#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:20:33 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178646 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/57/4075762.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_4075762
loop_
_publ_author_name
'Zhu, Hongping'
'Chai, Jianfang'
'He, Cheng'
'Bai, Guangcai'
'Roesky, Herbert W.'
'Jancik, Vojtech'
'Schmidt, Hans-Georg'
'Noltemeyer, Mathias'
_publ_section_title
;
 Stepwise Hydrolysis of Aluminum Chloride Iodide LAlClI (L =
 HC[(CMe)(NAr)]2, Ar = 2,6-iPr2C6H3) in the Presence ofN-Heterocyclic
 Carbene as Hydrogen Halide Acceptor†
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              380
_journal_paper_doi               10.1021/om049339a
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C64 H98 Al2 Cl2 N4 O2'
_chemical_formula_weight         1080.32
_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                 103.76(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.567(2)
_cell_length_b                   13.263(2)
_cell_length_c                   17.359(5)
_cell_measurement_temperature    133(2)
_cell_volume                     3033.9(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  IPDS2
_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  0.0802
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46371
_diffrn_reflns_theta_full        25.40
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.9646
_exptl_absorpt_correction_T_min  0.9475
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0338
_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)+(0.0457P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                4111
_reflns_number_total             5559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049339asi20040827_041507.cif
_cod_data_source_block           compound_3
_cod_original_cell_volume        3034.0(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4075762
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 0.48982(3) 0.91348(3) 0.05474(3) 0.01715(11) Uani 1 1 d . . .
Cl1 Cl 0.49586(3) 0.97568(3) 0.17260(2) 0.02490(11) Uani 1 1 d . . .
O1 O 0.58369(9) 0.98963(9) 0.01562(7) 0.0216(3) Uani 1 1 d . . .
N1 N 0.37219(9) 0.82140(10) 0.03997(8) 0.0186(3) Uani 1 1 d . . .
N2 N 0.58339(9) 0.79706(10) 0.08220(8) 0.0186(3) Uani 1 1 d . . .
C1 C 0.37426(12) 0.73945(12) 0.08595(9) 0.0198(3) Uani 1 1 d . . .
C2 C 0.46319(12) 0.69857(12) 0.13223(10) 0.0214(3) Uani 1 1 d . . .
H2A H 0.4568 0.6533 0.1732 0.026 Uiso 1 1 calc R . .
C3 C 0.56087(12) 0.71853(12) 0.12356(10) 0.0202(3) Uani 1 1 d . . .
C4 C 0.27777(12) 0.68204(13) 0.08674(10) 0.0237(4) Uani 1 1 d . . .
H4A H 0.2439 0.6624 0.0325 0.036 Uiso 1 1 calc R . .
H4B H 0.2324 0.7251 0.1086 0.036 Uiso 1 1 calc R . .
H4C H 0.2947 0.6216 0.1197 0.036 Uiso 1 1 calc R . .
C5 C 0.64048(13) 0.64145(13) 0.15989(11) 0.0260(4) Uani 1 1 d . . .
H5A H 0.7010 0.6760 0.1907 0.039 Uiso 1 1 calc R . .
H5B H 0.6586 0.6017 0.1177 0.039 Uiso 1 1 calc R . .
H5C H 0.6135 0.5967 0.1949 0.039 Uiso 1 1 calc R . .
C11 C 0.27248(12) 0.84076(12) -0.01206(10) 0.0195(3) Uani 1 1 d . . .
C12 C 0.19727(12) 0.88911(12) 0.01853(10) 0.0213(4) Uani 1 1 d . . .
C13 C 0.10005(12) 0.89693(13) -0.03129(11) 0.0269(4) Uani 1 1 d . . .
H13A H 0.0486 0.9314 -0.0130 0.032 Uiso 1 1 calc R . .
C14 C 0.07715(13) 0.85575(14) -0.10643(11) 0.0305(4) Uani 1 1 d . . .
H14A H 0.0100 0.8605 -0.1386 0.037 Uiso 1 1 calc R . .
C15 C 0.15141(13) 0.80770(14) -0.13510(10) 0.0273(4) Uani 1 1 d . . .
H15A H 0.1345 0.7789 -0.1867 0.033 Uiso 1 1 calc R . .
C16 C 0.25113(12) 0.80069(12) -0.08945(10) 0.0218(4) Uani 1 1 d . . .
C121 C 0.21656(12) 0.92727(13) 0.10350(10) 0.0236(4) Uani 1 1 d . . .
H12A H 0.2810 0.8962 0.1345 0.028 Uiso 1 1 calc R . .
C122 C 0.13085(13) 0.89824(15) 0.14373(11) 0.0297(4) Uani 1 1 d . . .
H12B H 0.1176 0.8257 0.1375 0.044 Uiso 1 1 calc R . .
H12C H 0.0691 0.9356 0.1190 0.044 Uiso 1 1 calc R . .
H12D H 0.1513 0.9149 0.2003 0.044 Uiso 1 1 calc R . .
C123 C 0.22904(14) 1.04154(14) 0.10752(11) 0.0311(4) Uani 1 1 d . . .
H12E H 0.2844 1.0612 0.0832 0.047 Uiso 1 1 calc R . .
H12F H 0.2449 1.0633 0.1631 0.047 Uiso 1 1 calc R . .
H12G H 0.1658 1.0736 0.0788 0.047 Uiso 1 1 calc R . .
C161 C 0.33281(13) 0.74745(13) -0.12176(10) 0.0254(4) Uani 1 1 d . . .
H16A H 0.3995 0.7781 -0.0950 0.030 Uiso 1 1 calc R . .
C162 C 0.31997(15) 0.76101(16) -0.21090(11) 0.0352(4) Uani 1 1 d . . .
H16B H 0.3750 0.7260 -0.2276 0.053 Uiso 1 1 calc R . .
H16C H 0.3221 0.8330 -0.2232 0.053 Uiso 1 1 calc R . .
H16D H 0.2546 0.7328 -0.2391 0.053 Uiso 1 1 calc R . .
C163 C 0.33907(17) 0.63543(15) -0.10197(13) 0.0420(5) Uani 1 1 d . . .
H16E H 0.3594 0.6267 -0.0443 0.063 Uiso 1 1 calc R . .
H16F H 0.3893 0.6034 -0.1263 0.063 Uiso 1 1 calc R . .
H16G H 0.2726 0.6042 -0.1225 0.063 Uiso 1 1 calc R . .
C21 C 0.68514(12) 0.79353(12) 0.06831(10) 0.0195(3) Uani 1 1 d . . .
C22 C 0.69969(12) 0.74493(12) -0.00045(10) 0.0226(4) Uani 1 1 d . . .
C23 C 0.79844(13) 0.74044(14) -0.01140(11) 0.0272(4) Uani 1 1 d . . .
H23A H 0.8100 0.7069 -0.0568 0.033 Uiso 1 1 calc R . .
C24 C 0.87941(13) 0.78319(14) 0.04173(11) 0.0297(4) Uani 1 1 d . . .
H24A H 0.9453 0.7816 0.0318 0.036 Uiso 1 1 calc R . .
C25 C 0.86403(13) 0.82844(14) 0.10952(11) 0.0278(4) Uani 1 1 d . . .
H25A H 0.9200 0.8580 0.1460 0.033 Uiso 1 1 calc R . .
C26 C 0.76813(12) 0.83169(13) 0.12564(10) 0.0230(4) Uani 1 1 d . . .
C221 C 0.61423(13) 0.69466(13) -0.06082(10) 0.0268(4) Uani 1 1 d . . .
H22A H 0.5504 0.7017 -0.0420 0.032 Uiso 1 1 calc R . .
C222 C 0.59720(14) 0.74389(15) -0.14242(11) 0.0324(4) Uani 1 1 d . . .
H22B H 0.5737 0.8133 -0.1395 0.049 Uiso 1 1 calc R . .
H22C H 0.5459 0.7057 -0.1806 0.049 Uiso 1 1 calc R . .
H22D H 0.6610 0.7442 -0.1595 0.049 Uiso 1 1 calc R . .
C223 C 0.63572(17) 0.58158(15) -0.06777(13) 0.0409(5) Uani 1 1 d . . .
H22E H 0.6463 0.5500 -0.0154 0.061 Uiso 1 1 calc R . .
H22F H 0.6967 0.5730 -0.0881 0.061 Uiso 1 1 calc R . .
H22G H 0.5778 0.5497 -0.1043 0.061 Uiso 1 1 calc R . .
C261 C 0.75909(13) 0.87028(13) 0.20638(10) 0.0243(4) Uani 1 1 d . . .
H26A H 0.6903 0.8516 0.2134 0.029 Uiso 1 1 calc R . .
C262 C 0.76888(14) 0.98473(14) 0.21149(12) 0.0337(4) Uani 1 1 d . . .
H26B H 0.7161 1.0155 0.1696 0.051 Uiso 1 1 calc R . .
H26C H 0.8359 1.0047 0.2048 0.051 Uiso 1 1 calc R . .
H26D H 0.7609 1.0075 0.2634 0.051 Uiso 1 1 calc R . .
C263 C 0.83869(13) 0.82177(15) 0.27403(11) 0.0323(4) Uani 1 1 d . . .
H26E H 0.8320 0.7482 0.2707 0.048 Uiso 1 1 calc R . .
H26F H 0.8281 0.8448 0.3251 0.048 Uiso 1 1 calc R . .
H26G H 0.9068 0.8413 0.2695 0.048 Uiso 1 1 calc R . .
C1A C 0.9322(12) 0.5442(8) 0.1635(9) 0.053(2) Uani 0.635(7) 1 d P A 1
H1AA H 0.8751 0.5228 0.1851 0.079 Uiso 0.635(7) 1 calc PR A 1
H1AB H 0.9312 0.6178 0.1578 0.079 Uiso 0.635(7) 1 calc PR A 1
H1AC H 0.9961 0.5234 0.1994 0.079 Uiso 0.635(7) 1 calc PR A 1
C2A C 0.9231(3) 0.4957(3) 0.0827(2) 0.0491(13) Uani 0.635(7) 1 d P A 1
H2AA H 0.8571 0.5155 0.0478 0.059 Uiso 0.635(7) 1 calc PR A 1
H2AB H 0.9222 0.4216 0.0893 0.059 Uiso 0.635(7) 1 calc PR A 1
C3A C 1.0069(4) 0.5223(4) 0.0410(4) 0.0413(16) Uani 0.635(7) 1 d P . 1
H3AA H 1.0105 0.5966 0.0369 0.050 Uiso 0.635(7) 1 calc PR A 1
H3AB H 1.0726 0.4989 0.0743 0.050 Uiso 0.635(7) 1 calc PR A 1
C1B C 0.947(2) 0.539(2) 0.1656(19) 0.080(8) Uani 0.365(7) 1 d P A 2
H1BA H 0.9792 0.5754 0.2143 0.120 Uiso 0.365(7) 1 calc PR A 2
H1BB H 0.9410 0.4676 0.1778 0.120 Uiso 0.365(7) 1 calc PR A 2
H1BC H 0.8800 0.5673 0.1430 0.120 Uiso 0.365(7) 1 calc PR A 2
C2B C 1.0109(5) 0.5493(6) 0.1078(5) 0.054(2) Uani 0.365(7) 1 d P A 2
H2BA H 1.0794 0.5222 0.1315 0.065 Uiso 0.365(7) 1 calc PR A 2
H2BB H 1.0183 0.6218 0.0966 0.065 Uiso 0.365(7) 1 calc PR A 2
C3B C 0.9674(7) 0.4950(7) 0.0307(7) 0.047(4) Uani 0.365(7) 1 d P . 2
H3BA H 0.8988 0.5219 0.0073 0.057 Uiso 0.365(7) 1 calc PR A 2
H3BB H 0.9601 0.4226 0.0421 0.057 Uiso 0.365(7) 1 calc PR A 2
H1 H 0.6351(17) 0.9838(18) 0.0275(14) 0.046(8) Uiso 1 1 d . . .
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'
O O 0.0106 0.0060 '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
O1 Al1 O1 72.46(7) . 3_675
O1 Al1 N1 151.96(6) . .
O1 Al1 N1 92.91(6) 3_675 .
O1 Al1 N2 93.17(6) . .
O1 Al1 N2 153.56(6) 3_675 .
N1 Al1 N2 90.05(6) . .
O1 Al1 Cl1 104.94(5) . .
O1 Al1 Cl1 104.18(5) 3_675 .
N1 Al1 Cl1 101.75(5) . .
N2 Al1 Cl1 100.90(5) . .
Al1 O1 Al1 107.55(7) . 3_675
C1 N1 C11 113.26(13) . .
C1 N1 Al1 121.33(11) . .
C11 N1 Al1 124.91(10) . .
C3 N2 C21 114.14(13) . .
C3 N2 Al1 121.27(10) . .
C21 N2 Al1 124.22(10) . .
N1 C1 C2 123.42(14) . .
N1 C1 C4 120.98(14) . .
C2 C1 C4 115.52(14) . .
C1 C2 C3 125.44(15) . .
N2 C3 C2 123.28(15) . .
N2 C3 C5 121.16(14) . .
C2 C3 C5 115.45(14) . .
C16 C11 C12 121.80(15) . .
C16 C11 N1 118.26(14) . .
C12 C11 N1 119.59(14) . .
C13 C12 C11 117.45(16) . .
C13 C12 C121 119.61(15) . .
C11 C12 C121 122.86(15) . .
C14 C13 C12 121.50(16) . .
C13 C14 C15 120.25(16) . .
C14 C15 C16 121.11(16) . .
C15 C16 C11 117.82(15) . .
C15 C16 C161 120.71(15) . .
C11 C16 C161 121.42(14) . .
C12 C121 C123 111.50(14) . .
C12 C121 C122 112.44(14) . .
C123 C121 C122 108.37(14) . .
C163 C161 C162 109.30(16) . .
C163 C161 C16 111.99(15) . .
C162 C161 C16 113.55(15) . .
C26 C21 C22 120.86(14) . .
C26 C21 N2 120.09(14) . .
C22 C21 N2 118.89(14) . .
C23 C22 C21 117.75(15) . .
C23 C22 C221 119.09(15) . .
C21 C22 C221 123.13(14) . .
C24 C23 C22 121.93(16) . .
C23 C24 C25 119.45(16) . .
C24 C25 C26 121.44(17) . .
C25 C26 C21 118.32(16) . .
C25 C26 C261 118.53(15) . .
C21 C26 C261 123.03(14) . .
C22 C221 C222 112.00(15) . .
C22 C221 C223 110.74(15) . .
C222 C221 C223 109.51(15) . .
C26 C261 C262 111.28(14) . .
C26 C261 C263 111.53(14) . .
C262 C261 C263 109.70(15) . .
C1A C2A C3A 115.7(6) . .
C3A C3A C2A 114.6(6) 3_765 .
C1B C2B C3B 112.9(13) . .
C2B C3B C3B 113.7(10) . 3_765
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 O1 1.8746(13) .
Al1 O1 1.8864(13) 3_675
Al1 N1 1.9773(14) .
Al1 N2 1.9837(14) .
Al1 Cl1 2.1893(7) .
O1 Al1 1.8864(14) 3_675
N1 C1 1.345(2) .
N1 C11 1.460(2) .
N2 C3 1.341(2) .
N2 C21 1.4574(19) .
C1 C2 1.391(2) .
C1 C4 1.517(2) .
C2 C3 1.394(2) .
C3 C5 1.512(2) .
C11 C16 1.409(2) .
C11 C12 1.411(2) .
C12 C13 1.398(2) .
C12 C121 1.522(2) .
C13 C14 1.380(3) .
C14 C15 1.381(3) .
C15 C16 1.399(2) .
C16 C161 1.529(2) .
C121 C123 1.525(2) .
C121 C122 1.541(2) .
C161 C163 1.523(3) .
C161 C162 1.526(2) .
C21 C26 1.408(2) .
C21 C22 1.411(2) .
C22 C23 1.398(2) .
C22 C221 1.520(2) .
C23 C24 1.377(3) .
C24 C25 1.380(3) .
C25 C26 1.395(2) .
C26 C261 1.524(2) .
C221 C222 1.527(3) .
C221 C223 1.538(3) .
C261 C262 1.525(3) .
C261 C263 1.535(2) .
C1A C2A 1.520(16) .
C2A C3A 1.527(6) .
C3A C3A 1.512(12) 3_765
C1B C2B 1.48(3) .
C2B C3B 1.511(13) .
C3B C3B 1.55(2) 3_765
