ZnCl<sub>2</sub>-catalysed transfer hydrogenation of carbonyls and chemoselective reduction of the CC bond in α,β-unsaturated ketones.
Sheokand, Sonu; Sharma, Sunita; Mohite, Manali A.; Rajaraman, Gopalan; Balakrishna, Maravanji S.; Chemical communications (Cambridge, England) 60 (2024) 7733–7736; doi:10.1039/d4cc02700k

data_7133255
_publ_section_title
;
 ZnCl<sub>2</sub>-catalysed transfer hydrogenation of carbonyls and
 chemoselective reduction of the C&#xe001;C bond in
 &#x3b1;,&#x3b2;-unsaturated ketones.
;
_journal_issue                   60
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7733
_journal_page_last               7736
_journal_paper_doi               10.1039/d4cc02700k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '2(C25 H18 O)'
_chemical_formula_sum            'C50 H36 O2'
_chemical_formula_weight         668.79
_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             2023-11-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-02-03 deposited with the CCDC.	2024-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.508(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.155(4)
_cell_length_b                   10.5253(19)
_cell_length_c                   19.426(3)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.20
_cell_volume                     3506.4(12)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      160.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1431
_diffrn_reflns_av_unetI/netI     0.1515
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19774
_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         2.097
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4419
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1532 before and 0.0995 after correction.
The Ratio of minimum to maximum transmission is 0.5926.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1381
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0853P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.2064
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3466
_reflns_number_total             6129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02700k2.cif
_cod_data_source_block           msb_sss_om_1_0m_a
_cod_depositor_comments          'Adding full bibliography for 7133255.cif.'
_cod_original_cell_volume        3506.4(11)
_cod_database_code               7133255
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.993
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C2'(H2'), C3'(H3')
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C13(H13), C12(H12), C11(H11), C10(H10), C7(H7),
 C6(H6), C25(H25), C24(H24), C23(H23), C22(H22), C21(H21), C15(H15), C16(H16),
 C17'(H17'), C18'(H18'), C19'(H19'), C13'(H13'), C12'(H12'), C25'(H25'),
 C24'(H24'), C23'(H23'), C22'(H22'), C21'(H21'), C7'(H7'), C6'(H6'), C11'(H11'),
  C10'(H10'), C15'(H15'), C16'(H16')
;
_shelx_res_checksum              22290
_shelx_hkl_checksum              3266
_olex2_submission_special_instructions 'No special instructions were received'