Ruthenium Catalyzed Hydroboration of Terminal Alkynes toZ-Vinylboronates
Chidambaram Gunanathan; Markus Hölscher; Fangfang Pan; Walter Leitner; Journal of the American Chemical Society 134 (2012) 14349–14352; doi:10.1021/ja307233p

data_4118584
_publ_section_title
;
 Ruthenium Catalyzed Hydroboration of Terminal Alkynes toZ-Vinylboronates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14349
_journal_page_last               14352
_journal_paper_doi               10.1021/ja307233p
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C29 H58 B N O2 P2 Ru'
_chemical_formula_sum            'C29 H58 B N O2 P2 Ru'
_chemical_formula_weight         626.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 104.573(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.865(3)
_cell_length_b                   16.434(3)
_cell_length_c                   17.172(4)
_cell_measurement_reflns_used    4714
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.3342
_cell_measurement_theta_min      2.1636
_cell_volume                     3240.6(13)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_source         'Incoatec microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42134
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.8729
_exptl_absorpt_correction_T_min  0.8020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.147(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         14881
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0278P)^2^+0.8926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                14136
_reflns_number_total             14881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307233p_si_001.cif
_cod_data_source_block           test
_cod_original_cell_volume        3240.7(12)
_cod_original_sg_symbol_Hall     P2yb
_cod_database_code               4118584