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_4065490
_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 H28 P2 W1'
_chemical_formula_sum            'C18 H28 P2 W'
_chemical_formula_weight         490.19
_chemical_name_systematic
;
 [{<i>\h</i>^5^-1-[2-di<i>tert</i>butyldiphosphane
--<i>\kP^1^</i>]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                 110.513(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7151(5)
_cell_length_b                   10.9810(3)
_cell_length_c                   11.4561(4)
_cell_measurement_reflns_used    5097
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.5313
_cell_measurement_theta_min      2.3085
_cell_measurement_wavelength     0.71073
_cell_volume                     1851.60(11)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
        (compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
        (compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
        (compiled Feb 27 2009,15:38:38)
;
_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      0.0020733202
_diffrn_orient_matrix_UB_12      0.0388023014
_diffrn_orient_matrix_UB_13      -0.0355416341
_diffrn_orient_matrix_UB_21      0.0062362081
_diffrn_orient_matrix_UB_22      -0.0515601448
_diffrn_orient_matrix_UB_23      -0.0252974028
_diffrn_orient_matrix_UB_31      -0.065806133
_diffrn_orient_matrix_UB_32      -0.0036802444
_diffrn_orient_matrix_UB_33      -0.0204550259
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7093
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    6.404
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_correction_T_min  0.276
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
        (compiled Feb 27 2009,15:38:38)
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            yellow
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.3251
_exptl_crystal_size_mid          0.0826
_exptl_crystal_size_min          0.0439
_refine_diff_density_max         1.51
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.94
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3438
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.94
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0521
_reflns_number_gt                2852
_reflns_number_total             3438
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om2008452_si_002.cif
_cod_data_source_block           I
_cod_original_cell_volume        1851.60(10)
_cod_database_code               4065490