Carboxylate-Functionalized Mesoionic Carbene Precursors: Decarboxylation, Ruthenium Bonding, and Catalytic Activity in Hydrogen Transfer Reactions
Sabater, Sara; Müller-Bunz, Helge; Albrecht, Martin; Organometallics 35 (2016) 2256–; doi:10.1021/acs.organomet.6b00322

data_4088697
_publ_section_title
;
 Carboxylate-Functionalized Mesoionic Carbene Precursors: Decarboxylation,
 Ruthenium Bonding, and Catalytic Activity in Hydrogen Transfer Reactions
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2256
_journal_paper_doi               10.1021/acs.organomet.6b00322
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C21 H26 Cl N4 O2 Ru, C F3 O3 S'
_chemical_formula_sum            'C22 H26 Cl F3 N4 O5 Ru S'
_chemical_formula_weight         652.05
_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_Hall  '-P 2yn'
_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                 93.6884(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8088(1)
_cell_length_b                   14.5983(2)
_cell_length_c                   15.4772(2)
_cell_measurement_reflns_used    33105
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2630
_cell_measurement_theta_min      3.5220
_cell_volume                     2662.56(6)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3196
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0085
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            64804
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.3031
_exptl_crystal_size_mid          0.2414
_exptl_crystal_size_min          0.1652
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         6600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+1.4977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                5874
_reflns_number_total             6600
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om6b00322_si_002.cif
_cod_data_source_block           alb305_9
_cod_original_cell_volume        2662.56(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088697