#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:31:44 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178569 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/78/4067828.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_4067828
loop_
_publ_author_name
'Maheswari, K.'
'Reddy, N. Dastagiri'
_publ_section_title
;
 Reactions of N-Monosubstituted Amidines with AlMe3and AlMeCl2: Formation
 of Fused Triazaalane Heterocycles
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              197
_journal_paper_doi               10.1021/om2007375
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C56 H86 Al3 Cl6 N8, C7 H8, Cl'
_chemical_formula_sum            'C63 H94 Al3 Cl7 N8'
_chemical_formula_weight         1292.55
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 112.737(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.8732(7)
_cell_length_b                   15.3876(3)
_cell_length_c                   19.2603(9)
_cell_measurement_reflns_used    12330
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6898
_cell_measurement_theta_min      2.6313
_cell_volume                     7345.5(5)
_computing_cell_refinement
;
'Tue Mar 08 16:54:23 2011'
;
_computing_data_collection
;
'Tue Mar 08 16:54:23 2011'
;
_computing_data_reduction
;
'Tue Mar 08 16:54:23 2011'
;
_computing_molecular_graphics    'ORTEP-III & Olex 2.1'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28443
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.76
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_T_max  0.9213
_exptl_absorpt_correction_T_min  0.8737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Tue Mar 08 16:54:23 2011'
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         8552
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0605P)²+8.4497P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1283
_reflns_number_gt                6650
_reflns_number_total             8552
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            om2007375_si_001.cif
_cod_data_source_block           Compound_12
_cod_original_cell_volume        7345.5(4)
_cod_database_code               4067828
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Al1 Al 0.0000 0.62300(5) 0.2500 0.0295(2) Uani 1 2 d S . .
Al2 Al 0.17587(2) 0.37502(4) 0.32141(3) 0.02213(13) Uani 1 1 d . . .
Cl3 Cl 0.23066(2) 0.34577(4) 0.27054(3) 0.03630(14) Uani 1 1 d . . .
Cl2 Cl 0.21899(2) 0.41422(4) 0.43478(3) 0.03982(14) Uani 1 1 d . . .
Cl1 Cl 0.03004(3) 0.69707(5) 0.35087(5) 0.0648(2) Uani 1 1 d . . .
N1 N 0.05384(6) 0.55644(10) 0.23779(9) 0.0244(3) Uani 1 1 d . . .
H1 H 0.0577 0.5660 0.1951 0.029 Uiso 1 1 calc R . .
C6 C 0.16800(8) 0.56296(13) 0.20522(12) 0.0306(4) Uani 1 1 d . . .
C17 C 0.09517(8) 0.07474(12) 0.37775(11) 0.0283(4) Uani 1 1 d . . .
C10 C 0.10450(8) 0.45223(14) 0.12851(11) 0.0309(4) Uani 1 1 d . . .
C2 C 0.13750(7) 0.20631(12) 0.35062(10) 0.0235(4) Uani 1 1 d . . .
C3 C 0.08011(8) 0.47137(14) 0.35139(11) 0.0283(4) Uani 1 1 d . . .
H3A H 0.0441 0.4464 0.3383 0.042 Uiso 1 1 calc R . .
H3B H 0.0841 0.5226 0.3834 0.042 Uiso 1 1 calc R . .
H3C H 0.1074 0.4281 0.3786 0.042 Uiso 1 1 calc R . .
C22 C 0.10017(9) 0.00079(14) 0.33874(14) 0.0373(5) Uani 1 1 d . . .
C11 C 0.06666(9) 0.37628(16) 0.12064(12) 0.0381(5) Uani 1 1 d . . .
H11 H 0.0611 0.3715 0.1689 0.046 Uiso 1 1 calc R . .
C18 C 0.08606(9) 0.07160(14) 0.44441(12) 0.0366(5) Uani 1 1 d . . .
C4 C 0.19302(8) 0.17303(14) 0.39368(13) 0.0347(5) Uani 1 1 d . . .
H4A H 0.1912 0.1229 0.4240 0.052 Uiso 1 1 calc R . .
H4B H 0.2148 0.2189 0.4269 0.052 Uiso 1 1 calc R . .
H4C H 0.2095 0.1555 0.3585 0.052 Uiso 1 1 calc R . .
C9 C 0.11232(10) 0.48421(19) 0.06573(13) 0.0461(6) Uani 1 1 d . . .
H9 H 0.0940 0.4576 0.0181 0.055 Uiso 1 1 calc R . .
C14 C 0.19846(9) 0.60704(15) 0.27976(14) 0.0391(5) Uani 1 1 d . . .
H14 H 0.1922 0.5728 0.3198 0.047 Uiso 1 1 calc R . .
C20 C 0.08744(13) -0.08447(17) 0.43530(19) 0.0616(8) Uani 1 1 d . . .
H20 H 0.0847 -0.1399 0.4552 0.074 Uiso 1 1 calc R . .
C23 C 0.10729(10) 0.00844(17) 0.26421(15) 0.0456(6) Uani 1 1 d . . .
H23 H 0.1292 0.0620 0.2677 0.055 Uiso 1 1 calc R . .
C8 C 0.14599(10) 0.5534(2) 0.07146(14) 0.0516(7) Uani 1 1 d . . .
H8 H 0.1503 0.5746 0.0278 0.062 Uiso 1 1 calc R . .
C26 C 0.07976(12) 0.15322(17) 0.48472(14) 0.0479(6) Uani 1 1 d . . .
H26 H 0.0695 0.2016 0.4471 0.058 Uiso 1 1 calc R . .
C21 C 0.09609(11) -0.07918(15) 0.36979(17) 0.0522(7) Uani 1 1 d . . .
H21 H 0.0994 -0.1311 0.3452 0.063 Uiso 1 1 calc R . .
C7 C 0.17343(9) 0.59221(16) 0.13992(14) 0.0425(6) Uani 1 1 d . . .
H7 H 0.1966 0.6399 0.1429 0.051 Uiso 1 1 calc R . .
C12 C 0.01137(10) 0.39032(19) 0.05775(13) 0.0460(6) Uani 1 1 d . . .
H12A H 0.0146 0.3864 0.0089 0.069 Uiso 1 1 calc R . .
H12B H -0.0023 0.4479 0.0632 0.069 Uiso 1 1 calc R . .
H12C H -0.0137 0.3456 0.0609 0.069 Uiso 1 1 calc R . .
C15 C 0.25924(10) 0.60835(18) 0.29867(17) 0.0536(7) Uani 1 1 d . . .
H15A H 0.2719 0.5491 0.2966 0.080 Uiso 1 1 calc R . .
H15B H 0.2780 0.6320 0.3494 0.080 Uiso 1 1 calc R . .
H15C H 0.2667 0.6448 0.2621 0.080 Uiso 1 1 calc R . .
C13 C 0.09093(12) 0.29130(19) 0.10913(18) 0.0635(8) Uani 1 1 d . . .
H13A H 0.0675 0.2430 0.1104 0.095 Uiso 1 1 calc R . .
H13B H 0.1267 0.2837 0.1493 0.095 Uiso 1 1 calc R . .
H13C H 0.0943 0.2922 0.0602 0.095 Uiso 1 1 calc R . .
C24 C 0.13813(19) -0.0661(2) 0.2489(3) 0.0984(14) Uani 1 1 d . . .
H24A H 0.1171 -0.1197 0.2421 0.148 Uiso 1 1 calc R . .
H24B H 0.1727 -0.0730 0.2915 0.148 Uiso 1 1 calc R . .
H24C H 0.1446 -0.0540 0.2031 0.148 Uiso 1 1 calc R . .
C27 C 0.03544(12) 0.1455(2) 0.51514(18) 0.0584(7) Uani 1 1 d . . .
H27A H 0.0017 0.1276 0.4745 0.088 Uiso 1 1 calc R . .
H27B H 0.0302 0.2019 0.5350 0.088 Uiso 1 1 calc R . .
H27C H 0.0458 0.1021 0.5555 0.088 Uiso 1 1 calc R . .
C16 C 0.17727(12) 0.69948(17) 0.2808(2) 0.0587(8) Uani 1 1 d . . .
H16A H 0.1818 0.7340 0.2409 0.088 Uiso 1 1 calc R . .
H16B H 0.1976 0.7264 0.3298 0.088 Uiso 1 1 calc R . .
H16C H 0.1389 0.6970 0.2725 0.088 Uiso 1 1 calc R . .
C25 C 0.05273(14) 0.0229(3) 0.19892(18) 0.0840(12) Uani 1 1 d . . .
H25A H 0.0584 0.0310 0.1521 0.126 Uiso 1 1 calc R . .
H25B H 0.0354 0.0748 0.2089 0.126 Uiso 1 1 calc R . .
H25C H 0.0295 -0.0277 0.1941 0.126 Uiso 1 1 calc R . .
N3 N 0.13057(6) 0.28302(11) 0.31780(9) 0.0269(3) Uani 1 1 d . . .
H3 H 0.0969 0.2927 0.2874 0.032 Uiso 1 1 calc R . .
C19 C 0.08268(12) -0.01064(17) 0.47281(15) 0.0531(7) Uani 1 1 d . . .
H19 H 0.0771 -0.0158 0.5184 0.064 Uiso 1 1 calc R . .
C28 C 0.13212(15) 0.1783(3) 0.5470(3) 0.1123(18) Uani 1 1 d . . .
H28A H 0.1447 0.1305 0.5832 0.168 Uiso 1 1 calc R . .
H28B H 0.1266 0.2303 0.5726 0.168 Uiso 1 1 calc R . .
H28C H 0.1592 0.1906 0.5259 0.168 Uiso 1 1 calc R . .
N4 N 0.09519(6) 0.15871(10) 0.34497(9) 0.0246(3) Uani 1 1 d . . .
H4 H 0.0634 0.1809 0.3181 0.030 Uiso 1 1 calc R . .
N2 N 0.12670(6) 0.46085(10) 0.26506(8) 0.0203(3) Uani 1 1 d . . .
C5 C 0.13301(7) 0.49273(12) 0.19762(10) 0.0231(4) Uani 1 1 d . . .
C1 C 0.08739(7) 0.49745(11) 0.28099(10) 0.0202(3) Uani 1 1 d . . .
Cl4 Cl 0.0000 0.28410(5) 0.2500 0.03276(16) Uani 1 2 d S . .
C1S C 0.2669(2) 0.7902(4) 0.4898(4) 0.084(2) Uani 0.50 1 d PGDU A -1
C2S C 0.2939(2) 0.7114(4) 0.4982(5) 0.139(5) Uani 0.50 1 d PGDU A -1
H2S H 0.3282 0.7092 0.4947 0.167 Uiso 0.50 1 calc PR A -1
C3S C 0.2708(3) 0.6359(4) 0.5117(6) 0.148(4) Uani 0.50 1 d PGDU A -1
H3S H 0.2892 0.5820 0.5175 0.177 Uiso 0.50 1 calc PR A -1
C4S C 0.2206(3) 0.6391(5) 0.5168(5) 0.163(6) Uani 0.50 1 d PGDU A -1
H4S H 0.2048 0.5875 0.5260 0.196 Uiso 0.50 1 calc PR A -1
C5S C 0.1936(2) 0.7179(6) 0.5084(5) 0.172(5) Uani 0.50 1 d PGDU A -1
H5S H 0.1593 0.7202 0.5119 0.207 Uiso 0.50 1 calc PR A -1
C6S C 0.2168(2) 0.7934(5) 0.4949(4) 0.095(3) Uani 0.50 1 d PGDU A -1
H6S H 0.1984 0.8473 0.4891 0.114 Uiso 0.50 1 calc PR A -1
C7S C 0.2911(4) 0.8733(5) 0.4745(5) 0.225(10) Uani 0.50 1 d PGDU A -1
H7SA H 0.2665 0.9218 0.4705 0.337 Uiso 0.50 1 calc PR A -1
H7SB H 0.2965 0.8675 0.4273 0.337 Uiso 0.50 1 calc PR A -1
H7SC H 0.3258 0.8843 0.5159 0.337 Uiso 0.50 1 calc PR A -1
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
N1 Al1 N1 113.20(10) 2 .
N1 Al1 Cl1 102.65(5) 2 .
N1 Al1 Cl1 111.83(5) . .
N1 Al1 Cl1 111.83(5) 2 2
N1 Al1 Cl1 102.65(5) . 2
Cl1 Al1 Cl1 115.10(6) . 2
N3 Al2 N2 102.09(7) . .
N3 Al2 Cl3 112.75(6) . .
N2 Al2 Cl3 109.98(5) . .
N3 Al2 Cl2 110.19(6) . .
N2 Al2 Cl2 112.01(6) . .
Cl3 Al2 Cl2 109.67(3) . .
C1 N1 Al1 132.27(13) . .
C7 C6 C5 117.0(2) . .
C7 C6 C14 120.31(19) . .
C5 C6 C14 122.70(18) . .
C18 C17 C22 123.55(19) . .
C18 C17 N4 117.66(18) . .
C22 C17 N4 118.61(18) . .
C9 C10 C5 117.2(2) . .
C9 C10 C11 120.3(2) . .
C5 C10 C11 122.50(17) . .
N3 C2 N4 119.96(17) . .
N3 C2 C4 120.03(17) . .
N4 C2 C4 120.01(17) . .
C21 C22 C17 116.7(2) . .
C21 C22 C23 122.2(2) . .
C17 C22 C23 121.1(2) . .
C13 C11 C10 111.7(2) . .
C13 C11 C12 110.4(2) . .
C10 C11 C12 112.29(19) . .
C19 C18 C17 116.9(2) . .
C19 C18 C26 120.8(2) . .
C17 C18 C26 122.29(19) . .
C8 C9 C10 121.3(2) . .
C6 C14 C15 111.6(2) . .
C6 C14 C16 111.2(2) . .
C15 C14 C16 110.6(2) . .
C21 C20 C19 121.1(2) . .
C24 C23 C22 113.8(3) . .
C24 C23 C25 111.9(3) . .
C22 C23 C25 110.8(2) . .
C7 C8 C9 120.4(2) . .
C28 C26 C18 111.4(3) . .
C28 C26 C27 110.0(2) . .
C18 C26 C27 113.0(2) . .
C20 C21 C22 121.2(2) . .
C8 C7 C6 121.4(2) . .
C2 N3 Al2 134.27(13) . .
C20 C19 C18 120.6(2) . .
C2 N4 C17 127.46(16) . .
C1 N2 C5 115.99(14) . .
C1 N2 Al2 127.18(12) . .
C5 N2 Al2 116.81(11) . .
C10 C5 C6 122.74(17) . .
C10 C5 N2 119.19(17) . .
C6 C5 N2 118.06(17) . .
N1 C1 N2 123.58(16) . .
N1 C1 C3 117.23(15) . .
N2 C1 C3 119.19(16) . .
C6S C1S C2S 120.0 . .
C6S C1S C7S 118.9 . .
C2S C1S C7S 121.1 . .
C3S C2S C1S 120.0 . .
C4S C3S C2S 120.0 . .
C3S C4S C5S 120.0 . .
C6S C5S C4S 120.0 . .
C1S C6S C5S 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 N1 1.8603(15) 2
Al1 N1 1.8603(15) .
Al1 Cl1 2.1243(8) .
Al1 Cl1 2.1243(8) 2
Al2 N3 1.8509(17) .
Al2 N2 1.8867(16) .
Al2 Cl3 2.1083(7) .
Al2 Cl2 2.1256(8) .
N1 C1 1.323(2) .
C6 C7 1.396(3) .
C6 C5 1.402(3) .
C6 C14 1.511(3) .
C17 C18 1.398(3) .
C17 C22 1.398(3) .
C17 N4 1.438(2) .
C10 C9 1.395(3) .
C10 C5 1.400(3) .
C10 C11 1.518(3) .
C2 N3 1.318(2) .
C2 N4 1.321(2) .
C2 C4 1.490(3) .
C3 C1 1.498(2) .
C22 C21 1.391(3) .
C22 C23 1.524(3) .
C11 C13 1.515(4) .
C11 C12 1.526(3) .
C18 C19 1.396(3) .
C18 C26 1.520(3) .
C9 C8 1.374(4) .
C14 C15 1.530(3) .
C14 C16 1.535(3) .
C20 C21 1.371(4) .
C20 C19 1.378(4) .
C23 C24 1.510(4) .
C23 C25 1.535(4) .
C8 C7 1.374(4) .
C26 C28 1.505(4) .
C26 C27 1.522(4) .
N2 C1 1.333(2) .
N2 C5 1.458(2) .
C1S C6S 1.3889 .
C1S C2S 1.3895 .
C1S C7S 1.5128 .
C2S C3S 1.3895 .
C3S C4S 1.3888 .
C4S C5S 1.3898 .
C5S C6S 1.3894 .
