En Route to a Molecular Sheaf: Active Metal Template Synthesis of a [3]Rotaxane with Two Axles Threaded through One Ring
Hei Man Cheng; David A. Leigh; Francesca Maffei; Paul R. McGonigal; Alexandra M. Z. Slawin; Jhenyi Wu; Journal of the American Chemical Society 133 (2011) 12298–12303; doi:10.1021/ja205167e

data_4106535
_publ_section_title
;
 En Route to a Molecular Sheaf: Active Metal Template Synthesis of a
 [3]Rotaxane with Two Axles Threaded through One Ring
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12298
_journal_page_last               12303
_journal_paper_doi               10.1021/ja205167e
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C207 H245 N3 O6,10(C H Cl3)'
_chemical_formula_sum            'C217 H255 Cl30 N3 O6'
_chemical_formula_weight         4064.74
_chemical_name_systematic
; 
 ? 
;
_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                91.765(10)
_cell_angle_beta                 100.119(9)
_cell_angle_gamma                90.483(13)
_cell_formula_units_Z            2
_cell_length_a                   14.886(3)
_cell_length_b                   25.124(6)
_cell_length_c                   29.790(7)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.8
_cell_measurement_theta_min      21.3
_cell_volume                     10962(4)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            143749
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.52
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    3.817
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4272
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.731
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1909
_refine_ls_number_reflns         37247
_refine_ls_number_restraints     1308
_refine_ls_restrained_S_all      1.713
_refine_ls_R_factor_all          0.2215
_refine_ls_R_factor_gt           0.1900
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4756
_refine_ls_wR_factor_ref         0.5084
_reflns_number_gt                21402
_reflns_number_total             37247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205167e_si_005.cif
_cod_data_source_block           5
_cod_database_code               4106535