Cavity-containing supramolecular gels as a crystallization tool for hydrophobic pharmaceuticals.
Kaufmann, Lena; Kennedy, Stuart R.; Jones, Christopher D.; Steed, Jonathan W.; Chemical communications (Cambridge, England) 52 (2016) 10113–10116; doi:10.1039/c6cc04037c

data_7124711
_publ_section_title
;
 Cavity-containing supramolecular gels as a crystallization tool for
 hydrophobic pharmaceuticals.
;
_journal_issue                   66
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10113
_journal_page_last               10116
_journal_paper_doi               10.1039/c6cc04037c
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C18 H22 Cl2 O6'
_chemical_formula_weight         405.25
_chemical_name_common            Chlorphenesin
_chemical_name_systematic        3-(p-Chlorophenoxy)propane-1,2-diol
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-05-06 deposited with the CCDC.
2016-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3202(14)
_cell_length_b                   4.6501(5)
_cell_length_c                   32.022(4)
_cell_measurement_reflns_used    113
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      37.40
_cell_measurement_theta_min      8.399
_cell_volume                     1834.5(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_unetI/netI     0.1066
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            13672
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.439
_diffrn_reflns_theta_min         2.544
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.23(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3747
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.963
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2489
_reflns_number_total             3747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc04037c2.cif
_cod_data_source_block           Chlorphen2
_cod_database_code               7124711
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.939
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              62789
_shelx_hkl_checksum              51276