Identification of a Foldaxane Kinetic Byproduct during Guest-Induced Single to Double Helix Conversion
Quan Gan; Yann Ferrand; Nagula Chandramouli; Brice Kauffmann; Christophe Aube; Didier Dubreuil; Ivan Huc; Journal of the American Chemical Society 134 (2012) 15656–15659; doi:10.1021/ja3064364

data_4118666
_publ_section_title
;
 Identification of a Foldaxane Kinetic Byproduct during Guest-Induced
 Single to Double Helix Conversion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15656
_journal_page_last               15659
_journal_paper_doi               10.1021/ja3064364
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C126 H134 Cl12 N22 O25'
_chemical_formula_weight         2781.96
_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
_audit_update_record
;
2012-07-02 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.388(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.097(4)
_cell_length_b                   31.196(5)
_cell_length_c                   40.446(6)
_cell_measurement_reflns_used    1832
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      52.6
_cell_measurement_theta_min      1.8
_cell_volume                     28665(8)
_computing_cell_refinement       SAINT
_computing_data_collection       'Bruker Proteum2 suite'
_computing_data_reduction        SAINT
_computing_molecular_graphics    wingx
_computing_publication_material  wingx
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.897
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  'four circles'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Helios optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            165090
_diffrn_reflns_theta_full        52.63
_diffrn_reflns_theta_max         52.63
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    2.727
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.354
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       plate
_exptl_crystal_F_000             10402
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.596
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       0.00012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.802
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3312
_refine_ls_number_reflns         29514
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.807
_refine_ls_R_factor_all          0.1867
_refine_ls_R_factor_gt           0.1429
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.051
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3437
_refine_ls_wR_factor_ref         0.3910
_reflns_number_gt                20072
_reflns_number_total             29514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3064364_si_003.cif
_cod_data_source_block           complexe
_cod_original_cell_volume        28666(8)
_cod_database_code               4118666