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_4330645
_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_moiety         'C72 H56 O6 Zr, C4 H8 O'
_chemical_formula_sum            'C76 H64 O7 Zr'
_chemical_formula_weight         1180.49
_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                 116.030(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.394(5)
_cell_length_b                   24.050(7)
_cell_length_c                   20.545(5)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.24
_cell_volume                     6391(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0675
_diffrn_reflns_av_sigmaI/netI    0.1089
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41783
_diffrn_reflns_theta_full        28.05
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.9562
_exptl_absorpt_correction_T_min  0.8954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       prism
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
 The residual electron density was assigned to one molecule of the
 tetrahydrofuran solvent [91/4 = 23 e per asymmetric unit; one molecule
 of C4H8O would give 40e].
;
_refine_diff_density_max         1.464
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         15221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1570
_refine_ls_R_factor_gt           0.0877
_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^)+(0.0971P)^2^+3.6133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1972
_refine_ls_wR_factor_ref         0.2210
_reflns_number_gt                8185
_reflns_number_total             15221
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic301352t_si_002_1.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4330645