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_4324782
_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         'C53.88 H84 N2 O8 Zr2, C2 H4 Cl2 '
_chemical_formula_sum            'C27.94 H44 Cl N O4 Zr'
_chemical_formula_weight         584.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 99.814(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6139(8)
_cell_length_b                   26.9865(19)
_cell_length_c                   11.2087(8)
_cell_measurement_temperature    173(2)
_cell_volume                     3163.5(4)
_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, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.861
_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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.1007
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            22079
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  0.9597
_exptl_absorpt_correction_T_min  0.9054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       block
_exptl_crystal_F_000             1231
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.968
_refine_diff_density_min         -2.175
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         12340
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0881
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+19.7014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2212
_refine_ls_wR_factor_ref         0.2373
_reflns_number_gt                9475
_reflns_number_total             12340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1025262_si_002_2.cif
_cod_data_source_block           Zr
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               4324782