#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/76/7007613.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_7007613
loop_
_publ_author_name
'Cheng, Yanxiang'
'Doyle, David J.'
'Hitchcock, Peter B.'
'Lappert, Michael F.'
_publ_section_title
;
 The beta-dialdiminato ligand [{N(C6H3Pri(2)-2,6)C(H)}2CPh]-: the
 conjugate acid and Li, Al, Ga and In derivatives.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4449
_journal_page_last               4460
_journal_paper_doi               10.1039/b607782j
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H41 Al1 Cl2 N2'
_chemical_formula_sum            'C33 H41 Al Cl2 N2'
_chemical_formula_weight         563.56
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2003-07-03T16:09:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.394(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0584(1)
_cell_length_b                   11.9404(1)
_cell_length_c                   26.9485(3)
_cell_measurement_reflns_used    24299
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     3201.88(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.797134E-1
_diffrn_orient_matrix_UB_12      0.42401E-1
_diffrn_orient_matrix_UB_13      0.168999E-1
_diffrn_orient_matrix_UB_21      0.43721E-2
_diffrn_orient_matrix_UB_22      -0.50365E-1
_diffrn_orient_matrix_UB_23      0.298421E-1
_diffrn_orient_matrix_UB_31      0.610415E-1
_diffrn_orient_matrix_UB_32      -0.517636E-1
_diffrn_orient_matrix_UB_33      -0.151926E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.032
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            28547
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.71
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0347P)²+1.5984P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                4826
_reflns_number_total             5581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b607782j.txt
_cod_data_source_block           (4)-jul203
_cod_original_cell_volume        3201.88(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C33 H41 Al1 Cl2 N2'
_cod_database_code               7007613
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
Al Al 0.51700(4) 0.76500(4) 0.116527(17) 0.02420(12) Uani 1 1 d . . .
Cl1 Cl 0.69470(4) 0.82138(4) 0.090759(18) 0.04376(14) Uani 1 1 d . . .
Cl2 Cl 0.55205(5) 0.60820(4) 0.152512(16) 0.03919(13) Uani 1 1 d . . .
N1 N 0.44797(12) 0.87105(11) 0.15764(4) 0.0227(3) Uani 1 1 d . . .
N2 N 0.37023(13) 0.76520(11) 0.06459(5) 0.0236(3) Uani 1 1 d . . .
C1 C 0.35400(15) 0.94411(13) 0.13909(6) 0.0240(3) Uani 1 1 d . . .
H1 H 0.3347 1.003 0.1606 0.029 Uiso 1 1 calc R . .
C2 C 0.28096(15) 0.94229(13) 0.09082(6) 0.0234(3) Uani 1 1 d . . .
C3 C 0.28597(15) 0.85160(13) 0.05851(6) 0.0238(3) Uani 1 1 d . . .
H3 H 0.222 0.8516 0.0288 0.029 Uiso 1 1 calc R . .
C4 C 0.18238(15) 1.03266(14) 0.07445(6) 0.0265(4) Uani 1 1 d . . .
C5 C 0.09383(17) 1.07324(16) 0.10545(7) 0.0378(4) Uani 1 1 d . . .
H5 H 0.094 1.0415 0.1378 0.045 Uiso 1 1 calc R . .
C6 C 0.00581(19) 1.15919(18) 0.08967(7) 0.0466(5) Uani 1 1 d . . .
H6 H -0.0534 1.1862 0.1114 0.056 Uiso 1 1 calc R . .
C7 C 0.00299(19) 1.20626(16) 0.04266(7) 0.0429(5) Uani 1 1 d . . .
H7 H -0.0567 1.2662 0.0322 0.052 Uiso 1 1 calc R . .
C8 C 0.08752(19) 1.16540(16) 0.01118(7) 0.0420(5) Uani 1 1 d . . .
H8 H 0.085 1.1963 -0.0214 0.05 Uiso 1 1 calc R . .
C9 C 0.17623(17) 1.07953(15) 0.02681(6) 0.0338(4) Uani 1 1 d . . .
H9 H 0.234 1.052 0.0047 0.041 Uiso 1 1 calc R . .
C10 C 0.49121(15) 0.87647(13) 0.21170(5) 0.0243(3) Uani 1 1 d . . .
C11 C 0.60278(16) 0.94175(15) 0.23091(6) 0.0306(4) Uani 1 1 d . . .
C12 C 0.64115(18) 0.94191(17) 0.28288(6) 0.0378(4) Uani 1 1 d . . .
H12 H 0.7169 0.9848 0.297 0.045 Uiso 1 1 calc R . .
C13 C 0.57166(19) 0.88136(17) 0.31403(6) 0.0398(4) Uani 1 1 d . . .
H13 H 0.5998 0.8826 0.3492 0.048 Uiso 1 1 calc R . .
C14 C 0.46110(18) 0.81873(16) 0.29432(6) 0.0344(4) Uani 1 1 d . . .
H14 H 0.4135 0.7776 0.3162 0.041 Uiso 1 1 calc R . .
C15 C 0.41828(16) 0.81490(14) 0.24298(6) 0.0269(4) Uani 1 1 d . . .
C16 C 0.67885(18) 1.01448(17) 0.19850(7) 0.0414(5) Uani 1 1 d . . .
H16 H 0.6408 1.0004 0.1627 0.05 Uiso 1 1 calc R . .
C17 C 0.8281(2) 0.9848(3) 0.20523(9) 0.0720(8) Uani 1 1 d . . .
H17A H 0.874 1.0331 0.1837 0.108 Uiso 1 1 calc R . .
H17B H 0.8387 0.9063 0.1959 0.108 Uiso 1 1 calc R . .
H17C H 0.8673 0.996 0.2404 0.108 Uiso 1 1 calc R . .
C18 C 0.6575(3) 1.1381(2) 0.20958(9) 0.0719(8) Uani 1 1 d . . .
H18A H 0.7065 1.1844 0.1883 0.108 Uiso 1 1 calc R . .
H18B H 0.6908 1.1535 0.2449 0.108 Uiso 1 1 calc R . .
H18C H 0.5614 1.1558 0.2026 0.108 Uiso 1 1 calc R . .
C19 C 0.29127(17) 0.74983(15) 0.22283(6) 0.0317(4) Uani 1 1 d . . .
H19 H 0.2909 0.7389 0.186 0.038 Uiso 1 1 calc R . .
C20 C 0.16599(19) 0.81673(19) 0.22941(9) 0.0515(5) Uani 1 1 d . . .
H20A H 0.0857 0.7736 0.2162 0.077 Uiso 1 1 calc R . .
H20B H 0.1661 0.8877 0.2112 0.077 Uiso 1 1 calc R . .
H20C H 0.1656 0.8319 0.2651 0.077 Uiso 1 1 calc R . .
C21 C 0.2866(2) 0.63437(18) 0.24643(8) 0.0503(5) Uani 1 1 d . . .
H21A H 0.2035 0.5963 0.2321 0.075 Uiso 1 1 calc R . .
H21B H 0.2892 0.6422 0.2828 0.075 Uiso 1 1 calc R . .
H21C H 0.3641 0.5903 0.2396 0.075 Uiso 1 1 calc R . .
C22 C 0.33557(15) 0.67313(13) 0.02956(6) 0.0254(3) Uani 1 1 d . . .
C23 C 0.37940(17) 0.67567(15) -0.01777(6) 0.0301(4) Uani 1 1 d . . .
C24 C 0.33888(19) 0.58738(16) -0.05036(7) 0.0388(4) Uani 1 1 d . . .
H24 H 0.367 0.5863 -0.0825 0.047 Uiso 1 1 calc R . .
C25 C 0.2594(2) 0.50179(17) -0.03725(7) 0.0446(5) Uani 1 1 d . . .
H25 H 0.2336 0.4426 -0.0602 0.054 Uiso 1 1 calc R . .
C26 C 0.2170(2) 0.50181(16) 0.00939(7) 0.0412(5) Uani 1 1 d . . .
H26 H 0.161 0.4429 0.0179 0.049 Uiso 1 1 calc R . .
C27 C 0.25512(16) 0.58668(14) 0.04394(6) 0.0304(4) Uani 1 1 d . . .
C28 C 0.4635(2) 0.77012(17) -0.03414(7) 0.0406(5) Uani 1 1 d . . .
H28 H 0.5152 0.8046 -0.0034 0.049 Uiso 1 1 calc R . .
C29 C 0.5635(2) 0.7296(2) -0.06746(9) 0.0572(6) Uani 1 1 d . . .
H29A H 0.6159 0.7934 -0.0769 0.086 Uiso 1 1 calc R . .
H29B H 0.5149 0.695 -0.0978 0.086 Uiso 1 1 calc R . .
H29C H 0.6241 0.6745 -0.0492 0.086 Uiso 1 1 calc R . .
C30 C 0.3756(3) 0.8613(2) -0.06230(10) 0.0733(8) Uani 1 1 d . . .
H30A H 0.433 0.9213 -0.0721 0.11 Uiso 1 1 calc R . .
H30B H 0.3148 0.892 -0.0404 0.11 Uiso 1 1 calc R . .
H30C H 0.3229 0.8291 -0.0924 0.11 Uiso 1 1 calc R . .
C31 C 0.20674(18) 0.58563(16) 0.09497(6) 0.0350(4) Uani 1 1 d . . .
H31 H 0.2711 0.6327 0.1179 0.042 Uiso 1 1 calc R . .
C32 C 0.0688(2) 0.6406(2) 0.09223(8) 0.0610(7) Uani 1 1 d . . .
H32A H 0.0405 0.6396 0.1255 0.092 Uiso 1 1 calc R . .
H32B H 0.0034 0.5993 0.0685 0.092 Uiso 1 1 calc R . .
H32C H 0.0739 0.7182 0.0809 0.092 Uiso 1 1 calc R . .
C33 C 0.2085(3) 0.46976(19) 0.11816(9) 0.0675(7) Uani 1 1 d . . .
H33A H 0.1772 0.4744 0.1509 0.101 Uiso 1 1 calc R . .
H33B H 0.3002 0.44 0.1225 0.101 Uiso 1 1 calc R . .
H33C H 0.1491 0.42 0.0961 0.101 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 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'
Cl Cl 0.1484 0.1585 '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'
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
N2 Al N1 96.91(6) . . ?
N2 Al Cl2 113.75(5) . . ?
N1 Al Cl2 112.16(5) . . ?
N2 Al Cl1 111.34(5) . . ?
N1 Al Cl1 112.37(5) . . ?
Cl2 Al Cl1 109.84(3) . . ?
C1 N1 C10 115.99(13) . . ?
C1 N1 Al 121.59(10) . . ?
C10 N1 Al 122.41(10) . . ?
C3 N2 C22 114.67(12) . . ?
C3 N2 Al 120.64(10) . . ?
C22 N2 Al 124.66(10) . . ?
N1 C1 C2 126.03(15) . . ?
C3 C2 C1 122.07(14) . . ?
C3 C2 C4 117.46(13) . . ?
C1 C2 C4 120.10(14) . . ?
N2 C3 C2 127.28(14) . . ?
C9 C4 C5 117.78(15) . . ?
C9 C4 C2 120.15(15) . . ?
C5 C4 C2 122.06(15) . . ?
C6 C5 C4 120.71(18) . . ?
C5 C6 C7 120.71(18) . . ?
C8 C7 C6 119.29(17) . . ?
C7 C8 C9 120.28(18) . . ?
C8 C9 C4 121.19(17) . . ?
C11 C10 C15 122.00(14) . . ?
C11 C10 N1 119.93(14) . . ?
C15 C10 N1 118.07(13) . . ?
C12 C11 C10 117.38(16) . . ?
C12 C11 C16 119.20(15) . . ?
C10 C11 C16 123.37(14) . . ?
C13 C12 C11 121.40(16) . . ?
C12 C13 C14 120.20(16) . . ?
C13 C14 C15 121.11(17) . . ?
C14 C15 C10 117.89(15) . . ?
C14 C15 C19 119.56(15) . . ?
C10 C15 C19 122.47(14) . . ?
C11 C16 C17 111.64(18) . . ?
C11 C16 C18 110.11(17) . . ?
C17 C16 C18 111.4(2) . . ?
C21 C19 C20 110.47(16) . . ?
C21 C19 C15 112.83(15) . . ?
C20 C19 C15 110.81(15) . . ?
C27 C22 C23 122.41(15) . . ?
C27 C22 N2 118.01(14) . . ?
C23 C22 N2 119.55(14) . . ?
C24 C23 C22 116.90(16) . . ?
C24 C23 C28 120.27(15) . . ?
C22 C23 C28 122.80(15) . . ?
C25 C24 C23 121.84(16) . . ?
C24 C25 C26 120.04(17) . . ?
C25 C26 C27 121.07(17) . . ?
C26 C27 C22 117.73(16) . . ?
C26 C27 C31 120.30(16) . . ?
C22 C27 C31 121.95(15) . . ?
C23 C28 C29 112.40(17) . . ?
C23 C28 C30 111.58(17) . . ?
C29 C28 C30 108.46(17) . . ?
C33 C31 C27 113.16(16) . . ?
C33 C31 C32 111.56(19) . . ?
C27 C31 C32 111.13(15) . . ?
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 N2 1.8801(13) . ?
Al N1 1.8808(14) . ?
Al Cl2 2.1143(7) . ?
Al Cl1 2.1195(6) . ?
N1 C1 1.329(2) . ?
N1 C10 1.4597(19) . ?
N2 C3 1.330(2) . ?
N2 C22 1.4579(19) . ?
C1 C2 1.398(2) . ?
C2 C3 1.395(2) . ?
C2 C4 1.488(2) . ?
C4 C9 1.394(2) . ?
C4 C5 1.394(2) . ?
C5 C6 1.381(3) . ?
C6 C7 1.382(3) . ?
C7 C8 1.375(3) . ?
C8 C9 1.384(2) . ?
C10 C11 1.402(2) . ?
C10 C15 1.404(2) . ?
C11 C12 1.397(2) . ?
C11 C16 1.516(2) . ?
C12 C13 1.374(3) . ?
C13 C14 1.380(3) . ?
C14 C15 1.388(2) . ?
C15 C19 1.526(2) . ?
C16 C17 1.527(3) . ?
C16 C18 1.528(3) . ?
C19 C21 1.522(3) . ?
C19 C20 1.524(3) . ?
C22 C27 1.401(2) . ?
C22 C23 1.409(2) . ?
C23 C24 1.394(2) . ?
C23 C28 1.514(3) . ?
C24 C25 1.375(3) . ?
C25 C26 1.385(3) . ?
C26 C27 1.392(2) . ?
C27 C31 1.524(2) . ?
C28 C29 1.522(3) . ?
C28 C30 1.532(3) . ?
C31 C33 1.517(3) . ?
C31 C32 1.527(3) . ?
