Ruthenium(ii) arene complexes bearing simple dioxime ligands: effective catalysts for the one-pot transfer hydrogenation/N-methylation of nitroarenes with methanol
Colaiezzi, Roberta; Saviozzi, Chiara; di Nicola, Nicola; Zacchini, Stefano; Pampaloni, Guido; Crucianelli, Marcello; Marchetti, Fabio; Di Giuseppe, Andrea; Biancalana, Lorenzo; Catalysis Science & Technology 13 (2023) 2160–2183; doi:10.1039/D3CY00218G

data_1568562
_publ_section_title
;
 Ruthenium(ii) arene complexes bearing simple dioxime ligands: effective
 catalysts for the one-pot transfer hydrogenation/N-methylation of
 nitroarenes with methanol
;
_journal_issue                   7
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              2160
_journal_page_last               2183
_journal_paper_doi               10.1039/D3CY00218G
_journal_volume                  13
_journal_year                    2023
_chemical_formula_sum            'C16 H28 Cl N2 O3.5 Ru'
_chemical_formula_weight         440.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-02-10 deposited with the CCDC.	2023-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.356(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.4589(10)
_cell_length_b                   13.1592(8)
_cell_length_c                   17.7332(11)
_cell_measurement_reflns_used    9669
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.652
_cell_measurement_theta_min      2.4425
_cell_volume                     3569.1(4)
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'PHOTONII area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59880
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.398
_diffrn_reflns_theta_min         1.934
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.047
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5477
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1403 (selected reflections only, before parameter refinement)
 R(int) =  0.0609 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       prism
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         6515
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0122P)^2^+3.8388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0468
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5946
_reflns_number_total             6515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cy00218g2.cif
_cod_data_source_block           4H
_cod_depositor_comments
'Adding full bibliography for 1568560--1568562.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C16 H28 Cl N2 O3.50 Ru'
_cod_database_code               1568562
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.802
_shelx_estimated_absorpt_t_max   0.859
_shelx_res_checksum              8728