Nitrone [2]Rotaxanes: Simultaneous Chemical Protection and Electrochemical Activation of a Functional Group
Daniel M. D'Souza; David A. Leigh; Loïc Mottier; Kathleen M. Mullen; Francesco Paolucci; Simon J. Teat; Songwei Zhang; Journal of the American Chemical Society 132 (2010) 9465–9470; doi:10.1021/ja1034683

data_4102657
_publ_section_title
;
 Nitrone [2]Rotaxanes: Simultaneous Chemical Protection and
 Electrochemical Activation of a Functional Group
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9465
_journal_page_last               9470
_journal_paper_doi               10.1021/ja1034683
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C62 H56 N6 O6'
_chemical_formula_weight         981.13
_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                81.4610(10)
_cell_angle_beta                 70.9250(10)
_cell_angle_gamma                76.3450(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1989(6)
_cell_length_b                   12.7110(6)
_cell_length_c                   18.6558(10)
_cell_measurement_reflns_used    5030
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     2648.6(2)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'SHELXTL PC (Siemens, 1994)'
_computing_publication_material  'SHELXTL PC (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Siemens SMART diffractometer'
_diffrn_measurement_method       '\w 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  0.0504
_diffrn_reflns_av_sigmaI/netI    0.1171
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16274
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.16
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.189
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.0129(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   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         9087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1214
_reflns_number_gt                4739
_reflns_number_total             9087
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1034683_si_001.cif
_cod_data_source_block           swrot1
_cod_database_code               4102657