#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:11:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179743 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/39/7003984.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_7003984
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            'C45 H41 Al N P'
_chemical_formula_weight         653.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.741(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8623(11)
_cell_length_b                   19.289(2)
_cell_length_c                   19.463(2)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3689.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35173
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.482415
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.156
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0471
_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)+(0.0791P)²+0.6720P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1409
_reflns_number_gt                4729
_reflns_number_total             6494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801772g.txt
_cod_data_source_block           (2-C6H4-Ph)2NAlMe2(CH2PPh3)
_cod_original_cell_volume        3689.7(7)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7003984
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 -0.22559(7) 0.67491(3) 0.41456(3) 0.05426(19) Uani 1 1 d . . .
P1 P 0.05403(5) 0.62467(3) 0.33517(3) 0.04937(17) Uani 1 1 d . . .
N1 N -0.27882(17) 0.76942(9) 0.41571(9) 0.0521(4) Uani 1 1 d . . .
C1 C -0.1819(2) 0.82266(11) 0.42884(11) 0.0539(5) Uani 1 1 d . . .
C2 C -0.1864(2) 0.88524(12) 0.39129(12) 0.0585(6) Uani 1 1 d . . .
C3 C -0.0886(3) 0.93591(13) 0.40961(14) 0.0740(7) Uani 1 1 d . . .
H3A H -0.0948 0.9785 0.3872 0.089 Uiso 1 1 calc R . .
C4 C 0.0161(3) 0.92525(16) 0.45928(16) 0.0806(8) Uani 1 1 d . . .
H4A H 0.0806 0.9597 0.4697 0.097 Uiso 1 1 calc R . .
C5 C 0.0242(3) 0.86341(16) 0.49325(15) 0.0763(7) Uani 1 1 d . . .
H5A H 0.0963 0.8547 0.5260 0.092 Uiso 1 1 calc R . .
C6 C -0.0745(2) 0.81378(13) 0.47905(13) 0.0663(6) Uani 1 1 d . . .
H6A H -0.0691 0.7726 0.5041 0.080 Uiso 1 1 calc R . .
C7 C -0.2825(3) 0.89853(12) 0.32939(12) 0.0636(6) Uani 1 1 d . . .
C8 C -0.3847(3) 0.94763(14) 0.32864(14) 0.0772(7) Uani 1 1 d . . .
H8A H -0.3980 0.9716 0.3690 0.093 Uiso 1 1 calc R . .
C9 C -0.4677(3) 0.96207(16) 0.26950(16) 0.0914(9) Uani 1 1 d . . .
H9A H -0.5368 0.9947 0.2706 0.110 Uiso 1 1 calc R . .
C10 C -0.4478(4) 0.92836(18) 0.20994(17) 0.1047(11) Uani 1 1 d . . .
H10A H -0.5027 0.9382 0.1699 0.126 Uiso 1 1 calc R . .
C11 C -0.3472(4) 0.8800(2) 0.20898(16) 0.1099(12) Uani 1 1 d . . .
H11A H -0.3331 0.8573 0.1680 0.132 Uiso 1 1 calc R . .
C12 C -0.2657(4) 0.86434(16) 0.26825(14) 0.0901(9) Uani 1 1 d . . .
H12A H -0.1989 0.8304 0.2669 0.108 Uiso 1 1 calc R . .
C13 C -0.4162(2) 0.79176(11) 0.40659(11) 0.0517(5) Uani 1 1 d . . .
C14 C -0.4738(2) 0.83344(11) 0.45612(12) 0.0548(5) Uani 1 1 d . . .
C15 C -0.6066(2) 0.85787(13) 0.44272(14) 0.0672(6) Uani 1 1 d . . .
H15A H -0.6433 0.8869 0.4745 0.081 Uiso 1 1 calc R . .
C16 C -0.6839(3) 0.83986(15) 0.38357(16) 0.0772(7) Uani 1 1 d . . .
H16A H -0.7724 0.8564 0.3755 0.093 Uiso 1 1 calc R . .
C17 C -0.6299(3) 0.79727(14) 0.33631(15) 0.0729(7) Uani 1 1 d . . .
H17A H -0.6826 0.7842 0.2966 0.087 Uiso 1 1 calc R . .
C18 C -0.4980(2) 0.77375(12) 0.34738(13) 0.0630(6) Uani 1 1 d . . .
H18A H -0.4628 0.7453 0.3147 0.076 Uiso 1 1 calc R . .
C19 C -0.3996(2) 0.85103(12) 0.52383(12) 0.0572(5) Uani 1 1 d . . .
C20 C -0.3759(3) 0.91933(14) 0.54369(14) 0.0746(7) Uani 1 1 d . . .
H20A H -0.4025 0.9549 0.5132 0.089 Uiso 1 1 calc R . .
C21 C -0.3136(3) 0.93560(16) 0.60774(16) 0.0878(8) Uani 1 1 d . . .
H21A H -0.2972 0.9817 0.6197 0.105 Uiso 1 1 calc R . .
C22 C -0.2760(3) 0.88400(18) 0.65356(15) 0.0861(8) Uani 1 1 d . . .
H22A H -0.2356 0.8949 0.6971 0.103 Uiso 1 1 calc R . .
C23 C -0.2981(3) 0.81652(16) 0.63516(14) 0.0800(8) Uani 1 1 d . . .
H23A H -0.2723 0.7814 0.6663 0.096 Uiso 1 1 calc R . .
C24 C -0.3587(2) 0.79981(14) 0.57058(13) 0.0670(6) Uani 1 1 d . . .
H24A H -0.3720 0.7535 0.5585 0.080 Uiso 1 1 calc R . .
C25 C -0.1594(3) 0.63733(14) 0.50704(13) 0.0789(8) Uani 1 1 d . . .
H25A H -0.2342 0.6341 0.5355 0.118 Uiso 1 1 calc R . .
H25B H -0.0913 0.6677 0.5284 0.118 Uiso 1 1 calc R . .
H25C H -0.1211 0.5921 0.5017 0.118 Uiso 1 1 calc R . .
C26 C -0.3700(3) 0.61481(14) 0.36995(16) 0.0788(7) Uani 1 1 d . . .
H26A H -0.4416 0.6095 0.4001 0.118 Uiso 1 1 calc R . .
H26B H -0.3325 0.5702 0.3607 0.118 Uiso 1 1 calc R . .
H26C H -0.4058 0.6356 0.3274 0.118 Uiso 1 1 calc R . .
C27 C -0.0745(2) 0.68453(11) 0.34782(12) 0.0566(5) Uani 1 1 d . . .
H27A H -0.1214 0.6921 0.3027 0.068 Uiso 1 1 calc R . .
H27B H -0.0282 0.7276 0.3603 0.068 Uiso 1 1 calc R . .
C28 C -0.0161(2) 0.53998(11) 0.31885(11) 0.0536(5) Uani 1 1 d . . .
C29 C -0.0735(3) 0.50412(13) 0.37104(14) 0.0759(7) Uani 1 1 d . . .
H29A H -0.0729 0.5236 0.4148 0.091 Uiso 1 1 calc R . .
C30 C -0.1313(3) 0.43994(15) 0.35860(17) 0.0894(9) Uani 1 1 d . . .
H30A H -0.1685 0.4160 0.3940 0.107 Uiso 1 1 calc R . .
C31 C -0.1343(3) 0.41155(15) 0.29471(18) 0.0955(10) Uani 1 1 d . . .
H31A H -0.1752 0.3686 0.2861 0.115 Uiso 1 1 calc R . .
C32 C -0.0776(4) 0.44575(17) 0.24342(17) 0.1105(12) Uani 1 1 d . . .
H32A H -0.0791 0.4259 0.1998 0.133 Uiso 1 1 calc R . .
C33 C -0.0176(3) 0.50968(14) 0.25525(14) 0.0839(8) Uani 1 1 d . . .
H33A H 0.0221 0.5323 0.2198 0.101 Uiso 1 1 calc R . .
C34 C 0.1756(2) 0.61889(12) 0.40904(11) 0.0550(5) Uani 1 1 d . . .
C35 C 0.2162(3) 0.67910(15) 0.44356(13) 0.0725(7) Uani 1 1 d . . .
H35A H 0.1749 0.7211 0.4311 0.087 Uiso 1 1 calc R . .
C36 C 0.3181(3) 0.6767(2) 0.49646(15) 0.0929(9) Uani 1 1 d . . .
H36A H 0.3463 0.7172 0.5193 0.111 Uiso 1 1 calc R . .
C37 C 0.3778(3) 0.6149(2) 0.51547(16) 0.1016(11) Uani 1 1 d . . .
H37A H 0.4471 0.6138 0.5509 0.122 Uiso 1 1 calc R . .
C38 C 0.3361(3) 0.5541(2) 0.48274(18) 0.0976(10) Uani 1 1 d . . .
H38A H 0.3750 0.5120 0.4969 0.117 Uiso 1 1 calc R . .
C39 C 0.2367(3) 0.55646(15) 0.42894(14) 0.0756(7) Uani 1 1 d . . .
H39A H 0.2101 0.5159 0.4057 0.091 Uiso 1 1 calc R . .
C40 C 0.1500(2) 0.64821(11) 0.26299(11) 0.0530(5) Uani 1 1 d . . .
C41 C 0.2773(3) 0.62048(14) 0.25663(14) 0.0747(7) Uani 1 1 d . . .
H41A H 0.3137 0.5886 0.2889 0.090 Uiso 1 1 calc R . .
C42 C 0.3506(3) 0.63992(18) 0.20246(16) 0.0924(9) Uani 1 1 d . . .
H42A H 0.4368 0.6214 0.1987 0.111 Uiso 1 1 calc R . .
C43 C 0.2976(3) 0.68612(17) 0.15433(15) 0.0867(9) Uani 1 1 d . . .
H43A H 0.3471 0.6985 0.1176 0.104 Uiso 1 1 calc R . .
C44 C 0.1714(3) 0.71438(16) 0.16011(13) 0.0827(8) Uani 1 1 d . . .
H44A H 0.1356 0.7463 0.1277 0.099 Uiso 1 1 calc R . .
C45 C 0.0980(3) 0.69507(14) 0.21438(12) 0.0679(6) Uani 1 1 d . . .
H45A H 0.0121 0.7140 0.2182 0.082 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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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 C26 112.20(10) . . ?
N1 Al1 C25 114.06(10) . . ?
C26 Al1 C25 110.60(13) . . ?
N1 Al1 C27 97.80(8) . . ?
C26 Al1 C27 107.88(11) . . ?
C25 Al1 C27 113.60(11) . . ?
C27 P1 C28 110.69(10) . . ?
C27 P1 C34 111.84(11) . . ?
C28 P1 C34 107.91(10) . . ?
C27 P1 C40 111.99(11) . . ?
C28 P1 C40 108.02(10) . . ?
C34 P1 C40 106.17(10) . . ?
C1 N1 C13 115.27(17) . . ?
C1 N1 Al1 121.14(14) . . ?
C13 N1 Al1 123.54(14) . . ?
C6 C1 C2 117.3(2) . . ?
C6 C1 N1 120.2(2) . . ?
C2 C1 N1 122.5(2) . . ?
C3 C2 C1 118.3(2) . . ?
C3 C2 C7 117.7(2) . . ?
C1 C2 C7 123.8(2) . . ?
C4 C3 C2 122.6(3) . . ?
C5 C4 C3 119.0(3) . . ?
C4 C5 C6 119.9(3) . . ?
C5 C6 C1 122.7(3) . . ?
C8 C7 C12 117.2(3) . . ?
C8 C7 C2 122.7(2) . . ?
C12 C7 C2 120.0(2) . . ?
C7 C8 C9 121.8(3) . . ?
C10 C9 C8 119.8(3) . . ?
C9 C10 C11 119.7(3) . . ?
C10 C11 C12 120.8(3) . . ?
C7 C12 C11 120.7(3) . . ?
C18 C13 C14 117.9(2) . . ?
C18 C13 N1 120.6(2) . . ?
C14 C13 N1 121.46(19) . . ?
C15 C14 C13 119.3(2) . . ?
C15 C14 C19 118.2(2) . . ?
C13 C14 C19 122.53(19) . . ?
C16 C15 C14 121.3(2) . . ?
C15 C16 C17 119.6(2) . . ?
C16 C17 C18 120.4(2) . . ?
C17 C18 C13 121.4(2) . . ?
C24 C19 C20 117.5(2) . . ?
C24 C19 C14 121.0(2) . . ?
C20 C19 C14 121.4(2) . . ?
C21 C20 C19 121.3(3) . . ?
C22 C21 C20 120.0(3) . . ?
C23 C22 C21 119.7(3) . . ?
C22 C23 C24 120.6(3) . . ?
C19 C24 C23 120.8(3) . . ?
P1 C27 Al1 126.80(12) . . ?
C33 C28 C29 118.4(2) . . ?
C33 C28 P1 121.65(18) . . ?
C29 C28 P1 119.97(18) . . ?
C30 C29 C28 120.5(3) . . ?
C31 C30 C29 120.1(3) . . ?
C32 C31 C30 120.0(3) . . ?
C31 C32 C33 120.7(3) . . ?
C28 C33 C32 120.4(3) . . ?
C35 C34 C39 119.4(2) . . ?
C35 C34 P1 118.91(19) . . ?
C39 C34 P1 121.50(19) . . ?
C36 C35 C34 119.9(3) . . ?
C37 C36 C35 120.2(3) . . ?
C36 C37 C38 120.7(3) . . ?
C39 C38 C37 119.3(3) . . ?
C38 C39 C34 120.5(3) . . ?
C45 C40 C41 118.9(2) . . ?
C45 C40 P1 120.50(17) . . ?
C41 C40 P1 120.60(18) . . ?
C42 C41 C40 120.1(3) . . ?
C43 C42 C41 120.4(3) . . ?
C42 C43 C44 120.1(3) . . ?
C43 C44 C45 119.5(3) . . ?
C40 C45 C44 120.9(2) . . ?
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 1.8977(18) . ?
Al1 C26 1.980(3) . ?
Al1 C25 1.999(3) . ?
Al1 C27 2.064(2) . ?
P1 C27 1.747(2) . ?
P1 C28 1.792(2) . ?
P1 C34 1.798(2) . ?
P1 C40 1.815(2) . ?
N1 C1 1.412(3) . ?
N1 C13 1.419(3) . ?
C1 C6 1.391(3) . ?
C1 C2 1.410(3) . ?
C2 C3 1.399(3) . ?
C2 C7 1.492(3) . ?
C3 C4 1.370(4) . ?
C4 C5 1.363(4) . ?
C5 C6 1.377(3) . ?
C7 C8 1.382(4) . ?
C7 C12 1.382(4) . ?
C8 C9 1.385(4) . ?
C9 C10 1.357(4) . ?
C10 C11 1.363(5) . ?
C11 C12 1.384(4) . ?
C13 C18 1.395(3) . ?
C13 C14 1.410(3) . ?
C14 C15 1.396(3) . ?
C14 C19 1.492(3) . ?
C15 C16 1.372(4) . ?
C16 C17 1.373(4) . ?
C17 C18 1.377(3) . ?
C19 C24 1.381(3) . ?
C19 C20 1.387(3) . ?
C20 C21 1.379(4) . ?
C21 C22 1.367(4) . ?
C22 C23 1.363(4) . ?
C23 C24 1.385(4) . ?
C28 C33 1.368(3) . ?
C28 C29 1.388(3) . ?
C29 C30 1.376(4) . ?
C30 C31 1.357(4) . ?
C31 C32 1.355(4) . ?
C32 C33 1.379(4) . ?
C34 C35 1.384(3) . ?
C34 C39 1.387(3) . ?
C35 C36 1.378(4) . ?
C36 C37 1.367(5) . ?
C37 C38 1.380(5) . ?
C38 C39 1.375(4) . ?
C40 C45 1.377(3) . ?
C40 C41 1.379(3) . ?
C41 C42 1.379(4) . ?
C42 C43 1.365(4) . ?
C43 C44 1.372(4) . ?
C44 C45 1.380(3) . ?
