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_4021777
_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         'C56 H64 N2 O11 '
_chemical_formula_sum            'C56 H64 N2 O11'
_chemical_formula_weight         941.13
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             2003-04-04
_audit_creation_method           'by CrystalStructure v3.00'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9969(2)
_cell_length_b                   29.4294(4)
_cell_length_c                   11.8503(1)
_cell_measurement_reflns_used    67662
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.7
_cell_volume                     5230.1(1)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure Ver. 3.00'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9960
_diffrn_measured_fraction_theta_max 0.9982
_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  0.034
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6619
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.942
_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    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2008.00
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.28
_refine_ls_extinction_coef       2114.6(1)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     731
_refine_ls_number_reflns         6605
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.0050
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 1.0000\s^2^(Fo) + 0.0000]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                4216
_reflns_number_total             6618
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo0601563si20060409_031640.cif
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C56 H64 N2 O11 '
_cod_database_code               4021777