Synthesis and characterization of group 4 metal alkoxide complexes containing imine based bis-bidentate ligands: effective catalysts for the ring opening polymerization of lactides, epoxides and polymerization of ethylene.
Roymuhury, Sagnik K.; Chakraborty, Debashis; Ramkumar, Venkatachalam; Dalton transactions (Cambridge, England : 2003) 44 (2015) 10352–10367; doi:10.1039/c5dt01092f

data_7035121
_publ_section_title
;
 Synthesis and characterization of group 4 metal alkoxide complexes
 containing imine based bis-bidentate ligands: effective catalysts for the
 ring opening polymerization of lactides, epoxides and polymerization of
 ethylene.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10352
_journal_page_last               10367
_journal_paper_doi               10.1039/c5dt01092f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C138 H204 Hf3 N6 O12'
_chemical_formula_weight         2674.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_audit_update_record
;
2015-04-28 deposited with the CCDC.
2015-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.805(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1043(7)
_cell_length_b                   29.5065(11)
_cell_length_c                   30.3372(10)
_cell_measurement_reflns_used    6847
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.71
_cell_measurement_theta_min      2.27
_cell_volume                     16942.7(11)
_computing_cell_refinement       'APEXII/SAINT (Bruker, 2008)'
_computing_data_collection       'APEXII (Bruker, 2008)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2008)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997) '
_computing_publication_material  'SHELXL-97 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'Bruker kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.1101
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            116293
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.917
_diffrn_reflns_theta_min         0.967
_exptl_absorpt_coefficient_mu    1.880
_exptl_absorpt_correction_T_max  0.7821
_exptl_absorpt_correction_T_min  0.6912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_description       block
_exptl_crystal_F_000             5544
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
The solvent accessible cavity associated with toluene molecule
(estimated volume 2068 \%A^3^) contains disordered toulene molecule,
for which no reasonable model could be developed. Therefore, the observed
structure  were modified by PLATON SQUEEZE(Spek, 2009) to eliminate
the diffuse electron density (272 electrons) found in the cavity.  

;
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1544
_refine_ls_number_reflns         35986
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0613P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18642
_reflns_number_total             35986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01092f2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7035119--7035121.cif.'
_cod_database_code               7035121
_shelx_estimated_absorpt_t_min   0.602
_shelx_estimated_absorpt_t_max   0.705
_shelxl_version_number           2012-9
_shelx_res_checksum              78028