Dipyrrolylmethane-based Macrobicyclic Azacryptand: Synthesis, X-ray Structures, Conformational and Anion Binding Properties
Tapas Guchhait; Ganesan Mani; Journal of Organic Chemistry 76 (2011) 10114–10121; doi:10.1021/jo201969f

data_4026797
_publ_section_title
;
 Dipyrrolylmethane-based Macrobicyclic Azacryptand: Synthesis, X-ray
 Structures, Conformational and Anion Binding Properties
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              10114
_journal_page_last               10121
_journal_paper_doi               10.1021/jo201969f
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C45 H72 N10 O11'
_chemical_formula_weight         929.13
_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                 91.867(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.256(3)
_cell_length_b                   25.707(5)
_cell_length_c                   13.471(3)
_cell_measurement_reflns_used    9179
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.55
_cell_volume                     5280.3(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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 area detector'
_diffrn_measurement_method       hemisphere
_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  0.1314
_diffrn_reflns_av_sigmaI/netI    0.0867
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            61300
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.9908
_exptl_absorpt_correction_T_min  0.9686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         9179
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1845
_refine_ls_R_factor_gt           0.0950
_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^)+(0.1269P)^2^+4.6727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2265
_refine_ls_wR_factor_ref         0.2858
_reflns_number_gt                4499
_reflns_number_total             9179
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo201969f_si_003.cif
_cod_data_source_block           compound3
_cod_original_cell_volume        5280.2(17)
_cod_database_code               4026797