#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:27:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179378 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/75/4327522.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_4327522
loop_
_publ_author_name
'Bor-Hunn Huang'
'Te-Liang Yu'
'Yi-Lun Huang'
'Bao-Tsan Ko'
'Chu-Chieh Lin'
_publ_section_title
;
 Reactions of Amides with Organoaluminum Compounds: Factors Affecting the
 Coordination Mode of Aluminum Amidates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2987
_journal_page_last               2994
_journal_paper_doi               10.1021/ic011072+
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C11 H13 Al F3 N O'
_chemical_formula_weight         259.20
_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                 95.14(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1453(18)
_cell_length_b                   18.259(4)
_cell_length_c                   7.9391(16)
_cell_measurement_reflns_used    3381
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.909
_cell_measurement_theta_min      2.577
_cell_volume                     1320.4(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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  'Bruker P4'
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7259
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.346
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.237
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0521
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1686
_reflns_number_gt                2050
_reflns_number_total             2590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0110722B_11.cif
_cod_data_source_block           13
_cod_database_code               4327522
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
Al Al 0.40905(6) 0.10449(3) -0.00523(7) 0.0480(2) Uani 1 1 d .
F1 F 0.3709(2) -0.06367(10) -0.4792(2) 0.1042(6) Uani 1 1 d .
F2 F 0.1640(2) -0.07940(11) -0.3745(3) 0.1107(6) Uani 1 1 d .
F3 F 0.3450(3) -0.14899(9) -0.2990(3) 0.1196(7) Uani 1 1 d .
O O 0.41489(15) -0.06007(7) -0.05712(18) 0.0543(4) Uani 1 1 d .
N N 0.33742(17) 0.04158(9) -0.19916(18) 0.0491(4) Uani 1 1 d .
C1 C 0.4531(3) 0.20061(12) -0.0946(4) 0.0782(7) Uani 1 1 d .
H1A H 0.4881 0.2323 -0.0032 0.117 Uiso 1 1 calc R
H1B H 0.3657 0.2210 -0.1523 0.117 Uiso 1 1 calc R
H1C H 0.5271 0.1959 -0.1723 0.117 Uiso 1 1 calc R
C2 C 0.2824(3) 0.09377(14) 0.1778(3) 0.0723(7) Uani 1 1 d .
H2A H 0.3178 0.1244 0.2709 0.108 Uiso 1 1 calc R
H2B H 0.2827 0.0436 0.2140 0.108 Uiso 1 1 calc R
H2C H 0.1841 0.1080 0.1386 0.108 Uiso 1 1 calc R
C3 C 0.3566(2) -0.02812(11) -0.1915(2) 0.0512(5) Uani 1 1 d .
C4 C 0.3086(3) -0.08088(14) -0.3393(4) 0.0766(7) Uani 1 1 d .
C5 C 0.2594(2) 0.07884(13) -0.3483(3) 0.0617(6) Uani 1 1 d .
H5A H 0.2331 0.0430 -0.4360 0.074 Uiso 1 1 calc R
H5B H 0.3243 0.1145 -0.3931 0.074 Uiso 1 1 calc R
C6 C 0.1222(2) 0.11683(12) -0.3003(3) 0.0583(5) Uani 1 1 d .
C7 C 0.0185(3) 0.08037(15) -0.2152(3) 0.0737(7) Uani 1 1 d .
H7A H 0.0338 0.0318 -0.1832 0.088 Uiso 1 1 calc R
C8 C -0.1087(3) 0.1164(2) -0.1773(4) 0.0912(9) Uani 1 1 d .
H8A H -0.1786 0.0917 -0.1210 0.109 Uiso 1 1 calc R
C9 C -0.1310(3) 0.1874(2) -0.2220(5) 0.1047(11) Uani 1 1 d .
H9A H -0.2152 0.2114 -0.1943 0.126 Uiso 1 1 calc R
C10 C -0.0306(4) 0.22369(19) -0.3074(5) 0.1127(12) Uani 1 1 d .
H10A H -0.0469 0.2722 -0.3394 0.135 Uiso 1 1 calc R
C11 C 0.0949(3) 0.18838(15) -0.3462(4) 0.0859(8) Uani 1 1 d .
H11A H 0.1628 0.2135 -0.4048 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'
F F 0.0171 0.0103 '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
O Al C2 108.74(10) 3_655 .
O Al C1 106.98(9) 3_655 .
C2 Al C1 121.22(12) . .
O Al N 100.05(7) 3_655 .
C2 Al N 110.09(9) . .
C1 Al N 107.66(10) . .
C3 O Al 135.46(13) . 3_655
C3 N C5 122.91(17) . .
C3 N Al 120.13(13) . .
C5 N Al 116.95(14) . .
N C3 O 122.16(17) . .
N C3 C4 123.41(18) . .
O C3 C4 114.40(18) . .
F3 C4 F2 107.2(2) . .
F3 C4 F1 107.9(2) . .
F2 C4 F1 108.2(2) . .
F3 C4 C3 110.7(2) . .
F2 C4 C3 110.9(2) . .
F1 C4 C3 111.8(2) . .
N C5 C6 111.00(17) . .
C11 C6 C7 118.1(2) . .
C11 C6 C5 120.4(2) . .
C7 C6 C5 121.5(2) . .
C6 C7 C8 120.0(3) . .
C9 C8 C7 120.3(3) . .
C8 C9 C10 120.3(3) . .
C9 C10 C11 119.8(3) . .
C6 C11 C10 121.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al O 1.8310(14) 3_655
Al C2 1.948(2) .
Al C1 1.949(2) .
Al N 1.9845(17) .
F1 C4 1.330(4) .
F2 C4 1.327(3) .
F3 C4 1.319(3) .
O C3 1.288(2) .
O Al 1.8310(14) 3_655
N C3 1.285(3) .
N C5 1.491(3) .
C3 C4 1.551(3) .
C5 C6 1.512(3) .
C6 C11 1.373(3) .
C6 C7 1.384(3) .
C7 C8 1.393(4) .
C8 C9 1.354(5) .
C9 C10 1.361(5) .
C10 C11 1.375(4) .
