#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:28:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179482 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/79/4337906.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_4337906
loop_
_publ_author_name
'Cole, Bren E.'
'Wolbach, Jeffrey P.'
'Dougherty, Jr, William G.'
'Piro, Nicholas A.'
'Kassel, W. Scott'
'Graves, Christopher R.'
_publ_section_title
;
 Synthesis and Characterization of Aluminum-α-diimine Complexes over
 Multiple Redox States.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3899
_journal_paper_doi               10.1021/ic5003989
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C22 H28 Al Cl2 N2'
_chemical_formula_sum            'C22 H28 Al Cl2 N2'
_chemical_formula_weight         418.34
_chemical_name_common            (LMes1-)AlCl2
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.6845(14)
_cell_length_b                   14.1011(10)
_cell_length_c                   18.3747(14)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.20
_cell_measurement_theta_min      2.15
_cell_volume                     4582.1(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            73337
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         2.154
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       shard
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         6438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0473P)²+3.3885P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4769
_reflns_number_total             6438
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5003989_si_001.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4337906--4337908.cif.'
_cod_database_code               4337906
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cl1 Cl 0.16038(3) 0.94297(3) 0.06948(3) 0.02819(11) Uani 1 1 d . .
N2 N 0.15739(8) 1.18457(10) 0.08526(7) 0.0176(3) Uani 1 1 d . .
Cl2 Cl 0.29360(3) 1.06082(4) 0.17105(2) 0.03001(12) Uani 1 1 d . .
N1 N 0.25891(8) 1.12217(10) -0.00315(7) 0.0171(3) Uani 1 1 d . .
Al1 Al 0.21709(3) 1.07446(4) 0.08248(3) 0.01726(12) Uani 1 1 d . .
C11 C 0.31235(9) 1.07872(11) -0.05187(8) 0.0165(3) Uani 1 1 d . .
C12 C 0.28570(9) 1.02724(12) -0.11178(9) 0.0177(3) Uani 1 1 d . .
C13 C 0.33840(10) 0.98725(12) -0.15913(9) 0.0202(3) Uani 1 1 d . .
H13 H 0.3210 0.9522 -0.2000 0.024 Uiso 1 1 calc R U
C21 C 0.09967(9) 1.21267(12) 0.13674(9) 0.0186(3) Uani 1 1 d . .
C2 C 0.17519(9) 1.24424(13) 0.03055(9) 0.0196(3) Uani 1 1 d . .
C14 C 0.41604(10) 0.99732(12) -0.14809(9) 0.0218(3) Uani 1 1 d . .
C1 C 0.23149(9) 1.20944(12) -0.01922(9) 0.0197(3) Uani 1 1 d . .
C22 C 0.02461(10) 1.18595(13) 0.12334(10) 0.0236(4) Uani 1 1 d . .
C16 C 0.38989(10) 1.09018(12) -0.03920(9) 0.0201(3) Uani 1 1 d . .
C25 C 0.06149(11) 1.29620(14) 0.24384(10) 0.0279(4) Uani 1 1 d . .
H25 H 0.0738 1.3340 0.2850 0.034 Uiso 1 1 calc R U
C121 C 0.20184(10) 1.01693(14) -0.12551(9) 0.0244(4) Uani 1 1 d . .
H12A H 0.1782 0.9846 -0.0841 0.037 Uiso 1 1 calc R U
H12B H 0.1938 0.9797 -0.1699 0.037 Uiso 1 1 calc R U
H12C H 0.1791 1.0799 -0.1314 0.037 Uiso 1 1 calc R U
C26 C 0.11960(10) 1.26764(13) 0.19708(9) 0.0217(3) Uani 1 1 d . .
C15 C 0.44053(10) 1.04839(13) -0.08777(10) 0.0235(4) Uani 1 1 d . .
H15 H 0.4933 1.0550 -0.0794 0.028 Uiso 1 1 calc R U
C261 C 0.20057(11) 1.29582(15) 0.21114(11) 0.0290(4) Uani 1 1 d . .
H26A H 0.2303 1.2392 0.2229 0.043 Uiso 1 1 calc R U
H26B H 0.2025 1.3404 0.2520 0.043 Uiso 1 1 calc R U
H26C H 0.2215 1.3262 0.1676 0.043 Uiso 1 1 calc R U
C141 C 0.47222(12) 0.95548(15) -0.20089(11) 0.0321(4) Uani 1 1 d . .
H14A H 0.5152 0.9988 -0.2064 0.048 Uiso 1 1 calc R U
H14B H 0.4478 0.9461 -0.2482 0.048 Uiso 1 1 calc R U
H14C H 0.4902 0.8944 -0.1823 0.048 Uiso 1 1 calc R U
C3 C 0.25630(12) 1.26472(14) -0.08232(10) 0.0290(4) Uani 1 1 d . .
H3A H 0.2902 1.3155 -0.0662 0.044 Uiso 1 1 calc R U
H3B H 0.2122 1.2924 -0.1065 0.044 Uiso 1 1 calc R U
H3C H 0.2831 1.2232 -0.1164 0.044 Uiso 1 1 calc R U
C4 C 0.14008(11) 1.33837(14) 0.02232(11) 0.0275(4) Uani 1 1 d . .
H4A H 0.0873 1.3355 0.0383 0.041 Uiso 1 1 calc R U
H4B H 0.1421 1.3576 -0.0289 0.041 Uiso 1 1 calc R U
H4C H 0.1676 1.3846 0.0521 0.041 Uiso 1 1 calc R U
C23 C -0.03078(10) 1.21630(15) 0.17233(11) 0.0288(4) Uani 1 1 d . .
H23 H -0.0819 1.1985 0.1642 0.035 Uiso 1 1 calc R U
C24 C -0.01351(11) 1.27131(14) 0.23225(11) 0.0300(4) Uani 1 1 d . .
C221 C 0.00394(11) 1.12640(18) 0.05827(12) 0.0365(5) Uani 1 1 d . .
H22A H 0.0241 1.1559 0.0141 0.055 Uiso 1 1 calc R U
H22B H -0.0512 1.1218 0.0546 0.055 Uiso 1 1 calc R U
H22C H 0.0255 1.0628 0.0638 0.055 Uiso 1 1 calc R U
C241 C -0.07493(13) 1.30322(18) 0.28419(13) 0.0445(6) Uani 1 1 d . .
H24A H -0.1083 1.3484 0.2595 0.067 Uiso 1 1 calc R U
H24B H -0.0518 1.3337 0.3266 0.067 Uiso 1 1 calc R U
H24C H -0.1044 1.2481 0.3000 0.067 Uiso 1 1 calc R U
C161 C 0.41823(10) 1.14896(15) 0.02376(11) 0.0309(4) Uani 1 1 d . .
H16A H 0.4736 1.1497 0.0234 0.046 Uiso 1 1 calc R U
H16B H 0.4003 1.1214 0.0696 0.046 Uiso 1 1 calc R U
H16C H 0.3992 1.2139 0.0192 0.046 Uiso 1 1 calc R U
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'
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
C2 N2 C21 118.76(14)
C2 N2 Al1 111.37(11)
C21 N2 Al1 129.85(11)
C1 N1 C11 119.09(13)
C1 N1 Al1 111.69(11)
C11 N1 Al1 129.21(11)
N1 Al1 N2 87.00(6)
N1 Al1 Cl1 114.07(5)
N2 Al1 Cl1 117.38(5)
N1 Al1 Cl2 115.24(5)
N2 Al1 Cl2 114.33(5)
Cl1 Al1 Cl2 107.95(3)
C12 C11 C16 121.34(15)
C12 C11 N1 119.27(14)
C16 C11 N1 119.38(14)
C13 C12 C11 118.38(15)
C13 C12 C121 120.86(15)
C11 C12 C121 120.75(15)
C12 C13 C14 121.74(16)
C26 C21 C22 121.81(15)
C26 C21 N2 119.50(14)
C22 C21 N2 118.66(15)
N2 C2 C1 115.01(15)
N2 C2 C4 122.72(15)
C1 C2 C4 122.27(15)
C15 C14 C13 118.35(16)
C15 C14 C141 120.65(16)
C13 C14 C141 120.99(16)
N1 C1 C2 114.77(14)
N1 C1 C3 123.28(15)
C2 C1 C3 121.96(16)
C23 C22 C21 117.92(17)
C23 C22 C221 120.79(17)
C21 C22 C221 121.28(16)
C15 C16 C11 118.27(16)
C15 C16 C161 120.62(15)
C11 C16 C161 121.08(15)
C24 C25 C26 122.33(18)
C21 C26 C25 117.49(16)
C21 C26 C261 121.42(15)
C25 C26 C261 121.09(17)
C14 C15 C16 121.92(16)
C24 C23 C22 122.04(17)
C23 C24 C25 118.40(17)
C23 C24 C241 120.71(19)
C25 C24 C241 120.9(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cl1 Al1 2.1215(7)
N2 C2 1.348(2)
N2 C21 1.447(2)
N2 Al1 1.8782(15)
Cl2 Al1 2.1252(7)
N1 C1 1.355(2)
N1 C11 1.439(2)
N1 Al1 1.8643(14)
C11 C12 1.400(2)
C11 C16 1.400(2)
C12 C13 1.394(2)
C12 C121 1.511(2)
C13 C14 1.395(2)
C21 C26 1.398(2)
C21 C22 1.402(2)
C2 C1 1.438(2)
C2 C4 1.473(3)
C14 C15 1.391(3)
C14 C141 1.509(2)
C1 C3 1.464(2)
C22 C23 1.398(3)
C22 C221 1.506(3)
C16 C15 1.395(2)
C16 C161 1.509(2)
C25 C24 1.388(3)
C25 C26 1.399(2)
C26 C261 1.508(3)
C23 C24 1.381(3)
C24 C241 1.514(3)
