The effect of solvent choice on the gelation and final hydrogel properties of Fmoc-diphenylalanine.
Raeburn, Jaclyn; Mendoza-Cuenca, Cristina; Cattoz, Beatrice N.; Little, Marc A.; Terry, Ann E.; Zamith Cardoso, Andre; Griffiths, Peter C.; Adams, Dave J.; Soft matter 11 (2015) 927–935; doi:10.1039/c4sm02256d

data_1518451
_publ_section_title
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 The effect of solvent choice on the gelation and final hydrogel
 properties of Fmoc-diphenylalanine.
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_journal_issue                   5
_journal_name_full               'Soft matter'
_journal_page_first              927
_journal_page_last               935
_journal_paper_doi               10.1039/c4sm02256d
_journal_volume                  11
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C33 H30 N2 O5, 0.88(H2 O)'
_chemical_formula_sum            'C33 H31.75 N2 O5.88'
_chemical_formula_weight         550.35
_chemical_name_systematic        FmocFF
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-11-12 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.49(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   52.27(6)
_cell_length_b                   5.010(6)
_cell_length_c                   22.83(3)
_cell_measurement_reflns_used    556
_cell_measurement_temperature    100
_cell_measurement_theta_max      18.034
_cell_measurement_theta_min      2.542
_cell_volume                     5761(12)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Rigaku CrystalClear v2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.1630
_diffrn_reflns_av_unetI/netI     0.2634
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11789
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         0.78
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.4986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1325 before and 0.0745 after correction.
The Ratio of minimum to maximum transmission is 0.6697.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2326
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.009
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         5782
_refine_ls_number_restraints     396
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.2274
_refine_ls_R_factor_gt           0.1027
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1448P)^2^+3.4992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2387
_refine_ls_wR_factor_ref         0.3134
_reflns_number_gt                2644
_reflns_number_total             5782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sm02256d2.cif
_cod_data_source_block           fmocff_100K
_cod_depositor_comments          'Adding full bibliography for 1518451.cif.'
_cod_original_cell_volume        5761(11)
_cod_database_code               1518451
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Fixed Sof: O4W(0.125) O3W(0.125) O2W(0.5)
5.a Ternary CH refined with riding coordinates:
 C41(H41), C43(H43), C47(H47), C8(H8), C10(H10), C21(H21)
5.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C46(H46A,H46B), C60(H60A,H60B), C7(H7A,H7B), C12(H12A,H12B),
 C20(H20A,H20B)
5.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C36(H36), C35(H35), C34(H34), C39(H39), C38(H38), C49(H49),
 C50(H50), C51(H51), C52(H52), C55(H55), C56(H56), C57(H57), C58(H58), C62(H62),
  C63(H63), C64(H64), C65(H65), C66(H66), N1(H1), N2(H2A), C2(H2B), C3(H3A),
 C4(H4A), C5(H5), C6(H6), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30), C31(H31), C32(H32)
5.d Fitted hexagon refined as free rotating group:
 C37(C36,C35,C34,C39,C38)
5.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O7(H7)
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_plat201_alert_2_a
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Problem: Isotropic non-H Atoms in Main Residue(s) .......         44 Report        
Response: Single crystal sample of FmocFF were very weakly diffracting. Synchrotron radiation 
was required for structure solution and a 1 angstrom resolution was applied during integration. 
Due to limited number of reflections collected during the data collection is was not justifiable to refine 
the while structure anisotropically. Only the main residue atoms were refined anisotropically.
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_shelx_res_checksum              8053
_shelx_hkl_checksum              26523