Thermal annealing behaviour and gel to crystal transition of a low molecular weight hydrogelator.
Barker, Emily C.; Martin, Adam D.; Garvey, Christopher J.; Goh, Ching Yong; Jones, Franca; Mocerino, Mauro; Skelton, Brian W.; Ogden, Mark I.; Becker, Thomas; Soft matter 13 (2017) 1006–1011; doi:10.1039/c6sm02431a

data_1545007
_publ_section_title
;
 Thermal annealing behaviour and gel to crystal transition of a low
 molecular weight hydrogelator.
;
_journal_issue                   5
_journal_name_full               'Soft matter'
_journal_page_first              1006
_journal_page_last               1011
_journal_paper_doi               10.1039/c6sm02431a
_journal_volume                  13
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C52 H64 Mg N4 O14, 16(H2 O), 2(Cl)'
_chemical_formula_sum            'C52 H96 Cl2 Mg N4 O30'
_chemical_formula_weight         1352.54
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           75
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4'
_symmetry_space_group_name_H-M   'P 4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-04-01T16:23:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-10-08 deposited with the CCDC.
2017-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.12420(10)
_cell_length_b                   14.12420(10)
_cell_length_c                   16.61700(10)
_cell_measurement_reflns_used    28882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.021
_cell_measurement_theta_min      2.6538
_cell_volume                     3314.98(4)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100(2)
_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       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40081
_diffrn_reflns_theta_full        67.13
_diffrn_reflns_theta_max         67.13
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    1.728
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.76567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.074
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.16(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         5900
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0826
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1728P)^2^+2.6240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2396
_refine_ls_wR_factor_ref         0.2406
_reflns_number_gt                5773
_reflns_number_total             5900
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c6sm02431a2.cif
_cod_data_source_block           mm39
_cod_depositor_comments          'Adding full bibliography for 1545007.cif.'
_cod_original_sg_symbol_Hall     P_4
_cod_database_code               1545007