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_4336495
_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            'C39 H40 I N2 Rh S2'
_chemical_formula_weight         830.66
_chemical_name_systematic
;
 ?
;
_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                90.000(2)
_cell_angle_beta                 90.000(2)
_cell_angle_gamma                96.169(2)
_cell_formula_units_Z            8
_cell_length_a                   14.123(2)
_cell_length_b                   16.273(3)
_cell_length_c                   32.044(6)
_cell_measurement_reflns_used    9248
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.38
_cell_volume                     7322(2)
_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 0.934
_diffrn_measured_fraction_theta_max 0.934
_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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.1642
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            40138
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    1.453
_exptl_absorpt_correction_T_max  0.8683
_exptl_absorpt_correction_T_min  0.5644
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1997)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       plate
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.215
_refine_diff_density_min         -1.710
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1646
_refine_ls_number_reflns         31444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          1.276
_refine_ls_shift/su_mean         0.039
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1934
_reflns_number_gt                18710
_reflns_number_total             31444
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402301u_si_004.cif
_cod_data_source_block           9b
_cod_database_code               4336495