Titanocene-Mediated Formation of Phosphorus−Phosphorus Bonds
Schaffrath, Markus; Villinger, Alexander; Michalik, Dirk; Rosenthal, Uwe; Schulz, Axel; Organometallics 27 (2008) 1393–; doi:10.1021/om701038p

data_4070813
_publ_section_title
;
 Titanocene-Mediated Formation of Phosphorus&#x2212;Phosphorus Bonds
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1393
_journal_paper_doi               10.1021/om701038p
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C18 H54 Cl2 N4 P2 Si6'
_chemical_formula_sum            'C18 H54 Cl2 N4 P2 Si6'
_chemical_formula_weight         628.03
_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                77.45(3)
_cell_angle_beta                 83.69(3)
_cell_angle_gamma                63.81(3)
_cell_formula_units_Z            1
_cell_length_a                   8.7620(18)
_cell_length_b                   9.2460(18)
_cell_length_c                   12.340(3)
_cell_measurement_reflns_used    8704
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      83.833
_cell_measurement_theta_min      4.988
_cell_volume                     875.5(4)
_computing_cell_refinement       'Bruker Apex v2.0-2'
_computing_data_collection       'Bruker Apex v2.0-2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0138
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21470
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.9071
_exptl_absorpt_correction_T_min  0.8297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             338
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0200
_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^)+(0.0305P)^2^+0.2135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0583
_reflns_number_gt                3785
_reflns_number_total             3978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om701038p-file001.cif
_cod_data_source_block           avms07
_cod_original_cell_volume        875.5(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4070813