#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:26:03 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179721 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/23/7002372.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_7002372
loop_
_publ_author_name
'Kamps, Ina'
'Langlitz, Irina'
'Mix, Andreas'
'Neumann, Beate'
'Stammler, Hans-Georg'
'Mitzel, Norbert W.'
_publ_section_title
;
 Transmetallation and silylation products of aminal carbanions
;
_journal_issue                   39
_journal_name_full               'Dalton Transactions'
_journal_page_first              8363
_journal_page_last               8369
_journal_paper_doi               10.1039/b911925f
_journal_year                    2009
_chemical_formula_moiety         'C20 H48 Al2 N6'
_chemical_formula_sum            'C20 H48 Al2 N6'
_chemical_formula_weight         426.60
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.687(4)
_cell_angle_beta                 106.821(3)
_cell_angle_gamma                110.728(4)
_cell_formula_units_Z            1
_cell_length_a                   8.2897(7)
_cell_length_b                   9.0162(6)
_cell_length_c                   9.7438(8)
_cell_measurement_reflns_used    12671
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     621.47(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.073
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9581
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  0.9946
_exptl_absorpt_correction_T_min  0.9723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             236
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0496
_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)+(0.0398P)²+0.3427P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1234
_reflns_number_gt                2136
_reflns_number_total             2810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b911925f.txt
_cod_data_source_block           compound1b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               7002372
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.26872(8) 0.38822(7) 0.34152(7) 0.02001(17) Uani 1 1 d . . .
N1 N 0.5751(2) 0.36366(19) 0.59800(18) 0.0198(3) Uani 1 1 d . . .
N2 N 0.2410(2) 0.16484(19) 0.52466(19) 0.0218(4) Uani 1 1 d . . .
N3 N 0.4881(2) 0.13755(19) 0.70795(19) 0.0220(4) Uani 1 1 d . . .
C1 C 0.3669(2) 0.3300(2) 0.5329(2) 0.0202(4) Uani 1 1 d . . .
H1 H 0.3542 0.4067 0.6118 0.024 Uiso 1 1 calc R . .
C2 C 0.2971(3) 0.1254(2) 0.6637(2) 0.0235(4) Uani 1 1 d . . .
H2A H 0.2099 0.0111 0.6514 0.028 Uiso 1 1 calc R . .
H2B H 0.2903 0.2030 0.7445 0.028 Uiso 1 1 calc R . .
C3 C 0.6145(3) 0.3097(2) 0.7358(2) 0.0224(4) Uani 1 1 d . . .
H3A H 0.7445 0.3219 0.7712 0.027 Uiso 1 1 calc R . .
H3B H 0.6022 0.3828 0.8163 0.027 Uiso 1 1 calc R . .
C4 C 0.6291(3) 0.2768(2) 0.4868(2) 0.0216(4) Uani 1 1 d . . .
H4A H 0.7638 0.3103 0.5288 0.032 Uiso 1 1 calc R . .
H4B H 0.5961 0.3069 0.3939 0.032 Uiso 1 1 calc R . .
H4C H 0.5630 0.1562 0.4648 0.032 Uiso 1 1 calc R . .
C5 C 0.1784(3) 0.0258(2) 0.3908(2) 0.0247(4) Uani 1 1 d . . .
H5A H 0.2833 0.0002 0.3888 0.037 Uiso 1 1 calc R . .
H5B H 0.1308 0.0562 0.3005 0.037 Uiso 1 1 calc R . .
H5C H 0.0793 -0.0720 0.3933 0.037 Uiso 1 1 calc R . .
C6 C 0.5360(3) 0.0905(3) 0.8461(2) 0.0275(5) Uani 1 1 d . . .
H6A H 0.6652 0.1042 0.8782 0.041 Uiso 1 1 calc R . .
H6B H 0.4526 -0.0259 0.8270 0.041 Uiso 1 1 calc R . .
H6C H 0.5221 0.1619 0.9253 0.041 Uiso 1 1 calc R . .
C7 C 0.0071(3) 0.3489(2) 0.3124(2) 0.0255(4) Uani 1 1 d . . .
H7A H -0.0698 0.2275 0.2668 0.031 Uiso 1 1 calc R . .
H7B H 0.0043 0.3779 0.4140 0.031 Uiso 1 1 calc R . .
C8 C -0.0951(3) 0.4342(3) 0.2199(3) 0.0312(5) Uani 1 1 d . . .
H8A H -0.0384 0.5536 0.2729 0.047 Uiso 1 1 calc R . .
H8B H -0.2267 0.3857 0.2067 0.047 Uiso 1 1 calc R . .
H8C H -0.0853 0.4176 0.1211 0.047 Uiso 1 1 calc R . .
C9 C 0.2994(3) 0.2855(2) 0.1582(2) 0.0244(4) Uani 1 1 d . . .
H9A H 0.4135 0.3646 0.1517 0.029 Uiso 1 1 calc R . .
H9B H 0.3170 0.1844 0.1688 0.029 Uiso 1 1 calc R . .
C10 C 0.1336(3) 0.2380(3) 0.0111(3) 0.0376(6) Uani 1 1 d . . .
H10A H 0.0182 0.1674 0.0197 0.056 Uiso 1 1 calc R . .
H10B H 0.1513 0.1772 -0.0725 0.056 Uiso 1 1 calc R . .
H10C H 0.1256 0.3391 -0.0077 0.056 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'
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
C7 Al1 C9 114.43(9) . . ?
C7 Al1 N1 108.36(8) . 2_666 ?
C9 Al1 N1 107.02(8) . 2_666 ?
C7 Al1 C1 105.46(8) . . ?
C9 Al1 C1 117.90(8) . . ?
N1 Al1 C1 102.78(7) 2_666 . ?
C3 N1 C4 109.49(14) . . ?
C3 N1 C1 109.78(14) . . ?
C4 N1 C1 112.23(15) . . ?
C3 N1 Al1 107.85(12) . 2_666 ?
C4 N1 Al1 109.15(12) . 2_666 ?
C1 N1 Al1 108.23(10) . 2_666 ?
C2 N2 C1 112.40(15) . . ?
C2 N2 C5 113.26(15) . . ?
C1 N2 C5 118.77(16) . . ?
C3 N3 C6 109.38(15) . . ?
C3 N3 C2 107.97(14) . . ?
C6 N3 C2 109.59(15) . . ?
N2 C1 N1 113.14(14) . . ?
N2 C1 Al1 110.87(12) . . ?
N1 C1 Al1 119.14(12) . . ?
N2 C1 H1 103.9 . . ?
N1 C1 H1 103.9 . . ?
Al1 C1 H1 103.9 . . ?
N2 C2 N3 111.61(16) . . ?
N2 C2 H2A 109.3 . . ?
N3 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
N3 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N3 C3 N1 111.83(15) . . ?
N3 C3 H3A 109.2 . . ?
N1 C3 H3A 109.2 . . ?
N3 C3 H3B 109.2 . . ?
N1 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 Al1 122.53(14) . . ?
C8 C7 H7A 106.7 . . ?
Al1 C7 H7A 106.7 . . ?
C8 C7 H7B 106.7 . . ?
Al1 C7 H7B 106.7 . . ?
H7A C7 H7B 106.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 Al1 113.81(14) . . ?
C10 C9 H9A 108.8 . . ?
Al1 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
Al1 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
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
Al1 C7 1.994(2) . ?
Al1 C9 1.997(2) . ?
Al1 N1 2.0231(17) 2_666 ?
Al1 C1 2.042(2) . ?
N1 C3 1.491(2) . ?
N1 C4 1.494(2) . ?
N1 C1 1.550(2) . ?
N1 Al1 2.0231(16) 2_666 ?
N2 C2 1.447(2) . ?
N2 C1 1.457(2) . ?
N2 C5 1.463(3) . ?
N3 C3 1.457(2) . ?
N3 C6 1.466(2) . ?
N3 C2 1.473(2) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.542(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.537(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
