Investigating hydrogel formation using in situ variable-temperature scanning probe microscopy
Barker, Emily C.; Goh, Ching Yong; Jones, Franca; Mocerino, Mauro; Skelton, Brian W.; Becker, Thomas; Ogden, Mark I.; Chem. Sci. 6 (2015) 6133–; doi:10.1039/C5SC02196K

data_1529321
_publ_section_title
;
 Investigating hydrogel formation using in situ variable-temperature
 scanning probe microscopy
;
_journal_issue                   11
_journal_name_full               'Chem. Sci.'
_journal_page_first              6133
_journal_paper_doi               10.1039/C5SC02196K
_journal_volume                  6
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C52 H60 N4 O12, C4 H8 O'
_chemical_formula_sum            'C56 H68 N4 O13'
_chemical_formula_weight         1005.14
_chemical_properties_physical    Efflorescent
_space_group_IT_number           209
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      209
_symmetry_space_group_name_Hall  'F 4 2 3'
_symmetry_space_group_name_H-M   'F 4 3 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-06-12T08:07:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-06-12 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   36.2659(2)
_cell_length_b                   36.2659(2)
_cell_length_c                   36.2659(2)
_cell_measurement_reflns_used    22874
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.1515
_cell_measurement_theta_min      3.4389
_cell_volume                     47697.5(5)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
 Oxford Diffraction Gemini diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0325850736
_diffrn_orient_matrix_UB_12      0.0181666536
_diffrn_orient_matrix_UB_13      -0.0205828603
_diffrn_orient_matrix_UB_21      -0.0220258864
_diffrn_orient_matrix_UB_22      0.0361848342
_diffrn_orient_matrix_UB_23      -0.0026870676
_diffrn_orient_matrix_UB_31      0.0164277526
_diffrn_orient_matrix_UB_32      0.0128559698
_diffrn_orient_matrix_UB_33      0.0369859983
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_av_unetI/netI     0.1585
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            144382
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.28
_diffrn_reflns_theta_max         67.28
_diffrn_reflns_theta_min         3.447
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.85908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.84
_exptl_crystal_description       block
_exptl_crystal_F_000             12864
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: H2O/THF'
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 947 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.323
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3613
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.37
_refine_ls_R_factor_all          0.1253
_refine_ls_R_factor_gt           0.1157
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3037
_refine_ls_wR_factor_ref         0.3188
_reflns_number_gt                2883
_reflns_number_total             3613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02196k2.cif
_cod_data_source_block           mmcy04
_cod_depositor_comments          'Adding full bibliography for 1529321.cif.'
_cod_original_cell_volume        47697.5(8)
_cod_database_code               1529321
_shelx_res_checksum              70424
_shelx_hkl_checksum              28880