Synthesis, structures and properties of biferrocenyl- and ruthenocenyl-substituted diphosphenes
Sasamori, Takahiro; Hori, Akimi; Kaneko, Yoshikazu; Tokitoh, Norihiro; New Journal of Chemistry 34 (2010) 1560–; doi:10.1039/c0nj00062k

data_7053464
_publ_section_title
;
 Synthesis, structures and properties of biferrocenyl- and
 ruthenocenyl-substituted diphosphenes
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1560
_journal_paper_doi               10.1039/c0nj00062k
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         'C47 H76 Fe2 P2 Si6'
_chemical_formula_sum            'C47 H76 Fe2 P2 Si6'
_chemical_formula_weight         983.26
_chemical_name_common            biferrocenyldiphosphene
_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                107.7383(10)
_cell_angle_beta                 97.2601(10)
_cell_angle_gamma                93.3283(16)
_cell_formula_units_Z            2
_cell_length_a                   12.3334(3)
_cell_length_b                   12.9518(4)
_cell_length_c                   17.4667(5)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      1.66
_cell_volume                     2622.37(13)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  Rigaku_Mercury_CCD
_diffrn_measurement_method       'Omega scans'
_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  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0785
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23442
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  0.8918
_exptl_absorpt_correction_T_min  0.7715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                6707
_reflns_number_total             9703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00062k.txt
_cod_data_source_block           bfcpp
_cod_database_code               7053464