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_4114301
_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            'C30 H39 Mo2 O2 P'
_chemical_formula_weight         654.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.952(2)
_cell_length_b                   19.642(4)
_cell_length_c                   14.316(3)
_cell_measurement_temperature    100(2)
_cell_volume                     2798.4(10)
_computing_data_collection       'Bruker SMART CCD '
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19628
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.978
_exptl_crystal_colour            Dark_red
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       Block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0194
_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^)+(0.0270P)^2^+0.4145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                5920
_reflns_number_total             6410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja037293rsi20030926_015902.cif
_cod_data_source_block           molh
_cod_original_cell_volume        2798.3(10)
_cod_database_code               4114301