Protonation of a lanthanum phosphide-alkyl occurs at the P?La not the C?La bond: isolation of a cationic lanthanum alkyl complex
Izod, Keith; Liddle, Stephen T.; Clegg, William; Chemical Communications  (2004) 1748–1749; doi:10.1039/b404188g

data_7110293
_publ_section_title
;
 Protonation of a lanthanum phosphide-alkyl occurs at the P?La not the
 C?La bond: isolation of a cationic lanthanum alkyl complex
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1748
_journal_page_last               1749
_journal_paper_doi               10.1039/b404188g
_journal_year                    2004
_chemical_formula_moiety
'C32 H62 La N O4 +, B C24 H20 -, 0.6 C4 H8 O, 0.2 C6 H14'
_chemical_formula_sum            'C59.56 H85.57 B La N O4.57 P Si2'
_chemical_formula_weight         1125.55
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.678(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7843(15)
_cell_length_b                   20.861(2)
_cell_length_c                   17.8375(17)
_cell_measurement_reflns_used    22395
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.86
_cell_measurement_theta_min      2.26
_cell_volume                     5861.4(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_sigmaI/netI    0.0982
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25268
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2366
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.065
_refine_diff_density_min         -1.568
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         7640
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0790
_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^)+(0.0882P)^2^+12.5438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                5761
_reflns_number_total             7640
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b404188gsup1.cif
_cod_data_source_block           ki158
_cod_original_cell_volume        5861.5(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7110293