Synthesis and Clathrates of Oligomeric 2-O-Naphthoide Macrocycles
Tayel A. AlHujran; Louise N. Dawe; Julie Collins; Paris E. Georghiou; Journal of Organic Chemistry 76 (2011) 971–973; doi:10.1021/jo101959w

data_4026006
_publ_contact_author_email       parisg@mun.ca
_publ_contact_author_fax         '(709) 864-3702'
_publ_contact_author_name        'Paris E. Georghiou'
_publ_contact_author_phone       '(709) 864-8517'
_publ_section_title
;
 Synthesis and Clathrates of Oligomeric 2-O-Naphthoide Macrocycles
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              971
_journal_page_last               973
_journal_paper_doi               10.1021/jo101959w
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C90 H84 O12, 4(C H Cl3)'
_chemical_formula_sum            'C94 H88 Cl12 O12'
_chemical_formula_weight         1835.04
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   16.6442(16)
_cell_length_b                   16.6442(16)
_cell_length_c                   27.928(3)
_cell_measurement_reflns_used    7000
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.6346
_cell_measurement_theta_min      2.0306
_cell_volume                     6700.3(12)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            20958
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.9775
_exptl_absorpt_correction_T_min  0.9497
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(T. Higashi, 2000)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2622
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.912
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.1111
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3909
_refine_ls_wR_factor_ref         0.3914
_reflns_number_gt                2606
_reflns_number_total             2622
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo101959w_si_003.cif
_cod_data_source_block           hexamer6
_cod_original_sg_symbol_H-M      'R -3:H'
_cod_database_code               4026006