Synthesis, Characterization, and Coordination Chemistry of the 2-Azaphenalenyl Radical
Shijun Zheng; Jie Lan; Saeed I. Khan; Yves Rubin; Journal of the American Chemical Society 125 (2003) 5786–5791; doi:10.1021/ja029236o

data_4113722
_publ_section_title
;
 Synthesis, Characterization, and Coordination Chemistry of the
 2-Azaphenalenyl Radical
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5786
_journal_page_last               5791
_journal_paper_doi               10.1021/ja029236o
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C41 H25 Cu F12 N2 O4'
_chemical_formula_weight         901.17
_space_group_IT_number           15
_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                 130.540(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.593(3)
_cell_length_b                   14.056(3)
_cell_length_c                   16.127(3)
_cell_measurement_reflns_used    884
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.40
_cell_measurement_theta_min      3.01
_cell_volume                     3719.8(12)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0746
_diffrn_reflns_av_sigmaI/netI    0.1881
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11827
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4438
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.1711
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1530
_reflns_number_gt                1887
_reflns_number_total             4438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029236osi20021108_042438.cif
_cod_data_source_block           yr250
_cod_original_cell_volume        3719.7(12)
_cod_database_code               4113722