Singlet-Triplet Gap in Triplet Ground-State Biradicals Is Modulated by Substituent Effects
David A. Shultz; Scot H. Bodnar; Hyoyoung Lee; Jeff W. Kampf; Christopher D. Incarvito; Arnold L. Rheingold; Journal of the American Chemical Society 124 (2002) 10054–10061; doi:10.1021/ja020154+

data_4115068
_publ_section_title
;
 Singlet-Triplet Gap in Triplet Ground-State Biradicals Is Modulated by
 Substituent Effects
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10054
_journal_page_last               10061
_journal_paper_doi               10.1021/ja020154+
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C111 H123 B2 Cl6 N12 O4 Zn2'
_chemical_formula_weight         2054.27
_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                99.258(6)
_cell_angle_beta                 92.264(7)
_cell_angle_gamma                97.887(6)
_cell_formula_units_Z            2
_cell_length_a                   12.688(5)
_cell_length_b                   12.987(5)
_cell_length_c                   33.514(12)
_cell_measurement_reflns_used    6223
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.23
_cell_volume                     5388(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 0.950
_diffrn_measured_fraction_theta_max 0.950
_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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            65261
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       plate
_exptl_crystal_F_000             2154
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.821
_refine_diff_density_min         0.844
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.0026(5)
_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   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1543
_refine_ls_number_reflns         21029
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1447P)^2^+20.7815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2643
_refine_ls_wR_factor_ref         0.2880
_reflns_number_gt                15559
_reflns_number_total             21029
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0201542B_2.cif
_cod_data_source_block           s214[(TpCum,MeZn)21-t-Bu]
_cod_original_cell_volume        5388(3)
_cod_database_code               4115068