Z-Selective, Catalytic Internal Alkyne Semihydrogenation under H2/CO Mixtures by a Niobium(III) Imido Complex
Thomas L. Gianetti; Neil C. Tomson; John Arnold; Robert G. Bergman; Journal of the American Chemical Society 133 (2011) 14904–14907; doi:10.1021/ja206016s

data_4106822
_publ_section_title
;
 Z-Selective, Catalytic Internal Alkyne Semihydrogenation under H2/CO
 Mixtures by a Niobium(III) Imido Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14904
_journal_page_last               14907
_journal_paper_doi               10.1021/ja206016s
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C47 H67 N4 Nb'
_chemical_formula_sum            'C47 H67 N4 Nb'
_chemical_formula_weight         780.96
_chemical_melting_point          405(1)
_chemical_name_common            tlgxr20
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.094(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.702(3)
_cell_length_b                   17.670(4)
_cell_length_c                   20.776(5)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    154(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.35
_cell_volume                     4590.9(19)
_computing_cell_refinement       'Bruker APEX2v.2009.1'
_computing_data_collection       'Bruker APEX2v.2009.1'
_computing_data_reduction        'Bruker APEX2v.2009.1'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      154(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\f and \w 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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0233
_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       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            75656
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  0.9218
_exptl_absorpt_correction_T_min  0.9140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       cube
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         8411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0319
_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 w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+3.2169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                6936
_reflns_number_total             8411
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja206016s_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        4590.6(18)
_cod_database_code               4106822