Insertion Reactions and Catalytic Hydrophosphination of Heterocumulenes using α-MetalatedN,N-Dimethylbenzylamine Rare-Earth-Metal Complexes
Behrle, Andrew C.; Schmidt, Joseph A. R.; Organometallics 32 (2013) 1141–1149; doi:10.1021/om300807k

data_4080112
_publ_section_title
;
 Insertion Reactions and Catalytic Hydrophosphination of Heterocumulenes
 using \a-MetalatedN,N-Dimethylbenzylamine Rare-Earth-Metal Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1141
_journal_page_last               1149
_journal_paper_doi               10.1021/om300807k
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C57 H72 La N6 P3'
_chemical_formula_sum            'C57 H72 La N6 P3'
_chemical_formula_weight         1073.03
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.324(2)
_cell_angle_beta                 83.209(2)
_cell_angle_gamma                80.949(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0569(12)
_cell_length_b                   12.7890(16)
_cell_length_c                   21.968(3)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.07
_cell_measurement_theta_min      2.43
_cell_volume                     2751.6(6)
_computing_cell_refinement       'Bruker SAINT v6.22'
_computing_data_collection       'Bruker SMART v5.625'
_computing_data_reduction        'Bruker SAINT v6.622'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       \w-scan
_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  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32673
_diffrn_reflns_theta_full        26.08
_diffrn_reflns_theta_max         26.08
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         10895
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0201
_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^)+(0.0175P)^2^+1.2529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0476
_reflns_number_gt                10029
_reflns_number_total             10895
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300807k_si_003.cif
_cod_data_source_block           La[iPrNC(PPh2)NiPr]3_(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4080112