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_4114202
_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            'C114.5 H142 B2 Cl9 N12 O4 Zn2'
_chemical_formula_weight         2221.81
_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                100.534(3)
_cell_angle_beta                 96.673(3)
_cell_angle_gamma                113.552(3)
_cell_formula_units_Z            2
_cell_length_a                   15.8309(15)
_cell_length_b                   18.2583(18)
_cell_length_c                   24.387(2)
_cell_measurement_reflns_used    6810
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.82
_cell_volume                     6211.2(10)
_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      150(2)
_diffrn_detector_area_resol_mean 0.75
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0838
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            73436
_diffrn_reflns_theta_full        28.44
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.7109
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.58
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.0008(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.599
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1305
_refine_ls_number_reflns         30348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.599
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0821
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2337
_refine_ls_wR_factor_ref         0.2446
_reflns_number_gt                19922
_reflns_number_total             30348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0367849si20030615_022359.cif
_cod_data_source_block           rf441d
_cod_original_cell_volume        6211.1(10)
_cod_original_formula_sum        'C114.50 H142 B2 Cl9 N12 O4 Zn2'
_cod_database_code               4114202