#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/21/2222123.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2222123
loop_
_publ_author_name
'Li, Chen-Yu'
'Lin, Chia-Her'
'Ko, Bao-Tsan'
_publ_section_title
Bis[μ-2-(2H-benzotriazol-2-yl)-4-methylphenolato]bis[dimethylaluminium(III)]
_journal_coeditor_code           RK2147
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m670
_journal_paper_doi               10.1107/S1600536809018492
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Al2 (C H3)4 (C13 H10 N3 O)2]'
_chemical_formula_moiety         'C30 H32 Al2 N6 O2'
_chemical_formula_sum            'C30 H32 Al2 N6 O2'
_chemical_formula_weight         562.58
_chemical_name_systematic
;
Bis[μ-2-(2H-benzotriazol-2-yl)-4-
methylphenolato]bis[dimethylaluminium(III)]
;
_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           SHELXL97
_cell_angle_alpha                112.517(2)
_cell_angle_beta                 94.824(3)
_cell_angle_gamma                109.574(2)
_cell_formula_units_Z            1
_cell_length_a                   7.4220(4)
_cell_length_b                   9.7120(5)
_cell_length_c                   11.6331(6)
_cell_measurement_reflns_used    7401
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.48
_cell_volume                     707.79(7)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω'
_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  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11757
_diffrn_reflns_theta_full        28.21
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0385
_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/[σ²(Fo²)+(0.0679P)²+0.1915P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                2923
_reflns_number_total             3405
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            rk2147.cif
_cod_data_source_block           I
_cod_database_code               2222123
_cod_database_fobs_code          2222123
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al Al 0.05537(5) 0.05266(4) 0.89433(3) 0.03495(10) Uani d . 1 . .
O O 0.05448(13) 0.14683(10) 1.06417(8) 0.0383(2) Uani d . 1 . .
N N1 0.16914(16) 0.28879(13) 0.90600(11) 0.0394(2) Uani d . 1 . .
N N2 0.20710(15) 0.42899(12) 1.00733(10) 0.0366(2) Uani d . 1 . .
N N3 0.28396(18) 0.56192(13) 0.98973(12) 0.0457(3) Uani d . 1 . .
C C1 0.10477(17) 0.30216(14) 1.15315(12) 0.0347(3) Uani d . 1 . .
C C2 0.17660(18) 0.44012(14) 1.12950(12) 0.0348(3) Uani d . 1 . .
C C3 0.2281(2) 0.59650(15) 1.22664(13) 0.0420(3) Uani d . 1 . .
H H3B 0.2737 0.6849 1.2076 0.050 Uiso calc R 1 . .
C C4 0.2129(2) 0.62320(16) 1.35011(13) 0.0435(3) Uani d . 1 . .
C C5 0.1424(2) 0.48768(17) 1.37431(13) 0.0432(3) Uani d . 1 . .
H H5A 0.1312 0.5018 1.4567 0.052 Uiso calc R 1 . .
C C6 0.0886(2) 0.33235(16) 1.27846(13) 0.0421(3) Uani d . 1 . .
H H6A 0.0399 0.2447 1.2982 0.051 Uiso calc R 1 . .
C C7 0.22611(19) 0.33415(16) 0.81377(13) 0.0409(3) Uani d . 1 . .
C C8 0.2240(2) 0.2418(2) 0.68526(15) 0.0546(4) Uani d . 1 . .
H H8A 0.1766 0.1290 0.6486 0.065 Uiso calc R 1 . .
C C9 0.2959(2) 0.3281(2) 0.61786(16) 0.0588(4) Uani d . 1 . .
H H9A 0.2961 0.2715 0.5328 0.071 Uiso calc R 1 . .
C C10 0.3694(2) 0.4988(2) 0.67200(16) 0.0566(4) Uani d . 1 . .
H H10A 0.4178 0.5511 0.6219 0.068 Uiso calc R 1 . .
C C11 0.3719(2) 0.5895(2) 0.79461(16) 0.0534(4) Uani d . 1 . .
H H11A 0.4203 0.7023 0.8297 0.064 Uiso calc R 1 . .
C C12 0.29715(19) 0.50377(16) 0.86672(14) 0.0416(3) Uani d . 1 . .
C C13 0.2747(3) 0.7923(2) 1.45629(17) 0.0637(5) Uani d . 1 . .
H H13A 0.3229 0.8706 1.4231 0.096 Uiso calc R 1 . .
H H13B 0.3771 0.8112 1.5237 0.096 Uiso calc R 1 . .
H H13C 0.1635 0.8026 1.4896 0.096 Uiso calc R 1 . .
C C14 -0.1914(2) -0.00914(18) 0.77213(15) 0.0490(3) Uani d . 1 . .
H H14A -0.2766 -0.1197 0.7492 0.073 Uiso calc R 1 . .
H H14B -0.1613 0.0013 0.6964 0.073 Uiso calc R 1 . .
H H14C -0.2562 0.0610 0.8114 0.073 Uiso calc R 1 . .
C C15 0.2981(2) 0.02143(18) 0.86005(16) 0.0501(3) Uani d . 1 . .
H H15A 0.2845 -0.0846 0.8501 0.075 Uiso calc R 1 . .
H H15B 0.4081 0.1025 0.9306 0.075 Uiso calc R 1 . .
H H15C 0.3199 0.0312 0.7828 0.075 Uiso calc R 1 . .
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O Al C15 . . 115.55(6) ?
O Al C14 . . 114.97(6) ?
C15 Al C14 . . 129.44(7) ?
O Al O . 2_557 76.96(4) ?
C15 Al O . 2_557 94.55(6) ?
C14 Al O . 2_557 94.85(5) ?
O Al N1 . . 87.28(4) ?
C15 Al N1 . . 92.11(6) ?
C14 Al N1 . . 91.89(6) ?
O Al N1 2_557 . 164.24(4) ?
C1 O Al . . 134.46(8) ?
C1 O Al . 2_557 122.50(8) ?
Al O Al . 2_557 103.04(4) ?
N2 N1 C7 . . 103.95(11) ?
N2 N1 Al . . 127.89(9) ?
C7 N1 Al . . 128.13(9) ?
N3 N2 N1 . . 115.67(11) ?
N3 N2 C2 . . 120.79(11) ?
N1 N2 C2 . . 123.49(10) ?
N2 N3 C12 . . 103.53(11) ?
O C1 C6 . . 119.56(11) ?
O C1 C2 . . 124.65(11) ?
C6 C1 C2 . . 115.79(11) ?
C3 C2 C1 . . 121.32(12) ?
C3 C2 N2 . . 116.43(11) ?
C1 C2 N2 . . 122.22(11) ?
C4 C3 C2 . . 121.75(13) ?
C4 C3 H3B . . 119.1 ?
C2 C3 H3B . . 119.1 ?
C3 C4 C5 . . 117.29(12) ?
C3 C4 C13 . . 121.89(14) ?
C5 C4 C13 . . 120.80(14) ?
C6 C5 C4 . . 121.39(13) ?
C6 C5 H5A . . 119.3 ?
C4 C5 H5A . . 119.3 ?
C5 C6 C1 . . 122.45(13) ?
C5 C6 H6A . . 118.8 ?
C1 C6 H6A . . 118.8 ?
N1 C7 C12 . . 107.66(12) ?
N1 C7 C8 . . 131.38(13) ?
C12 C7 C8 . . 120.97(13) ?
C9 C8 C7 . . 116.14(15) ?
C9 C8 H8A . . 121.9 ?
C7 C8 H8A . . 121.9 ?
C8 C9 C10 . . 122.70(16) ?
C8 C9 H9A . . 118.7 ?
C10 C9 H9A . . 118.7 ?
C11 C10 C9 . . 122.11(15) ?
C11 C10 H10A . . 118.9 ?
C9 C10 H10A . . 118.9 ?
C10 C11 C12 . . 116.60(15) ?
C10 C11 H11A . . 121.7 ?
C12 C11 H11A . . 121.7 ?
N3 C12 C7 . . 109.19(12) ?
N3 C12 C11 . . 129.32(13) ?
C7 C12 C11 . . 121.48(14) ?
C4 C13 H13A . . 109.5 ?
C4 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C4 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
Al C14 H14A . . 109.5 ?
Al C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
Al C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
Al C15 H15A . . 109.5 ?
Al C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
Al C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Al O . 1.8337(10) ?
Al C15 . 1.9725(15) ?
Al C14 . 1.9767(15) ?
Al O 2_557 2.0918(10) ?
Al N1 . 2.1060(11) ?
O C1 . 1.3595(14) ?
O Al 2_557 2.0918(10) ?
N1 N2 . 1.3344(15) ?
N1 C7 . 1.3556(18) ?
N2 N3 . 1.3277(15) ?
N2 C2 . 1.4268(17) ?
N3 C12 . 1.3483(19) ?
C1 C6 . 1.3967(18) ?
C1 C2 . 1.4084(18) ?
C2 C3 . 1.3978(17) ?
C3 C4 . 1.380(2) ?
C3 H3B . 0.9300 ?
C4 C5 . 1.390(2) ?
C4 C13 . 1.5098(19) ?
C5 C6 . 1.3826(18) ?
C5 H5A . 0.9300 ?
C6 H6A . 0.9300 ?
C7 C12 . 1.3991(19) ?
C7 C8 . 1.414(2) ?
C8 C9 . 1.370(2) ?
C8 H8A . 0.9300 ?
C9 C10 . 1.407(2) ?
C9 H9A . 0.9300 ?
C10 C11 . 1.354(2) ?
C10 H10A . 0.9300 ?
C11 C12 . 1.417(2) ?
C11 H11A . 0.9300 ?
C13 H13A . 0.9600 ?
C13 H13B . 0.9600 ?
C13 H13C . 0.9600 ?
C14 H14A . 0.9600 ?
C14 H14B . 0.9600 ?
C14 H14C . 0.9600 ?
C15 H15A . 0.9600 ?
C15 H15B . 0.9600 ?
C15 H15C . 0.9600 ?
