#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:32:45 +0100 (vie 25 de mar de 2016) $
#$Revision: 179753 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/49/7004981.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_7004981
loop_
_publ_author_name
'Hitchcock, Peter B.'
'Lappert, Michael F.'
'Merle, Philippe G.'
_publ_section_title
;
 Synthesis and structures of selected benzamidinates of Li, Na, Al, Zr
 and Sn(II) using the C1-symmetric ligands [N(SiMe3)C(C6H4Me-4 or
 Ph)NPh]-.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              585
_journal_page_last               594
_journal_paper_doi               10.1039/b614351b
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C34.52 H43.56 Al Cl0.48 N4 Si2'
_chemical_formula_sum            'C34.52 H43.56 Al Cl0.48 N4 Si2'
_chemical_formula_weight         615.12
_chemical_name_common            '[Al{Me3SiNC(PhMe)NPh}2(Cl/Me)]'
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             1999-10-22T16:38:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                105.102(1)
_cell_angle_beta                 101.050(1)
_cell_angle_gamma                93.509(1)
_cell_formula_units_Z            2
_cell_length_a                   10.2505(3)
_cell_length_b                   12.4069(3)
_cell_length_c                   14.8217(3)
_cell_measurement_reflns_used    12633
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      4.246
_cell_measurement_wavelength     0.71073
_cell_volume                     1773.81(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22571
_diffrn_reflns_theta_full        27.92
_diffrn_reflns_theta_max         27.92
_diffrn_reflns_theta_min         4.35
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         8390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0527P)²+0.6867P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.117
_reflns_number_gt                6914
_reflns_number_total             8390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b614351b.txt
_cod_data_source_block           (3)-oct2499
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004981
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al Al 0.28006(4) 0.82155(3) 0.19397(3) 0.02412(11) Uani 1 1 d . . .
Si1 Si 0.22288(5) 1.10204(4) 0.22344(3) 0.03211(12) Uani 1 1 d . . .
Si2 Si 0.29537(5) 0.53089(3) 0.13829(3) 0.03170(12) Uani 1 1 d . . .
N1 N 0.31508(12) 0.98750(10) 0.21482(9) 0.0269(3) Uani 1 1 d . . .
N2 N 0.46285(12) 0.86746(10) 0.19152(9) 0.0250(3) Uani 1 1 d . . .
N3 N 0.28531(13) 0.66526(10) 0.20948(9) 0.0276(3) Uani 1 1 d . . .
N4 N 0.25584(14) 0.81464(10) 0.31854(9) 0.0289(3) Uani 1 1 d . . .
C1 C 0.43822(15) 0.97523(12) 0.20342(10) 0.0244(3) Uani 1 1 d . . .
C2 C 0.53612(15) 1.06940(12) 0.20317(11) 0.0257(3) Uani 1 1 d . . .
C3 C 0.52932(17) 1.10622(13) 0.12188(11) 0.0325(3) Uani 1 1 d . . .
H3 H 0.4619 1.0714 0.0663 0.039 Uiso 1 1 calc R . .
C4 C 0.62010(18) 1.19346(14) 0.12112(12) 0.0376(4) Uani 1 1 d . . .
H4 H 0.6149 1.2173 0.0647 0.045 Uiso 1 1 calc R . .
C5 C 0.71874(18) 1.24647(14) 0.20205(13) 0.0371(4) Uani 1 1 d . . .
C6 C 0.72245(18) 1.21065(15) 0.28315(13) 0.0397(4) Uani 1 1 d . . .
H6 H 0.7881 1.2469 0.3394 0.048 Uiso 1 1 calc R . .
C7 C 0.63263(17) 1.12282(14) 0.28461(12) 0.0345(4) Uani 1 1 d . . .
H7 H 0.6374 1.0995 0.3412 0.041 Uiso 1 1 calc R . .
C8 C 0.8187(2) 1.34028(18) 0.20051(17) 0.0582(6) Uani 1 1 d . . .
H8A H 0.8002 1.3538 0.1373 0.087 Uiso 0.5 1 calc PR . .
H8B H 0.9094 1.319 0.214 0.087 Uiso 0.5 1 calc PR . .
H8C H 0.8114 1.4089 0.2492 0.087 Uiso 0.5 1 calc PR . .
H8D H 0.8805 1.3673 0.2631 0.087 Uiso 0.5 1 calc PR . .
H8E H 0.7713 1.4021 0.1863 0.087 Uiso 0.5 1 calc PR . .
H8F H 0.8693 1.3122 0.1511 0.087 Uiso 0.5 1 calc PR . .
C9 C 0.0694(2) 1.05963(18) 0.26062(17) 0.0518(5) Uani 1 1 d . . .
H9A H 0.0941 1.0444 0.323 0.078 Uiso 1 1 calc R . .
H9B H 0.0209 0.9917 0.2131 0.078 Uiso 1 1 calc R . .
H9C H 0.0122 1.1204 0.2655 0.078 Uiso 1 1 calc R . .
C10 C 0.3178(2) 1.22868(16) 0.31506(17) 0.0578(6) Uani 1 1 d . . .
H10A H 0.3415 1.2119 0.3768 0.087 Uiso 1 1 calc R . .
H10B H 0.2623 1.2907 0.321 0.087 Uiso 1 1 calc R . .
H10C H 0.3995 1.2502 0.2957 0.087 Uiso 1 1 calc R . .
C11 C 0.1761(2) 1.13096(19) 0.10526(15) 0.0541(5) Uani 1 1 d . . .
H11A H 0.2573 1.1536 0.0857 0.081 Uiso 1 1 calc R . .
H11B H 0.1187 1.1916 0.1101 0.081 Uiso 1 1 calc R . .
H11C H 0.1278 1.0629 0.0576 0.081 Uiso 1 1 calc R . .
C12 C 0.58614(14) 0.82386(12) 0.18408(10) 0.0246(3) Uani 1 1 d . . .
C13 C 0.67241(16) 0.85425(14) 0.13033(11) 0.0323(3) Uani 1 1 d . . .
H13 H 0.6499 0.9079 0.0961 0.039 Uiso 1 1 calc R . .
C14 C 0.79060(17) 0.80669(15) 0.12653(13) 0.0373(4) Uani 1 1 d . . .
H14 H 0.849 0.829 0.0904 0.045 Uiso 1 1 calc R . .
C15 C 0.82525(17) 0.72746(15) 0.17428(13) 0.0376(4) Uani 1 1 d . . .
H15 H 0.9071 0.6959 0.1718 0.045 Uiso 1 1 calc R . .
C16 C 0.73862(17) 0.69474(14) 0.22575(12) 0.0362(4) Uani 1 1 d . . .
H16 H 0.7603 0.6391 0.2579 0.043 Uiso 1 1 calc R . .
C17 C 0.62058(16) 0.74230(12) 0.23079(11) 0.0299(3) Uani 1 1 d . . .
H17 H 0.5622 0.719 0.2666 0.036 Uiso 1 1 calc R . .
C18 C 0.26425(15) 0.70367(12) 0.29678(11) 0.0267(3) Uani 1 1 d . . .
C19 C 0.25686(16) 0.63529(12) 0.36538(11) 0.0291(3) Uani 1 1 d . . .
C20 C 0.14703(18) 0.55790(14) 0.35259(13) 0.0376(4) Uani 1 1 d . . .
H20 H 0.0739 0.5482 0.2999 0.045 Uiso 1 1 calc R . .
C21 C 0.1439(2) 0.49431(15) 0.41707(14) 0.0431(4) Uani 1 1 d . . .
H21 H 0.0676 0.4422 0.4081 0.052 Uiso 1 1 calc R . .
C22 C 0.2490(2) 0.50521(15) 0.49354(13) 0.0427(4) Uani 1 1 d . . .
C23 C 0.3580(2) 0.58361(17) 0.50643(13) 0.0467(4) Uani 1 1 d . . .
H23 H 0.431 0.593 0.5591 0.056 Uiso 1 1 calc R . .
C24 C 0.36200(18) 0.64866(15) 0.44341(13) 0.0404(4) Uani 1 1 d . . .
H24 H 0.4371 0.7026 0.4538 0.048 Uiso 1 1 calc R . .
C25 C 0.2458(3) 0.4337(2) 0.56205(17) 0.0644(6) Uani 1 1 d . . .
H25A H 0.1612 0.3842 0.5426 0.097 Uiso 0.5 1 calc PR . .
H25B H 0.2536 0.4826 0.627 0.097 Uiso 0.5 1 calc PR . .
H25C H 0.3207 0.3883 0.5609 0.097 Uiso 0.5 1 calc PR . .
H25D H 0.3291 0.4525 0.6111 0.097 Uiso 0.5 1 calc PR . .
H25E H 0.2367 0.3541 0.5267 0.097 Uiso 0.5 1 calc PR . .
H25F H 0.1697 0.4484 0.5927 0.097 Uiso 0.5 1 calc PR . .
C26 C 0.3402(2) 0.55400(16) 0.02890(13) 0.0472(5) Uani 1 1 d . . .
H26A H 0.2713 0.5921 -0.0019 0.071 Uiso 1 1 calc R . .
H26B H 0.3464 0.4814 -0.0154 0.071 Uiso 1 1 calc R . .
H26C H 0.4267 0.6007 0.0462 0.071 Uiso 1 1 calc R . .
C27 C 0.1307(2) 0.44337(16) 0.10517(16) 0.0544(5) Uani 1 1 d . . .
H27A H 0.1067 0.4309 0.1629 0.082 Uiso 1 1 calc R . .
H27B H 0.1361 0.3709 0.0605 0.082 Uiso 1 1 calc R . .
H27C H 0.0623 0.4822 0.0747 0.082 Uiso 1 1 calc R . .
C28 C 0.4250(2) 0.45989(16) 0.19937(16) 0.0531(5) Uani 1 1 d . . .
H28A H 0.3993 0.448 0.2568 0.08 Uiso 1 1 calc R . .
H28B H 0.5113 0.507 0.2177 0.08 Uiso 1 1 calc R . .
H28C H 0.4326 0.3872 0.1559 0.08 Uiso 1 1 calc R . .
C29 C 0.23557(16) 0.88247(13) 0.40681(11) 0.0302(3) Uani 1 1 d . . .
C30 C 0.31862(19) 0.98293(14) 0.45056(12) 0.0377(4) Uani 1 1 d . . .
H30 H 0.3894 1.0029 0.4228 0.045 Uiso 1 1 calc R . .
C31 C 0.2981(2) 1.05414(16) 0.53498(13) 0.0467(5) Uani 1 1 d . . .
H31 H 0.3546 1.1229 0.5643 0.056 Uiso 1 1 calc R . .
C32 C 0.1965(2) 1.02578(18) 0.57626(13) 0.0492(5) Uani 1 1 d . . .
H32 H 0.1828 1.0746 0.6339 0.059 Uiso 1 1 calc R . .
C33 C 0.1149(2) 0.92612(18) 0.53332(13) 0.0456(4) Uani 1 1 d . . .
H33 H 0.0455 0.906 0.5622 0.055 Uiso 1 1 calc R . .
C34 C 0.13251(18) 0.85429(15) 0.44827(12) 0.0373(4) Uani 1 1 d . . .
H34 H 0.0744 0.7864 0.4187 0.045 Uiso 1 1 calc R . .
Cl Cl 0.12739(7) 0.78623(6) 0.06902(5) 0.0374(3) Uani 0.479(3) 1 d P . .
C35 C 0.12739(7) 0.78623(6) 0.06902(5) 0.0374(3) Uani 0.521(3) 1 d P . .
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 0 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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
_geom_angle_publ_flag
N4 Al N2 113.69(6) . . ?
N4 Al N1 101.31(5) . . ?
N2 Al N1 67.98(5) . . ?
N4 Al N3 67.68(5) . . ?
N2 Al N3 103.75(5) . . ?
N1 Al N3 163.04(6) . . ?
N4 Al Cl 125.59(5) . . ?
N2 Al Cl 120.71(5) . . ?
N1 Al Cl 97.91(5) . . ?
N3 Al Cl 99.02(5) . . ?
N4 Al C1 112.35(5) . . ?
N2 Al C1 34.45(5) . . ?
N1 Al C1 33.57(5) . . ?
N3 Al C1 136.96(6) . . ?
Cl Al C1 111.61(4) . . ?
N4 Al C18 34.13(5) . . ?
N2 Al C18 113.00(5) . . ?
N1 Al C18 134.34(6) . . ?
N3 Al C18 33.55(5) . . ?
Cl Al C18 115.91(4) . . ?
C1 Al C18 132.47(5) . . ?
N1 Si1 C9 105.56(8) . . ?
N1 Si1 C11 110.44(8) . . ?
C9 Si1 C11 109.51(11) . . ?
N1 Si1 C10 110.96(8) . . ?
C9 Si1 C10 109.65(11) . . ?
C11 Si1 C10 110.59(11) . . ?
N3 Si2 C26 104.77(7) . . ?
N3 Si2 C27 110.67(8) . . ?
C26 Si2 C27 109.25(10) . . ?
N3 Si2 C28 111.56(8) . . ?
C26 Si2 C28 110.64(10) . . ?
C27 Si2 C28 109.83(10) . . ?
C1 N1 Si1 132.15(10) . . ?
C1 N1 Al 89.38(9) . . ?
Si1 N1 Al 137.63(7) . . ?
C1 N2 C12 127.32(12) . . ?
C1 N2 Al 91.30(9) . . ?
C12 N2 Al 141.37(10) . . ?
C18 N3 Si2 133.32(11) . . ?
C18 N3 Al 89.05(9) . . ?
Si2 N3 Al 137.34(7) . . ?
C18 N4 C29 125.83(13) . . ?
C18 N4 Al 91.99(9) . . ?
C29 N4 Al 142.19(10) . . ?
N1 C1 N2 111.20(12) . . ?
N1 C1 C2 123.73(13) . . ?
N2 C1 C2 125.07(13) . . ?
N1 C1 Al 57.05(7) . . ?
N2 C1 Al 54.25(7) . . ?
C2 C1 Al 176.68(10) . . ?
C7 C2 C3 119.16(14) . . ?
C7 C2 C1 120.57(13) . . ?
C3 C2 C1 120.25(13) . . ?
C2 C3 C4 120.53(15) . . ?
C3 C4 C5 120.75(15) . . ?
C6 C5 C4 118.10(15) . . ?
C6 C5 C8 121.29(17) . . ?
C4 C5 C8 120.61(16) . . ?
C5 C6 C7 121.70(15) . . ?
C2 C7 C6 119.74(15) . . ?
C17 C12 C13 118.10(14) . . ?
C17 C12 N2 117.60(13) . . ?
C13 C12 N2 124.25(13) . . ?
C14 C13 C12 120.36(15) . . ?
C15 C14 C13 121.25(15) . . ?
C14 C15 C16 118.76(15) . . ?
C15 C16 C17 120.58(15) . . ?
C16 C17 C12 120.91(14) . . ?
N3 C18 N4 111.27(13) . . ?
N3 C18 C19 125.26(13) . . ?
N4 C18 C19 123.41(13) . . ?
N3 C18 Al 57.39(8) . . ?
N4 C18 Al 53.89(7) . . ?
C19 C18 Al 177.01(11) . . ?
C20 C19 C24 118.97(15) . . ?
C20 C19 C18 121.28(14) . . ?
C24 C19 C18 119.75(14) . . ?
C19 C20 C21 119.91(16) . . ?
C22 C21 C20 121.56(17) . . ?
C21 C22 C23 118.20(16) . . ?
C21 C22 C25 121.13(19) . . ?
C23 C22 C25 120.68(19) . . ?
C22 C23 C24 120.96(17) . . ?
C19 C24 C23 120.36(17) . . ?
C34 C29 C30 119.33(15) . . ?
C34 C29 N4 122.26(15) . . ?
C30 C29 N4 118.35(14) . . ?
C29 C30 C31 120.04(17) . . ?
C32 C31 C30 120.56(18) . . ?
C33 C32 C31 119.39(17) . . ?
C32 C33 C34 121.07(18) . . ?
C29 C34 C33 119.60(17) . . ?
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
Al N4 1.9322(13) . ?
Al N2 1.9346(13) . ?
Al N1 1.9998(12) . ?
Al N3 2.0140(13) . ?
Al Cl 2.1101(8) . ?
Al C1 2.3831(14) . ?
Al C18 2.3904(15) . ?
Si1 N1 1.7450(13) . ?
Si1 C9 1.854(2) . ?
Si1 C11 1.858(2) . ?
Si1 C10 1.859(2) . ?
Si2 N3 1.7463(13) . ?
Si2 C26 1.8533(19) . ?
Si2 C27 1.858(2) . ?
Si2 C28 1.859(2) . ?
N1 C1 1.3179(19) . ?
N2 C1 1.3485(18) . ?
N2 C12 1.4169(19) . ?
N3 C18 1.3214(19) . ?
N4 C18 1.3419(19) . ?
N4 C29 1.4196(19) . ?
C1 C2 1.4940(19) . ?
C2 C7 1.386(2) . ?
C2 C3 1.387(2) . ?
C3 C4 1.387(2) . ?
C4 C5 1.391(2) . ?
C5 C6 1.381(2) . ?
C5 C8 1.511(2) . ?
C6 C7 1.390(2) . ?
C12 C17 1.394(2) . ?
C12 C13 1.394(2) . ?
C13 C14 1.384(2) . ?
C14 C15 1.379(2) . ?
C15 C16 1.383(2) . ?
C16 C17 1.385(2) . ?
C18 C19 1.494(2) . ?
C19 C20 1.384(2) . ?
C19 C24 1.388(2) . ?
C20 C21 1.392(2) . ?
C21 C22 1.377(3) . ?
C22 C23 1.386(3) . ?
C22 C25 1.515(2) . ?
C23 C24 1.389(2) . ?
C29 C34 1.390(2) . ?
C29 C30 1.391(2) . ?
C30 C31 1.392(2) . ?
C31 C32 1.376(3) . ?
C32 C33 1.376(3) . ?
C33 C34 1.392(2) . ?
