#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:17:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179808 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/04/7010437.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_7010437
loop_
_publ_author_name
'Huang, Yi-Lun'
'Huang, Bor-Hunn'
'Ko, Bao-Tsan'
'Lin, Chu-Chieh'
_publ_section_title
;
 Reactions of amides with organoaluminium: a useful synthetic route to
 aluminium diketiminates †
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1359
_journal_paper_doi               10.1039/b009070k
_journal_year                    2001
_chemical_formula_sum            'C16 H18 Al N O2'
_chemical_formula_weight         283.29
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.007(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1019(8)
_cell_length_b                   9.7458(8)
_cell_length_c                   16.2491(13)
_cell_measurement_temperature    293(2)
_cell_volume                     1552.2(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0142
_diffrn_reflns_av_sigmaI/netI    0.0124
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8412
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             600
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                2594
_reflns_number_total             3034
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b009070k.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010437
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Al Al 0.34664(4) 0.09287(4) 0.02461(2) 0.04560(18) Uani 1 1 d . . .
O1 O 0.36443(10) -0.04653(10) -0.04625(6) 0.0482(3) Uani 1 1 d . . .
O2 O 0.67599(14) -0.02952(15) -0.43204(8) 0.0762(4) Uani 1 1 d . . .
N N 0.51227(11) -0.05019(11) -0.12786(7) 0.0436(3) Uani 1 1 d . . .
C1 C 0.38617(13) -0.03770(13) -0.12171(8) 0.0415(3) Uani 1 1 d . . .
C2 C 0.26343(13) -0.01996(14) -0.19293(8) 0.0427(3) Uani 1 1 d . . .
C3 C 0.14189(16) -0.07772(16) -0.18302(10) 0.0550(4) Uani 1 1 d . . .
H3A H 0.1402 -0.1238 -0.1332 0.066 Uiso 1 1 calc R . .
C4 C 0.02375(16) -0.06675(17) -0.24709(12) 0.0634(4) Uani 1 1 d . . .
H4A H -0.0566 -0.1071 -0.2406 0.076 Uiso 1 1 calc R . .
C5 C 0.02501(16) 0.00375(18) -0.32028(11) 0.0615(4) Uani 1 1 d . . .
H5A H -0.0541 0.0095 -0.3636 0.074 Uiso 1 1 calc R . .
C6 C 0.14269(17) 0.06557(18) -0.32952(10) 0.0604(4) Uani 1 1 d . . .
H6A H 0.1423 0.1155 -0.3783 0.072 Uiso 1 1 calc R . .
C7 C 0.26204(15) 0.05381(16) -0.26631(9) 0.0510(3) Uani 1 1 d . . .
H7A H 0.3416 0.0955 -0.2731 0.061 Uiso 1 1 calc R . .
C8 C 0.54891(13) -0.04844(13) -0.20842(8) 0.0415(3) Uani 1 1 d . . .
C9 C 0.62222(15) 0.06262(15) -0.22775(9) 0.0503(3) Uani 1 1 d . . .
H9A H 0.6440 0.1354 -0.1899 0.060 Uiso 1 1 calc R . .
C10 C 0.66279(16) 0.06519(17) -0.30282(10) 0.0565(4) Uani 1 1 d . . .
H10A H 0.7113 0.1401 -0.3155 0.068 Uiso 1 1 calc R . .
C11 C 0.63191(15) -0.04295(17) -0.35941(9) 0.0524(4) Uani 1 1 d . . .
C12 C 0.56037(16) -0.15465(16) -0.34002(9) 0.0549(4) Uani 1 1 d . . .
H12A H 0.5397 -0.2280 -0.3775 0.066 Uiso 1 1 calc R . .
C13 C 0.51968(15) -0.15667(15) -0.26430(9) 0.0496(3) Uani 1 1 d . . .
H13A H 0.4721 -0.2320 -0.2512 0.059 Uiso 1 1 calc R . .
C14 C 0.6498(3) -0.1376(3) -0.49175(13) 0.0942(7) Uani 1 1 d . . .
H14A H 0.6860 -0.1143 -0.5394 0.141 Uiso 1 1 calc R . .
H14B H 0.5532 -0.1518 -0.5106 0.141 Uiso 1 1 calc R . .
H14C H 0.6926 -0.2201 -0.4658 0.141 Uiso 1 1 calc R . .
C15 C 0.3826(2) 0.26585(17) -0.02632(11) 0.0718(5) Uani 1 1 d . . .
H15A H 0.4713 0.2626 -0.0379 0.108 Uiso 1 1 calc R . .
H15B H 0.3792 0.3398 0.0121 0.108 Uiso 1 1 calc R . .
H15C H 0.3148 0.2802 -0.0783 0.108 Uiso 1 1 calc R . .
C16 C 0.17021(17) 0.0769(2) 0.05384(12) 0.0688(5) Uani 1 1 d . . .
H16A H 0.1632 -0.0119 0.0781 0.103 Uiso 1 1 calc R . .
H16B H 0.0980 0.0879 0.0036 0.103 Uiso 1 1 calc R . .
H16C H 0.1630 0.1467 0.0942 0.103 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'
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'
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
O1 Al C15 108.67(6) . . ?
O1 Al C16 109.23(7) . . ?
C15 Al C16 116.45(9) . . ?
O1 Al N 102.72(5) . 3_655 ?
C15 Al N 111.98(7) . 3_655 ?
C16 Al N 106.90(6) . 3_655 ?
C1 O1 Al 127.83(8) . . ?
C11 O2 C14 118.45(15) . . ?
C1 N C8 122.44(11) . . ?
C1 N Al 118.25(9) . 3_655 ?
C8 N Al 118.97(8) . 3_655 ?
O1 C1 N 117.14(11) . . ?
O1 C1 C2 116.25(11) . . ?
N C1 C2 126.56(11) . . ?
C7 C2 C3 118.79(12) . . ?
C7 C2 C1 124.14(12) . . ?
C3 C2 C1 117.04(12) . . ?
C4 C3 C2 120.29(15) . . ?
C5 C4 C3 120.11(15) . . ?
C6 C5 C4 120.20(13) . . ?
C5 C6 C7 120.23(15) . . ?
C6 C7 C2 120.32(14) . . ?
C13 C8 C9 119.26(12) . . ?
C13 C8 N 121.85(11) . . ?
C9 C8 N 118.79(12) . . ?
C10 C9 C8 120.21(13) . . ?
C9 C10 C11 120.46(13) . . ?
O2 C11 C10 115.68(14) . . ?
O2 C11 C12 124.74(14) . . ?
C10 C11 C12 119.58(14) . . ?
C11 C12 C13 119.71(14) . . ?
C8 C13 C12 120.76(13) . . ?
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
Al O1 1.8177(10) . ?
Al C15 1.9503(17) . ?
Al C16 1.9587(17) . ?
Al N 1.9650(11) 3_655 ?
O1 C1 1.2997(15) . ?
O2 C11 1.3648(17) . ?
O2 C14 1.413(3) . ?
N C1 1.3073(18) . ?
N C8 1.4442(16) . ?
N Al 1.9650(11) 3_655 ?
C1 C2 1.4872(18) . ?
C2 C7 1.390(2) . ?
C2 C3 1.395(2) . ?
C3 C4 1.385(2) . ?
C4 C5 1.376(2) . ?
C5 C6 1.373(3) . ?
C6 C7 1.386(2) . ?
C8 C13 1.3764(19) . ?
C8 C9 1.3897(19) . ?
C9 C10 1.378(2) . ?
C10 C11 1.384(2) . ?
C11 C12 1.385(2) . ?
C12 C13 1.3885(18) . ?
