Light-Mediated C-C σ-Bond Driven Crystallization of a Phenalenyl Radical Dimer
Puhong Liao; Mikhail E. Itkis; Richard T. Oakley; Fook S. Tham; Robert C. Haddon; Journal of the American Chemical Society 126 (2004) 14297–14302; doi:10.1021/ja046243z

data_4113117
_publ_section_title
;
 Light-Mediated C-C \s-Bond Driven Crystallization of a Phenalenyl Radical
 Dimer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14297
_journal_page_last               14302
_journal_paper_doi               10.1021/ja046243z
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C70 H74 B2 N4 O2'
_chemical_formula_weight         1024.95
_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                73.246(4)
_cell_angle_beta                 67.638(4)
_cell_angle_gamma                69.852(4)
_cell_formula_units_Z            2
_cell_length_a                   14.457(3)
_cell_length_b                   14.650(3)
_cell_length_c                   16.026(3)
_cell_measurement_temperature    218(2)
_cell_volume                     2898.2(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      218(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         'Normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50226
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_correction_T_min  0.9741
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_meas      0
_exptl_crystal_description       'prism frag.'
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         14399
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+0.9857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1631
_reflns_number_gt                9750
_reflns_number_total             14399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046243zsi20040628_100151.cif
_cod_data_source_block           rh47r1m
_cod_original_cell_volume        2898.2(9)
_cod_database_code               4113117