Stereoselective Synthesis of Biphenolate/Binaphtolate Titanate and Zirconate Alkoxide Species: Structural Characterization and Use in the Controlled ROP of Lactide
Laurine Azor; Corinne Bailly; Lydia Brelot; Marc Henry; Pierre Mobian; Samuel Dagorne; Inorganic Chemistry 51 (2012) 10876–10883; doi:10.1021/ic301352t

data_4330648
_publ_contact_author_address
;
Institut Le Bel, rue Blaise Pascal, 67000 STRASBOURG, FRANCE
;
_publ_contact_author_email       welter@unistra.fr
_publ_contact_author_fax         0383681232
_publ_contact_author_name
;
Richard Welter
;
_publ_contact_author_phone       0383681593
_publ_section_title
;
 Stereoselective Synthesis of Biphenolate/Binaphtolate Titanate and
 Zirconate Alkoxide Species: Structural Characterization and Use in the
 Controlled ROP of Lactide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10876
_journal_page_last               10883
_journal_paper_doi               10.1021/ic301352t
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C56 H48 O6 Zr'
_chemical_formula_weight         908.16
_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                89.13(2)
_cell_angle_beta                 85.11(2)
_cell_angle_gamma                73.82
_cell_formula_units_Z            2
_cell_length_a                   9.785(3)
_cell_length_b                   13.750(3)
_cell_length_c                   17.194(5)
_cell_measurement_reflns_used    18647
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2213.5(11)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_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  0.0927
_diffrn_reflns_av_sigmaI/netI    0.0839
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31198
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.183
_refine_diff_density_min         -1.270
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         12911
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0955P)^2^+0.2223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1507
_refine_ls_wR_factor_ref         0.1741
_reflns_number_gt                9455
_reflns_number_total             12911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301352t_si_002_4.cif
_cod_data_source_block           laurine_zr_oct_2010
_cod_database_code               4330648