Iron(II) Bis(acetylide) Complexes as Key Intermediates in the Catalytic Hydrofunctionalization of Terminal Alkynes
Gorgas, Nikolaus; Stöger, Berthold; Veiros, Luis F.; Kirchner, Karl; ACS Catalysis 8 (2018) 7973–; doi:10.1021/acscatal.8b01942

data_4515723
_publ_section_title
;
 Iron(II) Bis(acetylide) Complexes as Key Intermediates in the Catalytic
 Hydrofunctionalization of Terminal Alkynes
;
_journal_issue                   9
_journal_name_full               'ACS Catalysis'
_journal_page_first              7973
_journal_paper_doi               10.1021/acscatal.8b01942
_journal_volume                  8
_journal_year                    2018
_chemical_formula_sum            'C40 H50 Fe N6 P2'
_chemical_formula_weight         732.65
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.665(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6843(14)
_cell_length_b                   11.1179(9)
_cell_length_c                   18.9515(14)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.26
_cell_volume                     3683.5(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            84287
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.102
_diffrn_reflns_theta_min         2.171
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.675
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         10766
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_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+2.1990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9066
_reflns_number_total             10766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b01942_si_002.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4515723
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.740
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              23095
_shelx_hkl_checksum              730