Reactivity of Diphenylbutadiyne with a Hexaruthenium Dihydride. Unusual 1,1- andtrans-1,2-Additions of Two Hydrogen Atoms to an Internal CC Triple Bond
Cabeza, Javier A.; del Río, Ignacio; Fernández-Colinas, José M.; García-Álvarez, Pablo; Miguel, Daniel; Organometallics 25 (2006) 1492–1499; doi:10.1021/om050941q

data_4074848
_publ_section_title
;
 Reactivity of Diphenylbutadiyne with a Hexaruthenium Dihydride. Unusual
 1,1- andtrans-1,2-Additions of Two Hydrogen Atoms to an Internal CC
 Triple Bond
;
_journal_coden_ASTM              ORGND7
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1492
_journal_page_last               1499
_journal_paper_doi               10.1021/om050941q
_journal_volume                  25
_journal_year                    2006
_chemical_compound_source
;
Synthesis. Crystallization from a CH~2~Cl~2~ /
  hexanes solution
at room temperature by slow liquid-liquid difussion.
;
_chemical_formula_moiety         'C37 H18 N2 O15 Ru6, C H2 Cl2'
_chemical_formula_sum            'C38 H20 Cl2 N2 O15 Ru6'
_chemical_formula_weight         1421.88
_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                 117.6780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.57970(10)
_cell_length_b                   31.0551(4)
_cell_length_c                   12.7125(2)
_cell_measurement_temperature    293(2)
_cell_volume                     4398.03(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39853
_diffrn_reflns_theta_full        68.44
_diffrn_reflns_theta_max         68.44
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    17.991
_exptl_absorpt_correction_T_max  0.105
_exptl_absorpt_correction_T_min  0.070
_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    2.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.860
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         8077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0410P)^2^+5.6307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0801
_reflns_number_gt                7470
_reflns_number_total             8077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050941qsi20051102_064754.cif
_cod_data_source_block           4_(pg41f1)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4074848