Synthesis and characterisation of BODIPY radical anions
Victoria J. Richards; Alexandra L. Gower; Jasper E. H. B. Smith; E. Stephen Davies; Dorothee Lahaye; Anna G. Slater; William Lewis; Alexander J. Blake; Neil R. Champness; Deborah L. Kays; Chem.Commun. 48 (2012) 1751–; doi:10.1039/c2cc16047a

data_7107317
_publ_section_title
;
 Synthesis and characterisation of BODIPY radical anions
;
_journal_name_full               Chem.Commun.
_journal_page_first              1751
_journal_paper_doi               10.1039/c2cc16047a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C21 H15 B N2 O2'
_chemical_formula_weight         338.16
_chemical_name_systematic
;
?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            44
_cell_length_a                   25.1377(7)
_cell_length_b                   25.1377(7)
_cell_length_c                   27.1775(8)
_cell_measurement_reflns_used    4944
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.47
_cell_measurement_theta_min      3.51
_cell_volume                     17173.6(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_computing_molecular_graphics    ' ?'
_computing_publication_material
'enCIFer( Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'microfocus copper tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_av_sigmaI/netI    0.104
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            19436
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         74.64
_diffrn_reflns_theta_min         3.52
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  1.62
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       rod
_exptl_crystal_F_000             7744
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.032
_platon_squeeze_details
;
The residual electron density is attributed to three overlapping molecules,
of the same composition as the fully-occupied molecules, and each of
occupancy 0.25.
;
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.27
_refine_diff_density_rms         0.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.95
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8505
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      0.94
_refine_ls_R_factor_all          0.114
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.088P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.170
_refine_ls_wR_factor_ref         0.186
_reflns_number_gt                4628
_reflns_number_total             8505
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc16047a.txt
_cod_data_source_block           bjsona
_cod_original_cell_volume        17173.5(8)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7107317