A Conformationally Flexible, Urea-Based Tripodal Anion Receptor: Solid-State, Solution, and Theoretical Studies
David R. Turner; Martin J. Paterson; Jonathan W. Steed; Journal of Organic Chemistry 71 (2006) 1598–1608; doi:10.1021/jo052339f

data_4021510
_publ_section_title
;
 A Conformationally Flexible, Urea-Based Tripodal Anion Receptor:
 Solid-State, Solution, and Theoretical Studies
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1598
_journal_page_last               1608
_journal_paper_doi               10.1021/jo052339f
_journal_volume                  71
_journal_year                    2006
_chemical_formula_sum            'C59.67 H82.67 Br3 N9 O8.67'
_chemical_formula_weight         1304.51
_chemical_name_common            3aptolBr
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.923(5)
_cell_angle_beta                 90.040(4)
_cell_angle_gamma                106.804(5)
_cell_formula_units_Z            4
_cell_length_a                   14.3365(9)
_cell_length_b                   19.7335(19)
_cell_length_c                   26.4104(19)
_cell_measurement_temperature    120(2)
_cell_volume                     7077.9(10)
_computing_cell_refinement       Denzo-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'XSeed interface to POVRay'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.869
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       \w
_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  0.0983
_diffrn_reflns_av_sigmaI/netI    0.3401
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21211
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.757
_exptl_absorpt_correction_T_max  0.7202
_exptl_absorpt_correction_T_min  0.5401
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1156
_refine_ls_number_reflns         17110
_refine_ls_number_restraints     1059
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.2527
_refine_ls_R_factor_gt           0.1228
_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^)+(0.1455P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2976
_refine_ls_wR_factor_ref         0.3475
_reflns_number_gt                5171
_reflns_number_total             17110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo052339fsi20051111_082448.cif
_cod_original_formula_sum        'C59.67 H82.67 N9 O8.67 Br3'
_cod_database_code               4021510