Salen Complexes of Zirconium and Hafnium: Synthesis, Structural Characterization, Controlled Hydrolysis, and Solvent-Free Ring-Opening Polymerization of Cyclic Esters and Lactides
Tanmoy Kumar Saha; Venkatachalam Ramkumar; Debashis Chakraborty; Inorganic Chemistry 50 (2011) 2720–2722; doi:10.1021/ic1025262

data_4324781
_publ_section_title
;
 Salen Complexes of Zirconium and Hafnium: Synthesis, Structural
 Characterization, Controlled Hydrolysis, and Solvent-Free Ring-Opening
 Polymerization of Cyclic Esters and Lactides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2720
_journal_page_last               2722
_journal_paper_doi               10.1021/ic1025262
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C40 H61 Hf N2 O4'
_chemical_formula_sum            'C40 H61 Hf N2 O4'
_chemical_formula_weight         812.40
_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                 112.0480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3458(5)
_cell_length_b                   17.1552(4)
_cell_length_c                   19.7831(5)
_cell_measurement_temperature    173(2)
_cell_volume                     4827.2(2)
_computing_cell_refinement       'APEXII/SAINT (Bruker, 2004)'
_computing_data_collection       'APEXII (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997) '
_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 0.999
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker ApexII CCD area detector'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34001
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    2.193
_exptl_absorpt_correction_T_max  0.8105
_exptl_absorpt_correction_T_min  0.6440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.766
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         11493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0924P)^2^+34.8372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.1862
_reflns_number_gt                9043
_reflns_number_total             11493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1025262_si_002_1.cif
_cod_data_source_block           Hf
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4324781