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_4088698
_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         'C18 H22 Cl2 N4 Ru, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C19.5 H25 Cl5 N4 Ru'
_chemical_formula_weight         593.75
_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                 101.5298(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.4316(2)
_cell_length_b                   20.1958(2)
_cell_length_c                   18.1570(2)
_cell_measurement_reflns_used    19621
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.2640
_cell_measurement_theta_min      3.2860
_cell_volume                     4825.91(10)
_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      100(2)
_diffrn_detector_area_resol_mean 10.3196
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56186
_diffrn_reflns_theta_full        76.90
_diffrn_reflns_theta_max         76.90
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    10.470
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_correction_T_min  0.136
_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    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.2567
_exptl_crystal_size_mid          0.0775
_exptl_crystal_size_min          0.0413
_refine_diff_density_max         2.463
_refine_diff_density_min         -2.243
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         10104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+31.6892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1505
_reflns_number_gt                8885
_reflns_number_total             10104
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om6b00322_si_002.cif
_cod_data_source_block           alb317_6
_cod_depositor_comments
;

2026-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C39 H50 Cl10 N8 Ru2'
_cod_original_formula_weight         1187.51
_cod_original_formula_moiety         '2 (C18 H22 Cl2 N4 Ru), 3 (C H2 Cl2)'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088698