Hydrogen-Bonded Aryl Amide Macrocycles: Synthesis, Single-Crystal Structures, and Stacking Interactions with Fullerenes and Coronene
Yuan-Yuan Zhu; Chuang Li; Guang-Yu Li; Xi-Kui Jiang; Zhan-Ting Li; Journal of Organic Chemistry 73 (2008) 1745–1751; doi:10.1021/jo702046f

data_4023300
_publ_section_title
;
 Hydrogen-Bonded Aryl Amide Macrocycles: Synthesis, Single-Crystal
 Structures, and Stacking Interactions with Fullerenes and Coronene
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1745
_journal_page_last               1751
_journal_paper_doi               10.1021/jo702046f
_journal_volume                  73
_journal_year                    2008
_chemical_formula_sum            'C51 H48 N6 O12'
_chemical_formula_weight         936.95
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                60.759(10)
_cell_angle_beta                 85.196(12)
_cell_angle_gamma                87.987(11)
_cell_formula_units_Z            2
_cell_length_a                   8.299(5)
_cell_length_b                   17.925(10)
_cell_length_c                   18.125(10)
_cell_measurement_reflns_used    925
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40.039
_cell_measurement_theta_min      4.474
_cell_volume                     2344(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1466
_diffrn_reflns_av_sigmaI/netI    0.2280
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12385
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67213
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.0017(6)
_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   0.838
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         8582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.2208
_refine_ls_R_factor_gt           0.0811
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0976P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.2723
_reflns_number_gt                2707
_reflns_number_total             8582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo702046f-File002.cif
_cod_data_source_block           cd26514
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4023300