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_7053465
_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         'C37 H68 P2 Ru Si6'
_chemical_formula_sum            'C37 H68 P2 Ru Si6'
_chemical_formula_weight         844.46
_chemical_name_common            ruthenocenyldiphosphene
_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                97.9195(7)
_cell_angle_beta                 96.8663(6)
_cell_angle_gamma                110.1667(8)
_cell_formula_units_Z            2
_cell_length_a                   9.61510(10)
_cell_length_b                   10.6365(2)
_cell_length_c                   24.8520(4)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.09
_cell_volume                     2324.61(6)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            20542
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_T_max  0.9884
_exptl_absorpt_correction_T_min  0.9439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            deep-red
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0300P)^2^+2.8152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                7880
_reflns_number_total             8550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00062k.txt
_cod_data_source_block           rcpp
_cod_database_code               7053465