Zr(iv) complexes containing salan-type ligands: synthesis, structural characterization and role as catalysts towards the polymerization of ε-caprolactone, rac-lactide, ethylene, homopolymerization and copolymerization of epoxides with CO2
Mandal, Mrinmay; Chakraborty, Debashis; Ramkumar, Venkatachalam; RSC Advances 5 (2015) 28536–; doi:10.1039/C4RA17201A

data_7235734
_publ_section_title
;
 Zr(iv) complexes containing salan-type ligands: synthesis, structural
 characterization and role as catalysts towards the polymerization of
 \e-caprolactone, rac-lactide, ethylene, homopolymerization and
 copolymerization of epoxides with CO2
;
_journal_issue                   36
_journal_name_full               'RSC Advances'
_journal_page_first              28536
_journal_paper_doi               10.1039/C4RA17201A
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C49 H86 N2 O8 Zr2'
_chemical_formula_sum            'C49 H86 N2 O8 Zr2'
_chemical_formula_weight         1013.64
_chemical_name_systematic        Zr
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2014-07-22 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.6790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8978(5)
_cell_length_b                   13.4806(4)
_cell_length_c                   24.3958(7)
_cell_measurement_temperature    296(2)
_cell_volume                     5421.7(3)
_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-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            45770
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.711
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.9327
_exptl_absorpt_correction_T_min  0.8905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             2152
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.357
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.853
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         9539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.853
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.055
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1120P)^2^+12.5437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7833
_reflns_number_total             9539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra17201a2.cif
_cod_data_source_block           Zr2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7235734
_shelxl_version_number           2014-3
_shelx_res_checksum              95987
_shelx_hkl_checksum              34363