Synthesis of Aluminum Complexes of Triaza Framework Ligands and Their Catalytic Activity toward Polymerization of ε-Caprolactone
Bakthavachalam, K.; Reddy, N. Dastagiri; Organometallics 32 (2013) 3174–; doi:10.1021/om3011432

data_4089386
_publ_section_title
;
 Synthesis of Aluminum Complexes of Triaza Framework Ligands and Their
 Catalytic Activity toward Polymerization of \e-Caprolactone
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3174
_journal_paper_doi               10.1021/om3011432
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C39 H47 Al Cl N3'
_chemical_formula_sum            'C39 H47 Al Cl N3'
_chemical_formula_weight         620.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-07-23
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.660(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.0597(5)
_cell_length_b                   12.3654(4)
_cell_length_c                   31.8609(11)
_cell_measurement_reflns_used    10454
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3204
_cell_measurement_theta_min      2.7379
_cell_volume                     7014.1(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega    3.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2928   37.0000   90.0000 85

  2 omega  -48.00  -22.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2928  -77.0000  -60.0000 26

  3 omega   39.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2928 -113.0000   87.0000 30

  4 omega   -4.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2928   77.0000  150.0000 87
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0327536000
_diffrn_orient_matrix_UB_12      0.0091197000
_diffrn_orient_matrix_UB_13      -0.0153157000
_diffrn_orient_matrix_UB_21      -0.0224892000
_diffrn_orient_matrix_UB_22      -0.0053101000
_diffrn_orient_matrix_UB_23      0.0161060000
_diffrn_orient_matrix_UB_31      0.0031613000
_diffrn_orient_matrix_UB_32      0.0563769000
_diffrn_orient_matrix_UB_33      0.0039846000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0910
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            26708
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.81
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.524
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         12341
_refine_ls_number_restraints     528
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0853P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1666
_reflns_number_gt                7404
_reflns_number_total             12341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3011432_si_002.cif
_cod_data_source_block           '[L1AlMeCl]'
_cod_database_code               4089386
_chemical_oxdiff_formula         c50h49al1n3cl1
_chemical_oxdiff_usercomment     'at 150K'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32