One-pot synthesis of cyclic triamides with a triangular cavity from trans-stilbene and diphenylacetylene monomers.
Yokoyama, Akihiro; Maruyama, Takurou; Tagami, Kei; Masu, Hyuma; Katagiri, Kosuke; Azumaya, Isao; Yokozawa, Tsutomu; Organic letters 10 (2008) 3207–3210; doi:10.1021/ol801083r

data_1504767
_publ_section_title
;
 One-pot synthesis of cyclic triamides with a triangular cavity from
 trans-stilbene and diphenylacetylene monomers.
;
_journal_issue                   15
_journal_name_full               'Organic letters'
_journal_page_first              3207
_journal_page_last               3210
_journal_paper_doi               10.1021/ol801083r
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C54 H45 N3 O3, 4(C7 H8)'
_chemical_formula_sum            'C82 H77 N3 O3'
_chemical_formula_weight         1152.47
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 118.19(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.473(12)
_cell_length_b                   8.427(5)
_cell_length_c                   43.282(19)
_cell_measurement_reflns_used    5951
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.15
_cell_measurement_theta_min      2.26
_cell_volume                     6582(6)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 '
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1158
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            22069
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.9794
_exptl_absorpt_correction_T_min  0.9726
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.986
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.191
_refine_ls_extinction_coef       0.0030(5)
_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   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         22070
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1635
_refine_ls_R_factor_gt           0.1187
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1340P)^2^+27.0045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3111
_refine_ls_wR_factor_ref         0.3357
_reflns_number_gt                13861
_reflns_number_total             22070
_reflns_threshold_expression     >2sigma
_cod_data_source_file            ol801083r-file005.cif
_cod_data_source_block           a0701181kka(compound4)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P21/c   '
_cod_database_code               1504767