Simultaneous Freezing of Chirality and In-Out Conformation of a Macropentacyclic Cryptand by Protonation
Clément Bonnot; Jean-Claude Chambron; Enrique Espinosa; Journal of the American Chemical Society 126 (2004) 11412–11413; doi:10.1021/ja048441w

data_4112953
_publ_contact_author
; Dr. Jean-Claude Chambron,

  LIMSAG, CNRS UMR 5633, 

  Universite de Bourgogne, Faculte des Sciences, 

  6 boulevard Gabriel, 21100 Dijon, 

  France 

;
_publ_contact_author_email       Jean-Claude.Chambron@u-bourgogne.fr
_publ_contact_author_fax         '+33 3 80 39 61 17'
_publ_contact_author_phone       '+33 3 80 39 61 16'
_publ_section_title
;
 Simultaneous Freezing of Chirality and In-Out Conformation of a
 Macropentacyclic Cryptand by Protonation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11412
_journal_page_last               11413
_journal_paper_doi               10.1021/ja048441w
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety
'C129 H163 N8 O12 S12,1(C F3 O3 S),0.5(C H2 Cl2),3(C4 H8 O2),3(H2 O)'
_chemical_formula_sum            'C142.5 H194 Cl F3 N8 O24 S13'
_chemical_formula_weight         2912.29
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.007(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.6378(2)
_cell_length_b                   18.6415(2)
_cell_length_c                   37.3315(5)
_cell_measurement_reflns_used    26597
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.23
_cell_volume                     15409.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1178
_diffrn_reflns_av_sigmaI/netI    0.2126
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            45543
_diffrn_reflns_theta_full        24.93
_diffrn_reflns_theta_max         24.93
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       Prism
_exptl_crystal_F_000             6196
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1969
_refine_ls_number_reflns         26597
_refine_ls_number_restraints     973
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.2095
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1127P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.2312
_reflns_number_gt                11526
_reflns_number_total             26597
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048441wsi20040325_041403.cif
_cod_data_source_block           cbo002
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C142.50 H194 Cl F3 N8 O24 S13'
_cod_database_code               4112953