Synthesis and Structural Characterization of Group 4 Metal Alkoxide Complexes of N,N,N',N'-Tetrakis(2-hydroxyethyl)ethylenediamine and Their Use As Initiators in the Ring-Opening Polymerization (ROP) of rac-Lactide under Industrially Relevant Conditions
Christopher J. Chuck; Matthew G. Davidson; Gerrit Gobius du Sart; Petya K. Ivanova-Mitseva; Gabriele I. Kociok-Köhn; Lois B. Manton; Inorganic Chemistry 52 (2013) 10804–10811; doi:10.1021/ic400667z

data_4336129
_publ_section_title
;
 Synthesis and Structural Characterization of Group 4 Metal Alkoxide
 Complexes of N,N,N',N'-Tetrakis(2-hydroxyethyl)ethylenediamine and Their
 Use As Initiators in the Ring-Opening Polymerization (ROP) of rac-Lactide
 under Industrially Relevant Conditions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10804
_journal_page_last               10811
_journal_paper_doi               10.1021/ic400667z
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C42 H88 N6 O16 Ti4, 2(C H2 Cl2)'
_chemical_formula_sum            'C44 H92 Cl4 N6 O16 Ti4'
_chemical_formula_weight         1294.64
_space_group_IT_number           2
_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
_cell_angle_alpha                83.6010(10)
_cell_angle_beta                 78.3720(10)
_cell_angle_gamma                80.9510(10)
_cell_formula_units_Z            1
_cell_length_a                   8.84810(10)
_cell_length_b                   9.8772(2)
_cell_length_c                   17.3948(3)
_cell_measurement_reflns_used    18996
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     1465.47(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 DENZO-SCALEPACK Z. Otwinowski and W. Minor, " 
 Processing of x-ray Diffraction Data Collected in Oscillation Mode ", 
 Methods in Enzymology, Volume 276: Macromolecular Crystallography, 
 part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
 SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). 
 Sheldrick, G.M., Institut f\"ur Anorganische Chemie der Universit\"at, 
 Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 
;
_computing_structure_solution
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '285 2.0 degree images with \f and \w 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  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28775
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.9060
_exptl_absorpt_correction_T_min  0.8299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourles
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0162P)^2^+2.0197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                5631
_reflns_number_total             6714
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400667z_si_002_1.cif
_cod_data_source_block           3
_cod_database_code               4336129