Oxidant-free Synthesis of Benzimidazoles from Alcohols and Aromatic Diamines Catalysed by New Ru(II)-PNS(O) Pincer Complexes
Luo, Qi; Dai, Zengjin; Cong, Hengjiang; Li, Renjie; Peng, Tianyou; Zhang, Jing; Dalton Trans.  (2017) –; doi:10.1039/C7DT02584J

data_7044376
_publ_section_title
;
 Oxidant-free Synthesis of Benzimidazoles from Alcohols and Aromatic
 Diamines Catalysed by New Ru(II)-PNS(O) Pincer Complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02584J
_journal_year                    2017
_chemical_formula_sum            'C48 H43 Cl2 F6 N3 O P2 Ru S'
_chemical_formula_weight         1057.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1n5tm8
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-29 deposited with the CCDC.
2017-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                73.1800(10)
_cell_angle_beta                 71.4470(10)
_cell_angle_gamma                66.8320(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4078(6)
_cell_length_b                   14.0340(8)
_cell_length_c                   16.4595(9)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.64
_cell_measurement_theta_min      2.27
_cell_volume                     2255.6(2)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEX-Duo CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45069
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.712
_diffrn_reflns_theta_min         1.883
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1 (Bruker,2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.612
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         11590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+2.0069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9604
_reflns_number_total             11590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02584j2.cif
_cod_data_source_block           x_a_CCDC1
_cod_database_code               7044376
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.915
_shelx_estimated_absorpt_t_max   0.932