Hydrogels formed from Fmoc amino acids
Draper, Emily R.; Morris, Kyle L.; Little, Marc A.; Raeburn, Jaclyn; Colquhoun, Catherine; Cross, Emily R.; McDonald, Tom. O.; Serpell, Louise C.; Adams, Dave J.; CrystEngComm 17 (2015) 8047–; doi:10.1039/C5CE00801H

data_7220754
_publ_section_title
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 Hydrogels formed from Fmoc amino acids
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_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              8047
_journal_paper_doi               10.1039/C5CE00801H
_journal_volume                  17
_journal_year                    2015
_chemical_absolute_configuration L
_chemical_formula_moiety         'C24 H21 N O4, 2(C H4 O)'
_chemical_formula_sum            'C26 H29 N O6'
_chemical_formula_weight         451.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-28 deposited with the CCDC.
2015-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.417(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.076(6)
_cell_length_b                   4.887(2)
_cell_length_c                   18.998(9)
_cell_measurement_reflns_used    1653
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.47
_cell_measurement_theta_min      2.22
_cell_volume                     1164.5(9)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_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  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1336
_diffrn_reflns_av_unetI/netI     0.0956
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16474
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        21.935
_diffrn_reflns_theta_max         21.935
_diffrn_reflns_theta_min         1.691
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.4759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1408 before and 0.0950 after correction.
The Ratio of minimum to maximum transmission is 0.6390.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       needle
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Flack x determined using 744 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         2788
_refine_ls_number_restraints     253
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.1269
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1533P)^2^+8.4284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3191
_refine_ls_wR_factor_ref         0.3389
_reflns_Friedel_coverage         0.726
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                2138
_reflns_number_total             2788
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00801h1.cif
_cod_data_source_block           DA_FmocF_MeOH_100K
_cod_depositor_comments
'Adding full bibliography for 7220753--7220755.cif.'
_cod_original_cell_volume        1164.4(10)
_cod_database_code               7220754
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.992
_olex2_refinement_description
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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 C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(N1)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16)
4.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C18(H18A,H18B)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3A), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
4.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
4.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O5(H5A), O6(H6)
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_thetm01_alert_3_a
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Problem: The value of sine(theta_max)/wavelength is less than 0.550
Calculated sin(theta_max)/wavelength = 0.5256
Response: Single crystals of FmocF_MeOH were weakly diffracting, diffuse 
scatter beyond 0.95 angstroms was omitted during refinement.    
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_plat340_alert_3_b
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Problem: Low Bond Precision on C-C Bonds ............... 0.0212 Ang.
Response: Low bond precision is related to quality of the diffraction data. 
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_shelx_res_checksum              93934
_olex2_submission_special_instructions 'No special instructions were received'