Reactivity of a (Bis-NHC)tricarbonylruthenium(0) Complex with Methyl Triflate and Methyl Iodide. Formation of Methyl- and Acetylruthenium(II) Derivatives: Experimental Results and Mechanistic DFT Calculations
Cabeza, Javier A.; Damonte, Marina; García-Álvarez, Pablo; Pérez-Carre Enrique; Organometallics 32 (2013) 4382–; doi:10.1021/om400534n

data_4081169
_publ_section_title
;
 Reactivity of a (Bis-NHC)tricarbonylruthenium(0) Complex with Methyl
 Triflate and Methyl Iodide. Formation of Methyl- and Acetylruthenium(II)
 Derivatives: Experimental Results and Mechanistic DFT Calculations
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4382
_journal_paper_doi               10.1021/om400534n
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C15 H19 N4 O3 Ru, C F3 O3 S'
_chemical_formula_sum            'C32 H38 F6 N8 O12 Ru2 S2'
_chemical_formula_weight         1106.96
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 93.070(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.4685(8)
_cell_length_b                   6.5425(2)
_cell_length_c                   25.8504(8)
_cell_measurement_temperature    123(2)
_cell_volume                     4132.3(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7779
_diffrn_reflns_theta_full        72.44
_diffrn_reflns_theta_max         72.44
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    7.730
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.0803
_exptl_crystal_size_mid          0.0688
_exptl_crystal_size_min          0.0647
_refine_diff_density_max         0.591
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         3956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0561P)^2^+6.6092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                3673
_reflns_number_total             3956
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om400534n_si_002.cif
_cod_data_source_block           xn12010-md401
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4081169