A Thermally Stable and Sterically Unprotected Terminal Electrophilic Phosphinidene Complex of Cobalt and Its Conversion to an η1-Phosphirene
Javier Sánchez-Nieves; Brian T. Sterenberg; Konstantin A. Udachin; Arthur J. Carty; Journal of the American Chemical Society 125 (2003) 2404–2405; doi:10.1021/ja028303b

data_4113509
_publ_contact_author_address
;
Steacie Institute for Molecular Sciences, National Research Council Canada, 
100 Sussex Drive, Ottawa, Ontario, Canada K1A 0R6
;
_publ_contact_author_email       Arthur.Carty@nrc.ca
_publ_contact_author_name        'Arthur J. Carty'
_publ_section_title
;
 A Thermally Stable and Sterically Unprotected Terminal Electrophilic
 Phosphinidene Complex of Cobalt and Its Conversion to an \h1-Phosphirene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2404
_journal_page_last               2405
_journal_paper_doi               10.1021/ja028303b
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C41.5 H40 Al Cl5 Co N O3 P2'
_chemical_formula_weight         925.84
_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                88.1930(10)
_cell_angle_beta                 75.2920(10)
_cell_angle_gamma                73.8360(10)
_cell_formula_units_Z            2
_cell_length_a                   12.3668(5)
_cell_length_b                   13.0461(6)
_cell_length_c                   15.9147(7)
_cell_measurement_temperature    173(2)
_cell_volume                     2383.22(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28558
_diffrn_reflns_theta_full        28.74
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.761
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_F_000             950
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         12275
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.239
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1092P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1650
_refine_ls_wR_factor_ref         0.1794
_reflns_number_gt                8004
_reflns_number_total             12275
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028303b-2_s2_3.cif
_cod_data_source_block           jav36
_cod_original_formula_sum        'C41.50 H40 Al Cl5 Co N O3 P2'
_cod_database_code               4113509