Probing Cucurbituril Assemblies in Water with TEMPO-like Nitroxides: A Trinitroxide Supraradical with Spin-Spin Interactions
David Bardelang; Karol Banaszak; Hakim Karoui; Antal Rockenbauer; Mélanie Waite; Konstantin Udachin; John A. Ripmeester; Christopher I. Ratcliffe; Olivier Ouari; Paul Tordo; Journal of the American Chemical Society 131 (2009) 5402–5404; doi:10.1021/ja900306m

data_4104219
_publ_section_title
;
 Probing Cucurbituril Assemblies in Water with TEMPO-like Nitroxides: A
 Trinitroxide Supraradical with Spin-Spin Interactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5402
_journal_page_last               5404
_journal_paper_doi               10.1021/ja900306m
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C348 H412.4 N198 O111.2'
_chemical_formula_weight         9148.36
_chemical_name_common            cucurbit[8]uril
_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                 105.33(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   44.283(9)
_cell_length_b                   31.672(6)
_cell_length_c                   37.209(7)
_cell_measurement_reflns_used    9225
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      41.63
_cell_measurement_theta_min      2.169
_cell_volume                     50330(18)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'ATOMS V.5.0'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            52620
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         0.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9636
_exptl_absorpt_correction_T_min  0.9504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             19104
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.361
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     6154
_refine_ls_number_reflns         52620
_refine_ls_number_restraints     8904
_refine_ls_restrained_S_all      1.288
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.1048
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3196
_refine_ls_wR_factor_ref         0.3393
_reflns_number_gt                35950
_reflns_number_total             52620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja900306m_si_002.cif
_cod_data_source_block           dav84
_cod_original_cell_volume        50330(17)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C348 H412.40 N198 O111.20'
_cod_database_code               4104219