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_4104374
_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         'C96 H72 Co N6 O6, C3 H6 O, 2 (Cl O4)'
_chemical_formula_sum            'C99 H78 Cl2 Co N6 O15'
_chemical_formula_weight         1721.50
_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                103.808(2)
_cell_angle_beta                 98.2280(10)
_cell_angle_gamma                101.688(2)
_cell_formula_units_Z            2
_cell_length_a                   13.9680(4)
_cell_length_b                   16.0410(3)
_cell_length_c                   20.7350(6)
_cell_measurement_reflns_used    45681
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     4327.6(2)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41339
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1790
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
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_refine_diff_density_max         1.312
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_parameters     1174
_refine_ls_number_reflns         19615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1023P)^2^+0.7867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1918
_reflns_number_gt                13812
_reflns_number_total             19615
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja809267z_si_004.cif
_cod_data_source_block           sauv6
_cod_original_cell_volume        4327.61(19)
_cod_database_code               4104374