Unraveling the Self-Assembly Modes in Multicomponent Supramolecular Gels Using Single-Crystal X-ray Diffraction
Ghosh, Dipankar; Farahani, Abbas D.; Martin, Adam D.; Thordarson, Pall; Damodaran, Krishna K.; Chemistry of Materials 32 (2020) 3517–3527; doi:10.1021/acs.chemmater.0c00475

data_4003523
_publ_section_title
;
 Unraveling the Self-Assembly Modes in Multicomponent Supramolecular Gels
 Using Single-Crystal X-ray Diffraction
;
_journal_issue                   8
_journal_name_full               'Chemistry of Materials'
_journal_page_first              3517
_journal_page_last               3527
_journal_paper_doi               10.1021/acs.chemmater.0c00475
_journal_volume                  32
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_formula_sum            'C20 H28 N2 O6'
_chemical_formula_weight         392.44
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.721(2)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   9.9327(5)
_cell_length_b                   9.8290(5)
_cell_length_c                   33.1100(18)
_cell_measurement_reflns_used    9021
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.11
_cell_measurement_theta_min      4.53
_cell_volume                     3210.3(3)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_collection       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_computing_molecular_graphics    'MERCURY CSD 4.2.0'
_computing_publication_material  'MERCURY CSD 4.2.0'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SAINT V8.35A (?, 2016)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            66905
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.154
_diffrn_reflns_theta_min         2.687
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1116 before and 0.0516 after correction.
The Ratio of minimum to maximum transmission is 0.8751.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 5337 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         12386
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0475P)^2^+0.8899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.850
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                12045
_reflns_number_total             12386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c00475_si_003.cif
_cod_data_source_block           cu_DG02176_7_0m_a_SS
_cod_depositor_comments
;Adding full bibliography for 4003523--4003526.cif.

 Adding full bibliography for 4003523--4003526.cif.
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4003523
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.685
_shelx_estimated_absorpt_t_max   0.916
_shelx_res_checksum              26501
_shelx_hkl_checksum              52579