Sequential O- and N-Acylation Protocol for High-Yield Preparation and Modification of Rotaxanes: Synthesis, Functionalization, Structure, and Intercomponent Interaction of Rotaxanes
Yuya Tachibana; Hiroaki Kawasaki; Nobuhiro Kihara; Toshikazu Takata; Journal of Organic Chemistry 71 (2006) 5093–5104; doi:10.1021/jo0601563

data_4021778
_publ_contact_author_email       ttakata@polymer.titech.ac.jp
_publ_contact_author_name        'Toshikazu Takata'
_publ_section_title
;
 Sequential O- and N-Acylation Protocol for High-Yield Preparation
 and Modification of Rotaxanes: Synthesis, Functionalization,
 Structure, and Intercomponent Interaction of Rotaxanes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5093
_journal_page_last               5104
_journal_paper_doi               10.1021/jo0601563
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C46 H59 N O11 '
_chemical_formula_sum            'C46 H59 N O11'
_chemical_formula_weight         801.97
_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'
_audit_creation_date             2001-07-06
_audit_creation_method           'by CrystalStructure v2.00'
_cell_angle_alpha                90
_cell_angle_beta                 93.445(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6538(4)
_cell_length_b                   19.8519(5)
_cell_length_c                   15.3287(5)
_cell_measurement_reflns_used    25405
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     4451.1(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure Ver. 2.00'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9916
_diffrn_measured_fraction_theta_max 0.9930
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40179
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.35
_refine_ls_extinction_coef       1218.7(1)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     693
_refine_ls_number_reflns         10120
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.0060
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.003Fo^2^ + 1.000\s^2^(Fo)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1910
_reflns_number_gt                5384
_reflns_number_total             10412
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo0601563si20060409_031711.cif
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C46 H59 N O11 '
_cod_database_code               4021778