A Redox-Neutral Fe-Catalyzed Cycloisomerization of Enyne Acetates
Teske, Johannes; Plietker, Bernd; ACS Catalysis 6 (2016) 7148–; doi:10.1021/acscatal.6b02260

data_4516707
_publ_section_title
;
 A Redox-Neutral Fe-Catalyzed Cycloisomerization of Enyne Acetates
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              7148
_journal_paper_doi               10.1021/acscatal.6b02260
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C39 H33 Fe N2 O2 P2, B F4, C H Cl3'
_chemical_formula_sum            'C40 H34 B Cl3 F4 Fe N2 O2 P2'
_chemical_formula_weight         885.64
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.636(3)
_cell_angle_beta                 69.027(3)
_cell_angle_gamma                83.561(3)
_cell_formula_units_Z            2
_cell_length_a                   12.2695(7)
_cell_length_b                   12.9467(7)
_cell_length_c                   14.1404(8)
_cell_measurement_reflns_used    8472
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      1.56
_cell_volume                     2054.1(2)
_computing_cell_refinement       'Bruker APEX Software Suite, 2008'
_computing_data_collection       'Bruker APEX Software Suite, 2008'
_computing_data_reduction        'Bruker APEX Software Suite, 2008'
_computing_molecular_graphics    'SHELXTL-plus, XP (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50690
_diffrn_reflns_theta_full        30.56
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.8894
_exptl_absorpt_correction_T_min  0.8459
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS, 2008'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         12473
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0423P)^2^+0.5410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                8472
_reflns_number_total             12473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs6b02260_si_003.cif
_cod_data_source_block           s2129lm
_cod_database_code               4516707