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_4106532
_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         'C47 H49 N3 O2'
_chemical_formula_sum            'C47 H49 N3 O2'
_chemical_formula_weight         687.89
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 107.210(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.463(4)
_cell_length_b                   22.062(8)
_cell_length_c                   15.984(6)
_cell_measurement_reflns_used    3340
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.3
_cell_measurement_theta_min      21.3
_cell_volume                     3861(2)
_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 0.949
_diffrn_measured_fraction_theta_max 0.939
_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  0.1331
_diffrn_reflns_av_sigmaI/netI    0.0962
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49816
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.34
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.7584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         13003
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.1409
_refine_ls_R_factor_gt           0.1077
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.003
_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          0.2891
_refine_ls_wR_factor_ref         0.3276
_reflns_number_gt                8798
_reflns_number_total             13003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205167e_si_002.cif
_cod_data_source_block           1
_cod_database_code               4106532