Remarkable Effects of Terminal Groups and Solvents on Helical Folding of o-Phenylene Oligomers
Shinji Ando; Eisuke Ohta; Atsuko Kosaka; Daisuke Hashizume; Hiroyuki Koshino; Takanori Fukushima; Takuzo Aida; Journal of the American Chemical Society 134 (2012) 11084–11087; doi:10.1021/ja303117z

data_4118220
_publ_section_title
;
 Remarkable Effects of Terminal Groups and Solvents on Helical Folding of
 o-Phenylene Oligomers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11084
_journal_page_last               11087
_journal_paper_doi               10.1021/ja303117z
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C48 H46 O12, C7 H8'
_chemical_formula_sum            'C55 H54 O12'
_chemical_formula_weight         906.98
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.7630(10)
_cell_angle_beta                 73.9210(10)
_cell_angle_gamma                70.6880(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1381(2)
_cell_length_b                   13.5002(3)
_cell_length_c                   16.7786(3)
_cell_measurement_reflns_used    39586
_cell_measurement_temperature    150
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.5
_cell_volume                     2287.43(8)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku RAXIS-Rapid'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0110
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42744
_diffrn_reflns_theta_full        68.19
_diffrn_reflns_theta_max         68.19
_diffrn_reflns_theta_min         3.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_T_max  0.8871
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
    Higashi, T. (1999). Program for Absorption Correction. 
    Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         8252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.8478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0823
_reflns_number_gt                7606
_reflns_number_total             8252
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja303117z_si_002.cif
_cod_data_source_block           benzylester
_cod_original_cell_volume        2287.42(8)
_cod_database_code               4118220