Lactide Cyclopolymerization Kinetics, X-ray Structure, and Solution Dynamics of (tBu-SalAmEE)Al and a Cautionary Tale Of Polymetalate Formation
Reisberg, Solomon H.; Hurley, Harry J.; Mathers, Robert T.; Tanski, Joseph M.; Getzler, Yutan D. Y. L.; Macromolecules 46 (2013) 3273–; doi:10.1021/ma400046x

data_1512018
_publ_contact_author             'Yutan D. Y. L. Getzler'
_publ_section_title
;
 Lactide Cyclopolymerization Kinetics, X-ray Structure, and Solution
 Dynamics of (tBu-SalAmEE)Al and a Cautionary Tale Of Polymetalate
 Formation
;
_journal_issue                   9
_journal_name_full               Macromolecules
_journal_page_first              3273
_journal_paper_doi               10.1021/ma400046x
_journal_volume                  46
_journal_year                    2013
_chemical_formula_moiety         'C34 H52 Al N O4'
_chemical_formula_sum            'C34 H52 Al N O4'
_chemical_formula_weight         565.75
_chemical_name_common
'(N,N-Bis(3,5-di-tert-butyl-2-benzyloxy)-2-(2-aminoethoxy)ethoxy)aluminum [(tBu-SalAmEE)Al]'
_chemical_name_systematic        ?
_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                102.7490(10)
_cell_angle_beta                 113.6440(10)
_cell_angle_gamma                93.7200(10)
_cell_formula_units_Z            4
_cell_length_a                   14.8694(9)
_cell_length_b                   14.9782(10)
_cell_length_c                   16.7758(11)
_cell_measurement_reflns_used    8512
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      28.88
_cell_measurement_theta_min      2.45
_cell_volume                     3288.7(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\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  0.0911
_diffrn_reflns_av_sigmaI/netI    0.1356
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            50334
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.9971
_exptl_absorpt_correction_T_min  0.9528
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.307
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         18393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1645
_refine_ls_R_factor_gt           0.0707
_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^)+(0.0741P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                9051
_reflns_number_total             18393
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ma400046x_si_002.cif
_cod_data_source_block           yg1447al
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1512018