In Situ Formation of Bis(phosphinimino)methanide Rare Earth Alkoxide Initiators for the Ring-Opening Polymerization of ε-Caprolactone
Gamer, Michael T.; Roesky, Peter W.; Palard, Isabelle; Le Hellaye, Maude; Guillaume, Sophie M.; Organometallics 26 (2007) 651–; doi:10.1021/om0608307

data_4072566
_publ_section_title
;
 In Situ Formation of Bis(phosphinimino)methanide Rare Earth Alkoxide
 Initiators for the Ring-Opening Polymerization of \e-Caprolactone
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              651
_journal_paper_doi               10.1021/om0608307
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C41 H54 Cl N2 P2 Si2 Y, 0.5(C7 H8)'
_chemical_formula_sum            'C44.5 H58 Cl N2 P2 Si2 Y'
_chemical_formula_weight         863.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 105.547(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.8649(10)
_cell_length_b                   15.6124(8)
_cell_length_c                   14.6317(9)
_cell_measurement_temperature    203(2)
_cell_volume                     4591.9(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'STOE IPDS '
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.1137
_diffrn_reflns_av_sigmaI/netI    0.1122
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38476
_diffrn_reflns_theta_full        24.09
_diffrn_reflns_theta_max         24.09
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            cubes
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       colorless
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .15
_refine_diff_density_max         1.167
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         14482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.0745
_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^)+(0.0663P)^2^+10.3704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1856
_reflns_number_gt                8434
_reflns_number_total             14482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0608307si20060911_102029.cif
_cod_data_source_block           1a
_cod_original_sg_symbol_H-M      P2(1)/C
_cod_original_formula_sum        'C44.50 H58 Cl N2 P2 Si2 Y'
_cod_database_code               4072566