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_4114200
_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            'C108 H128 B2 Cl4 N12 O4 Zn2'
_chemical_formula_weight         1952.38
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_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 116.337(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.376(2)
_cell_length_b                   18.9790(12)
_cell_length_c                   18.4471(12)
_cell_measurement_reflns_used    7402
_cell_measurement_temperature    118(2)
_cell_measurement_theta_max      22.33
_cell_measurement_theta_min      2.80
_cell_volume                     10158.5(11)
_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      118(2)
_diffrn_detector_area_resol_mean 0.90
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0636
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33091
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.8942
_exptl_absorpt_correction_T_min  0.8625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       block
_exptl_crystal_F_000             4120
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         7306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0903
_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^)+(0.1925P)^2^+48.5126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2638
_refine_ls_wR_factor_ref         0.3128
_reflns_number_gt                4627
_reflns_number_total             7306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0367849si20030615_021751.cif
_cod_data_source_block           rfnor
_cod_original_cell_volume        10158.4(11)
_cod_database_code               4114200