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_4311817
_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_formula_sum            'C48.5 H34 N2 O14 P2 Ru6'
_chemical_formula_weight         1537.14
_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                 95.471(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.354(3)
_cell_length_b                   23.584(6)
_cell_length_c                   20.941(5)
_cell_measurement_temperature    299(2)
_cell_volume                     5582(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20435
_diffrn_reflns_theta_full        23.49
_diffrn_reflns_theta_max         23.49
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    1.701
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.805349
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            BLACK
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             2980
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.48
_refine_diff_density_max         1.587
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.239
_refine_ls_extinction_coef       0.00052(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         7755
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+124.7108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1650
_reflns_number_gt                6477
_reflns_number_total             7755
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0492789si20040603_085619_6.cif
_cod_data_source_block           8_(pg50f1am)
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5582(3)
_cod_original_formula_sum        'C48.50 H34 N2 O14 P2 Ru6'
_cod_database_code               4311817