#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:39:14 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178575 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/85/4068574.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_4068574
loop_
_publ_author_name
'Pi, Chengfu'
'Wan, Li'
'Wu, Haoyu'
'Gu, Yingying'
'Zheng, Wenjun'
'Weng, Linhong'
'Chen, Zhenxia'
'Wu, Limin'
_publ_section_title
;
 Synthesis of Fused Aminocarbaaluminum Hydrides by the Hydroalumination of
 Bulky Isocyanides⊥
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1263
_journal_paper_doi               10.1021/om800961h
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C22.17 H37.33 Al3 N3'
_chemical_formula_weight         426.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_space_group_name_H-M   'R -3 :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.299(2)
_cell_angle_beta                 105.299(2)
_cell_angle_gamma                105.299(2)
_cell_formula_units_Z            6
_cell_length_a                   16.422(4)
_cell_length_b                   16.422(4)
_cell_length_c                   16.422(4)
_cell_measurement_reflns_used    997
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.060
_cell_measurement_theta_min      2.601
_cell_volume                     3846.6(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17761
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_correction_T_min  0.9688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1382
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0533
_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)+(0.0816P)²+1.9014P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1564
_reflns_number_gt                3920
_reflns_number_total             5041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800961h_si_001.cif
_cod_data_source_block           f80111a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3846.8(16)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4068574
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
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
Al1 Al 0.84269(5) 0.71892(5) 0.12502(5) 0.0396(2) Uani 1 1 d .
Al2 Al 0.71708(5) 0.55373(5) 0.02515(5) 0.0386(2) Uani 1 1 d .
Al3 Al 0.92316(5) 0.57471(5) 0.17161(5) 0.0350(2) Uani 1 1 d .
N1 N 0.76193(13) 0.62893(13) 0.15420(13) 0.0339(4) Uani 1 1 d .
N2 N 0.83077(14) 0.62273(14) 0.01744(14) 0.0373(5) Uani 1 1 d .
N3 N 0.92150(15) 0.44919(14) 0.16361(14) 0.0416(5) Uani 1 1 d .
C1 C 0.9426(3) 0.4461(2) 0.2554(2) 0.0698(9) Uani 1 1 d .
H1A H 0.9422 0.3870 0.2532 0.105 Uiso 1 1 calc R
H1B H 0.8981 0.4590 0.2792 0.105 Uiso 1 1 calc R
H1C H 1.0013 0.4903 0.2938 0.105 Uiso 1 1 calc R
C2 C 0.8343(2) 0.3748(2) 0.1051(2) 0.0678(9) Uani 1 1 d .
H2A H 0.8397 0.3180 0.1052 0.102 Uiso 1 1 calc R
H2B H 0.8190 0.3747 0.0445 0.102 Uiso 1 1 calc R
H2C H 0.7877 0.3834 0.1276 0.102 Uiso 1 1 calc R
C3 C 0.9934(3) 0.4352(3) 0.1294(3) 0.0939(15) Uani 1 1 d .
H3A H 0.9946 0.3760 0.1248 0.141 Uiso 1 1 calc R
H3B H 1.0508 0.4800 0.1705 0.141 Uiso 1 1 calc R
H3C H 0.9814 0.4404 0.0709 0.141 Uiso 1 1 calc R
C4 C 0.90004(17) 0.57981(18) 0.04681(17) 0.0405(6) Uani 1 1 d .
H4A H 0.9568 0.6136 0.0441 0.049 Uiso 1 1 calc R
H4B H 0.8794 0.5187 0.0038 0.049 Uiso 1 1 calc R
C5 C 0.82131(16) 0.59065(17) 0.21012(16) 0.0367(5) Uani 1 1 d .
H5A H 0.7835 0.5325 0.2067 0.044 Uiso 1 1 calc R
H5B H 0.8460 0.6307 0.2729 0.044 Uiso 1 1 calc R
C6 C 0.83375(19) 0.6407(2) -0.06498(18) 0.0461(6) Uani 1 1 d .
C7 C 0.7781(2) 0.5759(2) -0.1507(2) 0.0572(8) Uani 1 1 d .
C8 C 0.7841(3) 0.5956(3) -0.2276(2) 0.0824(12) Uani 1 1 d .
H8A H 0.7471 0.5533 -0.2848 0.099 Uiso 1 1 calc R
C9 C 0.8435(4) 0.6759(4) -0.2202(3) 0.0954(15) Uani 1 1 d .
H9A H 0.8457 0.6885 -0.2718 0.114 Uiso 1 1 calc R
C10 C 0.8984(3) 0.7364(3) -0.1377(3) 0.0803(12) Uani 1 1 d .
H10A H 0.9390 0.7904 -0.1334 0.096 Uiso 1 1 calc R
C11 C 0.8969(2) 0.7214(2) -0.0587(2) 0.0587(8) Uani 1 1 d .
C12 C 0.7136(3) 0.4852(3) -0.1651(2) 0.0750(10) Uani 1 1 d .
H12A H 0.7160 0.4803 -0.1076 0.113 Uiso 1 1 calc R
H12B H 0.7303 0.4385 -0.1979 0.113 Uiso 1 1 calc R
H12C H 0.6534 0.4785 -0.1990 0.113 Uiso 1 1 calc R
C13 C 0.9653(3) 0.7914(3) 0.0297(3) 0.0854(12) Uani 1 1 d .
H13A H 1.0015 0.8405 0.0184 0.128 Uiso 1 1 calc R
H13B H 1.0035 0.7646 0.0593 0.128 Uiso 1 1 calc R
H13C H 0.9345 0.8137 0.0676 0.128 Uiso 1 1 calc R
C14 C 0.69919(16) 0.65012(17) 0.19788(17) 0.0380(5) Uani 1 1 d .
C15 C 0.72520(18) 0.73500(18) 0.26502(18) 0.0442(6) Uani 1 1 d .
C16 C 0.6655(2) 0.7529(2) 0.3075(2) 0.0566(8) Uani 1 1 d .
H16A H 0.6820 0.8097 0.3509 0.068 Uiso 1 1 calc R
C17 C 0.5830(2) 0.6889(3) 0.2867(2) 0.0663(9) Uani 1 1 d .
H17A H 0.5437 0.7020 0.3153 0.080 Uiso 1 1 calc R
C18 C 0.5592(2) 0.6049(2) 0.2232(2) 0.0630(9) Uani 1 1 d .
H18A H 0.5033 0.5612 0.2095 0.076 Uiso 1 1 calc R
C19 C 0.61608(18) 0.58320(19) 0.1788(2) 0.0473(6) Uani 1 1 d .
C20 C 0.5849(2) 0.4876(2) 0.1133(2) 0.0581(8) Uani 1 1 d .
H20A H 0.6297 0.4813 0.0871 0.087 Uiso 1 1 calc R
H20B H 0.5288 0.4745 0.0664 0.087 Uiso 1 1 calc R
H20C H 0.5763 0.4463 0.1448 0.087 Uiso 1 1 calc R
C21 C 0.8162(2) 0.8080(2) 0.2971(2) 0.0586(8) Uani 1 1 d .
H21A H 0.8192 0.8601 0.3430 0.088 Uiso 1 1 calc R
H21B H 0.8252 0.8241 0.2471 0.088 Uiso 1 1 calc R
H21C H 0.8626 0.7864 0.3216 0.088 Uiso 1 1 calc R
H1 H 0.9393(19) 0.7453(19) 0.1948(19) 0.055(8) Uiso 1 1 d .
H3 H 0.7062(19) 0.4547(19) 0.0093(19) 0.051(8) Uiso 1 1 d .
H4 H 0.643(2) 0.580(2) -0.026(2) 0.064(9) Uiso 1 1 d .
H2 H 0.796(2) 0.783(2) 0.101(2) 0.063(9) Uiso 1 1 d .
H5 H 1.0199(19) 0.6253(19) 0.2372(19) 0.056(8) Uiso 1 1 d .
C25 C 0.523(4) 0.431(2) 0.503(4) 0.453(17) Uiso 1 1 d .
C26 C 0.515(3) 0.405(4) 0.559(4) 0.140(13) Uiso 0.17 1 d P
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'
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
N2 Al1 N1 89.46(9) . .
N2 Al1 Al2 46.95(6) . .
N1 Al1 Al2 46.97(6) . .
N2 Al1 H1 106.3(11) . .
N1 Al1 H1 105.8(10) . .
Al2 Al1 H1 129.0(10) . .
N2 Al1 H2 112.0(12) . .
N1 Al1 H2 109.2(12) . .
Al2 Al1 H2 103.5(12) . .
H1 Al1 H2 127.4(16) . .
N2 Al2 N1 89.02(9) . .
N2 Al2 Al1 46.68(6) . .
N1 Al2 Al1 46.76(6) . .
N2 Al2 H3 112.3(10) . .
N1 Al2 H3 112.9(10) . .
Al1 Al2 H3 138.6(10) . .
N2 Al2 H4 107.2(12) . .
N1 Al2 H4 108.5(12) . .
Al1 Al2 H4 99.4(12) . .
H3 Al2 H4 121.9(16) . .
C5 Al3 C4 108.77(10) . .
C5 Al3 N3 107.11(10) . .
C4 Al3 N3 107.72(10) . .
C5 Al3 H5 119.9(11) . .
C4 Al3 H5 115.2(11) . .
N3 Al3 H5 96.5(11) . .
C14 N1 C5 108.87(18) . .
C14 N1 Al1 122.25(15) . .
C5 N1 Al1 106.87(14) . .
C14 N1 Al2 120.61(15) . .
C5 N1 Al2 109.80(14) . .
Al1 N1 Al2 86.27(8) . .
C6 N2 C4 110.13(18) . .
C6 N2 Al1 120.90(16) . .
C4 N2 Al1 107.58(15) . .
C6 N2 Al2 121.72(17) . .
C4 N2 Al2 107.50(14) . .
Al1 N2 Al2 86.37(8) . .
C1 N3 C3 109.4(3) . .
C1 N3 C2 107.6(2) . .
C3 N3 C2 109.4(3) . .
C1 N3 Al3 108.12(19) . .
C3 N3 Al3 107.12(19) . .
C2 N3 Al3 115.15(17) . .
N3 C1 H1A 109.5 . .
N3 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N3 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N3 C2 H2A 109.5 . .
N3 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N3 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N3 C3 H3A 109.5 . .
N3 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N3 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N2 C4 Al3 115.07(16) . .
N2 C4 H4A 108.5 . .
Al3 C4 H4A 108.5 . .
N2 C4 H4B 108.5 . .
Al3 C4 H4B 108.5 . .
H4A C4 H4B 107.5 . .
N1 C5 Al3 114.72(15) . .
N1 C5 H5A 108.6 . .
Al3 C5 H5A 108.6 . .
N1 C5 H5B 108.6 . .
Al3 C5 H5B 108.6 . .
H5A C5 H5B 107.6 . .
C7 C6 C11 119.1(3) . .
C7 C6 N2 120.7(3) . .
C11 C6 N2 120.1(3) . .
C6 C7 C8 118.7(3) . .
C6 C7 C12 123.5(3) . .
C8 C7 C12 117.8(3) . .
C9 C8 C7 121.3(4) . .
C9 C8 H8A 119.3 . .
C7 C8 H8A 119.3 . .
C10 C9 C8 119.4(4) . .
C10 C9 H9A 120.3 . .
C8 C9 H9A 120.3 . .
C9 C10 C11 122.5(4) . .
C9 C10 H10A 118.7 . .
C11 C10 H10A 118.7 . .
C10 C11 C6 118.9(3) . .
C10 C11 C13 117.9(3) . .
C6 C11 C13 123.2(3) . .
C7 C12 H12A 109.5 . .
C7 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C7 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C15 C14 C19 119.4(2) . .
C15 C14 N1 120.1(2) . .
C19 C14 N1 120.2(2) . .
C16 C15 C14 119.2(3) . .
C16 C15 C21 117.1(3) . .
C14 C15 C21 123.7(2) . .
C17 C16 C15 121.4(3) . .
C17 C16 H16A 119.3 . .
C15 C16 H16A 119.3 . .
C16 C17 C18 119.1(3) . .
C16 C17 H17A 120.4 . .
C18 C17 H17A 120.4 . .
C17 C18 C19 121.9(3) . .
C17 C18 H18A 119.1 . .
C19 C18 H18A 119.1 . .
C18 C19 C14 118.8(3) . .
C18 C19 C20 117.5(3) . .
C14 C19 C20 123.7(2) . .
C19 C20 H20A 109.5 . .
C19 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C19 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C15 C21 H21A 109.5 . .
C15 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C15 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C26 C25 C26 120(3) . 6_666
C26 C25 C25 149(6) . 6_666
C26 C25 C25 50(5) 6_666 6_666
C26 C25 C25 61(5) . 5_666
C26 C25 C25 137(4) 6_666 5_666
C25 C25 C25 105(3) 6_666 5_666
C25 C26 C25 70(3) . 5_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 N2 1.959(2) .
Al1 N1 1.961(2) .
Al1 Al2 2.6867(13) .
Al1 H1 1.56(3) .
Al1 H2 1.53(3) .
Al2 N2 1.967(2) .
Al2 N1 1.968(2) .
Al2 H3 1.53(3) .
Al2 H4 1.52(3) .
Al3 C5 1.992(2) .
Al3 C4 2.012(3) .
Al3 N3 2.023(2) .
Al3 H5 1.52(3) .
N1 C14 1.465(3) .
N1 C5 1.531(3) .
N2 C6 1.469(3) .
N2 C4 1.528(3) .
N3 C1 1.473(4) .
N3 C3 1.479(4) .
N3 C2 1.483(4) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 C7 1.402(4) .
C6 C11 1.410(4) .
C7 C8 1.406(5) .
C7 C12 1.499(5) .
C8 C9 1.371(7) .
C8 H8A 0.9300 .
C9 C10 1.345(6) .
C9 H9A 0.9300 .
C10 C11 1.388(5) .
C10 H10A 0.9300 .
C11 C13 1.506(5) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 C15 1.403(4) .
C14 C19 1.403(4) .
C15 C16 1.392(4) .
C15 C21 1.502(4) .
C16 C17 1.368(5) .
C16 H16A 0.9300 .
C17 C18 1.372(5) .
C17 H17A 0.9300 .
C18 C19 1.390(4) .
C18 H18A 0.9300 .
C19 C20 1.509(4) .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C25 C26 1.12(8) .
C25 C26 1.29(8) 6_666
C25 C25 1.38(3) 6_666
C25 C25 1.38(3) 5_666
C26 C25 1.29(8) 5_666
