#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:07:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179277 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/97/4319763.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_4319763
loop_
_publ_author_name
'Matthias Stender'
'Barrett E. Eichler'
'Ned J. Hardman'
'Philip P. Power'
'Jörg Prust'
'Mathias Noltemeyer'
'Herbert W. Roesky'
_publ_section_title
;
 Synthesis and Characterization of HC{C(Me)N(C6H3-2,6-i-Pr2)}2MX2 (M = Al,
 X = Cl, I; M = Ga, In, X = Me, Cl, I): Sterically Encumbered
 β-Diketiminate Group 13 Metal Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2794
_journal_page_last               2799
_journal_paper_doi               10.1021/ic001311d
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C29 H41 Al Cl2 N2'
_chemical_formula_weight         515.52
_chemical_name_common            NacNacAlCl2
_chemical_name_systematic
; 

 ? 

;
_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                 108.8420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9413(7)
_cell_length_b                   9.9216(4)
_cell_length_c                   17.1167(7)
_cell_measurement_reflns_used    6886
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.45
_cell_measurement_theta_min      2.38
_cell_volume                     2883.6(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL v. 5.10'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 5.10'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 5.10'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 5.10'
_computing_structure_solution    'XS, Bruker SHELXTL v. 5.10'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38601
_diffrn_reflns_theta_full        31.48
_diffrn_reflns_theta_max         31.48
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        <0.01
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_T_max  0.9677
_exptl_absorpt_correction_T_min  0.8793
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS: an empirical absorption program by G. M. Sheldrick

using the method described by Blessing, R. H.; Acta Cryst.

A51, 1995, 33.

;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         9070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.098
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0689P)²+1.0885P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                7440
_reflns_number_total             9070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001311d_4.cif
_cod_data_source_block           mas05a
_cod_database_code               4319763
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
Cl1 Cl 0.315663(15) 0.03762(3) 0.100005(16) 0.02076(6) Uani 1 1 d . . .
Cl2 Cl 0.221919(16) -0.22579(3) 0.160234(17) 0.02168(7) Uani 1 1 d . . .
Al1 Al 0.268697(18) -0.02998(3) 0.192931(19) 0.01409(7) Uani 1 1 d . . .
N1 N 0.19805(5) 0.10060(8) 0.20746(5) 0.01417(15) Uani 1 1 d . . .
N2 N 0.34308(5) -0.02693(8) 0.29836(5) 0.01538(16) Uani 1 1 d . . .
C1 C 0.22452(6) 0.19595(10) 0.26537(6) 0.01562(18) Uani 1 1 d . . .
C2 C 0.30008(6) 0.19358(10) 0.32448(6) 0.01783(19) Uani 1 1 d . . .
H2A H 0.3166 0.2729 0.3539 0.021 Uiso 1 1 calc R . .
C3 C 0.35323(6) 0.08632(11) 0.34418(6) 0.01692(19) Uani 1 1 d . . .
C4 C 0.17267(7) 0.31260(11) 0.27120(7) 0.0209(2) Uani 1 1 d . . .
H4A H 0.1184 0.2865 0.2487 0.031 Uiso 1 1 calc R . .
H4B H 0.1826 0.3878 0.2406 0.031 Uiso 1 1 calc R . .
H4C H 0.1840 0.3378 0.3280 0.031 Uiso 1 1 calc R . .
C5 C 0.42298(7) 0.09840(12) 0.42159(7) 0.0229(2) Uani 1 1 d . . .
H5A H 0.4707 0.0874 0.4083 0.034 Uiso 1 1 calc R . .
H5B H 0.4200 0.0299 0.4601 0.034 Uiso 1 1 calc R . .
H5C H 0.4227 0.1856 0.4458 0.034 Uiso 1 1 calc R . .
C6 C 0.11686(6) 0.10751(10) 0.15309(6) 0.01524(18) Uani 1 1 d . . .
C7 C 0.06079(6) 0.02135(10) 0.16889(6) 0.01614(18) Uani 1 1 d . . .
C8 C -0.01749(6) 0.03173(11) 0.11812(7) 0.0201(2) Uani 1 1 d . . .
H8A H -0.0553 -0.0233 0.1282 0.024 Uiso 1 1 calc R . .
C9 C -0.04001(6) 0.12258(12) 0.05292(7) 0.0219(2) Uani 1 1 d . . .
H9A H -0.0924 0.1280 0.0197 0.026 Uiso 1 1 calc R . .
C10 C 0.01606(7) 0.20506(11) 0.03766(7) 0.0208(2) Uani 1 1 d . . .
H10A H 0.0007 0.2651 -0.0064 0.025 Uiso 1 1 calc R . .
C11 C 0.09527(6) 0.20010(10) 0.08699(6) 0.01747(19) Uani 1 1 d . . .
C12 C 0.15383(7) 0.29405(11) 0.06681(7) 0.0209(2) Uani 1 1 d . . .
H12A H 0.2048 0.2855 0.1104 0.025 Uiso 1 1 calc R . .
C13 C 0.12729(9) 0.44274(13) 0.06265(8) 0.0302(3) Uani 1 1 d . . .
H13A H 0.1154 0.4652 0.1119 0.045 Uiso 1 1 calc R . .
H13B H 0.0812 0.4555 0.0154 0.045 Uiso 1 1 calc R . .
H13C H 0.1688 0.5000 0.0580 0.045 Uiso 1 1 calc R . .
C14 C 0.16441(8) 0.25407(13) -0.01560(7) 0.0258(2) Uani 1 1 d . . .
H14A H 0.1810 0.1617 -0.0130 0.039 Uiso 1 1 calc R . .
H14B H 0.2035 0.3108 -0.0260 0.039 Uiso 1 1 calc R . .
H14C H 0.1153 0.2647 -0.0593 0.039 Uiso 1 1 calc R . .
C15 C 0.08265(6) -0.07865(11) 0.24022(6) 0.01802(19) Uani 1 1 d . . .
H15A H 0.1400 -0.0899 0.2583 0.022 Uiso 1 1 calc R . .
C16 C 0.06093(9) -0.02561(13) 0.31407(8) 0.0302(3) Uani 1 1 d . . .
H16A H 0.0878 0.0579 0.3325 0.045 Uiso 1 1 calc R . .
H16B H 0.0762 -0.0903 0.3581 0.045 Uiso 1 1 calc R . .
H16C H 0.0051 -0.0112 0.2979 0.045 Uiso 1 1 calc R . .
C17 C 0.04586(7) -0.21765(12) 0.21450(8) 0.0242(2) Uani 1 1 d . . .
H17A H 0.0619 -0.2517 0.1699 0.036 Uiso 1 1 calc R . .
H17B H -0.0105 -0.2102 0.1969 0.036 Uiso 1 1 calc R . .
H17C H 0.0631 -0.2783 0.2606 0.036 Uiso 1 1 calc R . .
C18 C 0.39097(6) -0.14284(10) 0.33607(6) 0.01727(19) Uani 1 1 d . . .
C19 C 0.36263(7) -0.22842(11) 0.38601(7) 0.0200(2) Uani 1 1 d . . .
C20 C 0.41114(7) -0.33389(12) 0.42760(7) 0.0245(2) Uani 1 1 d . . .
H20A H 0.3940 -0.3907 0.4615 0.029 Uiso 1 1 calc R . .
C21 C 0.48451(8) -0.35480(12) 0.41886(7) 0.0262(2) Uani 1 1 d . . .
H21A H 0.5166 -0.4240 0.4478 0.031 Uiso 1 1 calc R . .
C22 C 0.50998(7) -0.27264(12) 0.36708(7) 0.0242(2) Uani 1 1 d . . .
H22A H 0.5586 -0.2894 0.3604 0.029 Uiso 1 1 calc R . .
C23 C 0.46409(6) -0.16499(11) 0.32463(7) 0.01919(19) Uani 1 1 d . . .
C24 C 0.49491(7) -0.08080(12) 0.26750(7) 0.0217(2) Uani 1 1 d . . .
H24A H 0.4595 -0.0039 0.2482 0.026 Uiso 1 1 calc R . .
C25 C 0.57841(8) -0.02637(14) 0.31032(10) 0.0333(3) Uani 1 1 d . . .
H25A H 0.5793 0.0231 0.3588 0.050 Uiso 1 1 calc R . .
H25B H 0.5933 0.0321 0.2732 0.050 Uiso 1 1 calc R . .
H25C H 0.6148 -0.1003 0.3257 0.050 Uiso 1 1 calc R . .
C26 C 0.49393(8) -0.16547(13) 0.19210(8) 0.0290(3) Uani 1 1 d . . .
H26A H 0.4411 -0.1946 0.1636 0.043 Uiso 1 1 calc R . .
H26B H 0.5273 -0.2427 0.2099 0.043 Uiso 1 1 calc R . .
H26C H 0.5128 -0.1120 0.1556 0.043 Uiso 1 1 calc R . .
C27 C 0.28242(7) -0.21011(12) 0.39665(7) 0.0236(2) Uani 1 1 d . . .
H27A H 0.2538 -0.1415 0.3571 0.028 Uiso 1 1 calc R . .
C28 C 0.23394(8) -0.34055(15) 0.37765(9) 0.0337(3) Uani 1 1 d . . .
H28A H 0.2298 -0.3711 0.3232 0.051 Uiso 1 1 calc R . .
H28B H 0.1822 -0.3237 0.3806 0.051 Uiso 1 1 calc R . .
H28C H 0.2595 -0.4084 0.4172 0.051 Uiso 1 1 calc R . .
C29 C 0.28956(9) -0.16012(15) 0.48349(8) 0.0343(3) Uani 1 1 d . . .
H29A H 0.3148 -0.0736 0.4925 0.051 Uiso 1 1 calc R . .
H29B H 0.3203 -0.2230 0.5237 0.051 Uiso 1 1 calc R . .
H29C H 0.2380 -0.1525 0.4886 0.051 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'
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
N2 Al1 N1 99.36(4) . . ?
N2 Al1 Cl2 111.65(3) . . ?
N1 Al1 Cl2 116.07(3) . . ?
N2 Al1 Cl1 112.60(3) . . ?
N1 Al1 Cl1 109.06(3) . . ?
Cl2 Al1 Cl1 108.019(17) . . ?
C1 N1 C6 118.80(8) . . ?
C1 N1 Al1 119.33(7) . . ?
C6 N1 Al1 121.68(6) . . ?
C3 N2 C18 116.80(8) . . ?
C3 N2 Al1 119.73(7) . . ?
C18 N2 Al1 123.45(7) . . ?
N1 C1 C2 123.30(9) . . ?
N1 C1 C4 120.76(9) . . ?
C2 C1 C4 115.93(9) . . ?
C3 C2 C1 127.70(10) . . ?
N2 C3 C2 122.78(9) . . ?
N2 C3 C5 119.74(9) . . ?
C2 C3 C5 117.45(9) . . ?
C7 C6 C11 121.33(9) . . ?
C7 C6 N1 118.50(9) . . ?
C11 C6 N1 120.16(9) . . ?
C8 C7 C6 118.16(9) . . ?
C8 C7 C15 119.59(9) . . ?
C6 C7 C15 122.23(9) . . ?
C9 C8 C7 121.39(10) . . ?
C10 C9 C8 119.62(10) . . ?
C9 C10 C11 121.53(10) . . ?
C10 C11 C6 117.96(10) . . ?
C10 C11 C12 118.77(9) . . ?
C6 C11 C12 123.28(9) . . ?
C11 C12 C14 110.42(9) . . ?
C11 C12 C13 111.68(10) . . ?
C14 C12 C13 109.40(10) . . ?
C7 C15 C17 112.39(9) . . ?
C7 C15 C16 111.69(9) . . ?
C17 C15 C16 110.23(10) . . ?
C23 C18 C19 121.72(10) . . ?
C23 C18 N2 120.38(9) . . ?
C19 C18 N2 117.87(9) . . ?
C20 C19 C18 118.12(10) . . ?
C20 C19 C27 119.09(10) . . ?
C18 C19 C27 122.79(9) . . ?
C21 C20 C19 120.85(11) . . ?
C22 C21 C20 120.08(10) . . ?
C21 C22 C23 121.38(11) . . ?
C22 C23 C18 117.78(10) . . ?
C22 C23 C24 118.56(10) . . ?
C18 C23 C24 123.65(9) . . ?
C23 C24 C26 109.42(10) . . ?
C23 C24 C25 112.79(10) . . ?
C26 C24 C25 109.75(10) . . ?
C19 C27 C29 111.68(10) . . ?
C19 C27 C28 111.59(10) . . ?
C29 C27 C28 110.04(11) . . ?
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
Cl1 Al1 2.1344(4) . ?
Cl2 Al1 2.1185(4) . ?
Al1 N2 1.8663(9) . ?
Al1 N1 1.8843(9) . ?
N1 C1 1.3412(13) . ?
N1 C6 1.4550(13) . ?
N2 C3 1.3485(13) . ?
N2 C18 1.4557(13) . ?
C1 C2 1.4058(14) . ?
C1 C4 1.5082(14) . ?
C2 C3 1.3956(14) . ?
C3 C5 1.5051(14) . ?
C6 C7 1.4112(14) . ?
C6 C11 1.4110(14) . ?
C7 C8 1.3964(14) . ?
C7 C15 1.5230(14) . ?
C8 C9 1.3893(16) . ?
C9 C10 1.3855(17) . ?
C10 C11 1.3999(15) . ?
C11 C12 1.5253(15) . ?
C12 C14 1.5350(16) . ?
C12 C13 1.5448(17) . ?
C15 C17 1.5309(15) . ?
C15 C16 1.5313(16) . ?
C18 C23 1.4048(15) . ?
C18 C19 1.4110(15) . ?
C19 C20 1.3997(15) . ?
C19 C27 1.5187(17) . ?
C20 C21 1.3876(18) . ?
C21 C22 1.3857(18) . ?
C22 C23 1.4001(15) . ?
C23 C24 1.5196(16) . ?
C24 C26 1.5352(17) . ?
C24 C25 1.5375(17) . ?
C27 C29 1.5326(18) . ?
C27 C28 1.5344(18) . ?
