#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:45:19 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179934 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/29/7022922.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_7022922
loop_
_publ_author_name
'Han, Hong-Ling'
'Liu, Yan'
'Liu, Jing-Yu'
'Nomura, Kotohiro'
'Li, Yue-Sheng'
_publ_section_title
;
 Synthesis of binuclear phenoxyimino organoaluminum complexes and their
 use as the catalyst precursors for efficient ring-opening polymerisation
 of ε-caprolactone.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12346
_journal_page_last               12353
_journal_paper_doi               10.1039/c3dt50264c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C27 H40 Al2 Cl2 N2 O2'
_chemical_formula_weight         549.47
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 121.377(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.697(2)
_cell_length_b                   12.5736(14)
_cell_length_c                   16.2599(19)
_cell_measurement_temperature    185(2)
_cell_volume                     3089.0(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8379
_diffrn_reflns_theta_full        26.22
_diffrn_reflns_theta_max         26.22
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_T_max  0.9466
_exptl_absorpt_correction_T_min  0.9124
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0421
_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)+(0.0418P)²+2.7273P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1087
_reflns_number_gt                2278
_reflns_number_total             3100
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50264c.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7022922
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Al1 Al 0.24083(4) 0.47765(5) 0.14203(4) 0.03071(17) Uani 1 1 d .
C2 C 0.15614(15) 0.5855(2) 0.05759(17) 0.0517(6) Uani 1 1 d .
H2A H 0.1440 0.6348 0.0960 0.078 Uiso 1 1 calc R
H2B H 0.1010 0.5508 0.0094 0.078 Uiso 1 1 calc R
H2C H 0.1810 0.6248 0.0251 0.078 Uiso 1 1 calc R
C1 C 0.23369(17) 0.33202(19) 0.0965(2) 0.0564(7) Uani 1 1 d .
H1A H 0.2652 0.3271 0.0618 0.085 Uiso 1 1 calc R
H1B H 0.1715 0.3125 0.0532 0.085 Uiso 1 1 calc R
H1C H 0.2608 0.2834 0.1517 0.085 Uiso 1 1 calc R
O1 O 0.35082(8) 0.52368(11) 0.18861(9) 0.0328(3) Uani 1 1 d .
N1 N 0.24532(10) 0.48324(12) 0.26561(12) 0.0285(4) Uani 1 1 d .
C10 C 0.17271(13) 0.43845(17) 0.27850(16) 0.0394(5) Uani 1 1 d .
C13 C 0.14842(16) 0.5155(2) 0.3330(2) 0.0649(8) Uani 1 1 d .
H13A H 0.1977 0.5209 0.3999 0.097 Uiso 1 1 calc R
H13B H 0.0956 0.4896 0.3318 0.097 Uiso 1 1 calc R
H13C H 0.1363 0.5857 0.3025 0.097 Uiso 1 1 calc R
C12 C 0.09082(16) 0.4216(3) 0.1792(2) 0.0700(9) Uani 1 1 d .
H12A H 0.0693 0.4904 0.1471 0.105 Uiso 1 1 calc R
H12B H 0.0446 0.3871 0.1858 0.105 Uiso 1 1 calc R
H12C H 0.1059 0.3762 0.1407 0.105 Uiso 1 1 calc R
C11 C 0.2050(2) 0.3334(2) 0.3297(3) 0.0926(12) Uani 1 1 d .
H11A H 0.2226 0.2876 0.2938 0.139 Uiso 1 1 calc R
H11B H 0.1575 0.2990 0.3339 0.139 Uiso 1 1 calc R
H11C H 0.2560 0.3454 0.3947 0.139 Uiso 1 1 calc R
C9 C 0.31197(12) 0.52645(15) 0.34036(14) 0.0298(4) Uani 1 1 d .
H9 H 0.3084 0.5302 0.3966 0.036 Uiso 1 1 calc R
C4 C 0.49000(12) 0.60636(14) 0.28932(14) 0.0261(4) Uani 1 1 d .
C3 C 0.40854(12) 0.56623(14) 0.27289(14) 0.0256(4) Uani 1 1 d .
C7 C 0.45346(12) 0.61413(15) 0.43761(14) 0.0314(4) Uani 1 1 d .
H7 H 0.4409 0.6172 0.4877 0.038 Uiso 1 1 calc R
C5 C 0.54991(12) 0.64776(15) 0.37940(15) 0.0315(4) Uani 1 1 d .
H5 H 0.6052 0.6734 0.3911 0.038 Uiso 1 1 calc R
C8 C 0.39134(12) 0.56974(14) 0.34840(14) 0.0268(4) Uani 1 1 d .
C6 C 0.53231(13) 0.65322(16) 0.45316(15) 0.0339(5) Uani 1 1 d .
H6 H 0.5743 0.6836 0.5136 0.041 Uiso 1 1 calc R
Cl1 Cl 0.51135(7) 0.74701(7) 0.66827(6) 0.0952(3) Uani 1 1 d .
C14 C 0.5000 0.6710(3) 0.7500 0.0582(10) Uani 1 2 d S
H14A H 0.5526 0.6246 0.7856 0.070 Uiso 0.50 1 calc PR
H14B H 0.4474 0.6246 0.7144 0.070 Uiso 0.50 1 calc PR
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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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 107.87(9) . .
O1 Al1 C2 110.01(9) . .
C1 Al1 C2 120.57(12) . .
O1 Al1 N1 95.74(6) . .
C1 Al1 N1 112.34(10) . .
C2 Al1 N1 107.47(9) . .
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 . .
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 . .
C3 O1 Al1 131.03(12) . .
C9 N1 C10 116.80(17) . .
C9 N1 Al1 120.42(13) . .
C10 N1 Al1 122.78(13) . .
C11 C10 N1 107.30(17) . .
C11 C10 C13 112.2(2) . .
N1 C10 C13 111.23(17) . .
C11 C10 C12 110.0(2) . .
N1 C10 C12 108.24(18) . .
C13 C10 C12 107.8(2) . .
C10 C13 H13A 109.5 . .
C10 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C10 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N1 C9 C8 127.62(18) . .
N1 C9 H9 116.2 . .
C8 C9 H9 116.2 . .
C5 C4 C3 118.48(17) . .
C5 C4 C4 120.82(18) . 2_655
C3 C4 C4 120.69(19) . 2_655
O1 C3 C8 120.93(16) . .
O1 C3 C4 120.06(16) . .
C8 C3 C4 118.98(17) . .
C6 C7 C8 120.50(18) . .
C6 C7 H7 119.7 . .
C8 C7 H7 119.7 . .
C4 C5 C6 122.58(17) . .
C4 C5 H5 118.7 . .
C6 C5 H5 118.7 . .
C7 C8 C3 120.31(16) . .
C7 C8 C9 116.40(17) . .
C3 C8 C9 123.27(17) . .
C7 C6 C5 119.12(18) . .
C7 C6 H6 120.4 . .
C5 C6 H6 120.4 . .
Cl1 C14 Cl1 113.0(2) . 2_656
Cl1 C14 H14A 109.0 . .
Cl1 C14 H14A 109.0 2_656 .
Cl1 C14 H14B 109.0 . .
Cl1 C14 H14B 109.0 2_656 .
H14A C14 H14B 107.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 O1 1.7782(13) .
Al1 C1 1.954(2) .
Al1 C2 1.956(2) .
Al1 N1 1.9706(17) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
O1 C3 1.323(2) .
N1 C9 1.293(2) .
N1 C10 1.514(2) .
C10 C11 1.506(3) .
C10 C13 1.518(3) .
C10 C12 1.522(3) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C9 C8 1.448(2) .
C9 H9 0.9500 .
C4 C5 1.387(3) .
C4 C3 1.415(2) .
C4 C4 1.494(4) 2_655
C3 C8 1.411(3) .
C7 C6 1.373(3) .
C7 C8 1.401(3) .
C7 H7 0.9500 .
C5 C6 1.389(3) .
C5 H5 0.9500 .
C6 H6 0.9500 .
Cl1 C14 1.731(2) .
C14 Cl1 1.731(2) 2_656
C14 H14A 0.9900 .
C14 H14B 0.9900 .
