#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:11:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179743 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/39/7003983.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_7003983
loop_
_publ_author_name
'Dureen, Meghan A.'
'Stephan, Douglas W.'
_publ_section_title
;
 Biphenylamide ligand complexes of Li and Al: hemilabile arene donors?
;
_journal_issue                   35
_journal_name_full               'Dalton Transactions'
_journal_page_first              4723
_journal_page_last               4731
_journal_paper_doi               10.1039/b801772g
_journal_year                    2008
_chemical_formula_sum            'C30 H32 Al N O'
_chemical_formula_weight         449.55
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.730(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6605(15)
_cell_length_b                   30.207(5)
_cell_length_c                   10.2180(18)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     2596.7(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24804
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.481298
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0569
_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)+(0.0871P)²+0.2828P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1666
_reflns_number_gt                2847
_reflns_number_total             4561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801772g.txt
_cod_data_source_block           (2-C6H4-Ph)2NAlMe2(THF)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7003983
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.71790(10) 0.06732(3) 0.16700(9) 0.0649(3) Uani 1 1 d . . .
N1 N 0.8277(3) 0.11222(6) 0.2739(2) 0.0574(5) Uani 1 1 d . . .
O1 O 0.5308(2) 0.09424(6) 0.05522(18) 0.0724(5) Uani 1 1 d . . .
C15 C 0.8468(3) 0.11486(9) 0.4163(3) 0.0574(7) Uani 1 1 d . . .
C16 C 0.8265(3) 0.15432(9) 0.4823(3) 0.0574(7) Uani 1 1 d . . .
C21 C 0.7799(3) 0.19681(9) 0.4077(2) 0.0572(6) Uani 1 1 d . . .
C3 C 0.9056(3) 0.14567(8) 0.2136(3) 0.0588(7) Uani 1 1 d . . .
C4 C 1.0670(3) 0.15641(9) 0.2622(3) 0.0648(7) Uani 1 1 d . . .
C20 C 0.8819(3) 0.07647(10) 0.4944(3) 0.0708(8) Uani 1 1 d . . .
H20A H 0.8966 0.0499 0.4528 0.085 Uiso 1 1 calc R . .
C9 C 1.1799(3) 0.13155(10) 0.3693(3) 0.0683(8) Uani 1 1 d . . .
C26 C 0.6253(3) 0.20281(9) 0.3332(3) 0.0634(7) Uani 1 1 d . . .
H26A H 0.5512 0.1803 0.3301 0.076 Uiso 1 1 calc R . .
C17 C 0.8442(3) 0.15420(11) 0.6215(3) 0.0720(8) Uani 1 1 d . . .
H17A H 0.8334 0.1807 0.6651 0.086 Uiso 1 1 calc R . .
C8 C 0.8191(4) 0.16818(9) 0.1010(3) 0.0702(8) Uani 1 1 d . . .
H8A H 0.7130 0.1608 0.0664 0.084 Uiso 1 1 calc R . .
C22 C 0.8866(3) 0.23099(9) 0.4124(3) 0.0674(7) Uani 1 1 d . . .
H22A H 0.9904 0.2278 0.4631 0.081 Uiso 1 1 calc R . .
C5 C 1.1294(4) 0.19114(9) 0.2006(3) 0.0761(8) Uani 1 1 d . . .
H5A H 1.2347 0.1994 0.2351 0.091 Uiso 1 1 calc R . .
C25 C 0.5799(4) 0.24150(10) 0.2639(3) 0.0718(8) Uani 1 1 d . . .
H25A H 0.4759 0.2449 0.2139 0.086 Uiso 1 1 calc R . .
C7 C 0.8867(4) 0.20123(10) 0.0391(3) 0.0813(9) Uani 1 1 d . . .
H7A H 0.8273 0.2151 -0.0377 0.098 Uiso 1 1 calc R . .
C24 C 0.6879(4) 0.27512(10) 0.2683(3) 0.0773(8) Uani 1 1 d . . .
H24A H 0.6576 0.3013 0.2211 0.093 Uiso 1 1 calc R . .
C19 C 0.8953(4) 0.07706(12) 0.6323(3) 0.0820(9) Uani 1 1 d . . .
H19A H 0.9166 0.0510 0.6818 0.098 Uiso 1 1 calc R . .
C23 C 0.8411(4) 0.26984(10) 0.3430(3) 0.0794(9) Uani 1 1 d . . .
H23A H 0.9145 0.2926 0.3468 0.095 Uiso 1 1 calc R . .
C18 C 0.8772(4) 0.11610(13) 0.6959(3) 0.0842(10) Uani 1 1 d . . .
H18A H 0.8872 0.1167 0.7886 0.101 Uiso 1 1 calc R . .
C10 C 1.1897(4) 0.08579(11) 0.3642(3) 0.0782(9) Uani 1 1 d . . .
H10A H 1.1158 0.0702 0.2998 0.094 Uiso 1 1 calc R . .
C1 C 0.6200(4) 0.02368(10) 0.2637(3) 0.0956(11) Uani 1 1 d . . .
H1A H 0.5695 0.0386 0.3253 0.143 Uiso 1 1 calc R . .
H1B H 0.7003 0.0041 0.3129 0.143 Uiso 1 1 calc R . .
H1C H 0.5422 0.0069 0.2004 0.143 Uiso 1 1 calc R . .
C6 C 1.0420(5) 0.21354(11) 0.0914(4) 0.0875(10) Uani 1 1 d . . .
H6A H 1.0869 0.2367 0.0532 0.105 Uiso 1 1 calc R . .
C11 C 1.3080(5) 0.06319(13) 0.4537(4) 0.0946(11) Uani 1 1 d . . .
H11A H 1.3129 0.0325 0.4486 0.113 Uiso 1 1 calc R . .
C2 C 0.8307(4) 0.04551(11) 0.0345(3) 0.0910(10) Uani 1 1 d . . .
H2A H 0.8729 0.0701 -0.0052 0.136 Uiso 1 1 calc R . .
H2B H 0.7582 0.0293 -0.0346 0.136 Uiso 1 1 calc R . .
H2C H 0.9160 0.0265 0.0784 0.136 Uiso 1 1 calc R . .
C28 C 0.3000(4) 0.09617(16) -0.1191(4) 0.1139(13) Uani 1 1 d . . .
H28A H 0.2731 0.1222 -0.1756 0.137 Uiso 1 1 calc R . .
H28B H 0.2440 0.0709 -0.1665 0.137 Uiso 1 1 calc R . .
C27 C 0.4735(4) 0.08843(16) -0.0870(3) 0.1140(13) Uani 1 1 d . . .
H27A H 0.4961 0.0587 -0.1128 0.137 Uiso 1 1 calc R . .
H27B H 0.5246 0.1093 -0.1352 0.137 Uiso 1 1 calc R . .
C14 C 1.2897(4) 0.15337(12) 0.4687(3) 0.0854(9) Uani 1 1 d . . .
H14A H 1.2837 0.1840 0.4762 0.102 Uiso 1 1 calc R . .
C30 C 0.4005(4) 0.11176(15) 0.1082(4) 0.1083(13) Uani 1 1 d . . .
H30A H 0.3980 0.0974 0.1926 0.130 Uiso 1 1 calc R . .
H30B H 0.4131 0.1434 0.1237 0.130 Uiso 1 1 calc R . .
C13 C 1.4094(4) 0.13020(18) 0.5579(4) 0.1060(13) Uani 1 1 d . . .
H13A H 1.4835 0.1454 0.6232 0.127 Uiso 1 1 calc R . .
C29 C 0.2565(5) 0.10260(18) 0.0074(5) 0.1335(16) Uani 1 1 d . . .
H29A H 0.1829 0.1272 0.0007 0.160 Uiso 1 1 calc R . .
H29B H 0.2056 0.0762 0.0313 0.160 Uiso 1 1 calc R . .
C12 C 1.4179(5) 0.0852(2) 0.5496(4) 0.1100(14) Uani 1 1 d . . .
H12A H 1.4978 0.0696 0.6086 0.132 Uiso 1 1 calc R . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Al1 O1 106.37(9) . . ?
N1 Al1 C1 114.70(13) . . ?
O1 Al1 C1 100.34(14) . . ?
N1 Al1 C2 112.48(13) . . ?
O1 Al1 C2 102.64(12) . . ?
C1 Al1 C2 117.93(15) . . ?
C15 N1 C3 116.5(2) . . ?
C15 N1 Al1 124.09(16) . . ?
C3 N1 Al1 119.33(17) . . ?
C27 O1 C30 108.0(2) . . ?
C27 O1 Al1 126.2(2) . . ?
C30 O1 Al1 123.2(2) . . ?
C20 C15 C16 117.8(2) . . ?
C20 C15 N1 119.5(2) . . ?
C16 C15 N1 122.7(2) . . ?
C17 C16 C15 119.5(3) . . ?
C17 C16 C21 118.2(2) . . ?
C15 C16 C21 122.3(2) . . ?
C22 C21 C26 118.3(3) . . ?
C22 C21 C16 121.8(2) . . ?
C26 C21 C16 120.0(2) . . ?
C8 C3 C4 118.3(2) . . ?
C8 C3 N1 118.9(2) . . ?
C4 C3 N1 122.8(2) . . ?
C5 C4 C3 118.2(3) . . ?
C5 C4 C9 117.0(3) . . ?
C3 C4 C9 124.6(2) . . ?
C19 C20 C15 121.5(3) . . ?
C14 C9 C10 117.7(3) . . ?
C14 C9 C4 121.2(3) . . ?
C10 C9 C4 120.8(3) . . ?
C25 C26 C21 121.0(3) . . ?
C18 C17 C16 121.7(3) . . ?
C7 C8 C3 121.8(3) . . ?
C21 C22 C23 120.8(3) . . ?
C6 C5 C4 122.7(3) . . ?
C24 C25 C26 120.1(3) . . ?
C6 C7 C8 119.9(3) . . ?
C23 C24 C25 119.5(3) . . ?
C18 C19 C20 120.0(3) . . ?
C24 C23 C22 120.3(3) . . ?
C17 C18 C19 119.4(3) . . ?
C11 C10 C9 120.7(3) . . ?
C5 C6 C7 118.9(3) . . ?
C12 C11 C10 121.1(4) . . ?
C29 C28 C27 106.9(3) . . ?
O1 C27 C28 107.2(3) . . ?
C9 C14 C13 121.0(4) . . ?
C29 C30 O1 106.2(3) . . ?
C12 C13 C14 120.1(4) . . ?
C30 C29 C28 107.4(3) . . ?
C11 C12 C13 119.3(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 N1 1.856(2) . ?
Al1 O1 1.927(2) . ?
Al1 C1 1.957(3) . ?
Al1 C2 1.962(3) . ?
N1 C15 1.427(3) . ?
N1 C3 1.433(3) . ?
O1 C27 1.430(4) . ?
O1 C30 1.461(4) . ?
C15 C20 1.399(4) . ?
C15 C16 1.401(4) . ?
C16 C17 1.395(4) . ?
C16 C21 1.498(4) . ?
C21 C22 1.379(4) . ?
C21 C26 1.386(4) . ?
C3 C8 1.393(4) . ?
C3 C4 1.405(4) . ?
C4 C5 1.397(4) . ?
C4 C9 1.487(4) . ?
C20 C19 1.387(4) . ?
C9 C14 1.383(4) . ?
C9 C10 1.387(4) . ?
C26 C25 1.375(4) . ?
C17 C18 1.372(4) . ?
C8 C7 1.384(4) . ?
C22 C23 1.379(4) . ?
C5 C6 1.369(4) . ?
C25 C24 1.374(4) . ?
C7 C6 1.375(5) . ?
C24 C23 1.374(4) . ?
C19 C18 1.373(5) . ?
C10 C11 1.381(4) . ?
C11 C12 1.365(6) . ?
C28 C29 1.443(6) . ?
C28 C27 1.479(5) . ?
C14 C13 1.395(5) . ?
C30 C29 1.443(5) . ?
C13 C12 1.366(6) . ?
