Efficient <i>Z</i>-Selective Semihydrogenation of Internal Alkynes Catalyzed by Cationic Iron(II) Hydride Complexes.
Gorgas, Nikolaus; Brünig, Julian; Stöger, Berthold; Vanicek, Stefan; Tilset, Mats; Veiros, Luis F.; Kirchner, Karl; Journal of the American Chemical Society 141 (2019) 17452–17458; doi:10.1021/jacs.9b09907

data_4127855
_publ_section_title
;
 Efficient <i>Z</i>-Selective Semihydrogenation of Internal Alkynes
 Catalyzed by Cationic Iron(II) Hydride Complexes.
;
_journal_issue                   43
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17452
_journal_page_last               17458
_journal_paper_doi               10.1021/jacs.9b09907
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C38 H84 Al2 Fe2 N6 P4'
_chemical_formula_weight         914.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.062(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2241(7)
_cell_length_b                   9.8503(6)
_cell_length_c                   22.2709(15)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.57
_cell_measurement_theta_min      2.27
_cell_volume                     2398.6(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II CCD'
_diffrn_measurement_method       '\w- and \f-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            41390
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.665
_diffrn_reflns_theta_min         2.793
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.495
_exptl_absorpt_correction_T_min  0.432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       rod
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         8768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+0.7526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7279
_reflns_number_total             8768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09907_si_003.cif
_cod_data_source_block           FePNPAl
_cod_database_code               4127855
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.788
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_checksum              7778
_shelx_hkl_checksum              53806