Formation of a cationic alkylidene complex via formal hydride abstraction: synthesis and structural characterization of [W(PMe3)4(n\2-CHPMe2)H]X (X = Br, I)
Aaron Sattler; Gerard Parkin; Chem.Commun. 47 (2011) 12828–; doi:10.1039/c1cc15457e

data_7107102
_publ_section_title
;
 Formation of a cationic alkylidene complex via formal hydride
 abstraction: synthesis and structural characterization of
 [W(PMe3)4(n\2-CHPMe2)H]X (X = Br, I)
;
_journal_name_full               Chem.Commun.
_journal_page_first              12828
_journal_paper_doi               10.1039/c1cc15457e
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C15 H44 Br P5 W'
_chemical_formula_weight         643.11
_chemical_name_systematic
;
?
;
_space_group_IT_number           84
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4c'
_symmetry_space_group_name_H-M   'P 42/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.476(3)
_cell_length_b                   13.476(3)
_cell_length_c                   14.118(4)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      32.41
_cell_measurement_theta_min      2.58
_cell_volume                     2563.9(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44100
_diffrn_reflns_theta_full        31.76
_diffrn_reflns_theta_max         31.76
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    6.373
_exptl_absorpt_correction_T_max  0.8318
_exptl_absorpt_correction_T_min  0.3219
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            PURPLE
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.748
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         4516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0188
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+0.8663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0410
_refine_ls_wR_factor_ref         0.0433
_reflns_number_gt                3915
_reflns_number_total             4516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc15457e.txt
_cod_data_source_block           wp5brs10
_cod_original_cell_volume        2563.8(11)
_cod_original_sg_symbol_H-M      P4(2)/m
_cod_database_code               7107102