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_4516022
_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         'C46 H56 Ag2 N6 O2'
_chemical_formula_sum            'C46 H56 Ag2 N6 O2'
_chemical_formula_weight         940.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-12-21
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.10.28 svn.r3245 for OlexSys, GUI svn.r5128)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.163(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8105(3)
_cell_length_b                   15.9779(3)
_cell_length_c                   14.0138(4)
_cell_measurement_reflns_used    12795
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.3350
_cell_measurement_theta_min      2.2080
_cell_volume                     2109.85(10)
_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      150
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -59.00  70.00   0.50    5.00    --  -20.00  72.00-108.00  258
  2  \w    -58.50  49.00   0.50    5.00    --  -20.00  72.00-180.00  215
  3  \w    -35.00  -5.00   0.50    5.00    --  -20.00 -72.00-108.00   60
  4  \w   -110.00 -19.50   0.50    5.00    --  -20.00 -72.00-180.00  181
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0199414000
_diffrn_orient_matrix_UB_12      0.0364593000
_diffrn_orient_matrix_UB_13      -0.0294038000
_diffrn_orient_matrix_UB_21      0.0238932000
_diffrn_orient_matrix_UB_22      0.0252850000
_diffrn_orient_matrix_UB_23      0.0431146000
_diffrn_orient_matrix_UB_31      0.0684803000
_diffrn_orient_matrix_UB_32      0.0019082000
_diffrn_orient_matrix_UB_33      -0.0074723000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12562
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.601
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45924
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.296
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.127
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0402P)^2^+2.0622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3475
_reflns_number_total             3631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b02090_si_002.cif
_cod_data_source_block           2b_PG-DK-05-120_Mo
_cod_original_cell_volume        2109.86(9)
_cod_database_code               4516022
_chemical_oxdiff_formula         C23H23Ag1N3O1
_reflns_odcompleteness_completeness 90.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.11
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C14(H14), C15(H15), C16(H16)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              96904
_shelx_hkl_checksum              74030
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.481
_oxdiff_exptl_absorpt_empirical_full_min 0.707