Ruthenium Azocarboxamide Half-Sandwich Complexes: Influence of the Coordination Mode on the Electronic Structure and Activity in Base-Free Transfer Hydrogenation Catalysis
Sommer, Michael G.; Marinova, Sofiya; Krafft, Michael J.; Urankar, Damijana; Schweinfurth, David; Bubrin, Martina; Košmrlj, Janez; Sarkar, Biprajit; Organometallics 35 (2016) 2840–; doi:10.1021/acs.organomet.6b00424

data_4088776
_publ_section_title
;
 Ruthenium Azocarboxamide Half-Sandwich Complexes: Influence of the
 Coordination Mode on the Electronic Structure and Activity in Base-Free
 Transfer Hydrogenation Catalysis
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2840
_journal_paper_doi               10.1021/acs.organomet.6b00424
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C21 H22 Cl2 N5 O Ru, F6 P'
_chemical_formula_sum            'C21 H22 Cl2 F6 N5 O P Ru'
_chemical_formula_weight         677.38
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.977(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4895(15)
_cell_length_b                   21.739(4)
_cell_length_c                   12.834(2)
_cell_measurement_reflns_used    4156
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.26
_cell_measurement_theta_min      4.07
_cell_volume                     2532.2(8)
_computing_cell_refinement       'Bruker APEX II Software Suite, 2008'
_computing_data_collection       'Bruker APEX II Software Suite, 2008'
_computing_data_reduction        'Bruker APEX II Software Suite, 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Bruker Kappa APEX II Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1961
_diffrn_reflns_av_sigmaI/netI    0.2287
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12439
_diffrn_reflns_theta_full        66.26
_diffrn_reflns_theta_max         66.26
_diffrn_reflns_theta_min         4.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.201
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.697
_refine_diff_density_min         -1.534
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4156
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.2325
_refine_ls_R_factor_gt           0.1522
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+94.5586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3007
_refine_ls_wR_factor_ref         0.3344
_reflns_number_gt                2315
_reflns_number_total             4156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00424_si_002.cif
_cod_data_source_block           ac92
_cod_original_cell_volume        2532.3(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088776