#------------------------------------------------------------------------------
#$Date: 2019-11-26 16:25:35 +0200 (Tue, 26 Nov 2019) $
#$Revision: 243627 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/93/4089392.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4089392
loop_
_publ_author_name
'Bakthavachalam, K.'
'Reddy, N. Dastagiri'
_publ_section_title
;
 Synthesis of Aluminum Complexes of Triaza Framework Ligands and Their
 Catalytic Activity toward Polymerization of ε-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_sum            'C48 H60 Al4 O6'
_chemical_formula_weight         840.88
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.0954(3)
_cell_length_b                   21.0954(3)
_cell_length_c                   21.0954(3)
_cell_measurement_reflns_used    2797
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0838
_cell_measurement_theta_min      2.8909
_cell_volume                     9387.8(2)
_computing_cell_refinement
;
'Tue Jul 17 14:58:57 2012'
;
_computing_data_collection
;
'Tue Jul 17 14:58:57 2012'
;
_computing_data_reduction
;
'Tue Jul 17 14:58:57 2012'
;
_computing_molecular_graphics    ORTEP
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω 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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0781
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9685
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  0.9510
_exptl_absorpt_correction_T_min  0.9510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Tue Jul 17 14:58:57 2012'
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0784P)²+6.9396P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1587
_refine_ls_wR_factor_ref         0.1920
_reflns_number_gt                2146
_reflns_number_total             3677
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            om3011432_si_002.cif
_cod_data_source_block           alkoxide
_cod_database_code               4089392
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'y, z, x'
'-y+1/2, -z, x+1/2'
'y+1/2, -z+1/2, -x'
'-y, z+1/2, -x+1/2'
'z, x, y'
'-z, x+1/2, -y+1/2'
'-z+1/2, -x, y+1/2'
'z+1/2, -x+1/2, -y'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'-y, -z, -x'
'y-1/2, z, -x-1/2'
'-y-1/2, z-1/2, x'
'y, -z-1/2, x-1/2'
'-z, -x, -y'
'z, -x-1/2, y-1/2'
'z-1/2, x, -y-1/2'
'-z-1/2, x-1/2, y'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.78589(4) 0.28589(4) 0.21411(4) 0.0213(3) Uani 1 3 d S A .
Al2 Al 0.69619(4) 0.27252(4) 0.11000(4) 0.0321(3) Uani 1 1 d . A .
O2 O 0.85717(9) 0.25268(9) 0.17019(9) 0.0248(5) Uani 1 1 d . . .
C12 C 0.92694(15) 0.22431(14) 0.08147(14) 0.0308(7) Uani 1 1 d . . .
C11 C 0.88018(17) 0.27120(16) 0.10833(15) 0.0403(8) Uani 1 1 d . . .
H11A H 0.9003 0.3124 0.1115 0.048 Uiso 1 1 calc R . .
H11B H 0.8445 0.2751 0.0795 0.048 Uiso 1 1 calc R . .
C13 C 0.90809(18) 0.17635(16) 0.04167(15) 0.0426(9) Uani 1 1 d . . .
H13 H 0.8651 0.1708 0.0336 0.051 Uiso 1 1 calc R . .
C5 C 0.67597(16) 0.12603(15) 0.15429(19) 0.0446(9) Uani 1 1 d . . .
C1 C 0.60722(16) 0.29762(18) 0.11617(19) 0.0502(10) Uani 1 1 d . . .
H1A H 0.5924 0.2906 0.1586 0.075 Uiso 1 1 calc R . .
H1B H 0.5824 0.2729 0.0871 0.075 Uiso 1 1 calc R . .
H1C H 0.6031 0.3417 0.1058 0.075 Uiso 1 1 calc R . .
C17 C 0.99081(17) 0.23192(17) 0.09358(18) 0.0460(9) Uani 1 1 d . . .
H17 H 1.0046 0.2642 0.1202 0.055 Uiso 1 1 calc R . .
C6 C 0.61254(19) 0.1319(2) 0.1615(2) 0.0596(11) Uani 1 1 d . A .
H6 H 0.5975 0.1616 0.1904 0.072 Uiso 1 1 calc R . .
C15 C 1.0129(2) 0.1434(2) 0.0262(2) 0.0649(13) Uani 1 1 d . . .
H15 H 1.0418 0.1156 0.0079 0.078 Uiso 1 1 calc R . .
C14 C 0.9507(2) 0.13672(17) 0.01374(18) 0.0562(11) Uani 1 1 d . . .
H14 H 0.9369 0.1052 -0.0138 0.067 Uiso 1 1 calc R . .
C16 C 1.03442(18) 0.1910(2) 0.0657(2) 0.0667(13) Uani 1 1 d . . .
H16 H 1.0775 0.1955 0.0737 0.080 Uiso 1 1 calc R . .
C10 C 0.6988(2) 0.0825(2) 0.1122(3) 0.0788(15) Uani 1 1 d . A .
H10 H 0.7422 0.0775 0.1064 0.095 Uiso 1 1 calc R . .
C2 C 0.72058(19) 0.2382(2) 0.02735(17) 0.0584(11) Uani 1 1 d . . .
H2A H 0.7642 0.2483 0.0190 0.088 Uiso 1 1 calc R . .
H2B H 0.6943 0.2565 -0.0050 0.088 Uiso 1 1 calc R . .
H2C H 0.7152 0.1930 0.0275 0.088 Uiso 1 1 calc R . .
C8 C 0.5915(3) 0.0537(2) 0.0896(2) 0.0703(14) Uani 1 1 d . A .
H8 H 0.5618 0.0281 0.0693 0.084 Uiso 1 1 calc R . .
C9 C 0.6540(3) 0.0441(2) 0.0766(2) 0.0844(17) Uani 1 1 d . . .
H9 H 0.6673 0.0146 0.0467 0.101 Uiso 1 1 calc R A .
C7 C 0.5707(2) 0.0975(2) 0.1296(2) 0.0722(14) Uani 1 1 d . . .
H7 H 0.5275 0.1039 0.1352 0.087 Uiso 1 1 calc R A .
O1 O 0.72636(9) 0.22769(9) 0.17869(9) 0.0275(5) Uani 1 1 d . . .
C3 C 0.7106(5) 0.1664(4) 0.2055(4) 0.051(2) Uani 0.66(2) 1 d P A 1
H3A H 0.6833 0.1719 0.2421 0.061 Uiso 0.66(2) 1 calc PR A 1
H3B H 0.7489 0.1449 0.2191 0.061 Uiso 0.66(2) 1 calc PR A 1
C4 C 0.7347(7) 0.1599(5) 0.1747(11) 0.038(5) Uani 0.34(2) 1 d P A 2
H4A H 0.7476 0.1440 0.2159 0.045 Uiso 0.34(2) 1 calc PR A 2
H4B H 0.7684 0.1507 0.1449 0.045 Uiso 0.34(2) 1 calc PR A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Al1 O2 94.92(9) . 7_556
O2 Al1 O2 94.92(9) . 10_645
O2 Al1 O2 94.92(9) 7_556 10_645
O2 Al1 O1 95.31(8) . .
O2 Al1 O1 76.19(8) 7_556 .
O2 Al1 O1 166.97(8) 10_645 .
O2 Al1 O1 76.19(8) . 10_645
O2 Al1 O1 166.97(8) 7_556 10_645
O2 Al1 O1 95.31(8) 10_645 10_645
O1 Al1 O1 94.94(9) . 10_645
O2 Al1 O1 166.97(8) . 7_556
O2 Al1 O1 95.31(8) 7_556 7_556
O2 Al1 O1 76.19(8) 10_645 7_556
O1 Al1 O1 94.94(9) . 7_556
O1 Al1 O1 94.94(9) 10_645 7_556
O2 Al2 O1 79.44(9) 7_556 .
O2 Al2 C1 114.87(13) 7_556 .
O1 Al2 C1 114.72(14) . .
O2 Al2 C2 114.18(14) 7_556 .
O1 Al2 C2 114.82(15) . .
C1 Al2 C2 114.34(17) . .
C11 O2 Al2 130.07(18) . 10_645
C11 O2 Al1 127.30(17) . .
Al2 O2 Al1 102.54(10) 10_645 .
C13 C12 C17 118.8(3) . .
C13 C12 C11 121.6(3) . .
C17 C12 C11 119.5(3) . .
O2 C11 C12 112.4(2) . .
C14 C13 C12 121.7(4) . .
C6 C5 C10 118.9(4) . .
C6 C5 C4 138.1(8) . .
C10 C5 C4 102.5(9) . .
C6 C5 C3 109.6(6) . .
C10 C5 C3 130.8(6) . .
C4 C5 C3 31.7(6) . .
C12 C17 C16 119.7(4) . .
C7 C6 C5 123.4(4) . .
C14 C15 C16 121.0(4) . .
C15 C14 C13 119.7(4) . .
C15 C16 C17 119.2(4) . .
C5 C10 C9 118.8(4) . .
C7 C8 C9 123.4(4) . .
C8 C9 C10 116.3(4) . .
C8 C7 C6 119.0(5) . .
C4 O1 C3 33.6(6) . .
C4 O1 Al2 120.3(8) . .
C3 O1 Al2 133.2(3) . .
C4 O1 Al1 125.5(4) . .
C3 O1 Al1 124.9(3) . .
Al2 O1 Al1 101.82(10) . .
O1 C3 C5 109.0(5) . .
O1 C4 C5 112.9(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 O2 1.900(2) .
Al1 O2 1.900(2) 7_556
Al1 O2 1.900(2) 10_645
Al1 O1 1.908(2) .
Al1 O1 1.908(2) 10_645
Al1 O1 1.908(2) 7_556
Al2 O2 1.833(2) 7_556
Al2 O1 1.844(2) .
Al2 C1 1.954(3) .
Al2 C2 1.957(4) .
O2 C11 1.446(4) .
O2 Al2 1.833(2) 10_645
C12 C13 1.374(4) .
C12 C17 1.381(5) .
C12 C11 1.508(4) .
C13 C14 1.362(5) .
C5 C6 1.352(5) .
C5 C10 1.364(6) .
C5 C4 1.493(11) .
C5 C3 1.557(7) .
C17 C16 1.392(6) .
C6 C7 1.327(6) .
C15 C14 1.344(6) .
C15 C16 1.382(7) .
C10 C9 1.453(7) .
C8 C7 1.326(7) .
C8 C9 1.361(7) .
O1 C4 1.444(11) .
O1 C3 1.449(6) .
