Two Axles Threaded Using a Single Template Site: Active Metal Template Macrobicyclic [3]Rotaxanes
Stephen M. Goldup; David A. Leigh; Paul R. McGonigal; Vicki E. Ronaldson; Alexandra M. Z. Slawin; Journal of the American Chemical Society 132 (2010) 315–320; doi:10.1021/ja9080716

data_4101770
_publ_section_title
;
 Two Axles Threaded Using a Single Template Site: Active Metal Template
 Macrobicyclic [3]Rotaxanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              315
_journal_page_last               320
_journal_paper_doi               10.1021/ja9080716
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C51 H76 Cl2 N2 O6 Pd'
_chemical_formula_sum            'C51 H76 Cl2 N2 O6 Pd'
_chemical_formula_weight         990.44
_chemical_name_systematic
; 
 ? 
;
_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                 102.806(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.431(5)
_cell_length_b                   21.805(6)
_cell_length_c                   12.751(4)
_cell_measurement_reflns_used    11672
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.7613
_cell_measurement_theta_min      1.1329
_cell_volume                     4997(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            47896
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.0800
_refine_diff_density_max         1.716
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.0020(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         9169
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0855
_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^)+(0.1291P)^2^+12.5084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2288
_refine_ls_wR_factor_ref         0.2379
_reflns_number_gt                8137
_reflns_number_total             9169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9080716_si_001.cif
_cod_data_source_block           35.PdCl2(MeCN).
_cod_original_cell_volume        4997(3)
_cod_database_code               4101770