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_4072568
_publ_contact_author
;
      Prof. Dr. Peter Roesky
      Freie Universit\"at Berlin
      Fabeckstr. 34-36
      14195 Berlin
      Bundesrepublik Deutschland
;
_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 Yb, 0.5(C7 H8)'
_chemical_formula_sum            'C44.5 H58 Cl N2 P2 Si2 Yb'
_chemical_formula_weight         947.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_date             05-03-17
_audit_creation_method           'STOE X-RED'
_cell_angle_alpha                90.00
_cell_angle_beta                 105.870(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.731(2)
_cell_length_b                   15.4763(16)
_cell_length_c                   14.5358(16)
_cell_measurement_temperature    173(2)
_cell_volume                     4485.9(8)
_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_publication_material  'X-STEP32, Microsoft Word'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'area detector'
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19558
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    2.301
_exptl_absorpt_correction_T_max  0.6421
_exptl_absorpt_correction_T_min  0.5624
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.158
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0365P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0647
_reflns_number_gt                6463
_reflns_number_total             7850
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0608307si20060911_102029.cif
_cod_data_source_block           1c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C44.50 H58 Cl N2 P2 Si2 Yb'
_cod_database_code               4072568