Methyl Ether Derivatives of p-tert-Butyl[3.1.3.1]homooxacalixarene. Formation, Structure, and Complexes with Quaternary Ammonium Ions
Bernardo Masci; Stefano Levi Mortera; Daniela Persiani; Pierre Thuéry; Journal of Organic Chemistry 71 (2006) 504–511; doi:10.1021/jo051922t

data_4021386
_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       thuery@drecam.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
;
 Methyl Ether Derivatives of p-tert-Butyl[3.1.3.1]homooxacalixarene.
 Formation, Structure, and Complexes with
 Quaternary Ammonium Ions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              504
_journal_page_last               511
_journal_paper_doi               10.1021/jo051922t
_journal_volume                  71
_journal_year                    2006
_chemical_formula_sum            'C49.5 H69 Cl3 O7.5'
_chemical_formula_weight         890.40
_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                61.890(2)
_cell_angle_beta                 87.258(2)
_cell_angle_gamma                89.082(2)
_cell_formula_units_Z            4
_cell_length_a                   13.5059(5)
_cell_length_b                   20.4824(7)
_cell_length_c                   20.9212(9)
_cell_measurement_reflns_used    161520
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.92
_cell_volume                     5098.9(4)
_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); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two \f and three \w scans with 2\% steps'
_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  0.0682
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            161520
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    0.227
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.653
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1250
_refine_ls_number_reflns         19139
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0907
_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^)+(0.1335P)^2^+10.0774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2398
_refine_ls_wR_factor_ref         0.2598
_reflns_number_gt                14125
_reflns_number_total             19139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo051922tsi20050914_124544.cif
_cod_original_formula_sum        'C49.50 H69 Cl3 O7.50'
_cod_database_code               4021386