The Suzuki‒Miyaura reaction as a tool for modification of phenoxyl-nitroxyl radicals of the 4H-imidazole N-oxide series
Ten, Yury A.; Salnikov, Oleg G.; Amitina, Svetlana A.; Stass, Dmitri V.; Rybalova, Tatyana V.; Kazantsev, Maxim S.; Bogomyakov, Artem S.; Mostovich, Evgeny A.; Mazhukin, Dmitrii G.; RSC Advances 8 (2018) 26099–; doi:10.1039/C8RA05103H

data_7231209
_publ_section_title
;
 The Suzuki--Miyaura reaction as a tool for modification of
 phenoxyl-nitroxyl radicals of the 4H-imidazole N-oxide series
;
_journal_issue                   46
_journal_name_full               'RSC Advances'
_journal_page_first              26099
_journal_paper_doi               10.1039/C8RA05103H
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C31 H35 N2 O2'
_chemical_formula_sum            'C31 H35 N2 O2'
_chemical_formula_weight         467.61
_chemical_name_systematic
"'2,6-Di-tretbutyl-4-[1-oxi-(4-(biphenyl-4-yl)-5,5-dimethyl-1H-imidazol -2(5H)-yliden]cyclohexa-2,5-dienone'"
_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
_audit_update_record
;
2017-07-26 deposited with the CCDC.
2018-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.552(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5429(7)
_cell_length_b                   14.3317(8)
_cell_length_c                   16.9947(10)
_cell_measurement_reflns_used    9785
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.77
_cell_measurement_theta_min      3.11
_cell_volume                     2649.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50398
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.19
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.8623
_exptl_absorpt_correction_T_min  0.8158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1004
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent:  aprotone dipolar acetonitryl'
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.308
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         7602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.308
_refine_ls_R_factor_all          0.1501
_refine_ls_R_factor_gt           0.0954
_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^)+(0.1395P)^2^+1.7714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2911
_refine_ls_wR_factor_ref         0.3367
_reflns_number_gt                5116
_reflns_number_total             7602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ra05103h2.cif
_cod_data_source_block           comp11a_ten_75x
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               7231209