Complexation of Quaternary Ammonium Ions by Tetraester Derivatives of [3.1.3.1]Homooxacalixarene in Mobile and in Fixed Conformation
Bernardo Masci; Daniela Persiani; Pierre Thuéry; Journal of Organic Chemistry 71 (2006) 9784–9790; doi:10.1021/jo0617621

data_4022187
_publ_contact_author             'P. Thu\'ery'
_publ_contact_author_address
;
      CEA/Saclay, SCM (CNRS URA 331)
      B\^at. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_email       pierre.thuery@cea.fr
_publ_contact_author_fax         '33 1 69 08 66 40'
_publ_contact_author_phone       '33 01 69 08 63 29'
_publ_section_title
;
 Complexation of Quaternary Ammonium Ions by Tetraester Derivatives
 of [3.1.3.1]Homooxacalixarene in Mobile and in Fixed Conformation
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9784
_journal_page_last               9790
_journal_paper_doi               10.1021/jo0617621
_journal_volume                  71
_journal_year                    2006
_chemical_formula_sum            'C73 H106 O15'
_chemical_formula_weight         1223.58
_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                83.983(3)
_cell_angle_beta                 89.968(4)
_cell_angle_gamma                63.167(4)
_cell_formula_units_Z            2
_cell_length_a                   13.7593(8)
_cell_length_b                   13.9522(11)
_cell_length_c                   20.5857(16)
_cell_measurement_reflns_used    25083
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.43
_cell_volume                     3502.1(5)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f 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  0.0822
_diffrn_reflns_av_sigmaI/netI    0.1045
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11951
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         11951
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.0817
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+5.4753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1893
_refine_ls_wR_factor_ref         0.2273
_reflns_number_gt                7393
_reflns_number_total             11951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0617621si20060826_062657.cif
_cod_database_code               4022187