Reactions of Lithiated Diphosphanes R2P‒P(SiMe3)Li (R =tBu,iPr,iPr2N, Et2N) with [Cp2WCl2]. Syntheses and Structures of the First Terminal Phosphanylphosphido Complexes of Tungsten(IV)
Grubba, Rafał; Baranowska, Katarzyna; Gudat, Dietrich; Pikies, Jerzy; Organometallics 30 (2011) 6655–; doi:10.1021/om2008452

data_4065491
_publ_section_title
;
 Reactions of Lithiated Diphosphanes R2P--P(SiMe3)Li (R =tBu,iPr,iPr2N,
 Et2N) with [Cp2WCl2]. Syntheses and Structures of the First Terminal
 Phosphanylphosphido Complexes of Tungsten(IV)
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6655
_journal_paper_doi               10.1021/om2008452
_journal_volume                  30
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C18 H30 N2 P2 W'
_chemical_formula_sum            'C18 H30 N2 P2 W'
_chemical_formula_weight         520.22
_chemical_name_systematic
;
[{<i>\h</i>^5^-1-[2-bis(diethylamino)diphosphane--<i>\k</i>P]
cyclopentadienyl}-\
(<i>\h</i>^5^-cyclopentadienyl)-hydrido-tungsten(IV)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 97.857(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3230(7)
_cell_length_b                   8.6258(3)
_cell_length_c                   14.0541(10)
_cell_measurement_reflns_used    3942
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.5498
_cell_measurement_theta_min      2.3576
_cell_measurement_wavelength     0.71073
_cell_volume                     1960.23(18)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
        (compiled Jan  8 2009,16:24:04)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
        (compiled Jan  8 2009,16:24:04)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
        (compiled Jan  8 2009,16:24:04)

;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire2 (large Be window)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.004631409
_diffrn_orient_matrix_UB_12      0.0808024009
_diffrn_orient_matrix_UB_13      -0.0079888123
_diffrn_orient_matrix_UB_21      -0.0248559486
_diffrn_orient_matrix_UB_22      0.0087554303
_diffrn_orient_matrix_UB_23      0.0347556626
_diffrn_orient_matrix_UB_31      0.0442671942
_diffrn_orient_matrix_UB_32      0.0134102952
_diffrn_orient_matrix_UB_33      0.0255954233
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7121
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    6.057
_exptl_absorpt_correction_T_max  0.565
_exptl_absorpt_correction_T_min  0.448
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
        (compiled Jan  8 2009,16:24:04)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.2252
_exptl_crystal_size_mid          0.1746
_exptl_crystal_size_min          0.1346
_refine_diff_density_max         2.317
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3646
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                2806
_reflns_number_total             3646
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om2008452_si_002.cif
_cod_data_source_block           II
_cod_database_code               4065491