Trends in Metal-Biradical Exchange Interaction for First-Row MII(Nitronyl Nitroxide-Semiquinone) Complexes
David A. Shultz; Kira E. Vostrikova; Scot H. Bodnar; Hyun-Joo Koo; Myung-Hwan Whangbo; Martin L. Kirk; Ezra C. Depperman; Jeff W. Kampf; Journal of the American Chemical Society 125 (2003) 1607–1617; doi:10.1021/ja020715x

data_4113442
_publ_section_title
;
 Trends in Metal-Biradical Exchange Interaction for First-Row MII(Nitronyl
 Nitroxide-Semiquinone) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1607
_journal_page_last               1617
_journal_paper_doi               10.1021/ja020715x
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C62 H73 B N8 O4 Zn'
_chemical_formula_weight         1070.46
_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                80.091(5)
_cell_angle_beta                 75.019(6)
_cell_angle_gamma                82.382(6)
_cell_formula_units_Z            4
_cell_length_a                   14.230(5)
_cell_length_b                   17.950(6)
_cell_length_c                   25.171(8)
_cell_measurement_reflns_used    4116
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      21.32
_cell_measurement_theta_min      2.18
_cell_volume                     6092(4)
_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      158(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_sigmaI/netI    0.1030
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            54050
_diffrn_reflns_theta_full        23.42
_diffrn_reflns_theta_max         23.42
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.829
_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    1.167
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1369
_refine_ls_number_reflns         17667
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1545
_refine_ls_R_factor_gt           0.0845
_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^)+(0.1277P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2199
_refine_ls_wR_factor_ref         0.2512
_reflns_number_gt                9298
_reflns_number_total             17667
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja020715x_1.cif
_cod_data_source_block           s475[NN-PhSQZnTpCum,Me]
_cod_database_code               4113442