Programmed twisting of phenylene‒ethynylene linkages from aromatic stacking interactions
Mullin, William J.; Pawle, Robert H.; Sharber, Seth A.; Müller, Peter; Thomas, Samuel W.; Journal of Materials Chemistry C 7 (2019) 1198–; doi:10.1039/C8TC05612A

data_7237557
_publ_section_title
;
 Programmed twisting of phenylene--ethynylene linkages from aromatic
 stacking interactions
;
_journal_issue                   5
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              1198
_journal_paper_doi               10.1039/C8TC05612A
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C46 H30 O4, 0.84(C H Cl3)'
_chemical_formula_sum            'C46.84 H30.84 Cl2.52 O4'
_chemical_formula_weight         746.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/2
_audit_update_record
;
2018-10-24 deposited with the CCDC.
2018-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                80.595(2)
_cell_angle_beta                 84.255(2)
_cell_angle_gamma                88.725(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1455(7)
_cell_length_b                   9.8705(8)
_cell_length_c                   23.767(2)
_cell_measurement_reflns_used    9503
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.92
_cell_measurement_theta_min      2.39
_cell_volume                     1875.7(3)
_computing_cell_refinement       'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_data_collection       'APEX3 v2017.3.0 (Bruker-AXS, 2017)'
_computing_data_reduction        'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/2 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            59772
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.132
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Herbst-Irmer et al., 2015)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             773
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         11450
_refine_ls_number_restraints     291
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+0.8968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1523
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7572
_reflns_number_total             11450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8tc05612a2.cif
_cod_data_source_block           X18062
_cod_original_cell_volume        1875.6(3)
_cod_database_code               7237557
_shelx_shelxl_version_number     2017/2
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              75884
_shelx_hkl_checksum              12415