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_4113508
_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            'C27 H29 Al Cl4 Co N O3 P2'
_chemical_formula_weight         705.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   12.5260(6)
_cell_length_b                   12.8291(6)
_cell_length_c                   20.4241(10)
_cell_measurement_temperature    173(2)
_cell_volume                     3282.1(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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0402
_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       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31227
_diffrn_reflns_theta_full        28.78
_diffrn_reflns_theta_max         28.78
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.001
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_F_000             1440
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.005(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         8516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0466P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                6443
_reflns_number_total             8516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028303b-2_s2_2.cif
_cod_data_source_block           jav31
_cod_database_code               4113508