Application of Tautomerism of Ferrocenyl Secondary Phosphine Oxides in Suzuki−Miyaura Cross-Coupling Reactions
Jung, Lin-Ying; Tsai, Shih-Hung; Hong, Fung-E; Organometallics 28 (2009) 6044–; doi:10.1021/om900435y

data_4069832
_publ_section_title
;
 Application of Tautomerism of Ferrocenyl Secondary Phosphine Oxides in
 Suzuki&#x2212;Miyaura Cross-Coupling Reactions
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              6044
_journal_paper_doi               10.1021/om900435y
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C56 H74 Cl2 Fe4 O4 P4 Pd2, C4 H10 O'
_chemical_formula_sum            'C60 H84 Cl2 Fe4 O5 P4 Pd2'
_chemical_formula_weight         1516.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 124.311(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.058(3)
_cell_length_b                   20.034(2)
_cell_length_c                   16.7798(18)
_cell_measurement_reflns_used    4651
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.998
_cell_measurement_theta_min      2.7065
_cell_volume                     6402.5(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18046
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    1.661
_exptl_absorpt_correction_T_max  0.6627
_exptl_absorpt_correction_T_min  0.5786
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.010
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         9217
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1555
_reflns_number_gt                7203
_reflns_number_total             9217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900435y_si_001.cif
_cod_data_source_block           hong152m
_cod_original_cell_volume        6402.6(12)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4069832