Different Reactivity Patterns of Trimethylsilyl- and Phenyl-Substituted Propargylallenes: Fe2(CO)9- and [Ag]±Promoted Cyclizations
Oulié, Pascal; Altes, Lena; Milosevic, Sandra; Bouteille, Romain; Müller-Bunz, Helge; McGlinchey, Michael J.; Organometallics 29 (2010) 676–; doi:10.1021/om9009872

data_4067504
_publ_section_title
;
 Different Reactivity Patterns of Trimethylsilyl- and Phenyl-Substituted
 Propargylallenes: Fe2(CO)9- and [Ag]+-Promoted Cyclizations
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              676
_journal_paper_doi               10.1021/om9009872
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C45 H27 O3 Fe, 0.5(C H2 Cl2), 0.15(H2 O)'
_chemical_formula_sum            'C45.5 H27.3 Cl Fe O3.15'
_chemical_formula_weight         715.66
_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                 99.035(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.669(2)
_cell_length_b                   13.8982(13)
_cell_length_c                   19.1186(17)
_cell_measurement_reflns_used    5504
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.64
_cell_measurement_theta_min      2.17
_cell_volume                     6736.0(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40546
_diffrn_reflns_theta_full        22.08
_diffrn_reflns_theta_max         22.08
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  0.8943
_exptl_absorpt_correction_T_min  0.6258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS v.2.10 (Bruker,2003) was used for absorption correction. 
 R(int) for selected reflections was 0.070 before and 0.019 after 
 correction. The Ratio of minimum to maximum transmission is 0.699798. 
 The \l/2 correction factor is 0.0000 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2948.0
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         8285
_refine_ls_number_restraints     377
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0398P)^2^+5.3392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0902
_reflns_number_gt                7024
_reflns_number_total             8285
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om9009872_si_001.cif
_cod_data_source_block           mjm226(15)
_cod_depositor_comments
;

2025-11-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         1431.33
_cod_original_formula_moiety         '2 (C45 H27 O3 Fe), C H2 Cl2, 0.3 (H2 O)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        6736.1(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C91 H54.6 O6.3 Cl2 Fe2'
_cod_database_code               4067504