Chiral Spherical Molecule Constructed from Aromatic Amides: Facile Synthesis and Highly Ordered Network Structure in the Crystal
Hyuma Masu; Takako Kato; Masahide Tominaga; Journal of Organic Chemistry 73 (2008) 5143–5146; doi:10.1021/jo800585h

data_4023512
_publ_contact_author_address
;Faculty of Pharmaceutical Sciences at Kagawa Campus,
Tokushima Bunri University,
1314-1 Shido, Sanuki, Kagawa,
769-2193, JAPAN
;
_publ_contact_author_email       azumayai@kph.bunri-u.ac.jp
_publ_contact_author_fax         +81-87-894-0181
_publ_contact_author_name        'Isao Azumaya'
_publ_contact_author_phone       +81-87-894-5111x6308
_publ_section_title
;
 Chiral Spherical Molecule Constructed from Aromatic Amides: Facile
 Synthesis and Highly Ordered Network Structure in the Crystal
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5143
_journal_page_last               5146
_journal_paper_doi               10.1021/jo800585h
_journal_volume                  73
_journal_year                    2008
_chemical_formula_moiety         'C42 H42 N6 O6, 1.5(H2 O)'
_chemical_formula_sum            'C42 H45 N6 O7.5'
_chemical_formula_weight         753.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 92.224(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5799(15)
_cell_length_b                   27.514(3)
_cell_length_c                   9.2074(9)
_cell_measurement_reflns_used    1677
_cell_measurement_temperature    150
_cell_measurement_theta_max      21.39
_cell_measurement_theta_min      2.58
_cell_volume                     3943.9(7)
_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      150
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.914
_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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11003
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.9912
_exptl_absorpt_correction_T_min  0.9613
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         4466
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1010P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1676
_reflns_number_gt                3172
_reflns_number_total             4466
_reflns_threshold_expression     >2sigma
_cod_data_source_file            jo800585h-File003.cif
_cod_data_source_block           a0602281mas(compound_1)
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_sum        'C42 H45 N6 O7.50'
_cod_database_code               4023512