Getting Harder: Cobalt(III)-Template Synthesis of Catenanes and Rotaxanes
Leigh, David A.; Lusby, Paul J.; McBurney, Roy T.; Morelli, Alessandra; Slawin, Alexandra M. Z.; Thomson, Andrew R.; Walker, D. Barney; Journal of the American Chemical Society 131 (2009) 3762–3771; doi:10.1021/ja809627j

data_4104024
_publ_section_title
;
 Getting Harder: Cobalt(III)-Template Synthesis of Catenanes and Rotaxanes
;
_journal_coden_ASTM              JACSAT
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3762
_journal_page_last               3771
_journal_paper_doi               10.1021/ja809627j
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C62 H70 Co N6 O8,C6 H16 N'
_chemical_formula_sum            'C68 H86 Co N7 O8'
_chemical_formula_weight         1188.37
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.176(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4921(6)
_cell_length_b                   19.1721(8)
_cell_length_c                   21.3192(9)
_cell_measurement_reflns_used    17258
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      1.08
_cell_volume                     6232.5(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 0.992
_diffrn_measured_fraction_theta_max 0.991
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            57765
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.419
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         11312
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+11.7397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.1807
_reflns_number_gt                10412
_reflns_number_total             11312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809627j_si_002.cif
_cod_data_source_block           dled175
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-09
;
_cod_database_code               4104024