Phosphinidene Complexes of Scandium: Powerful PAr Group-Transfer Vehicles to Organic and Inorganic Substrates
Benjamin F. Wicker; Jennifer Scott; José G. Andino; Xinfeng Gao; Hyunsoo Park; Maren Pink; Daniel J. Mindiola; Journal of the American Chemical Society 132 (2010) 3691–3693; doi:10.1021/ja100214e

data_4102092
_publ_section_title
;
 Phosphinidene Complexes of Scandium: Powerful PAr Group-Transfer Vehicles
 to Organic and Inorganic Substrates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3691
_journal_page_last               3693
_journal_paper_doi               10.1021/ja100214e
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
'(C26 H40 N P2) (C24 H25 P) (C4 H10 O2) Br Li Sc, 0.5(C4 H10 O) '
_chemical_formula_sum            'C56 H80 Br Li N O2.5 P3 Sc'
_chemical_formula_weight         1031.93
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_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                   11.8898(12)
_cell_length_b                   21.318(3)
_cell_length_c                   22.944(3)
_cell_measurement_reflns_used    2433
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      1.30
_cell_volume                     5815.5(13)
_computing_cell_refinement       'APEX 2'
_computing_data_collection       'APEX 2 (Bruker-AXS, 2009)'
_computing_data_reduction        'APEX 2'
_computing_molecular_graphics    'APEX 2'
_computing_publication_material  'APEX 2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 53.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  kappa
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35804
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.30
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker APEX II'
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  0.9548
_exptl_absorpt_correction_T_min  0.8961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         8362
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0830P)^2^+4.9419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1510
_reflns_number_gt                6709
_reflns_number_total             8362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja100214e_si_003.cif
_cod_data_source_block           new
_cod_original_cell_volume        5815.7(11)
_cod_original_formula_sum        'C56 H80 Br Li N O2.50 P3 Sc'
_cod_database_code               4102092