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_4028569
_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 H65 N7 O11'
_chemical_formula_weight         904.06
_chemical_name_systematic
; 
 ? 
;
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_gamma                103.162(13)
_cell_formula_units_Z            2
_cell_length_a                   11.684(4)
_cell_length_b                   13.811(5)
_cell_length_c                   16.664(6)
_cell_measurement_reflns_used    3267
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.52
_cell_measurement_theta_min      2.32
_cell_volume                     2474.2(15)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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
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_diffrn_reflns_limit_l_min       -18
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_diffrn_reflns_theta_max         22.98
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLOURLESS
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_exptl_crystal_description       BLOCK
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_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6780
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_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.0853
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1794P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_cod_original_sg_symbol_H-M      'P -1 '
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