Ten-Electron Coordination and Reactivity of an Arylphosphinidene Ligand
M. Esther García; Víctor Riera; Miguel A. Ruiz; David Sáez; Hayrullo Hamidov; John C. Jeffery; Thomas Riis-Johannessen; Journal of the American Chemical Society 125 (2003) 13044–13045; doi:10.1021/ja037293r

data_4114302
_publ_section_title
;
 Ten-Electron Coordination and Reactivity of an Arylphosphinidene Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13044
_journal_page_last               13045
_journal_paper_doi               10.1021/ja037293r
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C62 H52 B F24 Mo2 O2 P'
_chemical_formula_weight         1518.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.6950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1853(3)
_cell_length_b                   21.1676(5)
_cell_length_c                   19.4760(4)
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.11
_cell_measurement_theta_min      2.65
_cell_volume                     6188.3(2)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'CCD Area detector'
_diffrn_measurement_method       'Frames each covering 0.3 \% in \w'
_diffrn_radiation_monochromator  'Osmic Confocal Maxflux mirrow optics'
_diffrn_radiation_source         '4.8 kW rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54185
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29239
_diffrn_reflns_theta_full        70.18
_diffrn_reflns_theta_max         70.18
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    4.608
_exptl_absorpt_correction_type   Hemisphere
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            Dark_orange
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         10733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0749
_reflns_number_gt                8388
_reflns_number_total             10733
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja037293rsi20030926_015920.cif
_cod_data_source_block           mobh
_cod_database_code               4114302