Synthesis of a Preorganized Hybrid Macrobicycle with Distinct Amide and Amine Clefts: Tetrahedral versus Spherical Anions Binding Studies
Subrata Saha; Bidyut Akhuli; Sourav Chakraborty; Pradyut Ghosh; Journal of Organic Chemistry 78 (2013) 8759–8765; doi:10.1021/jo401504f

data_4028571
_publ_section_title
;
 Synthesis of a Preorganized Hybrid Macrobicycle with Distinct Amide and
 Amine Clefts: Tetrahedral versus Spherical Anions Binding Studies
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8759
_journal_page_last               8765
_journal_paper_doi               10.1021/jo401504f
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C47 H63 Br3 N8 O7'
_chemical_formula_weight         1091.78
_chemical_name_systematic
; 
 ? 
;
_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                 113.740(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3205(7)
_cell_length_b                   11.8681(6)
_cell_length_c                   32.3426(15)
_cell_measurement_reflns_used    3158
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.62
_cell_measurement_theta_min      2.23
_cell_volume                     5031.7(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'MERCURY 2.3'
_computing_publication_material  'ORTEP 3V.2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1057
_diffrn_reflns_av_sigmaI/netI    0.0874
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            46097
_diffrn_reflns_theta_full        24.67
_diffrn_reflns_theta_max         24.67
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    2.462
_exptl_absorpt_correction_T_max  0.9524
_exptl_absorpt_correction_T_min  0.8664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
The unit cell contains one disordered acetonitrile molecule which has been 
treated as a diffuse contribution to the overall scatterin without 
specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.029
_refine_diff_density_min         -2.159
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         8522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0795
_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^)+(0.0864P)^2^+50.2271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2172
_reflns_number_gt                5376
_reflns_number_total             8522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo401504f_si_002_3.cif
_cod_data_source_block           COMPLEX_2
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4028571