Oxidation Products of Doubly Trimethylene-Bridged Tetrabenzyl p-Phenylenediamine Paracyclophane
Almaz S. Jalilov; Lu Han; Stephen F. Nelsen; Ilia A. Guzei; Journal of Organic Chemistry 78 (2013) 11373–11381; doi:10.1021/jo401921f

data_4028755
_publ_contact_author_address
;
Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI  53706
USA
;
_publ_contact_author_email       iguzei@chem.wisc.edu
_publ_contact_author_fax         608-262-0381
_publ_contact_author_name
;
Guzei, Ilia A. 
;
_publ_contact_author_phone       608-263-4694
_publ_section_title
;
 Oxidation Products of Doubly Trimethylene-Bridged Tetrabenzyl
 p-Phenylenediamine Paracyclophane
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              11373
_journal_page_last               11381
_journal_paper_doi               10.1021/jo401921f
_journal_volume                  78
_journal_year                    2013
_chemical_formula_moiety         'C46 H48 N4, 4(C3H6O), 2(F6 Sb)'
_chemical_formula_sum            'C58 H72 F12 N4 O4 Sb2'
_chemical_formula_weight         1360.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                81.6450(11)
_cell_angle_beta                 83.7998(12)
_cell_angle_gamma                79.6147(11)
_cell_formula_units_Z            1
_cell_length_a                   10.6821(3)
_cell_length_b                   11.5613(3)
_cell_length_c                   12.1911(3)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.3355
_cell_measurement_theta_min      2.8676
_cell_volume                     1460.02(7)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXTL, OLEX2 (Dolomanov et al., 2009)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.40\% \w and 0.5\% \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0128
_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       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36038
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  0.9056
_exptl_absorpt_correction_T_min  0.7788
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2007)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       block
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         7258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0174
_refine_ls_R_factor_gt           0.0164
_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^)+(0.0184P)^2^+0.6495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0411
_refine_ls_wR_factor_ref         0.0417
_reflns_number_gt                6965
_reflns_number_total             7258
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo401921f_si_002.cif
_cod_data_source_block           nelsen26
_cod_original_sg_symbol_Hall     '-P 1        '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4028755