(4) Uiso 1 1 d D . .
H42 H 0.3561 0.5139 0.0289 0.030 Uiso 1 1 calc R . .
C52 C 0.5409 0.6574 0.1388 0.025(4) Uiso 1 1 d D . .
H52 H 0.6670 0.6830 0.1370 0.030 Uiso 1 1 calc R . .
C62 C 0.4523 0.8151 0.1125 0.025(4) Uiso 1 1 d D . .
H62A H 0.3341 0.7843 0.0847 0.030 Uiso 1 1 calc R . .
H62B H 0.4491 0.8778 0.1916 0.030 Uiso 1 1 calc R . .
O22 O 0.5277 0.1664 0.2520 0.025(4) Uiso 1 1 d D . .
H22A H 0.5035 0.1593 0.3448 0.038 Uiso 0.57(14) 1 d PD . .
H22B H 0.4667 0.0793 0.1994 0.038 Uiso 0.43(14) 1 d PD . .
O32 O 0.4865 0.2326 -0.0081 0.025(4) Uiso 1 1 d D . .
H32 H 0.5104 0.2733 -0.0961 0.038 Uiso 1 1 d D . .
O12 O 0.5625 0.5859 -0.0806 0.025(4) Uiso 1 1 d D . .
O52 O 0.4850 0.6070 0.2639 0.025(4) Uiso 1 1 d D . .
O62 O 0.5420 0.9137 0.0169 0.025(4) Uiso 1 1 d D . .
H62A H 0.5184 1.0275 0.0326 0.038 Uiso 0.68(16) 1 d PD . .
H62B H 0.5345 0.8543 -0.0646 0.038 Uiso 0.32(16) 1 d PD . .
#==END
#Simplified Crystal Information File for Cellulose II.
data_cellii
_audit_creation_method
Adapted from Langan P, Nishiyama Y, Chanzy
H (2001) X-ray structure of mercerized cellulose II at 1 Å resolution.
Biomacromolecules 2:410–416. DOI:10.1021/bm005612q
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
_cell_length_a
_cell_length_b
_cell_length_c
_cell_angle_alpha
_cell_angle_beta
_cell_angle_gamma
8.10(5)
9.03(5)
10.31(5)
90.00
90.00
117.10(5)
_cell_volume
_cell_formula_units_Z
_cell_measurement_temperature
_exptl_crystal_density_diffrn
_exptl_crystal_density_method
_exptl_crystal_F_000
_exptl_absorpt_coefficient_mu
671(6)
2
293(2)
1.634
'not measured'
356
0.143
_diffrn_ambient_temperature
293(2)
_diffrn_radiation_wavelength
0.72080
_diffrn_radiation_type
?
_diffrn_radiation_source
'fine-focus sealed tube'
_diffrn_radiation_monochromator
graphite
_diffrn_reflns_number
235
_diffrn_reflns_av_R_equivalents
0.0000
_diffrn_reflns_av_sigmaI/netI
0.0671
_reflns_number_total
235
_reflns_number_gt
228
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C -0.043(6) 0.007(7) 0.381(2) 0.06(3) Uiso 1 1 d DU . .
H11 H -0.1257 -0.1115 0.3924 0.072 Uiso 1 1 calc R . .
C21 C -0.125(7) 0.086(7) 0.286(3) 0.05(2) Uiso 1 1 d DU . .
H21 H -0.0411 0.2049 0.2764 0.056 Uiso 1 1 calc R . .
C31 C -0.151(7) -0.003(9) 0.156(3) 0.05(2) Uiso 1 1 d DU . .
H31 H -0.2396 -0.1205 0.1677 0.066 Uiso 1 1 calc R . .
O21 O -0.299(7) 0.062(8) 0.334(4) 0.029(18) Uiso 1 1 d DU . .
H21A H -0.3801 0.0096 0.2806 0.043 Uiso 1 1 calc R . .
C41 C 0.034(7) 0.008(8) 0.112(3) 0.05(2) Uiso 1 1 d DU . .
H41 H 0.1198 0.1243 0.0929 0.055 Uiso 1 1 calc R . .
O31 O -0.224(10) 0.069(12) 0.066(4) 0.06(3) Uiso 1 1 d DU . .
H31A H -0.2428 0.0189 -0.0036 0.094 Uiso 1 1 calc R . .
C51 C 0.118(9) -0.057(9) 0.216(3) 0.04(2) Uiso 1 1 d DU . .
H51 H 0.0297 -0.1731 0.2320 0.046 Uiso 1 1 calc R . .
O11 O 0.011(6) -0.091(6) -0.001(2) 0.038(17) Uiso 1 1 d DU . .
O51 O 0.133(6) 0.034(8) 0.333(3) 0.047(18) Uiso 1 1 d DU . .
C61 C 0.298(13) -0.053(13) 0.183(5) 0.07(3) Uiso 1 1 d DU . .
H61A H 0.2935 -0.0928 0.0947 0.083 Uiso 1 1 calc R . .
H61B H 0.3960 0.0603 0.1874 0.083 Uiso 1 1 calc R . .
O61 O 0.337(12) -0.155(12) 0.270(8) 0.08(3) Uiso 1 1 d DU . .
H61 H 0.3446 -0.1196 0.3443 0.123 Uiso 1 1 calc R . .
C12 C 0.468(6) 0.522(6) -0.150(2) 0.04(2) Uiso 1 1 d DU . .
H12 H 0.5652 0.6374 -0.1577 0.049 Uiso 1 1 calc R . .
C22 C 0.318(7) 0.506(8) -0.054(3) 0.028(19) Uiso 1 1 d DU . .
H22 H 0.2243 0.3886 -0.0506 0.034 Uiso 1 1 calc R . .
C32 C 0.398(7) 0.559(8) 0.082(3) 0.04(2) Uiso 1 1 d DU . .
H32 H 0.4800 0.6792 0.0821 0.052 Uiso 1 1 calc R . .
O22 O 0.230(8) 0.603(9) -0.092(4) 0.038(19) Uiso 1 1 d DU . .
H22A H 0.2397 0.6679 -0.0333 0.057 Uiso 1 1 calc R . .
C42 C 0.509(6) 0.468(7) 0.119(3) 0.030(19) Uiso 1 1 d DU . .
H42 H 0.4232 0.3516 0.1370 0.036 Uiso 1 1 calc R . .
O32 O 0.250(8) 0.523(9) 0.170(4) 0.05(2) Uiso 1 1 d DU . .
H32A H 0.2909 0.5499 0.2434 0.076 Uiso 1 1 calc R . .
C52 C 0.640(7) 0.474(10) 0.011(3) 0.034(18) Uiso 1 1 d DU . .
H52 H 0.7246 0.5920 -0.0036 0.040 Uiso 1 1 calc R . .
O12 O 0.621(5) 0.539(6) 0.232(2) 0.034(16) Uiso 1 1 d DU . .
O52 O 0.541(8) 0.413(8) -0.108(3) 0.050(17) Uiso 1 1 d DU . .
C62 C 0.757(12) 0.392(17) 0.037(5) 0.06(3) Uiso 1 1 d DU . .
H62A H 0.8256 0.4356 0.1166 0.075 Uiso 1 1 calc R . .
H62B H 0.6794 0.2739 0.0479 0.075 Uiso 1 1 calc R . .
O62 O 0.886(13) 0.418(15) -0.067(8) 0.10(3) Uiso 1 1 d DU . .
H62 H 0.8303 0.3600 -0.1288 0.143 Uiso 1 1 calc R . .
#END
#Created Crystal Information File for Cellulose IIII (copy the following into a text editor like
notepad and save the file as a simple text file, e.g., cellulose_III.cif, for input to the Mercury
program.)
data_celliii(i) by ADFrench (format based on output from CSD Conquest program
for methyl cellobioside)
_audit_creation_date 1971-12-31
_audit_creation_method CSD-ConQuest-V1
_database_code_CSD MCELOB
_chemical_formula_sum 'C14 H28 O12'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21'
_symmetry_Int_Tables_number 4
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
_cell_length_a
_cell_length_b
_cell_length_c
_cell_angle_alpha
_cell_angle_beta
_cell_angle_gamma
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.20
O 0.68
loop_
_atom_site_label
_atom_site_type_symbol
4.45
7.85
10.33
90.00
90.00
105.1
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
C1 C 0.050961
C2 C 0.191389
C3 C 0.047193
C4 C 0.009263
C5 C -0.148745
C6 C -0.176129
O2 O 0.181636
O3 O 0.242720
O4 O -0.191038
O5 O 0.038639
O6 O -0.238242
H1 H -0.164524
H2 H 0.411219
H3 H -0.158495
H4 H 0.213656
H5 H -0.356184
H6A H -0.342927
H6B H 0.016046
oH2 H 0.40(2)
oH3 H 0.15(4)
oH6 H -0.12(6)
0.057262 0.380527
0.196135 0.287129
0.160362 0.153425
-0.031267 0.112801
-0.157932 0.218384
-0.348168 0.188882
0.366971 0.331722
0.281823 0.066537
-0.076143 0.000711
-0.114787 0.333349
-0.451795 0.303957
0.062564 0.393673
0.197152 0.278760
0.183912 0.154995
-0.050262 0.093348
-0.141547 0.235149
-0.390800 0.126975
-0.359921
0.150091
0.442(16) 0.33(3)
0.27(3)
-0.020(8)
-0.54(3)
0.30(2)
#END
#Created crystal information file for cellulose IIIII
data_celliii(ii) adapted by AD French from Wada M, Heux L, Nishiyama Y,
Langan P (2009) X-ray Crystallographic, Scanning Microprobe X-ray
Diffraction, and Cross-Polarized/Magic Angle Spinning 13C NMR Studies of the
Structure of Cellulose III(II). Biomacromolecules 10:302–309.
DOI:10.1021/bm8010227
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21'
_symmetry_Int_Tables_number 4
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
_cell_length_a
_cell_length_b
_cell_length_c
_cell_angle_alpha
_cell_angle_beta
_cell_angle_gamma
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
4.45
7.64
10.36
90.00
90.00
106.96
H 0.20
O 0.68
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
O2 O 0.68488 -0.37630 0.40489
O3 O 0.87119 -0.28100 0.66392
O4 O 1.02248 -0.11465 0.22064
O5 O 1.15127 0.10212 0.37810
O6 O 1.21602 0.49674 0.44536
C1 C 0.92234 -0.06377 0.33869
C2 C 0.91582 -0.21013 0.43949
C3 C 0.84574 -0.14684 0.57200
C4 C 0.93112 -0.04051 0.10489
C5 C 1.06807 0.17557 0.49643
C6 C 1.30366 0.35964 0.51557
H1 H 0.71466 -0.04491 0.33011
H2 H 1.12218 -0.23189 0.44173
H3 H 0.62980 -0.13903 0.57275
H4 H 0.71811 -0.03018 0.11550
H5 H 0.85745 0.19036 0.48815
H6A H 1.31803 0.39029 0.60667
H62B H 1.50878 0.35512 0.48691
O2 O 1.18281 1.38162 0.32614
O3 O 1.20116 1.28786 0.06276
O4 O 1.18130 1.09163 0.50024
O5 O 1.01778 0.88426 0.33876
O6 O 0.64790 0.51577 0.28795
C1 C 1.01893 1.06205 0.38261
C2 C 1.18683 1.20394 0.28520
C3 C 1.02633 1.15882 0.15457
C4 C 0.99814 1.03693 0.61541
C5 C 0.84177 0.83024 0.22131
C6 C 0.83586 0.63567 0.19505
H1 H 0.80317 1.06692 0.39496
H2 H 1.40526 1.20182 0.27763
H3 H 0.81407 1.17173 0.16076
H4 H 0.78655 1.04766 0.60109
H5 H 0.62667 0.83634 0.23349
H6A H 0.75191 0.60042 0.10939
H6B H 1.04826 0.62590 0.19779
#END