Synthesis of a stable 1,2-bis(ferrocenyl)diphosphene
Takahiro Sasamori; Michiyasu Sakagami; Masatoshi Niwa; Heisuke Sakai; Yukio Furukawa; Norihiro Tokitoh; Chem.Commun. 48 (2012) 8562–; doi:10.1039/c2cc33277a

data_7108178
_publ_section_title
;
 Synthesis of a stable 1,2-bis(ferrocenyl)diphosphene
;
_journal_name_full               Chem.Commun.
_journal_page_first              8562
_journal_paper_doi               10.1039/c2cc33277a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C52 H50 Fe2 P2, 0.25(C6 H14)'
_chemical_formula_sum            'C53.5 H53.5 Fe2 P2'
_chemical_formula_weight         870.10
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.8602(6)
_cell_angle_beta                 90.2326(5)
_cell_angle_gamma                103.7802(6)
_cell_formula_units_Z            4
_cell_length_a                   14.09510(10)
_cell_length_b                   17.4920(2)
_cell_length_c                   19.8743(2)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      1.70
_cell_volume                     4513.86(8)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
;
Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38846
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.9289
_exptl_absorpt_correction_T_min  0.8647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998) Private communication
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1826
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.653
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1053
_refine_ls_number_reflns         16401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0541P)^2^+3.3754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                14882
_reflns_number_total             16401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33277a.txt
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C53.50 H53.50 Fe2 P2'
_cod_database_code               7108178