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_4106534
_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,C80 H98 O2,1.5(C H Cl3)'
_chemical_formula_sum            'C128.5 H148.5 Cl4.5 N3 O4'
_chemical_formula_weight         1958.53
_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                105.149(7)
_cell_angle_beta                 102.006(4)
_cell_angle_gamma                96.112(6)
_cell_formula_units_Z            2
_cell_length_a                   15.632(6)
_cell_length_b                   19.012(8)
_cell_length_c                   20.288(9)
_cell_measurement_reflns_used    12879
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.1
_cell_volume                     5609(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      93(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1373
_diffrn_reflns_av_sigmaI/netI    0.1252
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58267
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.46
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.7593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             2098
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.421
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.704
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1279
_refine_ls_number_reflns         20614
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.700
_refine_ls_R_factor_all          0.2461
_refine_ls_R_factor_gt           0.2014
_refine_ls_shift/su_max          0.151
_refine_ls_shift/su_mean         0.009
_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          0.5020
_refine_ls_wR_factor_ref         0.5281
_reflns_number_gt                13060
_reflns_number_total             20614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205167e_si_004.cif
_cod_data_source_block           4
_cod_original_formula_sum        'C128.50 H148.50 Cl4.50 N3 O4'
_cod_database_code               4106534