Cyanosilylation of Aromatic Aldehydes by Cationic Ruthenium(II) Complexes of Benzimidazole-Derived O-Functionalized N-Heterocyclic Carbenes at Ambient Temperature under Solvent-Free Conditions.
Kumar, Dharmendra; Prakasham, A. P.; Das, Sharmistha; Datta, Anindya; Ghosh, Prasenjit; ACS omega 3 (2018) 1922–1938; doi:10.1021/acsomega.7b02090

data_4516021
_publ_section_title
;
 Cyanosilylation of Aromatic Aldehydes by Cationic Ruthenium(II) Complexes
 of Benzimidazole-Derived O-Functionalized N-Heterocyclic Carbenes at
 Ambient Temperature under Solvent-Free Conditions.
;
_journal_issue                   2
_journal_name_full               'ACS omega'
_journal_page_first              1922
_journal_page_last               1938
_journal_paper_doi               10.1021/acsomega.7b02090
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C30 H37 Cl N3 O Ru, Cl, H2 O'
_chemical_formula_sum            'C30 H39 Cl2 N3 O2 Ru'
_chemical_formula_weight         645.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-08-16
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_cell_angle_alpha                109.2536(19)
_cell_angle_beta                 99.6774(18)
_cell_angle_gamma                107.5084(18)
_cell_formula_units_Z            2
_cell_length_a                   9.9088(2)
_cell_length_b                   11.7379(2)
_cell_length_c                   14.6956(3)
_cell_measurement_reflns_used    14297
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.2860
_cell_measurement_theta_min      2.0330
_cell_volume                     1469.48(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15201
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.993
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         2.323
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5141
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0311P)^2^+0.7475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0616
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4865
_reflns_number_total             5141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b02090_si_002.cif
_cod_data_source_block           3c_PG-DK-05-133_Mo
_cod_database_code               4516021
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O2(H2A,H2B)
2.b Ternary CH refined with riding coordinates:
 C27(H27)
2.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B)
2.d Aromatic/amide H refined with riding coordinates:
 N3(H3), C5(H5), C3(H3A), C16(H16), C4(H4), C14(H14), C22(H22), C6(H6),
 C26(H26), C25(H25), C23(H23)
2.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C9(H9A,H9B,H9C), C29(H29A,H29B,
 H29C), C28(H28A,H28B,H28C), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'