Passing Two Strings through the Same Ring Using an Octahedral Metal Center as Template: A New Synthesis of [3]Rotaxanes
Alexander I. Prikhod'ko; Jean-Pierre Sauvage; Journal of the American Chemical Society 131 (2009) 6794–6807; doi:10.1021/ja809267z

data_4104372
_publ_section_title
;
 Passing Two Strings through the Same Ring Using an Octahedral Metal
 Center as Template: A New Synthesis of [3]Rotaxanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6794
_journal_page_last               6807
_journal_paper_doi               10.1021/ja809267z
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C117 H96 Co N6 O10, 2(C3 H6 O), 3(F6 P)'
_chemical_formula_sum            'C123 H108 Co F18 N6 O12 P3'
_chemical_formula_weight         2355.99
_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                89.2340(10)
_cell_angle_beta                 78.448(2)
_cell_angle_gamma                84.786(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4954(3)
_cell_length_b                   19.0943(6)
_cell_length_c                   25.8961(8)
_cell_measurement_reflns_used    189236
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     6510.7(3)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1692
_diffrn_reflns_av_sigmaI/netI    0.2851
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            80608
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2436
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.173
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1452
_refine_ls_number_reflns         29651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.3290
_refine_ls_R_factor_gt           0.1465
_refine_ls_shift/su_max          0.000
_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          0.3587
_refine_ls_wR_factor_ref         0.4388
_reflns_number_gt                9949
_reflns_number_total             29651
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja809267z_si_002.cif
_cod_data_source_block           sauv13
_cod_database_code               4104372