Half-rotation in a kinetically locked [2]catenane induced by transition metal ion substitution
David A. Leigh; Paul J. Lusby; Alexandra M. Z. Slawin; D. Barney Walker; Chem.Commun. 48 (2012) 5826–; doi:10.1039/c2cc32418k

data_7107815
_publ_section_title
;
 Half-rotation in a kinetically locked [2]catenane induced by transition
 metal ion substitution
;
_journal_name_full               Chem.Commun.
_journal_page_first              5826
_journal_paper_doi               10.1039/c2cc32418k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C93 H111 N7 O12 Pd,2(C2 H2 N)'
_chemical_formula_sum            'C97 H117 N9 O12 Pd'
_chemical_formula_weight         1707.40
_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                77.683(8)
_cell_angle_beta                 74.610(8)
_cell_angle_gamma                81.063(8)
_cell_formula_units_Z            2
_cell_length_a                   13.579(2)
_cell_length_b                   17.669(3)
_cell_length_c                   19.456(3)
_cell_measurement_reflns_used    9061
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.1
_cell_volume                     4372.8(12)
_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 0.995
_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  0.0905
_diffrn_reflns_av_sigmaI/netI    0.1045
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44474
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1081
_refine_ls_number_reflns         15933
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1641
_refine_ls_R_factor_gt           0.1191
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1653P)^2^+23.0733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2963
_refine_ls_wR_factor_ref         0.3327
_reflns_number_gt                10647
_reflns_number_total             15933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32418k.txt
_cod_data_source_block           Pd3H2
_cod_original_cell_volume        4373.2(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107815