Construction and Charge-Transfer Complexation of Adamantane-Based Macrocycles and a Cage with Aromatic Ring Moieties
Masahide Tominaga; Hyuma Masu; Isao Azumaya; Journal of Organic Chemistry 74 (2009) 8754–8760; doi:10.1021/jo9018842

data_4025051
_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
;
Construction and Charge-Transfer Complexation of Adamantane-Based
Macrocycles and a Cage with Aromatic Ring Moieties
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8754
_journal_page_last               8760
_journal_paper_doi               10.1021/jo9018842
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C64H68O12, 3(C6H3N3O6)'
_chemical_formula_sum            'C82 H77 N9 O30'
_chemical_formula_weight         1668.53
_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                 98.486(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.371(3)
_cell_length_b                   33.097(6)
_cell_length_c                   16.454(3)
_cell_measurement_reflns_used    3855
_cell_measurement_temperature    120
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2.23
_cell_volume                     7740(2)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_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      120
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.944
_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  0.0923
_diffrn_reflns_av_sigmaI/netI    0.1233
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38203
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.53
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.9945
_exptl_absorpt_correction_T_min  0.9571
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     989
_refine_ls_number_reflns         15192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1314
_refine_ls_R_factor_gt           0.0633
_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^)+(0.0730P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1848
_reflns_number_gt                8173
_reflns_number_total             15192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo9018842_si_001.cif
_cod_data_source_block           a0809291mas
_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      'P2(1)/c  '
_cod_database_code               4025051