Synthesis of New Dipyrido-Annulated N-Heterocyclic Carbenes with Ortho Substituents
Shin-ichi Fuku-en; Junki Yamamoto; Mao Minoura; Satoshi Kojima; Yohsuke Yamamoto; Inorganic Chemistry 52 (2013) 11700–11702; doi:10.1021/ic402301u

data_4336493
_publ_contact_author_email       yyama@hiroshima-u.ac.jp
_publ_section_title
;
 Synthesis of New Dipyrido-Annulated N-Heterocyclic Carbenes with Ortho
 Substituents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11700
_journal_page_last               11702
_journal_paper_doi               10.1021/ic402301u
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C35 H41 I N2 O S2'
_chemical_formula_weight         696.72
_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                 91.481(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.288(6)
_cell_length_b                   10.971(3)
_cell_length_c                   25.321(6)
_cell_measurement_reflns_used    3226
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.35
_cell_volume                     6745(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayered confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0866
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13855
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  0.9891
_exptl_absorpt_correction_T_min  0.7920
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1997)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       plate
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0885P)^2^+7.9391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1739
_reflns_number_gt                3210
_reflns_number_total             5564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402301u_si_002.cif
_cod_data_source_block           4b
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4336493