Reactivity of a Bis(N-heterocyclic carbene) with Ruthenium Carbonyl. Synthesis of Mono- and Trinuclear Derivatives and Ligand Modification via C‒H Bond Activation
Cabeza, Javier A.; Damonte, Marina; Pérez-Carreño, Enrique; Organometallics 31 (2012) 8355–; doi:10.1021/om3009298

data_4079680
_publ_section_title
;
 Reactivity of a Bis(N-heterocyclic carbene) with Ruthenium Carbonyl.
 Synthesis of Mono- and Trinuclear Derivatives and Ligand Modification via
 C--H Bond Activation
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8355
_journal_paper_doi               10.1021/om3009298
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         '2(C26 H18 N4 O10 Ru3), C H2 Cl2'
_chemical_formula_sum            'C53 H38 Cl2 N8 O20 Ru6'
_chemical_formula_weight         1784.23
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_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                 108.7340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1595(2)
_cell_length_b                   16.07780(10)
_cell_length_c                   21.4623(2)
_cell_measurement_reflns_used    10458
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      71.4989
_cell_measurement_theta_min      2.7798
_cell_volume                     5934.25(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_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 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19899
_diffrn_reflns_theta_full        69.98
_diffrn_reflns_theta_max         69.98
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    13.596
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.997
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3480
_exptl_crystal_size_max          0.0729
_exptl_crystal_size_mid          0.0510
_exptl_crystal_size_min          0.0284
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         10911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0229P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0631
_reflns_number_gt                8748
_reflns_number_total             10911
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om3009298_si_002.cif
_cod_data_source_block           md360f1
_cod_original_cell_volume        5934.25(9)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4079680