Reactivity of N-Heterocyclic Carbenes with [Ru3(CO)12] and [Os3(CO)12]. Influence of Ligand Volume and Electronic Effects
Cabeza, Javier A.; del Río, Ignacio; Miguel, Daniel; Pérez-Carreño, Enrique; Sánchez-Vega, M. Gabriela; Organometallics 27 (2008) 211–; doi:10.1021/om7009655

data_4070720
_publ_section_title
;
 Reactivity of N-Heterocyclic Carbenes with [Ru3(CO)12] and [Os3(CO)12].
 Influence of Ligand Volume and Electronic Effects
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              211
_journal_paper_doi               10.1021/om7009655
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C15 H5 N O12 Ru3'
_chemical_formula_sum            'C15 H5 N O12 Ru3'
_chemical_formula_weight         694.41
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.78(5)
_cell_angle_beta                 73.10(6)
_cell_angle_gamma                70.62(5)
_cell_formula_units_Z            2
_cell_length_a                   8.332(4)
_cell_length_b                   11.889(7)
_cell_length_c                   11.904(7)
_cell_measurement_temperature    293(2)
_cell_volume                     1064.3(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'EUCLID (Spek, 1982)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.866
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32216
_diffrn_reflns_theta_full        74.49
_diffrn_reflns_theta_max         74.49
_diffrn_reflns_theta_min         3.88
_exptl_absorpt_coefficient_mu    17.602
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.687
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
  [1.00000+-1.00000exp(-12.50(sin\q/\l)^2^)]/
    [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.1128P)^2^+0.0000sin\q/\l]
  where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1627
_reflns_number_gt                2866
_reflns_number_total             3765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7009655-file003.cif
_cod_data_source_block           2_(gt174f2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1064.3(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4070720