Synthesis and Characterization of Bidentate Rare-Earth Iminophosphoraneo-Aryl Complexes and Their Behavior As Catalysts for the Polymerization of 1,3-Butadiene
Martinez-Arripe, Elsa; Jean-Baptiste-dit-Dominique, François; Auffrant, Audrey; Le Goff, Xavier-Frédéric; Thuilliez, Julien; Nief, François; Organometallics 31 (2012) 4854–; doi:10.1021/om300389v

data_4078751
_publ_section_title
;
 Synthesis and Characterization of Bidentate Rare-Earth
 Iminophosphoraneo-Aryl Complexes and Their Behavior As Catalysts for the
 Polymerization of 1,3-Butadiene
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              4854
_journal_paper_doi               10.1021/om300389v
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C66 H69 La N3 P3, C4H8O, C7H8'
_chemical_formula_sum            'C77 H85 La N3 O P3'
_chemical_formula_weight         1300.30
_chemical_name_systematic
; 
 ? 
;
_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                88.449(1)
_cell_angle_beta                 69.426(1)
_cell_angle_gamma                84.688(1)
_cell_formula_units_Z            2
_cell_length_a                   13.154(1)
_cell_length_b                   15.279(1)
_cell_length_c                   18.133(1)
_cell_measurement_reflns_used    5503
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3397.2(4)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49417
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.9292
_exptl_absorpt_correction_T_min  0.8073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
 A highly disordered C4H8O and C5H12 molecule was accounted for using the
 Platon SQUEEZE function.
;
_refine_diff_density_max         1.160
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         15476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0498P)^2^+5.9274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1260
_reflns_number_gt                13581
_reflns_number_total             15476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300389v_si_002.cif
_cod_data_source_block           ema254
_cod_original_sg_symbol_H-M      'P-1     '
_cod_database_code               4078751