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_4118221
_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         'C64 H62 O16, 2(C2 H3 N)'
_chemical_formula_sum            'C68 H68 N2 O16'
_chemical_formula_weight         1169.24
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.999(5)
_cell_angle_beta                 76.081(5)
_cell_angle_gamma                75.721(5)
_cell_formula_units_Z            2
_cell_length_a                   12.5010(11)
_cell_length_b                   15.3747(15)
_cell_length_c                   16.5206(16)
_cell_measurement_reflns_used    7555
_cell_measurement_temperature    90
_cell_measurement_theta_max      32.5699
_cell_measurement_theta_min      1.3802
_cell_volume                     2957.5(5)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku AFC-8 with Saturn70 CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            77568
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         1.28
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9889
_exptl_absorpt_correction_T_min  0.9037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
abscor
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.0251(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         17261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0664
_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^)+(0.0894P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1779
_reflns_number_gt                12602
_reflns_number_total             17261
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja303117z_si_003.cif
_cod_data_source_block           6mer-Bn-ester
_cod_database_code               4118221