Synthesis and Structure of a Complex Having a Quartet Ground State with Three Entirely Different Spin Carriers: Nitronyl Nitroxide, o-Semiquinone, and CuII
David A. Shultz; Scot H. Bodnar; Kira E. Vostrikova; Jeff W. Kampf; Inorganic Chemistry 39 (2000) 6091–6093; doi:10.1021/ic0009122

data_4321715
_publ_section_title
;
 Synthesis and Structure of a Complex Having a Quartet Ground State with
 Three Entirely Different Spin Carriers: Nitronyl Nitroxide,
 o-Semiquinone, and CuII
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6091
_journal_page_last               6093
_journal_paper_doi               10.1021/ic0009122
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C56 H69 B N8 O4 Zn'
_chemical_formula_weight         994.37
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 98.240(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5781(12)
_cell_length_b                   17.7408(17)
_cell_length_c                   24.440(2)
_cell_measurement_reflns_used    6650
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      21.44
_cell_measurement_theta_min      2.26
_cell_volume                     5397.4(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1162
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            50007
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            maroon
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.0019(2)
_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   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         9202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+23.7979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1770
_refine_ls_wR_factor_ref         0.1907
_reflns_number_gt                7030
_reflns_number_total             9202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0009122.cif
_cod_data_source_block           znnsq
_cod_original_cell_volume        5397.3(9)
_cod_database_code               4321715