Synthesis of Aza-m-Xylylene Diradicals with Large Singlet-Triplet Energy Gap and Statistical Analyses of Their EPR Spectra.
Olankitwanit, Arnon; Pink, Maren; Rajca, Suchada; Rajca, Andrzej; Journal of the American Chemical Society 136 (2014) 14277–; doi:10.1021/ja508119d

data_4122705
_publ_section_title
;
 Synthesis of Aza-m-Xylylene Diradicals with Large Singlet-Triplet Energy
 Gap and Statistical Analyses of Their EPR Spectra.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14277
_journal_paper_doi               10.1021/ja508119d
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C38 H60 N2'
_chemical_formula_weight         544.88
_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                 100.198(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0042(15)
_cell_length_b                   9.8362(8)
_cell_length_c                   22.3583(19)
_cell_measurement_reflns_used    2006
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      15.45
_cell_measurement_theta_min      2.40
_cell_volume                     3464.1(5)
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2012)'
_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2012)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2012)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2012)'
_computing_publication_material  'SHELXTL (Bruker, 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2012)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details      '0.5 degree frames measured for 2 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'silicon  1 1 1 and 3 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1246
_diffrn_reflns_av_sigmaI/netI    0.1212
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28319
_diffrn_reflns_theta_full        15.59
_diffrn_reflns_theta_max         15.59
_diffrn_reflns_theta_min         0.75
_exptl_absorpt_coefficient_mu    0.029
_exptl_absorpt_correction_T_max  0.9999
_exptl_absorpt_correction_T_min  0.9997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.002
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1627
_reflns_number_gt                4097
_reflns_number_total             7581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja508119d_si_002.cif
_cod_data_source_block           12511
_cod_depositor_comments
'Adding full bibliography for 4122705--4122706.cif.'
_cod_original_cell_volume        3464.0(5)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4122705