Hexaruthenium Carbonyl Cluster Complexes with Basal Edge-Bridged Square Pyramidal Metallic Skeleton: Efficient Synthesis of 2-Imidopyridine Derivatives and Determination of Their Reactive Sites in Carbonyl Substitution Reactions
Javier A. Cabeza; Ignacio del Río; Pablo García-Álvarez; Daniel Miguel; Víctor Riera; Inorganic Chemistry 43 (2004) 5450–5458; doi:10.1021/ic0492789

data_4311816
_publ_contact_author_address
;
      Departamento de Qu\'imica Org\'anica e Inorg\'anica 
      Facultad de Qu\'imica 
      Universidad de Oviedo 
      33071 Oviedo 
      Spain 
;
_publ_contact_author_email       jac@fq.uniovi.es
_publ_contact_author_fax         '+34 985 103446'
_publ_contact_author_name        'Javier A. Cabeza'
_publ_contact_author_phone       '+34 985 103501'
_publ_section_title
;
 Hexaruthenium Carbonyl Cluster Complexes with Basal Edge-Bridged Square
 Pyramidal Metallic Skeleton: Efficient Synthesis of 2-Imidopyridine
 Derivatives and Determination of Their Reactive Sites in Carbonyl
 Substitution Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5450
_journal_page_last               5458
_journal_paper_doi               10.1021/ic0492789
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source
;
Synthesis. Crystallization from a CH~2~Cl~2~ /
 hexanes solution 
at room temperature by slow liquid-liquid difussion.
;
_chemical_formula_moiety
'C73 H53 N2 O13 P3 Ru6, 3(C0.33 H0.66 Cl0.66)'
_chemical_formula_sum            'C74 H55 Cl2 N2 O13 P3 Ru6'
_chemical_formula_weight         1950.43
_chemical_name_systematic
;
 ?
;
_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                90.276(3)
_cell_angle_beta                 95.087(3)
_cell_angle_gamma                104.990(3)
_cell_formula_units_Z            2
_cell_length_a                   13.9447(6)
_cell_length_b                   15.1141(6)
_cell_length_c                   18.9417(8)
_cell_measurement_temperature    150(2)
_cell_volume                     3839.5(3)
_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      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     1.54180
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62023
_diffrn_reflns_theta_full        68.41
_diffrn_reflns_theta_max         68.41
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    11.049
_exptl_absorpt_correction_T_max  0.435
_exptl_absorpt_correction_T_min  0.160
_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            black
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.075
_refine_diff_density_max         2.643
_refine_diff_density_min         -1.727
_refine_diff_density_rms         0.315
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         14041
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0764
_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
 [1.00000+-1.00000exp(-15.40(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+7.9362*P+(0.1945P)^2^+0.0000sin\q/\l]
 where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2321
_refine_ls_wR_factor_ref         0.2642
_reflns_number_gt                11643
_reflns_number_total             14041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0492789si20040603_085619_5.cif
_cod_data_source_block           7_(pg49f2)
_cod_database_code               4311816