Synthesis of Cyclophanes with Planar and Helical Chirality
Xiao Liu; Yudao Ma; Wenzeng Duan; Fuyan He; Lei Zhao; Chun Song; Journal of Organic Chemistry 76 (2011) 1953–1956; doi:10.1021/jo102538y

data_4026142
_publ_section_title
;
 Synthesis of Cyclophanes with Planar and Helical Chirality
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1953
_journal_page_last               1956
_journal_paper_doi               10.1021/jo102538y
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C36 H32 N4'
_chemical_formula_weight         520.66
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.498(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.1860(7)
_cell_length_b                   14.0335(15)
_cell_length_c                   13.2350(14)
_cell_measurement_temperature    273(2)
_cell_volume                     1330.6(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7549
_diffrn_reflns_theta_full        26.69
_diffrn_reflns_theta_max         26.69
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.9923
_exptl_absorpt_correction_T_min  0.9885
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         5178
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.124
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                3976
_reflns_number_total             5178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo102538y_si_001.cif
_cod_data_source_block           test
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4026142