Tuning the structure of 1,3,5-benzene tricarboxamide self-assemblies through stereochemistry.
Caumes, Xavier; Baldi, Arianna; Gontard, Geoffrey; Brocorens, Patrick; Lazzaroni, Roberto; Vanthuyne, Nicolas; Troufflard, Claire; Raynal, Matthieu; Bouteiller, Laurent; Chemical communications (Cambridge, England) 52 (2016) 13369–13372; doi:10.1039/c6cc07325e

data_7125182
_publ_section_title
;
 Tuning the structure of 1,3,5-benzene tricarboxamide self-assemblies
 through stereochemistry.
;
_journal_issue                   91
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13369
_journal_page_last               13372
_journal_paper_doi               10.1039/c6cc07325e
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         '(C45 H69 N3 O9), 0.25(C2 H3 N), 0.5(H2 O)'
_chemical_formula_sum            'C45.5 H70.75 N3.25 O9.5'
_chemical_formula_weight         815.30
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2016-07-08 deposited with the CCDC.
2016-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                61.491(2)
_cell_angle_beta                 83.352(2)
_cell_angle_gamma                79.502(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5502(4)
_cell_length_b                   15.7414(5)
_cell_length_c                   15.8302(5)
_cell_measurement_reflns_used    9164
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      66.62
_cell_measurement_theta_min      3.18
_cell_volume                     2485.47(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(1)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         micro-source
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43045
_diffrn_reflns_point_group_measured_fraction_full 0.785
_diffrn_reflns_point_group_measured_fraction_max 0.784
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.651
_diffrn_reflns_theta_min         3.179
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             885
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 4693 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1118
_refine_ls_number_reflns         13780
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0922P)^2^+0.1959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1234
_reflns_Friedel_coverage         0.571
_reflns_Friedel_fraction_full    0.572
_reflns_Friedel_fraction_max     0.570
_reflns_number_gt                13352
_reflns_number_total             13780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07325e2.cif
_cod_data_source_block           ab-bta-7
_cod_database_code               7125182
_shelx_res_checksum              7759
_shelx_hkl_checksum              52414