One pot tandem dual CC and CO bond reductions in the β-alkylation of secondary alcohols with primary alcohols by ruthenium complexes of amido and picolyl functionalized N-heterocyclic carbenes.
Prakasham, A. P.; Ta, Sabyasachi; Dey, Shreyata; Ghosh, Prasenjit; Dalton transactions (Cambridge, England : 2003) 50 (2021) 15640–15654; doi:10.1039/d1dt02849a

data_7708759
_publ_section_title
;
 One pot tandem dual C&#xE001;C and C&#xE001;O bond reductions in the
 \b-alkylation of secondary alcohols with primary alcohols by ruthenium
 complexes of amido and picolyl functionalized N-heterocyclic carbenes.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15640
_journal_page_last               15654
_journal_paper_doi               10.1039/d1dt02849a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C27 H31 Cl N3 Ru, Cl, 2(H2 O)'
_chemical_formula_sum            'C27 H35 Cl2 N3 O2 Ru'
_chemical_formula_weight         605.55
_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     dual
_audit_creation_date             2018-02-07
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2018-12-25 deposited with the CCDC.	2021-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                93.836(2)
_cell_angle_beta                 93.825(2)
_cell_angle_gamma                97.623(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2367(3)
_cell_length_b                   9.1208(3)
_cell_length_c                   17.8719(5)
_cell_measurement_reflns_used    7464
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.9600
_cell_measurement_theta_min      2.2430
_cell_volume                     1323.90(8)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0781
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11503
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.259
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81035
_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            Yellow
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       Block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.257
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.1674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3922
_reflns_number_total             4654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02849a2.cif
_cod_data_source_block           pg-app-10-16-1_mo
_cod_database_code               7708759
_shelx_shelxl_version_number     2018/1
_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, All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
2.b Ternary CH refined with riding coordinates:
 C25(H25)
2.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.d Aromatic/amide H refined with riding coordinates:
 C17(H17), C16(H16), C15(H15), C14(H14), C2(H2), C24(H24), C7(H7), C21(H21),
 C8(H8), C23(H23), C6(H6), C20(H20), C3(H3)
2.e Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C27(H27A,H27B,
 H27C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              40920
_shelx_hkl_checksum              98390
_olex2_submission_special_instructions 'No special instructions were received'