Aerobic dehydrogenation of amines to nitriles catalyzed by triazolylidene ruthenium complexes with O<sub>2</sub> as terminal oxidant.
Olivares, Marta; Knörr, Pascal; Albrecht, Martin; Dalton transactions (Cambridge, England : 2003) 49 (2020) 1981–1991; doi:10.1039/c9dt04873a

data_7703329
_publ_section_title
;
 Aerobic dehydrogenation of amines to nitriles catalyzed by triazolylidene
 ruthenium complexes with O<sub>2</sub> as terminal oxidant.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1981
_journal_page_last               1991
_journal_paper_doi               10.1039/c9dt04873a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C22 H28 Cl N4 O3 Ru, C F3 O3 S, 0.301(H2 O)'
_chemical_formula_sum            'C23 H28.6 Cl F3 N4 O6.3 Ru S'
_chemical_formula_weight         687.48
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-11-30T15:42:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-10-10 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                75.559(3)
_cell_angle_beta                 78.781(2)
_cell_angle_gamma                62.824(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7705(2)
_cell_length_b                   10.1541(3)
_cell_length_c                   16.0919(5)
_cell_measurement_reflns_used    13123
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.026
_cell_measurement_theta_min      2.278
_cell_volume                     1369.33(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0080388
_diffrn_orient_matrix_UB_12      -0.0162883
_diffrn_orient_matrix_UB_13      0.045702
_diffrn_orient_matrix_UB_21      -0.0331942
_diffrn_orient_matrix_UB_22      0.0780629
_diffrn_orient_matrix_UB_23      0.0009694
_diffrn_orient_matrix_UB_31      -0.0745102
_diffrn_orient_matrix_UB_32      0.0047444
_diffrn_orient_matrix_UB_33      -0.000654
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21468
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.196
_diffrn_reflns_theta_min         2.294
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       prism
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+1.3053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0
_reflns_number_gt                5734
_reflns_number_total             6208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04873a2.cif
_cod_data_source_block           complex4b_16ma145_mo-269
_cod_depositor_comments
'Adding full bibliography for 7703329--7703332.cif.'
_cod_original_formula_sum        'C23 H28.60 Cl F3 N4 O6.30 Ru S'
_cod_database_code               7703329
_shelx_res_checksum              41462