Exchange Coupling Mediated Through-Bonds and Through-Space in Conformationally Constrained Polyradical Scaffolds: Calix[4]arene Nitroxide Tetraradicals and Diradical
Andrzej Rajca; Sumit Mukherjee; Maren Pink; Suchada Rajca; Journal of the American Chemical Society 128 (2006) 13497–13507; doi:10.1021/ja063567+

data_4110968
_publ_section_title
;
 Exchange Coupling Mediated Through-Bonds and Through-Space in
 Conformationally Constrained Polyradical Scaffolds: Calix[4]arene
 Nitroxide Tetraradicals and Diradical
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13497
_journal_page_last               13507
_journal_paper_doi               10.1021/ja063567+
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C56 H80 N4 O12'
_chemical_formula_sum            'C56 H80 N4 O12'
_chemical_formula_weight         1001.24
_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                 100.379(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.920(4)
_cell_length_b                   35.167(9)
_cell_length_c                   10.593(3)
_cell_measurement_reflns_used    7499
_cell_measurement_temperature    137(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.2
_cell_volume                     5467(3)
_computing_cell_refinement       'SAINT (Bruker, current version)'
_computing_data_collection       'SMART (Bruker, current version)'
_computing_data_reduction        'SAINT (Bruker, current version)'
_computing_molecular_graphics    'SHELXTL (Bruker), XTEL (Local Library)'
_computing_publication_material  'SHELXTL (Bruker)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      137(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
'0.30 degree frames measured for 15 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_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
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_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            82665
_diffrn_reflns_theta_full        27.73
_diffrn_reflns_theta_max         27.73
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  606
_diffrn_standards_number         284
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.9915
_exptl_absorpt_correction_T_min  0.9791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing (1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         12675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+2.3431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                9499
_reflns_number_total             12675
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063567si20060522_033115.cif
_cod_data_source_block           03456
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        5467(2)
_cod_database_code               4110968