Facile Hydrometalation of Alkynes by nido-1,2-(Cp*RuH)2B3H7 Yielding Novel Ru-B Edge-Bridging Alkylidenes. Stepwise Conversion of HC\τbCC(O)OMe into nido-1,2-(Cp*RuH)2-3-HOB-4-MeC-5-MeOC-BH3, Cp* = η5-C5Me5
Hong Yan; Alicia M. Beatty; Thomas P. Fehlner; Journal of the American Chemical Society 124 (2002) 10280–10281; doi:10.1021/ja026738t

data_4115113
_publ_section_title
;
 Facile Hydrometalation of Alkynes by nido-1,2-(Cp*RuH)2B3H7 Yielding
 Novel Ru-B Edge-Bridging Alkylidenes. Stepwise Conversion of
 HC\\tbCC(O)OMe into nido-1,2-(Cp*RuH)2-3-HOB-4-MeC-5-MeOC-BH3, Cp* =
 \h5-C5Me5
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10280
_journal_page_last               10281
_journal_paper_doi               10.1021/ja026738t
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C24 H43 B3 O2 Ru2'
_chemical_formula_weight         598.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   'geom, except difmap for B-H and Ru-H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.0530(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4297(7)
_cell_length_b                   14.8019(9)
_cell_length_c                   15.4447(9)
_cell_measurement_reflns_used    8923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.66
_cell_volume                     2609.2(3)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31460
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8046
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.342
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.104
_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     287
_refine_ls_number_reflns         7964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0372P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                6440
_reflns_number_total             7964
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja026738t_s1_3.cif
_cod_data_source_block           tf902m
_cod_database_code               4115113