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_4516020
_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         'C33 H43 Cl N3 O Ru, Cl, C H Cl3'
_chemical_formula_sum            'C34 H44 Cl5 N3 O Ru'
_chemical_formula_weight         789.04
_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   geom
_audit_creation_date             2017-02-19
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.10.28 svn.r3245 for OlexSys, GUI svn.r5128)
;
_cell_angle_alpha                69.6572(18)
_cell_angle_beta                 83.3894(13)
_cell_angle_gamma                82.6029(13)
_cell_formula_units_Z            2
_cell_length_a                   11.04197(15)
_cell_length_b                   13.3361(3)
_cell_length_c                   13.4517(3)
_cell_measurement_reflns_used    24757
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.1230
_cell_measurement_theta_min      1.9070
_cell_volume                     1836.57(7)
_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 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0493
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27452
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.596
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74141
_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    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.778
_refine_diff_density_min         -1.552
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6219
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0510P)^2^+4.2850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5860
_reflns_number_total             6219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b02090_si_002.cif
_cod_data_source_block           2c_PG-DK-05-161_Mo
_cod_original_cell_volume        1836.58(6)
_cod_database_code               4516020
_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
2. Uiso/Uaniso restraints and constraints
Uanis(Cl4) \\sim Ueq, Uanis(Cl5) \\sim Ueq, Uanis(Cl3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C21(H21), C18(H18), C31(H31), C34(H34)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C2(H2A,H2B)
3.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C15(H15), C14(H14), C8(H8), C16(H16), C28(H28), C7(H7), C5(H5),
 C29(H29), C6(H6), C26(H26), C25(H25)
3.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C23(H23A,H23B,H23C), C22(H22A,H22B,
 H22C), C19(H19A,H19B,H19C), C3(H3A,H3B,H3C), C33(H33A,H33B,H33C), C20(H20A,
 H20B,H20C)
;
_shelx_res_checksum              19428
_shelx_hkl_checksum              96543
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'