#------------------------------------------------------------------------------
#$Date: 2016-09-10 02:25:13 +0300 (Sat, 10 Sep 2016) $
#$Revision: 186384 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/01/7040143.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_7040143
loop_
_publ_author_name
'Kirk, Sarah M.'
'Quilter, Helena C.'
'Buchard, Antoine'
'Thomas, Lynne H.'
'Kociok-Kohn, Gabriele'
'Jones, Matthew D.'
_publ_section_title
;
 Monomeric and dimeric Al(iii) complexes for the production of
 polylactide.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13846
_journal_page_last               13852
_journal_paper_doi               10.1039/c6dt02861f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C44 H60 Al2 N2 O2, 2(C7 H8)'
_chemical_formula_sum            'C58 H76 Al2 N2 O2'
_chemical_formula_weight         887.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-11 deposited with the CCDC.
2016-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.7450(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1650(3)
_cell_length_b                   13.0700(3)
_cell_length_c                   14.7260(4)
_cell_measurement_reflns_used    15765
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      3.51
_cell_volume                     2669.24(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'kappa CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23401
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.016
_diffrn_reflns_theta_max         25.016
_diffrn_reflns_theta_min         3.610
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   0.9952
_exptl_transmission_factor_min   0.9905
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0654P)²+1.7888P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1518
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3364
_reflns_number_total             4696
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02861f2.cif
_cod_data_source_block           Al2_5_Me4
_cod_depositor_comments
'Adding full bibliography for 7040140--7040144.cif.'
_cod_database_code               7040143
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.990
_shelx_estimated_absorpt_t_max   0.995
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Al1 Al 0.51966(6) 0.33344(5) 0.07308(5) 0.0283(2) Uani 1 1 d . .
O1 O 0.48816(13) 0.39617(12) 0.16934(12) 0.0331(4) Uani 1 1 d . .
N1 N 0.50245(14) 0.19635(14) 0.12118(13) 0.0260(5) Uani 1 1 d . .
C1 C 0.6546(2) 0.3587(2) 0.0693(2) 0.0404(7) Uani 1 1 d . .
H1A H 0.6630 0.4307 0.0541 0.061 Uiso 1 1 calc R U
H1B H 0.6735 0.3151 0.0219 0.061 Uiso 1 1 calc R U
H1C H 0.6951 0.3430 0.1299 0.061 Uiso 1 1 calc R U
C2 C 0.4203(2) 0.3434(2) -0.0401(2) 0.0444(7) Uani 1 1 d . .
H2A H 0.3566 0.3354 -0.0248 0.067 Uiso 1 1 calc R U
H2B H 0.4302 0.2894 -0.0834 0.067 Uiso 1 1 calc R U
H2C H 0.4244 0.4105 -0.0689 0.067 Uiso 1 1 calc R U
C3 C 0.43490(17) 0.36448(18) 0.22829(17) 0.0271(5) Uani 1 1 d . .
C4 C 0.40319(17) 0.43510(18) 0.28902(16) 0.0268(5) Uani 1 1 d . .
C5 C 0.34358(18) 0.39790(19) 0.34501(17) 0.0304(6) Uani 1 1 d . .
H5 H 0.3208 0.4453 0.3845 0.036 Uiso 1 1 calc R U
C6 C 0.31382(18) 0.29497(19) 0.34820(17) 0.0312(6) Uani 1 1 d . .
C7 C 0.35085(19) 0.22731(19) 0.29304(17) 0.0306(6) Uani 1 1 d . .
H7 H 0.3356 0.1567 0.2954 0.037 Uiso 1 1 calc R U
C8 C 0.41071(18) 0.25980(17) 0.23308(16) 0.0272(5) Uani 1 1 d . .
C9 C 0.43486(18) 0.54805(18) 0.29249(18) 0.0301(6) Uani 1 1 d . .
C10 C 0.3920(2) 0.60051(19) 0.20013(19) 0.0392(7) Uani 1 1 d . .
H10A H 0.4103 0.5623 0.1491 0.059 Uiso 1 1 calc R U
H10B H 0.4168 0.6706 0.2007 0.059 Uiso 1 1 calc R U
H10C H 0.3216 0.6022 0.1915 0.059 Uiso 1 1 calc R U
C11 C 0.54532(19) 0.5556(2) 0.3115(2) 0.0387(7) Uani 1 1 d . .
H11A H 0.5696 0.5207 0.2621 0.058 Uiso 1 1 calc R U
H11B H 0.5723 0.5233 0.3712 0.058 Uiso 1 1 calc R U
H11C H 0.5645 0.6278 0.3135 0.058 Uiso 1 1 calc R U
C12 C 0.4014(2) 0.6077(2) 0.3703(2) 0.0437(7) Uani 1 1 d . .
H12A H 0.4254 0.6781 0.3717 0.066 Uiso 1 1 calc R U
H12B H 0.4266 0.5746 0.4300 0.066 Uiso 1 1 calc R U
H12C H 0.3307 0.6084 0.3587 0.066 Uiso 1 1 calc R U
C13 C 0.2450(2) 0.2641(2) 0.41110(19) 0.0400(7) Uani 1 1 d . .
C14 C 0.1502(3) 0.3220(5) 0.3809(3) 0.1001(17) Uani 1 1 d . .
H14A H 0.1628 0.3958 0.3844 0.150 Uiso 1 1 calc R U
H14B H 0.1063 0.3042 0.4220 0.150 Uiso 1 1 calc R U
H14C H 0.1207 0.3033 0.3170 0.150 Uiso 1 1 calc R U
C15 C 0.2261(4) 0.1498(3) 0.4077(3) 0.120(2) Uani 1 1 d . .
H15A H 0.1957 0.1299 0.3444 0.179 Uiso 1 1 calc R U
H15B H 0.1831 0.1326 0.4499 0.179 Uiso 1 1 calc R U
H15C H 0.2872 0.1130 0.4267 0.179 Uiso 1 1 calc R U
C16 C 0.2875(2) 0.2922(3) 0.5110(2) 0.0527(8) Uani 1 1 d . .
H16A H 0.3499 0.2582 0.5308 0.079 Uiso 1 1 calc R U
H16B H 0.2436 0.2700 0.5507 0.079 Uiso 1 1 calc R U
H16C H 0.2963 0.3665 0.5161 0.079 Uiso 1 1 calc R U
C17 C 0.45018(18) 0.18131(18) 0.18318(16) 0.0280(6) Uani 1 1 d . .
H17 H 0.4369 0.1124 0.1967 0.034 Uiso 1 1 calc R U
C18 C 0.54110(18) 0.10939(17) 0.07987(16) 0.0266(5) Uani 1 1 d . .
C19 C 0.63891(18) 0.09939(18) 0.09444(17) 0.0303(6) Uani 1 1 d . .
H19 H 0.6792 0.1472 0.1327 0.036 Uiso 1 1 calc R U
C20 C 0.47880(17) 0.04108(17) 0.02070(16) 0.0234(5) Uani 1 1 d . .
C21 C 0.37650(18) 0.05020(18) 0.00229(17) 0.0276(5) Uani 1 1 d . .
H21 H 0.3474 0.1050 0.0290 0.033 Uiso 1 1 calc R U
C22 C 0.31987(18) -0.01866(18) -0.05306(17) 0.0301(6) Uani 1 1 d . .
H22 H 0.2517 -0.0120 -0.0638 0.036 Uiso 1 1 calc R U
C23 C -0.0114(3) 0.3948(2) 0.7288(3) 0.0563(9) Uani 1 1 d . .
C24 C 0.0081(3) 0.4198(3) 0.6406(3) 0.0640(10) Uani 1 1 d . .
H24 H -0.0429 0.4292 0.5884 0.077 Uiso 1 1 calc R U
C25 C 0.1000(3) 0.4296(3) 0.6327(3) 0.0693(10) Uani 1 1 d . .
H25 H 0.1125 0.4443 0.5731 0.083 Uiso 1 1 calc R U
C26 C 0.1778(3) 0.4197(3) 0.7053(4) 0.0836(13) Uani 1 1 d . .
H26 H 0.2418 0.4293 0.6967 0.100 Uiso 1 1 calc R U
C27 C 0.1595(3) 0.3959(3) 0.7892(3) 0.0737(11) Uani 1 1 d . .
H27 H 0.2115 0.3873 0.8407 0.088 Uiso 1 1 calc R U
C28 C 0.0630(2) 0.3836(2) 0.8013(2) 0.0479(8) Uani 1 1 d . .
H28 H 0.0510 0.3674 0.8608 0.057 Uiso 1 1 calc R U
C29 C -0.1100(3) 0.3806(3) 0.7406(3) 0.0817(12) Uani 1 1 d . .
H29A H -0.1301 0.3098 0.7254 0.122 Uiso 1 1 calc R U
H29B H -0.1528 0.4274 0.6993 0.122 Uiso 1 1 calc R U
H29C H -0.1137 0.3951 0.8051 0.122 Uiso 1 1 calc R U
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'
N N 0.0061 0.0033 '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
O1 Al1 C1 110.63(11) . .
O1 Al1 C2 113.37(11) . .
C1 Al1 C2 120.22(13) . .
O1 Al1 N1 93.66(8) . .
C1 Al1 N1 111.08(11) . .
C2 Al1 N1 104.38(11) . .
C3 O1 Al1 130.42(15) . .
C17 N1 C18 119.58(19) . .
C17 N1 Al1 121.44(16) . .
C18 N1 Al1 118.69(15) . .
Al1 C1 H1A 109.5 . .
Al1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Al1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
Al1 C2 H2A 109.5 . .
Al1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
Al1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
O1 C3 C8 120.7(2) . .
O1 C3 C4 120.3(2) . .
C8 C3 C4 119.1(2) . .
C5 C4 C3 117.2(2) . .
C5 C4 C9 121.7(2) . .
C3 C4 C9 121.1(2) . .
C4 C5 C6 125.2(2) . .
C4 C5 H5 117.4 . .
C6 C5 H5 117.4 . .
C7 C6 C5 116.1(2) . .
C7 C6 C13 123.7(2) . .
C5 C6 C13 120.2(2) . .
C6 C7 C8 121.8(2) . .
C6 C7 H7 119.1 . .
C8 C7 H7 119.1 . .
C7 C8 C3 120.4(2) . .
C7 C8 C17 116.8(2) . .
C3 C8 C17 122.7(2) . .
C10 C9 C11 109.7(2) . .
C10 C9 C12 107.9(2) . .
C11 C9 C12 106.8(2) . .
C10 C9 C4 109.8(2) . .
C11 C9 C4 110.3(2) . .
C12 C9 C4 112.2(2) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C9 C11 H11A 109.5 . .
C9 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C9 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C9 C12 H12A 109.5 . .
C9 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C9 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C16 C13 C15 107.6(3) . .
C16 C13 C14 108.3(3) . .
C15 C13 C14 109.8(4) . .
C16 C13 C6 110.4(2) . .
C15 C13 C6 111.7(2) . .
C14 C13 C6 108.9(3) . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C13 C16 H16A 109.5 . .
C13 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C13 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
N1 C17 C8 125.9(2) . .
N1 C17 H17 117.1 . .
C8 C17 H17 117.1 . .
C19 C18 C20 121.3(2) . .
C19 C18 N1 117.9(2) . .
C20 C18 N1 120.6(2) . .
C18 C19 C22 120.2(2) . 3_655
C18 C19 H19 119.9 . .
C22 C19 H19 119.9 3_655 .
C18 C20 C21 123.0(2) . .
C18 C20 C20 118.2(3) . 3_655
C21 C20 C20 118.8(3) . 3_655
C22 C21 C20 120.8(2) . .
C22 C21 H21 119.6 . .
C20 C21 H21 119.6 . .
C21 C22 C19 120.7(2) . 3_655
C21 C22 H22 119.6 . .
C19 C22 H22 119.6 3_655 .
C28 C23 C24 118.9(3) . .
C28 C23 C29 120.5(4) . .
C24 C23 C29 120.6(4) . .
C25 C24 C23 118.4(4) . .
C25 C24 H24 120.8 . .
C23 C24 H24 120.8 . .
C24 C25 C26 124.3(4) . .
C24 C25 H25 117.8 . .
C26 C25 H25 117.8 . .
C27 C26 C25 117.4(4) . .
C27 C26 H26 121.3 . .
C25 C26 H26 121.3 . .
C26 C27 C28 120.6(4) . .
C26 C27 H27 119.7 . .
C28 C27 H27 119.7 . .
C23 C28 C27 120.3(3) . .
C23 C28 H28 119.8 . .
C27 C28 H28 119.8 . .
C23 C29 H29A 109.5 . .
C23 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C23 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 O1 1.7716(17) .
Al1 C1 1.952(3) .
Al1 C2 1.955(3) .
Al1 N1 1.960(2) .
O1 C3 1.327(3) .
N1 C17 1.302(3) .
N1 C18 1.448(3) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C8 1.416(3) .
C3 C4 1.420(3) .
C4 C5 1.383(3) .
C4 C9 1.541(3) .
C5 C6 1.413(3) .
C5 H5 0.9500 .
C6 C7 1.375(3) .
C6 C13 1.529(3) .
C7 C8 1.408(3) .
C7 H7 0.9500 .
C8 C17 1.440(3) .
C9 C10 1.534(4) .
C9 C11 1.536(4) .
C9 C12 1.539(3) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 C16 1.517(4) .
C13 C15 1.518(5) .
C13 C14 1.527(5) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17 0.9500 .
C18 C19 1.364(3) .
C18 C20 1.422(3) .
C19 C22 1.404(3) 3_655
C19 H19 0.9500 .
C20 C21 1.424(3) .
C20 C20 1.426(4) 3_655
C21 C22 1.361(3) .
C21 H21 0.9500 .
C22 C19 1.404(3) 3_655
C22 H22 0.9500 .
C23 C28 1.346(5) .
C23 C24 1.421(5) .
C23 C29 1.455(5) .
C24 C25 1.336(5) .
C24 H24 0.9500 .
C25 C26 1.376(6) .
C25 H25 0.9500 .
C26 C27 1.349(6) .
C26 H26 0.9500 .
C27 C28 1.423(5) .
C27 H27 0.9500 .
C28 H28 0.9500 .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
