Recombination of an Fe-Si-P Linkage to an Fe-P-Si Linkage through an Isolable Intermediate Phosphasilaferracyclopropane
Masaaki Okazaki; Takahiko Yoshitomi; Junpei Naito; Akira Sato; Takashi Komuro; Hiromi Tobita; Journal of the American Chemical Society 130 (2008) 17674–17675; doi:10.1021/ja808443v

data_4108963
_publ_contact_author_address
'Department of Chemistry, Graduate School of Science, Tohoku University'
_publ_contact_author_email       tobita@m.tains.tohoku.ac.jp
_publ_contact_author_fax         81-22-795-6543
_publ_contact_author_name        'Hiromi Tobita'
_publ_contact_author_phone       81-22-795-6539
_publ_section_title
;
 Recombination of an Fe-Si-P Linkage to an Fe-P-Si Linkage through an
 Isolable Intermediate Phosphasilaferracyclopropane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17674
_journal_page_last               17675
_journal_paper_doi               10.1021/ja808443v
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration unk
_chemical_formula_sum            'C26 H31 Fe O2 P Si'
_chemical_formula_weight         490.42
_chemical_properties_physical    air-sensitive
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.5404(6)
_cell_length_b                   15.7053(8)
_cell_length_c                   22.1506(14)
_cell_measurement_reflns_used    42209
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.95
_cell_measurement_theta_min      3.20
_cell_volume                     5058.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35754
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.12
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.9646
_exptl_absorpt_correction_T_min  0.8115
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   Higashi
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         5726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+12.4867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1672
_reflns_number_gt                4624
_reflns_number_total             5726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808443v_si_002_1.cif
_cod_data_source_block           complex3
_cod_database_code               4108963