Ruthenium(II) Arene Complexes with Asymmetrical Guanidinate Ligands: Synthesis, Characterization, and Application in the Base-Free Catalytic Isomerization of Allylic Alcohols
Garc\?ía-Álvarez, Rocío; Suárez, Francisco J.; D\?íez, Josefina; Crochet, Pascale; Cadierno, Victorio; Antiñolo, Antonio; Fernández-Galán, Rafael; Carrillo-Hermosilla, Fernando; Organometallics 31 (2012) 8301–; doi:10.1021/om3009124

data_4079653
_publ_section_title
;
 Ruthenium(II) Arene Complexes with Asymmetrical Guanidinate Ligands:
 Synthesis, Characterization, and Application in the Base-Free Catalytic
 Isomerization of Allylic Alcohols
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8301
_journal_paper_doi               10.1021/om3009124
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C27 H42 Cl N3 Ru'
_chemical_formula_sum            'C27 H42 Cl N3 Ru'
_chemical_formula_weight         545.16
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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                 107.197(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.9253(9)
_cell_length_b                   13.8742(4)
_cell_length_c                   11.7132(3)
_cell_measurement_reflns_used    9003
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      74.6915
_cell_measurement_theta_min      3.4472
_cell_volume                     5422.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics    'PLATON (Spek, 2007)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device
; 
165 mm Onyx CCD detector in \k-geometry diffractometer
;
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15372
_diffrn_reflns_theta_full        74.86
_diffrn_reflns_theta_max         74.86
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    5.712
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.182
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         5371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0650P)^2^+9.6047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                4703
_reflns_number_total             5371
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om3009124_si_001.cif
_cod_data_source_block           2b
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4079653