Trends in Exchange Coupling for Trimethylenemethane-Type Bis(semiquinone) Biradicals and Correlation of Magnetic Exchange with Mixed Valency for Cross-Conjugated Systems
David A. Shultz; Rosario M. Fico; Scot H. Bodnar; R. Krishna Kumar; Kira E. Vostrikova; Jeff W. Kampf; Paul D. Boyle; Journal of the American Chemical Society 125 (2003) 11761–11771; doi:10.1021/ja0367849

data_4114199
_publ_section_title
;
 Trends in Exchange Coupling for Trimethylenemethane-Type Bis(semiquinone)
 Biradicals and Correlation of Magnetic Exchange with Mixed Valency for
 Cross-Conjugated Systems
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11761
_journal_page_last               11771
_journal_paper_doi               10.1021/ja0367849
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C113.5 H141 B2 Cl N12 O4 Zn2'
_chemical_formula_weight         1925.19
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.610(4)
_cell_angle_beta                 67.429(3)
_cell_angle_gamma                70.397(3)
_cell_formula_units_Z            2
_cell_length_a                   18.2397(13)
_cell_length_b                   18.3714(14)
_cell_length_c                   18.3630(13)
_cell_measurement_reflns_used    7401
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      21.18
_cell_measurement_theta_min      2.70
_cell_volume                     5351.6(7)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_sigmaI/netI    0.0987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36621
_diffrn_reflns_theta_full        22.01
_diffrn_reflns_theta_max         22.01
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.9489
_exptl_absorpt_correction_T_min  0.8322
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       plate
_exptl_crystal_F_000             2050
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1246
_refine_ls_number_reflns         13069
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.1488
_refine_ls_R_factor_gt           0.0814
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1367P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2151
_refine_ls_wR_factor_ref         0.2440
_reflns_number_gt                6997
_reflns_number_total             13069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0367849si20030615_021726.cif
_cod_data_source_block           flat
_cod_original_formula_sum        'C113.50 H141 B2 Cl N12 O4 Zn2'
_cod_database_code               4114199