Reactions of Ring-Slipped Iron Complexes Derived from P(S)Ph-Bridged [1]Ferrocenophane: Synthesis of Bis(half-sandwich) Heterodinuclear Complexes
Imamura, Yuki; Kubo, Kazuyuki; Mizuta, Tsutomu; Miyoshi, Katsuhiko; Organometallics 25 (2006) 2301–; doi:10.1021/om060020v

data_4075067
_publ_section_title
;
 Reactions of Ring-Slipped Iron Complexes Derived from P(S)Ph-Bridged
 [1]Ferrocenophane:&#x00A0; Synthesis of Bis(half-sandwich)
 Heterodinuclear Complexes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2301
_journal_paper_doi               10.1021/om060020v
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C25 H31 Fe O9 P3 S W'
_chemical_formula_weight         840.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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                   9.74300(10)
_cell_length_b                   13.24900(10)
_cell_length_c                   23.1550(2)
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.5
_cell_volume                     2988.96(5)
_computing_cell_refinement       HKL
_computing_data_collection       HKL
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Mac Science DIP2030 Imaging Plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            7065
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    4.610
_exptl_absorpt_correction_T_max  0.8022
_exptl_absorpt_correction_T_min  0.1592
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.854
_refine_diff_density_min         -1.599
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.370(8)
_refine_ls_extinction_coef       0.0033(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0730P)^2^+13.6135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                6778
_reflns_number_total             6824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060020vsi20060107_125139.cif
_cod_data_source_block           5W
_cod_database_code               4075067