Profluorescent verdazyl radicals ‒ synthesis and characterization
Matuschek, David; Eusterwiemann, Steffen; Stegemann, Linda; Doerenkamp, Carsten; Wibbeling, Birgit; Daniliuc, Constantin G.; Doltsinis, Nikos L.; Strassert, Cristian A.; Eckert, Hellmut; Studer, Armido; Chem. Sci. 6 (2015) 4712–; doi:10.1039/C5SC00724K

data_1520453
_publ_section_title
;
 Profluorescent verdazyl radicals -- synthesis and characterization
;
_journal_issue                   8
_journal_name_full               'Chem. Sci.'
_journal_page_first              4712
_journal_paper_doi               10.1039/C5SC00724K
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C28 H19 N4 O'
_chemical_formula_weight         427.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-24 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.773(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7763(13)
_cell_length_b                   5.8280(3)
_cell_length_c                   16.1543(9)
_cell_measurement_reflns_used    2545
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      66.60
_cell_measurement_theta_min      0.88
_cell_volume                     1072.06(15)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.080
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10206
_diffrn_reflns_theta_full        63.37
_diffrn_reflns_theta_max         63.37
_diffrn_reflns_theta_min         3.88
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.9870
_exptl_absorpt_correction_T_min  0.7137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             446
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.174
_refine_diff_density_min         -0.145
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.4(6)
_refine_ls_extinction_coef       0.0041(10)
_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   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3257
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0987P)^2^+0.2609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1681
_reflns_number_gt                2635
_reflns_number_total             3257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc00724k2.cif
_cod_data_source_block           stu7039
_cod_depositor_comments
'Adding full bibliography for 1520452--1520455.cif.'
_cod_original_cell_volume        1072.06(14)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               1520453