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_7235733
_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         'C55 H96 N2 O8 Zr2, 0.5(C8)'
_chemical_formula_sum            'C59 H96 N2 O8 Zr2'
_chemical_formula_weight         1143.82
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_update_record
;
2014-07-22 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                94.360(2)
_cell_angle_beta                 101.224(2)
_cell_angle_gamma                100.485(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1760(3)
_cell_length_b                   11.3344(3)
_cell_length_c                   26.2444(8)
_cell_measurement_temperature    298(2)
_cell_volume                     3184.95(16)
_computing_cell_refinement       APEXII,Bruker,2004
_computing_data_collection       APEXII,Bruker,2004
_computing_data_reduction        SAINT,Bruker,2004
_computing_molecular_graphics    'ORTEP-3 (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      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            38478
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.80
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.9424
_exptl_absorpt_correction_T_min  0.8798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         11145
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1672
_reflns_number_gt                8465
_reflns_number_total             11145
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra17201a2.cif
_cod_data_source_block           Zr3
_cod_original_cell_volume        3184.95(15)
_cod_database_code               7235733