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_4102658
_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_compound_source        ?
_chemical_formula_analytical     'C60 H54 N8 O6'
_chemical_formula_moiety         'C30 H26 N6 O4.C30 H28 N2 O2'
_chemical_formula_structural     'C60 H54 N8 O6'
_chemical_formula_sum            'C60 H54 N8 O6'
_chemical_formula_weight         983.11
_chemical_name_common            ?
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 108.408(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.547(4)
_cell_length_b                   11.196(3)
_cell_length_c                   16.222(4)
_cell_measurement_reflns_used    92
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      6
_cell_volume                     2506.9(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'CCLRC Daresbury Laboratory Station 9.8'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68840
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_sigmaI/netI    0.0878
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10380
_diffrn_reflns_theta_full        22.61
_diffrn_reflns_theta_max         22.61
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Siemens Madison WI USA'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       plate
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0093(35)
_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_all   1.053
_refine_ls_goodness_of_fit_obs   1.180
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3580
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.122
_refine_ls_restrained_S_obs      1.180
_refine_ls_R_factor_all          0.1499
_refine_ls_R_factor_obs          0.1012
_refine_ls_shift/esd_max         0.038
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1151P)^2^+4.8178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2693
_refine_ls_wR_factor_obs         0.2311
_reflns_number_observed          2455
_reflns_number_total             3630
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja1034683_si_002.cif
_cod_data_source_block           swrot3
_cod_depositor_comments
;
Replacing value '-' with '?' for the following tags:
'_chemical_compound_source', '_chemical_name_common', 
'_diffrn_standards_decay_%', '_diffrn_standards_interval_count', 
'_diffrn_standards_interval_time', '_diffrn_standards_number'.

Antanas Vaitkus, 2015-02-20

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1151P)^2^+4.8178P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1151P)^2^+4.8178P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4102658