Reactivity of Terminal, Electrophilic Phosphinidene Complexes of Molybdenum and Tungsten. Nucleophilic Addition at Phosphorus and P−P Bond Forming Reactions with Phosphines and Diphosphines
Sterenberg, Brian T.; Senturk, Ozan Sanli; Udachin, Konstantin A.; Carty, Arthur J.; Organometallics 26 (2007) 925–; doi:10.1021/om060685x

data_4072485
_publ_section_title
;
 Reactivity of Terminal, Electrophilic Phosphinidene Complexes of
 Molybdenum and Tungsten. Nucleophilic Addition at Phosphorus and
 P&#x2212;P Bond Forming Reactions with Phosphines and Diphosphines
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              925
_journal_paper_doi               10.1021/om060685x
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C24 H45 Al Cl4 N O2 P3 W'
_chemical_formula_weight         825.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                96.860(2)
_cell_angle_beta                 98.118(2)
_cell_angle_gamma                94.6010(10)
_cell_formula_units_Z            2
_cell_length_a                   8.6986(9)
_cell_length_b                   12.0265(9)
_cell_length_c                   16.6578(13)
_cell_measurement_temperature    173(2)
_cell_volume                     1704.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20223
_diffrn_reflns_theta_full        28.74
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    3.891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             824
_refine_diff_density_max         3.560
_refine_diff_density_min         -1.702
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         8726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0213P)^2^+25.9661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1406
_reflns_number_gt                8018
_reflns_number_total             8726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060685xsi20060731_105009.cif
_cod_data_source_block           oz10
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4072485