Structure and Properties of the Macrocyclic Tridentate Ferrocenylphosphine Ligand (−PhPC5H4FeC5H4−)3
Mizuta, Tsutomu; Aotani, Tomoyuki; Imamura, Yuki; Kubo, Kazuyuki; Miyoshi, Katsuhiko; Organometallics 27 (2008) 2457–; doi:10.1021/om800057w

data_4071244
_publ_section_title
;
 Structure and Properties of the Macrocyclic Tridentate
 Ferrocenylphosphine Ligand (&#x2212;PhPC5H4FeC5H4&#x2212;)3
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2457
_journal_paper_doi               10.1021/om800057w
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C56 H55 Fe3 O2 P3 S3'
_chemical_formula_weight         1116.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            42
_cell_length_a                   49.6210(2)
_cell_length_b                   49.621
_cell_length_c                   25.42500(10)
_cell_measurement_temperature    200(2)
_cell_volume                     54215.4(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Mac Science DIP2030 Imaging Plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       65
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            28659
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.088
_exptl_absorpt_correction_T_max  0.7745
_exptl_absorpt_correction_T_min  0.6746
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             24276
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.000025(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   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1374
_refine_ls_number_reflns         28659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.124
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+166.1471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1136
_reflns_number_gt                26606
_reflns_number_total             28659
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800057w-file009.cif
_cod_data_source_block           4a
_cod_database_code               4071244