Trapping of Unsaturated Small Molecules through Cyclization with Iron−Iminophosphorane Complexes
Kubo, Kazuyuki; Baba, Takayuki; Mizuta, Tsutomu; Miyoshi, Katsuhiko; Organometallics 25 (2006) 3238–; doi:10.1021/om0510728

data_4074977
_publ_section_title
;
 Trapping of Unsaturated Small Molecules through Cyclization with
 Iron&#x2212;Iminophosphorane Complexes
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3238
_journal_paper_doi               10.1021/om0510728
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C21 H30 Fe N2 O3 P 1+, F6 P 1-'
_chemical_formula_sum            'C21 H30 F6 Fe N2 O3 P2'
_chemical_formula_weight         590.26
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   8.5180(2)
_cell_length_b                   15.7840(4)
_cell_length_c                   19.4580(4)
_cell_measurement_reflns_used    3507
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      1.66
_cell_volume                     2616.09(11)
_computing_cell_refinement
'HKL Program package (Otwinowski and Minor, 1997)'
_computing_data_collection       'MAC Science DIP2030'
_computing_data_reduction
'HKL Program package (Otwinowski and Minor, 1997)'
_computing_molecular_graphics    'ORTEP-III (Burnett and Johnson, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'imaging plate area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3507
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0349P)^2^+8.6023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1411
_reflns_number_gt                3007
_reflns_number_total             3507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0510728si20051216_030331.cif
_cod_data_source_block           Complex4
_cod_database_code               4074977